SUMMA CANISTER CLEANING PROCEDURES - … CANISTER CLEANING PROCEDURES 1.0 SCOPE AND APPLICATION This standard operating procedure (SOP) is intended for use when cleaning Summa …

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SOP#: 1703DATE: 09/01/94

REV. #: 0.0

SUMMA CANISTERCLEANING PROCEDURES

1.0 SCOPE AND APPLICATION

This standard operating procedure (SOP) is intendedfor use when cleaning Summa polished stainless steelcanisters. Summa canisters provide a medium tosample gas-phase Volatile Organic Compounds(VOCs) on-site at concentrations of one part perbillion by volume (ppbv) and greater. This procedureis to assure that canisters have been sufficientlycleaned prior to sampling, to the extent that no VOCcontamination is present at concentrations greater than0.2 ppbv.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent on site conditions, equipmentlimitations or limitations imposed by the procedure orother procedure limitations. In all instances, theultimate procedures employed should be documentedand associated with the final report.

Mention of trade names or commercial products doesnot constitute U.S. EPA endorsement orrecommendation for use.

2.0 METHOD SUMMARY

After use, canisters are logged in and physicallyinspected. These canisters are vented to the outsideair under an operating exhaust hood. Canisters areconnected to a manifold which is attached to avacuum pump via a cryogenic trap. The canisters andlines are evacuated and then the canisters are heatedto an elevated temperature for a prescribed timeperiod. During the heating period, the canisters arefilled with humidified nitrogen and pressurized. Theprocess is repeated. The filling and pressurizingfunctions are followed by evacuation and heating andare performed a total of three times.

Canisters are confirmed free of VOC contaminationby pressurizing the canisters with ultra high puritynitrogen and analyzing on the GC/MS. If no VOCcontamination is present at concentrations greater than

0.2 ppbv, the canister is determined clean. Cleancanisters are leak-tested by pressurizing with nitrogenfor 24 hours. Canisters that have been determinedclean and without leaks are evacuated. Thesecanisters are logged in as cleaned and certified and arestored in the evacuated state with brass cap fittingsuntil needed for sampling.

3.0 SAMPLE PRESERVATION,CONTAINERS, HANDLING AND STORAGE

3.1 Canister Receipt

1. The overall condition of each sample canisteris observed. Any canister having physicaldefects requires corrective action.

2. Each canister should be observed for anattached sample identification number.

3. Each canister is recorded in the dedicatedlaboratory logbook by its Summa canisternumber.

3.2 Canister Storage

1. Canisters are stored in an evacuated state ofless than 0.05 mm Hg and with a brass cap inplace. The canisters remain in this state untilneeded.

2. An identification tag is attached to the neckof each canister for field notes and tocomplete the chain of custody record.

3. Each canister is recorded in the dedicatedlaboratory logbook stating the canister statusand storage location. Also noted on theidentification tag are the date cleaned anddate certified clean, as well as the initials ofthe operator.

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4.0 I N T E R F E R E N C E A N DPOTENTIAL PROBLEMS

Contamination may occur in the sample canisters ifthey are not properly cleaned before use. All otherequipment used in this process must be sufficientlyclean. All gases and solvents used must be certified Gas cylinders of nitrogen, ultra high purity grade.99.99% pure to avoid contamination. Canisters mustbe stored with the valve closed and the brass caps in Cryogen - liquid nitrogen (bp -195EC).place to avoid vacuum loss.

5.0 EQUIPMENT/APPARATUS

5.1 Canister

Sample canister - Leak-free stainless steel pressurevessels at desired volume (e.g., 6L), with valve and 1. All connections in the vacuum system exceptSumma passivated interior surfaces (Scientific the canisters and manifold are sealed. AllInstrumentation Specialists, Inc., P.O. Box 8941, connections, lines, and valves are checkedMoscow, ID, 83843 or Anderson Samplers, Inc., for leaks by pressurizing the line to 30 psig4215-C Wendell Dr., Atlanta, GA, 30336), or and using a soap solution. The septum isequivalent. checked for leaks by visual inspection.

5.2 Canister Cleaning System (Figure1, Appendix A)

Vacuum pump - capable of evacuating samplecanister(s) to an absolute pressure of <0.05 mm Hg.

Manifold - stainless steel manifold with connectionsfor simultaneously cleaning several canisters.

Shutoff valve(s) - two on/off toggle valves (Valves A,and B).

Stainless steel vacuum gauge (pressure gauge) -capable of measuring vacuum in the manifold to anabsolute pressure of <0.05 mm Hg or less.

Cryogenic trap - stainless steel U-shaped open tubulartrap cooled with liquid nitrogen to preventcontamination from back diffusion of oil from vacuumpump.

Stainless steel two-stage pressure regulator 0-690 kPa(0-100 psig) to regulate nitrogen pressure.

Teflon tee with a septum port - an injection portcapable of introducing distilled, deionized water toprovide moisture to the nitrogen supply line.

Isothermal oven - a system for heating canisters(Fisher Scientific, Pittsburgh, PA, Model 349) orequivalent.

6.0 REAGENTS

Distilled, deionized water, ultra high purity.

7.0 PROCEDURE

7.1 System Set-Up

2. The liquid nitrogen is added to the cryogenictrap and allowed to equilibrate.

3. Check the pump to assure proper workingorder by achieving a vacuum of 0.05 mm Hgin the line that normally attaches to themanifold but is now capped. Valve A isopen and Valve B is closed. After thevacuum test is completed, turn the pump offand remove the cap to break the vacuum.

4. Check the oven to assure proper workingorder by heating the oven to 100EC andmeasuring the internal temperature with athermometer.

5. Check reagents to assure proper purity.

6. Set the back pressure on the nitrogen to 30psig.

7.2 Cleaning

1. All canisters are vented to the outside airunder an operating exhaust hood.

2. Connect the canisters (with the valves closedon the canisters) to the manifold by theSwagelok fittings. Connect the manifold to

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the vacuum system by the Swagelok fitting. 18. Disconnect manifold from cleaning system.

3. Open Valve A, assure Valve B is closed, and 19. Disconnect canisters from the manifold andstart vacuum pump. place a brass cap on each canister.

4. Once a vacuum (0.05 mm Hg) is obtained in 20. Choose the one canister of this set of four,the line and the manifold, Valve A is closed. that was analyzed as being the most highlyThe system is then examined for leaks by contaminated previous to cleaning. Fill thiscomparing the initial vacuum reading and a canister with ultra high purity nitrogen to asecond vacuum reading three minutes later. pressure of 30 psig.If the vacuum deteriorates more than 5 mmHg, a leak exists and corrective action, such 21. Analyze the above canister for VOCas tightening all fittings, is necessary. contamination by GC/MS. If this canister is

5. If no leaks are observed, Valve A is opened contamination is present at concentrationsand the Canister 1 valve is opened. Evacuate greater than 0.2 ppbv, then all canisters inCanister 1 to 0.05 mm Hg, then close that set of four are considered clean.Canister 1 valve. By evacuating one canister Document the results.at a time, cross contamination betweencanisters is minimized. 22. Evacuate the above canister again to 0.05

6. Evacuate all other canisters in the same it with the other three of the lot. Documentmanner as described in the above step. the location.

7. After all four canisters are evacuated, open 23. If the above canister is not sufficiently cleanall canister valves. Turn on the oven and (i.e. VOC contamination is present atheat to 100EC. concentrations greater than 0.2 ppbv), then

8. Continue evacuating canisters for one hour at until the canisters meet the prescribed100EC. Document the time. criteria. Document the results.

9. After one hour, Valve A is closed and ValveB is opened, with the regulator metering theflow of nitrogen.

10. Inject 100 µL of distilled, deionized watervia a syringe through the humidity injectorport in the nitrogen line.

11. Allow the canisters to pressurize to 30 psigfor 15 minutes.

12. Close Valve B.

13. Close canister valves.

14. Repeat steps 5 through 13, twice.

15. Close valves on canisters.

16. Close Valve A.

17. Turn off vacuum pump.

sufficiently clean to the extent that no VOC

mm Hg, cap it with a brass fitting, and store

all canisters in that lot must be cleaned again

7.3 Leak-Testing

1. Once the canister lot is determined as beingclean, the canisters are pressurized to 30 psigwith nitrogen.

2. The initial pressure is measured via thepressure gauge, the canister valve is closed,and the brass cap is replaced. Document thetime and pressure.

3. After 24 hours, the final pressure is checked.Document the time and pressure.

4. If leak tight, the pressure should not varymore than ±13.8 kPa (±2 psig) over the 24-hour period. If this criterion is met, thecanister is capped with a brass fitting andstored. If a leak is present, corrective actionsuch as tightening all fittings, is required.Document the results.

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8.0 CALCULATIONS

There are no calculations for this SOP.

9.0 QUALITY ASSURANCE/QUALITY CONTROL

The following specific quality assurance/qualitycontrol procedures are applicable for Summa canistercleaning:

1. All connections, lines, and valves arechecked to assure no leaks are present.

2. The septum is checked, to assure no leaks arepresent, by removing the septum and visuallyexamining it.

3. The pump is checked to assure properworking order by achieving a vacuum of 0.05mm Hg prior to cleaning.

4. The oven is checked to assure properworking order by comparing the oven settingat 100EC to the internal temperature with athermometer.

5. The reagents are checked to assure sufficientpurity.

6. All canisters are to be evacuated to 0.05 mmHg during each cycle of the cleaning processand the results are to be documented.

7. All canisters are to be evacuated at 100ECfor one hour during each cycle of thecleaning process. Results are to bedocumented.

8. All canisters are to be evacuated, heated, andpressurized three times during the cleaningprocess. Document each cycle.

9. The selected canister from the cleaning lot tobe tested must be analyzed by GC/MS as ASTM Standards D1356-73A - Standard Definitionsshown to be sufficiently cleaned to the extent of Terms and Relating to Atmospheric Sampling andthat no VOC contamination is present at Analysis.concentrations greater than 0.2 ppbv for thecanister lot to be considered cleaned. If the Compendium of Methods for the Determination ofVOC contamination is greater than 0.2 ppbv, Toxic Organic Compounds in Ambient Airthe canister lot must be cleaned again. In EPA/600/4-87/006, September 1986, Method TO-14

either case, the results will be documented.

10. All canisters will be leak-tested for 24 hoursand the results will be documented.

11. All canisters will be stored evacuated andcapped with a brass fitting. The pressure andlocation will be documented.

10.0 DATA VALIDATION

This section is not applicable to this SOP.

11.0 HEALTH AND SAFETY

When working with potentially hazardous materials,follow U.S. EPA, OSHA or corporate health andsafety practices. More specifically, liquid nitrogen isused to cool the cryogenic trap. Its boiling point is-196EC. Insulated gloves, lab coat, face shield, andsafety glasses must be worn when using this material.Liquid nitrogen must be transported only in properlyconstructed containers.

Ultra high purity nitrogen is used to clean thecanisters and must be labeled properly. All cylindersmust be securely fastened to a stationary object. Thecylinder valve should only be opened by hand. Theproper regulator must be used and set correctly.

The oven is set to a temperature of 100EC. Insulatedgloves should be worn when handling items heated tothis temperature.

Prior to cleaning, canisters are to be vented to theatmosphere under an operating exhaust hood. Thehood must be in proper working order.

Canisters are pressurized during the cleaningoperation. No canister is to be pressurized above 30psig. The maximum pressure limit for the Summacanisters is 40 psig.

12.0 REFERENCES

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- Determination of Volatile Organic Compounds(VOCs) in Ambient Air Using Summa CanisterSampling and Gas Chromatographic Analysis.

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APPENDIX A

Figure

FIGURE 1. Canister Cleaning System

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SOP#: 1704DATE: 07/27/95

REV. #: 0.1 SUMMA CANISTER SAMPLING


The purpose of this standard operating procedure(SOP) is to describe a procedure for sampling ofvolatile organic compounds (VOCs) in ambient air.The method is based on samples collected as wholeair samples in Summa passivated stainless steelcanisters. The VOCs are subsequently separated bygas chromatography (GC) and measured bymass-selective detector or multidetector techniques.This method presents procedures for sampling intocanisters at final pressures both above and belowatmospheric pressure (respectively referred to aspressurized and subatmospheric pressure sampling).

This method is applicable to specific VOCs that havebeen tested and determined to be stable when stored inpressurized and subatmospheric pressure canisters.The organic compounds that have been successfullycollected in pressurized canisters by this method arelisted in the Volatile Organic Compound Data Sheet(Appendix A). These compounds have been measuredat the parts per billion by volume (ppbv) level.



2.0 METHOD SUMMARY

Both subatmospheric pressure and pressurizedsampling modes use an initially evacuated canister.Both modes may also use a mass flowcontroller/vacuum pump arrangement to regulate flow.With the above configuration, a sample of ambient air

is drawn through a sampling train comprised ofcomponents that regulate the rate and duration ofsampling into a pre-evacuated Summa passivatedcanister. Alternatively, subatmospheric pressuresampling may be performed using a fixed orifice,capillary, or adjustable micrometering valve in lieu ofthe mass flow controller/vacuum pump arrangementfor taking grab samples or short durationtime-integrated samples. Usually, the alternativetypes of flow controllers are appropriate only insituations where screening samples are taken to assessfor future sampling activities.

3.0 SAMPLE PRESERVATION,CONTAINERS, HANDLING,AND STORAGE

After the air sample is collected, the canister valve isclosed, an identification tag is attached to the canister,and the canister is transported to a laboratory foranalysis. Upon receipt at the laboratory, the canistertag data is recorded. Sample holding times andexpiration should be determined prior to initiatingfield activities.

4.0 INTERFERENCES ANDPOTENTIAL PROBLEMS

Contamination may occur in the sampling system ifcanisters are not properly cleaned before use.Additionally, all other sampling equipment (e.g.,pump and flow controllers) should be thoroughlycleaned.


The following equipment/apparatus (Figure 1,Appendix B) is required:

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5.1 Subatmospheric Pressure SamplingEquipment

1. VOC canister sampler - whole air samplercapable of filling an initially evacuatedcanister by action of the flow controlledpump from vacuum to near atmosphericpressure. (Andersen Samplers Inc., Model87-100 or equivalent).

2. Sampling inlet line - stainless steel tubing toconnect the sampler to the sample inlet.

3. Sample canister - leak-free stainless steelpressure vessels of desired volume withvalve and Summa passivated interiorsurfaces (Scientific InstrumentationSpecialist, Inc., ID 83843, AndersenSamplers, Inc., or equivalent).

4. Particulate matter filter - 2-µm sinteredstainless steel in-line filter (Nupro Co.,Model SS-2F-K4-2, or equivalent).

5. Chromatographic grade stainless steel tubingand fittings - for interconnections (AlltechAssociates, Cat. #8125, or equivalent). Allmaterials in contact with sample, analyte,and support gases should be chromatographicgrade stainless steel.

6. Fixed orifice, capillary, or adjustablemicrometering valve - used in lieu of theelectronic flow controller/vacuum pump forgrab samples or short durationtime-integrated samples.

5.2 Pressurized Sampling Equipment

1. VOC canister sampler - whole air samplercapable of filling an initially evacuatedcanister by action of the flow controlledpump from vacuum to near atmosphericpressure. (Andersen Samplers Inc., Model87-100).

2. Sampling inlet line - stainless steel tubing toconnect the sampler to the sample inlet.

3. Sample canister - leak-free stainless steelpressure vessels of desired volume withvalve and Summa passivated interior

surfaces (Scientific InstrumentationSpecialist, Inc., ID 83843, AndersenSamplers, Inc., or equivalent).

4. Particulate matter filter - 2-µm sinteredstainless steel in-line filter (Nupro Co.,Model SS-2F-K4-2, or equivalent).

5. Chromatographic grade stainless steel tubingand fittings - for interconnections (AlltechAssociates, Cat. #8125, or equivalent). Allmaterials in contact with sample, analyte,and support gases should be chromatographicgrade stainless steel.

6.0 REAGENTS


7.0 PROCEDURE

7.1 Subatmospheric Pressure Sampling

7.1.1 Sampling Using a Fixed Orifice,Capillary, or AdjustableMicrometering Valve

1. Prior to sample collection, the appropriateinformation is completed on the CanisterSampling Field Data Sheet (Appendix C).

2. A canister, which is evacuated to 0.05 mmHg and fitted with a flow restricting device,is opened to the atmosphere containing theVOCs to be sampled.

3. The pressure differential causes the sampleto flow into the canister.

4. This technique may be used to collect grabsamples (duration of 10 to 30 seconds) ortime-integrated samples (duration of 12 to 24hours). The sampling duration depends onthe degree to which the flow is restricted.

5. A critical orifice flow restrictor will have adecrease in the flow rate as the pressureapproaches atmospheric.

6. Upon sample completion at the location, theappropriate information is recorded on the

F '' (P)(V)(T)(60)

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Canister Sampling Field Data Sheet. VOCs to be sampled.

7.1.2 Sampling Using a Mass FlowCont ro l l e r /Vacuum PumpArrangement (Andersen SamplerModel 87-100)

1. Prior to sample collection the appropriateinformation is completed on the CanisterSampling Field Data Sheet (Appendix C).

2. A canister, which is evacuated to 0.05 mmHg and connected in line with the sampler, isopened to the atmosphere containing theVOCs to be sampled.

3. A whole air sample is drawn into the systemthrough a stainless steel inlet tube by a directdrive blower motor assembly.

4. A small portion of this whole air sample ispulled from the inlet tube by a speciallymodified inert vacuum pump in conjunctionwith a mass flow controller.

5. The initially evacuated canister is filled byaction of the flow controlled pump to nearatmospheric pressure.

6. A digital time-program is used to pre-selectsample duration and start and stop times.

7. Upon sample completion at the location, theappropriate information is recorded on theCanister Sampling Field Data Sheet.

7.2 Pressurized Sampling

7.2.1 Sampling Using a Mass FlowControl ler /Vacuum PumpArrangement (Anderson SamplerModel 87-100)

1. Prior to sample commencement at thelocation, the appropriate information iscompleted on the Canister Sampling FieldData Sheet.

2. A canister, which is evacuated to 0.05 mmHg and connected in line with the sampler, isopened to the atmosphere containing the

3. A whole air sample is drawn into the systemthrough a stainless steel inlet tube by a directdrive blower motor assembly.

4. A small portion of this whole air sample ispulled from the inlet tube by a speciallymodified inert vacuum pump in conjunctionwith a mass flow controller.

5. The initially evacuated canister is filled byaction of the flow controlled pump to apositive pressure not to exceed 25 psig.

6. A digital time-programmer is used topre-select sample duration and start and stoptimes.

7. Upon sample completion at the location, theappropriate information is recorded on theCanister Sampling Field Data Sheet.

8.0 CALCULATIONS

1. A flow control device is chosen to maintaina constant flow into the canister over thedesired sample period. This flow rate isdetermined so the canister is filled to about88.1 kPa for subatmospheric pressuresampling or to about one atmosphere aboveambient pressure for pressurized samplingover the desired sample period. The flowrate can be calculated by:

where:

F = flow rate (cm /min)3

P = final canister pressure,atmospheres absolute

V = volume of the canister(cm )3

T = sample period (hours)

For example, if a 6-L canister is to be filled to 202kPa (two atmospheres) absolute pressure in 24 hours,the flow rate can be calculated by:

F '' (2)(6000)(24)(60)

'' 8.3cm 3/min

DF '' YaXa

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2. If the canister pressure is increased, adilution factor (DF) is calculated andrecorded on the sampling data sheet.

where:

Xa = canister pressure (kPa,psia) absolute beforedilution.

Ya = canister pressure (kPa,psia) absolute afterdilution.

After sample analysis, detected VOC concentrationsare multiplied by the dilution factor to determineconcentration in the sampled air.


The following general quality assurance procedures VIP-8, EPA 600/9-87-010.apply:

1. All data must be documented on standard Volume Sets When Sampling Ambient Airchain of custody records, field data sheets, or Using Solid Adsorbents," Atmosphericsite logbooks. Environ., 18:855-859, 1984.

2. All instrumentation must be operated in 4. J. F. Walling, J. E. Bumgarner, J. D.accordance with operating instructions as Driscoll,C. M. Morris, A. E. Riley, and L. H.supplied by the manufacturer, unless Wright, "Apparent Reaction Productsotherwise specified in the work plan. Desorbed From Tenax Used to SampleEquipment checkout and calibration Ambient Air," Atmospheric Environ.,activities must occur prior to 20:51-57, 1986.sampling/operation, and they must bedocumented. 5. Portable Instruments User's Manual for




When working with potentially hazardous materials,follow U.S. EPA, OSHA, and corporate health andsafety practices. Specifically, pressurizing of Summacanisters should be performed in a well ventilatedroom, or preferably under a fume hood. Care must betaken not to exceed 40 psi in the canisters. Canistersare under pressure, albeit only 20-30 psi, and shouldnot be dented or punctured. They should be stored ina cool dry place and always be placed in their plasticshipping boxes during transport and storage.

12.0 REFERENCES

1. Ralph M. Riggin, Technical AssistanceDocument for Sampling and Analysis ofToxic Organic Compounds in Ambient Air,EPA-600/4-83-027 U. S. EnvironmentalProtection Agency, Research Triangle Park,NC, 1983.

2. W. A. McClenny, J. D. Pleil, T. A. Lumpkinand K. D. Oliver, "Update on Canister-BasedSamplers for VOCs," Proceedings of the1987 EPA/APCA Symposium onMeasurement of Toxic and Related AirPollutants, May, 1987 APCA Publication

3. J. F. Walling, "The Utility of Distributed Air

Moni to r ing VOC Sources,EPA-340/1-88-015, U.S. EnvironmentalProtection Agency, Office of Air QualityPlanning and Standards, Washington, D.C.,June 1986.

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6. R. A. Rasmussen and J. E. Lovelock, 8. EPA Method TO-14 "Determination ofAtmospheric Measurements Using Canister Volatile Organic Compounds (VOC's) inTechnology, J. Geophys. Res., 83: Ambient Air Using Summa Passivated8369-8378, 1983. Canister Sampling and Gas Chromatographic

7. R. A. Rasmussen and M. A. K. Khalil,"Atmospheric Halocarbon: Measurementsand Analysis of Selected Trace Gases," Proc.NATO ASI on Atmospheric Ozone, BO:209-23l.

Analysis", May 1988.

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APPENDIX A

Volatile Organic Compound Data Sheet

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APPENDIX B

FIGURE 1. Subatmospheric/Pressurized Sampling Equipment

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APPENDIX C

Canister Sampling Field Data SheetPage of

SUMMA AIR SAMPLING WORK SHEET

Site: Site#: Samplers: Work Assignment Manager: Date: Project Leader:

Sample #

Location

SUMMA ID

Orifice Used

Analysis/Method

Time (Start)

Time (Stop)

Total Time

SUMMA WENT TO YES/NO YES/NO YES/NO YES/NO YES/NOAMBIENT

Pressure Gauge

Pressure Gauge

Flow Rate (Pre)

Flow Rate (Post)

Flow Rate (Average)

MET Station On-site? Y / N

General Comments:

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SOP#: 1706DATE: 09/12/94

REV. #: 0.0

SUMMA CANISTERFIELD STANDARDS


The objective of this procedure is to establish standardoperating practices for the use of Summa canisters.Summa polished canisters are used to store calibrationgas standards for transport to field sampling sites.These standards contained in the Summa canisterswill be used for calibration of field instrumentation.In addition, a series of different concentrations of gasstandards, or dilutions in the field of a single canister,can be used to construct calibration curves and toascertain minimum detection limits on various fieldinstrumentation currently used by EPA/ERT.


2.0 METHOD SUMMARY

A clean evacuated Summa canister is obtained. Acertified gas standard cylinder is selected and adelivery pressure of 20-30 psi is set. The lines arebled with the gas standard. Then, the Summa canisteris opened while still attached to the gas standard line,and is charged to 20-30 psi with the certified gasstandard cylinder. The Summa canister is closed andthe gas standard lines are removed. A "tee" with aseptum is attached onto the Swagelok fitting of theSumma canister. The "tee" is purged with thecontents of the Summa canister. The Summa canistervalve is opened and samples can be taken via a gastight syringe through the septum on the "tee". Thevalve is closed when not in use. Tedlar bags can alsobe filled from the "tee".


Samples and gas standards can be kept several monthsin the Summa polished canisters. Care must be takento ensure no leaks occur when the "tee" and septum

are used. In addition, the needle valve on the Summacanister must be completely closed when not in use.When transporting and storing, the Summa canister isplaced in a plastic shipping container. This willprotect the canister from accidental punctures ordents.


As long as the gas standards and all transfer lines areclean, no interferences are expected. The initialpressure of the Summa canister should be recordedafter filling. In addition, the pressure should berecorded after each use. A dramatic drop in pressure(i.e., five psi or more) may invalidate the use of thatcanister.


C Summa Canister, 6-liter total volumeCat # 87-300, Anderson Samplers, Inc.4215 Wendell Drive, Atlanta, GA 30376PN # 0650, SIS, P.O. Box 8941, 815Courtney St., Moscow, Idaho 83843

C Certified gas standard from Scott Gas,Matheson or other reliable manufacturer

C Hamilton gas tight syringe with Teflon sealplugs in various sizes

C Clean Teflon tubing, 1/4" O.D.

C Swagelok "tee" 1/4" O.D. Teflon

C 1/4" Teflon swagelok nuts & ferrules

C 9-mm septa, preferably Teflon backed

C Swagelok on/off or needle valve, 1/4" O.D.stainless steel

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6.0 REAGENTS

All standards must be vapor phase pressurized gascylinders, certified by the manufacturer to be within±2% accuracy, and to be NBS traceable. ScottSpecialty Gas or Matheson Gas can provide thesestandards. If field dilution is required, a cylinder ofultra high purity air is required.

7.0 PROCEDURES

1. Obtain a Summa polished canister that hasbeen cleaned and evacuated and select acompressed gas cylinder of a certifiedstandard. This standard should be certifiedby the manufacturer to be within ±2% for theaccuracy of the concentration level and beNBS traceable.

2. A high purity dual stage regulator is attachedto the standard cylinder. This must deliver20-30 psi pressure at an accuracy of ±10% orbetter.

3. A section of clean, unused 1/4" O.D. Teflontubing is attached to the Teflon "tee".

4. The side port of the "tee" has an on/off valveor needle valve connected to it (Figure 1,Appendix A).

5. A vent line is temporally connected to theoutlet port of the side valve and placed in afume hood or on an outside vent. TheSumma canister charging system appears inFigure 2 (Appendix A).

6. The standard cylinder is opened at 20-30 psifrom the outlet of the cylinder regulator.

7. The needle valve on the Summa canister isstill closed at this point. The side valve onthe "tee" is opened and the standardcylinder's 1/4" Teflon feed lines are allowedto vent for one-two minutes.

8. The valve is then closed tightly and theneedle valve on the Summa canister isslowly opened. A hissing noise should beheard. Do not fill the Summa canisters toorapidly. Allow the canister to continuefilling.

9. Periodically check the pressure on the dualstage regulator attached to the standardcylinder to ensure 20-30 psi is beingdelivered.

10. Once the hissing stops, the canister should befilled to approximately the same pressure asthe line delivery pressure.

11. Close the needle valve on the Summacanister tightly.

12. Close the standard cylinder and vent the feedlines.

13. Remove the feed line from the top of theTeflon "tee".

14. Place a Swagelok back ferrule, in theinverted position, on the top of the "tee".This will provide a flat surface on which aTeflon-backed septum can be placed.

15. Place the Teflon-backed septum, Teflon sidedown. The septum should create a gas tightfit once a 1/4" Swagelok nut is tightenedonto the top of the "tee" (Figures 3 and 4,Appendix A).

16. Open the needle valve on the Summacanister to check for leaks throughout the"tee", particularly in the septum fitting. Dothis with the valve on the side of the "tee"closed.

17. Afterwards, slowly open the side valve of the"tee" and vent for 1/2 minute and re-close.The septum "tee" is now ready for samplingfrom the canister using a gas tight syringethrough the septum seal.

18. Close the Summa canister needle valvebetween sample taking with the gas tightsyringe.

19. Periodically, vent or flush the "tee" toprovide fresh standard for sampling. Theside valve can also be used, after flushing, tofill Tedlar bags with the standard from theSumma canister.

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8.0 CALCULATIONS 10.0 DATA VALIDATION

The procedure for performing field dilutions of the This section is not applicable to this SOP.standards from the Summa canisters must bedocumented. This allows for the recalculation ofconcentrations of standards if any discrepancies arisein the calibration of the field instrumentation. Simplevolumetric dilutions using Hamilton gas tightsyringes, are performed using Tedlar bags with ultrahigh purity air as the diluent.

9.0 QUALITY ASSURANCE/QUALTIY CONTROL

The concentration levels of the certified gas standardsmust be recorded. The vendor typically provides theanalysis of certification with each standards cylinder;a copy should be provided with the Summa canister. This section is not applicable to this SOP.

As previously stated, the pressure of the canister alongwith the date and time, should be recorded at theinitial filling and at the end of each use of the canister.A drop in pressure of 5-10 psi in between usages mayinvalidate the canister for use as a calibrationstandard. Certification of canister cleaning andevacuation should be noted prior to filling withstandards.


Pressurizing of Summa canisters should be performedin a well ventilated room, or preferably under a fumehood. Care must be taken not to exceed 40 psi in thecanisters. Canisters are under pressure, albeit only20-30 psi, and should not be dented or punctured.They should be stored in a cool dry place and alwaysbe placed in their plastic shipping boxes duringtransport and storage.

12.0 REFERENCES

4

APPENDIX A

Figures

FIGURE 1. Teflon "Tee" Setup

5

APPENDIX A - (Con't)

Figures

FIGURE 2. Summa Canister Charging System

6

APPENDIX A - (Con’t)

Figures

FIGURE 3. Septum "Tee" Setup

7

APPENDIX A - (Con't)

Figures

FIGURE 4. Teflon Nut with Septum

1

SOP#: 2001DATE: 08/11/94

REV. #: 0.0 GENERAL FIELD

SAMPLING GUIDELINES


The purpose of this Standard Operating Procedure(SOP) is to provide general field sampling guidelinesthat will assist REAC personnel in choosing samplingstrategies, location, and frequency for properassessment of site characteristics. This SOP isapplicable to all field activities that involve sampling.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent on site conditions, equipmentlimitations or limitations imposed by the procedure. Inall instances, the ultimate procedures employed shouldbe documented and associated with the final report.


2.0 METHOD SUMMARY

Sampling is the selection of a representative portion ofa larger population, universe, or body. Throughexamination of a sample, the characteristics of thelarger body from which the sample was drawn can beinferred. In this manner, sampling can be a valuabletool for determining the presence, type, and extent ofcontamination by hazardous substances in theenvironment.

The primary objective of all sampling activities is tocharacterize a hazardous waste site accurately so thatits impact on human health and the environment canbe properly evaluated. It is only through sampling andanalysis that site hazards can be measured and the jobof cleanup and restoration can be accomplishedeffectively with minimal risk. The sampling itselfmust be conducted so that every sample collectedretains its original physical form and chemicalcomposition. In this way, sample integrity is insured,quality assurance standards are maintained, and thesample can accurately represent the larger body of

material under investigation.

The extent to which valid inferences can be drawnfrom a sample depends on the degree to which thesampling effort conforms to the project's objectives.For example, as few as one sample may produceadequate, technically valid data to address theproject's objectives. Meeting the project's objectivesrequires thorough planning of sampling activities, andimplementation of the most appropriate sampling andanalytical procedures. These issues will be discussedin this procedure.


The amount of sample to be collected, and the propersample container type (i.e., glass, plastic), chemicalpreservation, and storage requirements are dependenton the matrix being sampled and the parameter(s) ofinterest. Sample preservation, containers, handling,and storage for air and waste samples are discussed inthe specific SOPs for air and waste samplingtechniques.


The nature of the object or materials being sampledmay be a potential problem to the sampler. If amaterial is homogeneous, it will generally have auniform composition throughout. In this case, anysample increment can be considered representative ofthe material. On the other hand, heterogeneoussamples present problems to the sampler because ofchanges in the material over distance, both laterallyand vertically.

Samples of hazardous materials may pose a safetythreat to both field and laboratory personnel. Properhealth and safety precautions should be implementedwhen handling this type of sample.

2

Environmental conditions, weather conditions, or The importance of making the distinction betweennon-target chemicals may cause problems and/or environmental and hazardous samples is two-fold:interferences when performing sampling activities orwhen sampling for a specific parameter. Refer to the (1) Personnel safety requirements: Any samplespecific SOPs for sampling techniques. thought to contain enough hazardous


The equipment/apparatus required to collect samplesmust be determined on a site specific basis. Due to thewide variety of sampling equipment available, refer tothe specific SOPs for sampling techniques whichinclude lists of the equipment/apparatus required forsampling.

6.0 REAGENTS

Reagents may be utilized for preservation of samplesand for decontamination of sampling equipment. Thepreservatives required are specified by the analysis tobe performed. Decontamination solutions arespecified in ERT SOP #2006, Sampling EquipmentDecontamination.

7.0 PROCEDURE

7.1 Types of Samples

In relation to the media to be sampled, two basic typesof samples can be considered: the environmentalsample and the hazardous sample.

Environmental samples are those collected fromstreams, ponds, lakes, wells, and are off-site samplesthat are not expected to be contaminated withhazardous materials. They usually do not require thespecial handling procedures typically used forconcentrated wastes. However, in certain instances,environmental samples can contain elevatedconcentrations of pollutants and in such cases wouldhave to be handled as hazardous samples.

Hazardous or concentrated samples are those collectedfrom drums, tanks, lagoons, pits, waste piles, freshspills, or areas previously identified as contaminated,and require special handling procedures because oftheir potential toxicity or hazard. These samples canbe further subdivided based on their degree of hazard;however, care should be taken when handling andshipping any wastes believed to be concentratedregardless of the degree.

materials to pose a safety threat should bedesignated as hazardous and handled in amanner which ensures the safety of both fieldand laboratory personnel.

(2) Transportation requirements: Hazardoussamples must be packaged, labeled, andshipped according to the International AirTransport Association (IATA) DangerousGoods Regulations or Department ofTransportation (DOT) regulations and U.S.EPA guidelines.

7.2 Sample Collection Techniques

In general, two basic types of sample collectiontechniques are recognized, both of which can be usedfor either environmental or hazardous samples.

Grab Samples

A grab sample is defined as a discrete aliquotrepresentative of a specific location at a given point intime. The sample is collected all at once at oneparticular point in the sample medium. Therepresentativeness of such samples is defined by thenature of the materials being sampled. In general, assources vary over time and distance, therepresentativeness of grab samples will decrease.

Composite Samples

Composites are nondiscrete samples composed ofmore than one specific aliquot collected at varioussampling locations and/or different points in time.Analysis of this type of sample produces an averagevalue and can in certain instances be used as analternative to analyzing a number of individual grabsamples and calculating an average value. It shouldbe noted, however, that compositing can maskproblems by diluting isolated concentrations of somehazardous compounds below detection limits.

Compositing is often used for environmental samplesand may be used for hazardous samples under certainconditions. For example, compositing of hazardouswaste is often performed after compatibility tests have

3

been completed to determine an average value over a concentration), and basis of thenumber of different locations (group of drums). This information/data.procedure generates data that can be useful by C Technical approach including media/matrixproviding an average concentration within a number to be sampled, sampling equipment to beof units, can serve to keep analytical costs down, and used, sample equipment decontamination (ifcan provide information useful to transporters and necessary), sampling design and rationale,waste disposal operations. and SOPs or description of the procedure to

For sampling situations involving hazardous wastes, C Project management and reporting, schedule,grab sampling techniques are generally preferred project organization and responsibilities,because grab sampling minimizes the amount of time manpower and cost projections, and requiredsampling personnel must be in contact with the deliverables.wastes, reduces risks associated with compositing C QA objectives and protocols including tablesunknowns, and eliminates chemical changes that summarizing field sampling and QA/QCmight occur due to compositing. analysis and objectives.

7.3 Types of Sampling Strategies

The number of samples that should be collected andanalyzed depends on the objective of the investigation.There are three basic sampling strategies: random,systematic, and judgmental sampling.

Random sampling involves collection of samples in anonsystematic fashion from the entire site or a specificportion of a site. Systematic sampling involvescollection of samples based on a grid or a patternwhich has been previously established. Whenjudgmental sampling is performed, samples arecollected only from the portion(s) of the site mostlikely to be contaminated. Often, a combination ofthese strategies is the best approach depending on thetype of the suspected/known contamination, theuniformity and size of the site, the level/type ofinformation desired, etc.

7.4 QA Work Plans (QAWP)

A QAWP is required when it becomes evident that afield investigation is necessary. It should be initiatedin conjunction with, or immediately following,notification of the field investigation. This plan shouldbe clear and concise and should detail the followingbasic components, with regard to sampling activities:

C Objective and purpose of the investigation.C Basis upon which data will be evaluated.C Information known about the site including

location, type and size of the facility, andlength of operations/abandonment.

C Type and volume of contaminated material,contaminants of concern (including

be implemented.

Note that this list of QAWP components is not all-inclusive and that additional elements may be addedor altered depending on the specific requirements ofthe field investigation. It should also be recognizedthat although a detailed QAWP is quite important, itmay be impractical in some instances. Emergencyresponses and accidental spills are prime examples ofsuch instances where time might prohibit thedevelopment of site-specific QAWPs prior to fieldactivities. In such cases, investigators would have torely on general guidelines and personal judgment, andthe sampling or response plans might simply be astrategy based on preliminary information andfinalized on site. In any event, a plan of action shouldbe developed, no matter how concise or informal, toaid investigators in maintaining a logical andconsistent order to the implementation of their task.

7.5 Legal Implications

The data derived from sampling activities are oftenintroduced as critical evidence during litigation of ahazardous waste site cleanup. Legal issues in whichsampling data are important may include cleanup costrecovery, identification of pollution sources andresponsible parties, and technical validation ofremedial design methodologies. Because of thepotential for involvement in legal actions, strictadherence to technical and administrative SOPs isessential during both the development andimplementation of sampling activities.

Technically valid sampling begins with thoroughplanning and continues through the sample collectionand analytical procedures. Administrativerequirements involve thorough, accurate

4

documentation of all sampling activities.Documentation requirements include maintenance ofa chain of custody, as well as accurate records of fieldactivities and analytical instructions. Failure toobserve these procedures fully and consistently mayresult in data that are questionable, invalid andnon-defensible in court, and the consequent loss ofenforcement proceedings.

8.0 CALCULATIONS

Refer to the specific SOPs for any calculations whichare associated with sampling techniques.


Refer to the specific SOPs for the type and frequencyof QA/QC samples to be analyzed, the acceptancecriteria for the QA/QC samples, and any other QA/QCactivities which are associated with samplingtechniques.


Refer to the specific SOPs for data validationactivities that are associated with samplingtechniques.


When working with potentially hazardous materials,follow U.S. EPA, OSHA, and corporate health andsafety procedures.

1

SOP#: 2006DATE: 08/11/94

REV. #: 0.0

SAMPLING EQUIPMENTDECONTAMINATION


The purpose of this Standard Operating Procedure(SOP) is to provide a description of the methods usedfor preventing, minimizing, or limitingcross-contamination of samples due to inappropriateor inadequate equipment decontamination and toprovide general guidelines for developingdecontamination procedures for sampling equipmentto be used during hazardous waste operations as per29 Code of Federal Regulations (CFR) 1910.120.This SOP does not address personneldecontamination.

These are standard (i.e. typically applicable) operatingprocedures which may be varied or changed asrequired, dependent upon site conditions, equipmentlimitation, or limitations imposed by the procedure.In all instances, the ultimate procedures employedshould be documented and associated with the finalreport.

Mention of trade names or commercial products doesnot constitute U.S. Environmental Protection Agency(U.S. EPA) endorsement or recommendation for use.

2.0 METHOD SUMMARY

Removing or neutralizing contaminants fromequipment minimizes the likelihood of sample crosscontamination, reduces or eliminates transfer ofcontaminants to clean areas, and prevents the mixingof incompatible substances.

Gross contamination can be removed by physicaldecontamination procedures. These abrasive andnon-abrasive methods include the use of brushes, airand wet blasting, and high and low pressure watercleaning.

The first step, a soap and water wash, removes al lvisible particulate matter and residual oils and grease.This may be preceded by a steam or high pressure

water wash to facilitate residuals removal. Thesecond step involves a tap water rinse and adistilled/deionized water rinse to remove thedetergent. An acid rinse provides a low pH media fortrace metals removal and is included in thedecontamination process if metal samples are to becollected. It is followed by another distilled/deionizedwater rinse. If sample analysis does not includemetals, the acid rinse step can be omitted. Next, ahigh purity solvent rinse is performed for traceorganics removal if organics are a concern at the site.Typical solvents used for removal of organiccontaminants include acetone, hexane, or water.Acetone is typically chosen because it is an excellentsolvent, miscible in water, and not a target analyte onthe Priority Pollutant List. If acetone is known to bea contaminant of concern at a given site or if TargetCompound List analysis (which includes acetone) isto be performed, another solvent may be substituted.The solvent must be allowed to evaporate completelyand then a final distilled/deionized water rinse isperformed. This rinse removes any residual traces ofthe solvent.

The decontamination procedure described above maybe summarized as follows:

1. Physical removal2. Non-phosphate detergent wash3. Tap water rinse4. Distilled/deionized water rinse5. 10% nitric acid rinse6. Distilled/deionized water rinse7. Solvent rinse (pesticide grade)8. Air dry9. Distilled/deionized water rinse

If a particular contaminant fraction is not present atthe site, the nine (9) step decontamination procedurespecified above may be modified for site specificity.For example, the nitric acid rinse may be eliminatedif metals are not of concern at a site. Similarly, thesolvent rinse may be eliminated if organics are not of

2

concern at a site. Modifications to the standard bristle scrub brushes or long-handled bottle brushesprocedure should be documented in the site specific can be used to remove contaminants. Largework plan or subsequent report. galvanized wash tubs, stock tanks, or buckets can hold


The amount of sample to be collected and the propersample container type (i.e., glass, plastic), chemicalpreservation, and storage requirements are dependenton the matrix being sampled and the parameter(s) ofinterest. More specifically, sample collection and analysis ofdecontamination waste may be required beforebeginning proper disposal of decontamination liquidsand solids generated at a site. This should bedetermined prior to initiation of site activities.


C The use of distilled/deionized watercommonly available from commercialvendors may be acceptable fordecontamination of sampling equipmentprovided that it has been verified bylaboratory analysis to be analyte free(specifically for the contaminants ofconcern).

C The use of an untreated potable water supplyis not an acceptable substitute for tap water.Tap water may be used from any municipalor industrial water treatment system.

C If acids or solvents are utilized indecontamination they raise health and safety,and waste disposal concerns.

C Damage can be incurred by acid and solventwashing of complex and sophisticatedsampling equipment.


Decontamination equipment, materials, and suppliesare generally selected based on availability. Otherconsiderations include the ease of decontaminating ordisposing of the equipment. Most equipment andsupplies can be easily procured. For example, soft-

wash and rinse solutions. Children's wading pools canalso be used. Large plastic garbage cans or othersimilar containers lined with plastic bags can helpsegregate contaminated equipment. Contaminatedliquid can be stored temporarily in metal or plasticcans or drums.

The following standard materials and equipment arerecommended for decontamination activities:

5.1 Decontamination Solutions

C Non-phosphate detergentC Selected solvents (acetone, hexane, nitric

acid, etc.)C Tap waterC Distilled or deionized water

5.2 Decontamination Tools/Supplies

C Long and short handled brushesC Bottle brushesC Drop cloth/plastic sheetingC Paper towelsC Plastic or galvanized tubs or bucketsC Pressurized sprayers (H O)2

C Solvent sprayersC Aluminum foil

5.3 Health and Safety Equipment

Appropriate personal protective equipment (i.e., safetyglasses or splash shield, appropriate gloves, aprons orcoveralls, respirator, emergency eye wash)

5.4 Waste Disposal

C Trash bagsC Trash containersC 55-gallon drumsC Metal/plastic buckets/containers for storage

and disposal of decontamination solutions

6.0 REAGENTS

There are no reagents used in this procedure asidefrom the actual decontamination solutions. Table 1(Appendix A) lists solvent rinses which may berequired for elimination of particular chemicals. In

3

general, the following solvents are typically utilized contaminants by neutralization, chemical reaction,for decontamination purposes: disinfection, or sterilization.

C 10% nitric acid is typically used for Physical decontamination techniques can be groupedinorganic compounds such as metals. An into two categories: abrasive methods andacid rinse may not be required if inorganics non-abrasive methods, as follows:are not a contaminant of concern.

C Acetone (pesticide grade)(1)

C Hexane (pesticide grade)(1)

C Methanol(1)

- Only if sample is to be analyzed for organics.(1)

7.0 PROCEDURES

As part of the health and safety plan, adecontamination plan should be developed andreviewed. The decontamination line should be set upbefore any personnel or equipment enter the areas ofpotential exposure. The equipment decontaminationplan should include:

C The number, location, and layout ofdecontamination stations.

C Decontamination equipment needed.

C Appropriate decontamination methods.

C Methods for disposal of contaminatedclothing, equipment, and solutions.

C Procedures can be established to minimizethe potential for contamination. This mayinclude: (1) work practices that minimizecontact with potential contaminants; (2)using remote sampling techniques; (3)covering monitoring and sampling equipmentwith plastic, aluminum foil, or otherprotective material; (4) watering down dustyareas; (5) avoiding laying down equipment inareas of obvious contamination; and (6) useof disposable sampling equipment.

7.1 Decontamination Methods

All samples and equipment leaving the contaminatedarea of a site must be decontaminated to remove anycontamination that may have adhered to equipment.Various decontamination methods will removecontaminants by: (1) flushing or other physicalaction, or (2) chemical complexing to inactivate

7.1.1 Abrasive Cleaning Methods

Abrasive cleaning methods work by rubbing andwearing away the top layer of the surface containingthe contaminant. The mechanical abrasive cleaningmethods are most commonly used at hazardous wastesites. The following abrasive methods are available:

Mechanical

Mechanical methods of decontamination include usingmetal or nylon brushes. The amount and type ofcontaminants removed will vary with the hardness ofbristles, length of time brushed, degree of brushcontact, degree of contamination, nature of the surfacebeing cleaned, and degree of contaminant adherenceto the surface.

Air Blasting

Air blasting equipment uses compressed air to forceabrasive material through a nozzle at high velocities.The distance between nozzle and surface cleaned, airpressure, time of application, and angle at which theabrasive strikes the surface will dictate cleaningefficiency. Disadvantages of this method are theinability to control the amount of material removedand the large amount of waste generated.

Wet Blasting

Wet blast cleaning involves use of a suspended fineabrasive. The abrasive/water mixture is delivered bycompressed air to the contaminated area. By using avery fine abrasive, the amount of materials removedcan be carefully controlled.

7.1.2 Non-Abrasive Cleaning Methods

Non-abrasive cleaning methods work by forcing thecontaminant off a surface with pressure. In general,the equipment surface is not removed usingnon-abrasive methods.

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Low-Pressure Water

This method consists of a container which is filledwith water. The user pumps air out of the container tocreate a vacuum. A slender nozzle and hose allow theuser to spray in hard-to-reach places.

High-Pressure Water

This method consists of a high-pressure pump, anoperator controlled directional nozzle, and a high-pressure hose. Operating pressure usually rangesfrom 340 to 680 atmospheres (atm) and flow ratesusually range from 20 to 140 liters per minute.

Ultra-High-Pressure Water

This system produces a water jet that is pressuredfrom 1,000 to 4,000 atmospheres. Thisultra-high-pressure spray can remove tightly-adheredsurface films. The water velocity ranges from 500meters/second (m/s) (1,000 atm) to 900 m/s (4,000atm). Additives can be used to enhance the cleaningaction.

Rinsing

Contaminants are removed by rinsing throughdilution, physical attraction, and solubilization.

Damp Cloth Removal

In some instances, due to sensitive, non-waterproofequipment or due to the unlikelihood of equipmentbeing contaminated, it is not necessary to conduct anextensive decontamination procedure. For example,air sampling pumps hooked on a fence, placed on adrum, or wrapped in plastic bags are not likely tobecome heavily contaminated. A damp cloth shouldbe used to wipe off contaminants which may haveadhered to equipment through airborne contaminantsor from surfaces upon which the equipment was set .

Disinfection/Sterilization

Disinfectants are a practical means of inactivatinginfectious agents. Unfortunately, standardsterilization methods are impractical for largeequipment. This method of decontamination istypically performed off-site.

7.2 Field Sampling EquipmentDecontamination Procedures

The decontamination line is setup so that the firststation is used to clean the most contaminated item.It progresses to the last station where the leastcontaminated item is cleaned. The spread ofcontaminants is further reduced by separating eachdecontamination station by a minimum of three (3)feet. Ideally, the contamination should decrease as theequipment progresses from one station to anotherfarther along in the line.

A site is typically divided up into the followingboundaries: Hot Zone or Exclusion Zone (EZ), theContamination Reduction Zone (CRZ), and theSupport or Safe Zone (SZ). The decontamination lineshould be setup in the Contamination ReductionCorridor (CRC) which is in the CRZ. Figure 1(Appendix B) shows a typical contaminant reductionzone layout. The CRC controls access into and out ofthe exclusion zone and confines decontaminationactivities to a limited area. The CRC boundariesshould be conspicuously marked. The far end is thehotline, the boundary between the exclusion zone andthe contamination reduction zone. The size of thedecontamination corridor depends on the number ofstations in the decontamination process, overalldimensions of the work zones, and amount of spaceavailable at the site. Whenever possible, it should bea straight line.

Anyone in the CRC should be wearing the level ofprotection designated for the decontamination crew.Another corridor may be required for the entry andexit of heavy equipment. Sampling and monitoringequipment and sampling supplies are all maintainedoutside of the CRC. Personnel don their equipmentaway from the CRC and enter the exclusion zonethrough a separate access control point at the hotline.One person (or more) dedicated to decontaminatingequipment is recommended.

7.2.1 Decontamination Setup

Starting with the most contaminated station, thedecontamination setup should be as follows:

Station 1: Segregate Equipment Drop

Place plastic sheeting on the ground (Figure 2,Appendix B). Size will depend on amount of

5

equipment to be decontaminated. Provide containers pool with tap water. Several bottle and bristle brusheslined with plastic if equipment is to be segregated. should be dedicated to this station. ApproximatelySegregation may be required if sensitive equipment or 10-50 gallons of water may be required initiallymildly contaminated equipment is used at the same depending upon the amount of equipment totime as equipment which is likely to be heavily decontaminate and the amount of gross contamination.contaminated.

Station 2: Physical Removal With A High-PressureWasher (Optional) Fill a low-pressure sprayer with distilled/deionized

As indicated in 7.1.2, a high-pressure wash may be the water during the rinsing process. Approximatelyrequired for compounds which are difficult to remove 10-20 gallons of water may be required initiallyby washing with brushes. The elevated temperature of depending upon the amount of equipment tothe water from the high-pressure washers is excellent decontaminate and the amount of gross contamination.at removing greasy/oily compounds. High pressurewashers require water and electricity. Station 6: Nitric Acid Sprayers

A decontamination pad may be required for the high- Fill a spray bottle with 10% nitric acid. An acid rinsepressure wash area. An example of a wash pad may may not be required if inorganics are not aconsist of an approximately 1 1/2 foot-deep basin contaminant of concern. The amount of acid willlined with plastic sheeting and sloped to a sump at one depend on the amount of equipment to becorner. A layer of sand can be placed over the plastic decontaminated. Provide a 5-gallon bucket or basin toand the basin is filled with gravel or shell. The sump collect acid during the rinsing process.is also lined with visqueen and a barrel is placed in thehole to prevent collapse. A sump pump is used to Station 7: Low-Pressure Sprayersremove the water from the sump for transfer into adrum. Fill a low-pressure sprayer with distilled/deionized

Typically heavy machinery is decontaminated at the water during the rinsate process. end of the day unless site sampling requires that themachinery be decontaminated frequently. A separate Station 8: Organic Solvent Sprayersdecontamination pad may be required for heavyequipment. Fill a spray bottle with an organic solvent. After each

Station 3: Physical Removal With Brushes And A distilled/deionized water and air dried. Amount ofWash Basin solvent will depend on the amount of equipment to

Prior to setting up Station 3, place plastic sheeting on collect the solvent during the rinsing process. the ground to cover areas under Station 3 throughStation 10. Solvent rinses may not be required unless organics areFill a wash basin, a large bucket, or child's swimming a contaminant of concern, and may be eliminated frompool with non-phosphate detergent and tap water. the station sequence. Several bottle and bristle brushes to physically removecontamination should be dedicated to this station . Station 9: Low-Pressure SprayersApproximately 10 - 50 gallons of water may berequired initially depending upon the amount of Fill a low-pressure sprayer with distilled/deionizedequipment to decontaminate and the amount of gross water. Provide a 5-gallon bucket or basin to collectcontamination. water during the rinsate process.

Station 4: Water Basin Station 10: Clean Equipment Drop

Fill a wash basin, a large bucket, or child's swimming Lay a clean piece of plastic sheeting over the bottom

Station 5: Low-Pressure Sprayers

water. Provide a 5-gallon bucket or basin to contain

water. Provide a 5-gallon bucket or basin to collect

solvent rinse, the equipment should be rinsed with

decontaminate. Provide a 5-gallon bucket or basin to

6

plastic layer. This will allow easy removal of the Using a spray bottle rinse sampling equipment withplastic in the event that it becomes dirty. Provide nitric acid. Begin spraying (inside and outside) at onealuminum foil, plastic, or other protective material to end of the equipment allowing the acid to drip to thewrap clean equipment. other end into a 5-gallon bucket. A rinsate blank may

7.2.2 Decontamination Procedures

Station 1: Segregate Equipment Drop

Deposit equipment used on-site (i.e., tools, samplingdevices and containers, monitoring instruments radios,clipboards, etc.) on the plastic drop cloth/sheet or indifferent containers with plastic liners. Each will becontaminated to a different degree. Segregation at thedrop reduces the probability of cross contamination.Loose leaf sampling data sheets or maps can be placedin plastic zip lock bags if contamination is evident.

Station 2: Physical Removal With A High-PressureWasher (Optional)

Use high pressure wash on grossly contaminatedequipment. Do not use high- pressure wash onsensitive or non-waterproof equipment.

Station 3: Physical Removal With Brushes And AWash Basin

Scrub equipment with soap and water using bottle andbristle brushes. Only sensitive equipment (i.e., radios,air monitoring and sampling equipment) which iswaterproof should be washed. Equipment which isnot waterproof should have plastic bags removed andwiped down with a damp cloth. Acids and organicrinses may also ruin sensitive equipment. Consult the 1. Collect high-pressure pad and heavymanufacturers for recommended decontamination equipment decontamination area liquid andsolutions. waste and store in appropriate drum or

Station 4: Equipment Rinse collection process. Refer to the Department

Wash soap off of equipment with water by immersing appropriate containers based on thethe equipment in the water while brushing. Repeat as contaminant of concern.many times as necessary.

Station 5: Low-Pressure Rinse equipment decontamination area solid waste

Rinse sampling equipment with distilled/deionized Refer to the DOT requirements forwater with a low-pressure sprayer. appropriate containers based on the

Station 6: Nitric Acid Sprayers ( required only ifmetals are a contaminant of concern) 3. Empty soap and water liquid wastes from

be required at this station. Refer to Section 9.


Rinse sampling equipment with distilled/deionizedwater with a low-pressure sprayer.

Station 8: Organic Solvent Sprayers

Rinse sampling equipment with a solvent. Beginspraying (inside and outside) at one end of theequipment allowing the solvent to drip to the otherend into a 5-gallon bucket. Allow the solvent toevaporate from the equipment before going to the nextstation. A QC rinsate sample may be required at thisstation.


Rinse sampling equipment with distilled/deionizedwater with a low-pressure washer.

Station 10 : Clean Equipment Drop

Lay clean equipment on plastic sheeting. Once airdried, wrap sampling equipment with aluminum foil,plastic, or other protective material.

7.2.3 Post Decontamination Procedures

container. A sump pump can aid in the

of Transportation (DOT) requirements for

2. Collect high-pressure pad and heavy

and store in appropriate drum or container.

contaminant of concern.

basins and buckets and store in appropriate

7

drum or container. Refer to the DOT equipment to test for residual contamination. Therequirements for appropriate containers blank water is collected in sample containers forbased on the contaminant of concern. handling, shipment, and analysis. These samples are

4. Empty acid rinse waste and place in rinsate blank is used to assess cross contaminationappropriate container or neutralize with a brought about by improper decontaminationbase and place in appropriate drum. pH procedures. Where dedicated sampling equipment ispaper or an equivalent pH test is required for not utilized, collect one rinsate blank per day per typeneutralization. Consult DOT requirements of sampling device samples to meet QA2 and QA3for appropriate drum for acid rinse waste. objectives.

5. Empty solvent rinse sprayer and solvent If sampling equipment requires the use of plasticwaste into an appropriate container. Consult tubing it should be disposed of as contaminated andDOT requirements for appropriate drum for replaced with clean tubing before additional samplingsolvent rinse waste. occurs.

6. Using low-pressure sprayers, rinse basins,and brushes. Place liquid generated fromthis process into the wash water rinsecontainer.

7. Empty low-pressure sprayer water onto theground.

8. Place all solid waste materials generatedfrom the decontamination area (i.e., glovesand plastic sheeting, etc.) in an approvedDOT drum. Refer to the DOT requirementsfor appropriate containers based on thecontaminant of concern.

9. Write appropriate labels for waste and makearrangements for disposal. Consult DOTregulations for the appropriate label for eachdrum generated from the decontaminationprocess.

8.0 CALCULATIONS


9.0 QUALITYASSURANCE/QUALITY CONTROL

A rinsate blank is one specific type of quality control substitutions should be made to eliminate the hazard.sample associated with the field decontamination The choice of respiratory protection based onprocess. This sample will provide information on the contaminants of concern from the site may not beeffectiveness of the decontamination process appropriate for solvents used in the decontaminationemployed in the field. process.

Rinsate blanks are samples obtained by running Safety considerations should be addressed when usinganalyte free water over decontaminated sampling abrasive and non-abrasive decontamination

treated identical to samples collected that day. A


Results of quality control samples will be evaluatedfor contamination. This information will be utilizedto qualify the environmental sample results inaccordance with the project's data quality objectives.


When working with potentially hazardous materials ,follow OSHA, U.S. EPA, corporate, and otherapplicable health and safety procedures.

Decontamination can pose hazards under certaincircumstances. Hazardous substances may beincompatible with decontamination materials. Forexample, the decontamination solution may react withcontaminants to produce heat, explosion, or toxicproducts. Also, vapors from decontaminationsolutions may pose a direct health hazard to workersby inhalation, contact, fire, or explosion.

The decontamination solutions must be determined tobe acceptable before use. Decontamination materialsmay degrade protective clothing or equipment; somesolvents can permeate protective clothing. Ifdecontamination materials do pose a health hazard,measures should be taken to protect personnel or

8

equipment. Maximum air pressure produced byabrasive equipment could cause physical injury.Displaced material requires control mechanisms.

Material generated from decontamination activitiesrequires proper handling, storage, and disposal.Personal Protective Equipment may be required forthese activities.

Material safety data sheets are required for alldecontamination solvents or solutions as required bythe Hazard Communication Standard (i.e., acetone,alcohol, and trisodiumphosphate).

In some jurisdictions, phosphate containing detergents(i.e., TSP) are banned.

12.0 REFERENCES

Field Sampling Procedures Manual, New JerseyDepartment of Environmental Protection, February,1988.

A Compendium of Superfund Field OperationsMethods, EPA 540/p-87/001.

Engineering Support Branch Standard OperatingProcedures and Quality Assurance Manual, USEPARegion IV, April 1, 1986.

Guidelines for the Selection of Chemical ProtectiveClothing, Volume 1, Third Edition, AmericanConference of Governmental Industrial Hygienists,Inc., February, 1987.

Occupational Safety and Health Guidance Manual forHazardous Waste Site Activities,NIOSH/OSHA/USCG/EPA, October, 1985.

9

APPENDIX A

Table

Table 1. Soluble Contaminants and Recommended Solvent Rinse

TABLE 1Soluble Contaminants and Recommended Solvent Rinse

SOLVENT EXAMPLES OF SOLUBLE(1)

SOLVENTS CONTAMINANTS

Water Deionized water Low-chain hydrocarbonsTap water Inorganic compounds

SaltsSome organic acids and other polarcompounds

Dilute Acids Nitric acid Basic (caustic) compounds (e.g., aminesAcetic acid and hydrazines)Boric acid

Dilute Bases Sodium bicarbonate (e.g., Acidic compoundssoap detergent) Phenol

ThiolsSome nitro and sulfonic compounds

Organic Solvents Alcohols Nonpolar compounds (e.g., some(2)

Ethers organic compounds) Ketones Aromatics Straight chain alkalines(e.g., hexane) Common petroleumproducts (e.g., fuel, oil,kerosene)

Organic Solvent Hexane PCBs(2)

- Material safety data sheets are required for all decontamination solvents or solutions as required(1)

by the Hazard Communication Standard

- WARNING: Some organic solvents can permeate and/or degrade the protective clothing(2)

10

APPENDIX B

Figures

Figure 1. Contamination Reduction Zone Layout

11

APPENDIX B (Cont’d.)

Figures

Figure 2. Decontamination Layout

1

SOP#: 2007DATE: 01/26/95

REV. #: 0.0 GROUNDWATER WELL

SAMPLING


The objective of this standard operating procedure(SOP) is to provide general reference information onsampling of ground water wells. This guideline isprimarily concerned with the collection of watersamples from the saturated zone of the subsurface.Every effort must be made to ensure that the sampleis representative of the particular zone of water beingsampled. These procedures are designed to be used inconjunction with analyses for the most common typesof ground water contaminants (e.g., volatile and semi-volatile organic compounds, pesticides, metals,biological parameters).

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent upon site conditions,equipment limitations or limitations imposed by theprocedure. In all instances, the ultimate proceduresemployed should be documented and associated withthe final report.

Mention of trade names or commercial products doesnot constitute U.S. Environmental Protection Agency(EPA) endorsement or recommendation for use.

2.0 METHOD SUMMARY

In order to obtain a representative groundwater samplefor chemical analysis it is important to removestagnant water in the well casing and the waterimmediately adjacent to the well before collection ofthe sample. This may be achieved with one of anumber of instruments. The most common of theseare the bailer, submersible pump, non-contact gasbladder pump, inertia pump and suction pump. At aminimum, three well volumes should be purged, ifpossible. Equipment must be decontaminated prior touse and between wells. Once purging is completedand the correct laboratory-cleaned sample containershave been prepared, sampling may proceed. Samplingmay be conducted with any of the above instruments,

and need not be the same as the device used forpurging. Care should be taken when choosing thesampling device as some will affect the integrity ofthe sample. Sampling should occur in a progressionfrom the least to most contaminated well, if thisinformation is known.

The growing concern over the past several years overlow levels of volatile organic compounds in watersupplies has led to the development of highlysophisticated analytical methods that can providedetection limits at part per trillion levels. While thelaboratory methods are extremely sensitive, wellcontrolled and quality assured, they cannotcompensate for a poorly collected sample. Thecollection of a sample should be as sensitive, highlydeveloped and quality assured as the analyticalprocedures.


The type of analysis for which a sample is beingcollected determines the type of bottle, preservative,holding time, and filtering requirements. Samplesshould be collected directly from the sampling deviceinto appropriate laboratory cleaned containers. Checkthat a Teflon liner is present in the cap, if required.Attach a sample identification label. Complete a fielddata sheet, a chain of custody form, and record allpertinent data in the site logbook.

Samples shall be appropriately preserved, labelled,logged, and placed in a cooler to be maintained at4EC. Samples must be shipped well before theholding time is up and ideally should be shippedwithin 24 hours of sample collection. It is imperativethat samples be shipped or delivered daily to theanalytical laboratory in order to maximize the timeavailable for the laboratory to perform the analyses.The bottles should be shipped with adequate packingand cooling to ensure that they arrive intact.

2

Sample retrieval systems suitable for the validcollection of volatile organic samples are: positivedisplacement bladder pumps, gear driven submersiblepumps, syringe samplers and bailers (Barcelona, 1984;Nielsen, 1985). Field conditions and other constraintswill limit the choice of appropriate systems. Thefocus of concern must remain to provide a validsample for analysis, one which has been subjected tothe least amount of turbulence possible.

Treatment of the sample with sodium thiosulfatepreservative is required only if there is residualchlorine in the water that could cause free radicalchlorination and change the identity of the originalcontaminants. It should not be used if there is nochlorine in the water.

Holding time for volatiles analysis is seven days. It isimperative that the sample be shipped or delivereddaily to the analytical laboratory. The bottles must beshipped on their sides to aid in maintaining the airtightseal during shipment, with adequate packing andcooling to ensure that they arrive intact.

For collection of volatile organic samples, refer to thework plan to ensure that 40 mL glass sample vialswith Teflon lined septa are ordered and in sufficientnumbers. Check sampling supplies; field kit forchlorine, preservatives, Parafilm, foam sleeves andcoolers. Due to the extreme trace levels at whichvolatile organics are detectable, cross contaminationand introduction of contaminants must be avoided.Trip blanks are incorporated into the shipmentpackage to provide a check against crosscontamination.


4.1 General

The primary goal in performing ground watersampling is to obtain a representative sample of theground water body. Analysis can be compromised byfield personnel in two primary ways: (1) taking anunrepresentative sample, or (2) by incorrect handlingof the sample. There are numerous ways ofintroducing foreign contaminants into a sample, andthese must be avoided by following strict samplingprocedures and utilizing trained field personnel.

4.2 Purging

In a nonpumping well, there will be little or novertical mixing of the water, and stratification willoccur. The well water in the screened section willmix with the ground water due to normal flowpatterns, but the well water above the screened sectionwill remain isolated, become stagnant, and may lackthe contaminants representative of the ground water.Persons sampling should realize that stagnant watermay contain foreign material inadvertently ordeliberately introduced from the surface, resulting inan unrepresentative sample. To safeguard againstcollecting nonrepresentative stagnant water, thefollowing guidelines and techniques should beadhered to during sampling:

1. As a general rule, all monitor wells should bepumped or bailed prior to sampling. Purgewater should be containerized on site orhandled as specified in the site specificproject plan. Evacuation of a minimum ofone volume of water in the well casing, andpreferably three to five volumes, isrecommended for a representative sample.In a high-yielding ground water formationand where there is no stagnant water in thewell above the screened section, evacuationprior to sample withdrawal is not as critical.However, in all cases where the monitoringdata is to be used for enforcement actions,evacuation is recommended.

2. When purging with a pump (not a bailer), thepump should be set at the screened interval,or if the well is an open-rock well, it shouldbe set at the same depth the sample will becollected. When sampling a screened well,the sample should also be collected from thesame depth the pump was set at.

3. The well should be sampled as soon aspossible after purging.

4. Analytical parameters typically dictatewhether the sample should be collectedthrough the purging device, or through aseparate sampling instrument.

5. For wells that can be pumped or bailed todryness with the equipment being used, thewell should be evacuated and allowed to

3

recover prior to collecting a sample. If the Advantagesrecovery rate is fairly rapid and time allows,evacuation of more than one volume of water C Only practical limitations on size andis preferred. If recovery is slow, sample the materialswell upon recovery after one evacuation.

6. A non-representative sample can also resultfrom excessive pre-pumping of the C Portablemonitoring well. Stratification of theleachate concentration in the ground water C Inexpensive, so it can be dedicated and hungformation may occur, or heavier-than-water in a well, thereby reducing the chances ofcompounds may sink to the lower portions of cross contaminationthe aquifer. Excessive pumping can dilute orincrease the contaminant concentrations from C Minimal outgassing of volatile organicswhat is representative of the sampling point while sample is in bailerof interest.

4.3 Materials

Materials of construction for samplers and evacuationequipment (bladders, pump, bailers, tubing, etc.)should be limited to stainless steel, Teflon , and glassR

in areas where concentrations are expected to be at ornear the detection limit. The tendency of organics toleach into and out of many materials make theselection of materials critical for trace analyses. Theuse of plastics, such as PVC or polyethylene, shouldbe avoided when analyzing for organics. However,PVC may be used for evacuation equipment as it willnot come in contact with the sample, and in highlycontaminated wells, disposable equipment (i.e.,polypropylene bailers) may be appropriate to avoidcross-contamination.

Materials of construction (bladders/ pumps, bailers,tubing, etc.) suitable for collecting and handlingVolatile Organic Samples should be limited tostainless steel, Teflon and glass in areas whichdetection limit range concentrations are expected.The tendency of organics to leach into and out ofmany materials, make the selection of materials Advantagescritical for these trace analyses. The use of plastics,e.g., PVC etc., should be avoided. There are C Portable and can be transported to severalnumerous ways of introducing foreign contaminants wellsinto a sample, and these must be avoided by followingstrict sampling procedures and utlization of trained C Depending upon the size of the pump and thepersonnel. pumping depths, relatively high pumping

4.4 Advantages/Disadvantages ofCertain Equipment

4.4.1 Bailers

C No power source needed

C Readily available

C Removes stagnant water first

C Rapid, simple method for removing smallvolumes of purge water

Disadvantages

C Time-consuming to flush a large well ofstagnant water

C Transfer of sample may cause aeration

C Stoppers at the bottom of the bailer usuallyleak thus the bailer must be brought to thesurface rapidly

C If the bailer is allowed to hit the bottom ofthe well boring, gravel can displace the ballvalve not allowing the bailer to hold water

4.4.2 Submersible Pumps

rates are possible

C Generally very reliable and does not requirepriming

4

Disadvantages C Restricted to areas with water levels within

C Potential for effects on analysis of traceorganics C Vacuum can cause loss of dissolved gasses

C Heavy and cumbersome to deal with,particularly in deeper wells C Pump must be primed and vacuum is often

C Expensive pumping

C Power source needed

C Sediment in water may cause problems withthe pumps

C Impractical in low yielding or shallow wells

4.4.3 Non-Contact Gas Bladder Pumps

Advantages Disadvantages

C Maintains integrity of sample C Restricted to areas with water levels within

C Easy to use

C Can sample from discrete locations within these manual pumpsthe monitor well

Disadvantages

C Difficulty in cleaning, though dedicated diameter wellstubing and bladder may be used

C Only useful to about 100 feet

C Supply of gas for operation, gas bottlesand/or compressors are often difficult toobtain and are cumbersome

C Relatively low pumping rates

C Requires air compressor or pressurized gassource and control box

4.4.4 Suction Pumps

Advantages

C Portable, inexpensive, and readily available

Disadvantages

20 to 25 feet of the ground surface

and volatile organics

difficult to maintain during initial stages of

4.4.5 Inertia Pumps

Advantages

C Portable, inexpensive, and readily available

C Offers a rapid method for purging relativelyshallow wells

70 feet of the ground surface

C May be time consuming to purge wells with

C Labor intensive

C WaTerra pumps are only effective in 2-inch

5.0 EQUIPMENT APPARATUS

5.1 Equipment Checklist

5.1.1 General

C Water level indicator - electric sounder- steel tape- transducer- reflection sounder- airline

C Depth sounderC Appropriate keys for well cap locksC Steel brushC HNU or OVA (whichever is most

appropriate)C LogbookC CalculatorC Field data sheets and samples labels

5

C Chain of custody records and seals - wire strippersC Sample containers - electrical tapeC Engineer's rule - heat shrinkC Sharp knife (locking blade) - hose connectorsC Tool box (to include at least: screwdrivers, - Teflon tape

pliers, hacksaw, hammer, flashlight, C Winch, pulley or hoistadjustable wrench) C Gasoline for generator/gas can

C Leather work gloves C Flow meter with gate valveC Appropriate Health & Safety gear C 1" nipples and various plumbing (i.e., pipeC 5-gallon pail connectors)C Plastic sheeting C Control box (if necessary)C Shipping containersC Packing materialsC Bolt cuttersC Ziploc plastic bags C Containers for evacuation liquidsC Decontamination solutions C Tap waterC Non phosphate soapC Several brushesC Pails or tubsC Aluminum foilC Garden sprayer C Preservatives C Distilled or deionized waterC Fire extinguisher (if using a generator for

your power source)

5.1.2 Bailers

C Clean, decontaminated bailers of appropriatesize and construction material

C Nylon line, enough to dedicate to each wellC Teflon coated bailer wireC Sharp knifeC Aluminum foil (to wrap clean bailers)C Five gallon bucket

5.1.3 Submersible Pump

C Pump(s)C Generator (110, 120, or 240 volt) or 12 volt

battery if inaccessible to field vehicle - ampmeter is useful

C 1" black PVC coil tubing - enough todedicate to each well

C Hose clampsC Safety cable C Tool box supplement

- pipe wrenches

5.1.4 Non-Gas Contact Bladder Pump

C Non-gas contact bladder pumpC Compressor or nitrogen gas tankC Batteries and chargerC Teflon tubing - enough to dedicate to each

wellC Swagelock fittingC Toolbox supplements - same as submersible

pumpC Control box (if necessary)

5.1.5 Suction Pump

C PumpC 1" black PVC coil tubing - enough to

dedicate to each wellC Gasoline - if requiredC ToolboxC Plumbing fittingsC Flow meter with gate valve

5.1.6 Inertia Pump

C Pump assembly (WaTerra pump, pistonpump)

C Five gallon bucket

6.0 REAGENTS

Reagents may be utilized for preservation of samplesand for decontamination of sampling equipment. Thepreservatives required are specified by the analysis tobe performed. Decontamination solutions arespecified in ERT SOP #2006, Sampling EquipmentDecontamination.

6

7.0 PROCEDURE

7.1 Preparation

1. Determine the extent of the sampling effort,the sampling methods to be employed, andthe types and amounts of equipment andsupplies needed (i.e, diameter and depth ofwells to be sampled).

2. Obtain necessary sampling and monitoringequipment, appropriate to type ofcontaminant being investigated. Forcollection of volatile organic samples, referto the work plan to ensure that 40 mL glasssample vials with Teflon lined septa areordered and in sufficient numbers. Checksampling supplies; field kit for chlorine,preservatives, Parafilm, foam sleeves andcoolers. Due to extreme trace levels atwhich volatile organics are detectable, crosscontamination and introduction ofcontaminants must be avoided. Trip blanksare incorporated into the shipment package toprovide a check against cross contamination.

3. Decontaminate or preclean equipment, andensure that it is in working order.

4. Prepare scheduling and coordinate with staff,clients, and regulatory agency, if appropriate.

5. Perform a general site survey prior to siteentry in accordance with the site specificHealth and Safety Plan.

6. Identify and mark all sampling locations.

7.2 Field Preparation

1. Start at the least contaminated well, ifknown.

2. Lay plastic sheeting around the well tominimize likelihood of contamination ofequipment from soil adjacent to the well.

3. Remove locking well cap, note location, timeof day, and date in field notebook orappropriate log form.

4. Remove well casing cap.

5. Screen headspace of well with an appropriatemonitoring instrument to determine thepresence of volatile organic compounds andrecord in site logbook.

6. Lower water level measuring device orequivalent (i.e., permanently installedtransducers or airline) into well until watersurface is encountered.

7. Measure distance from water surface toreference measuring point on well casing orprotective barrier post and record in sitelogbook. Alternatively, if no reference point,note that water level measurement is fromtop of steel casing, top of PVC riser pipe,from ground surface, or some other positionon the well head.

If floating organics are of concern, this canbe determined by measuring the water levelwith an oil/water interface probe whichmeasures floating organics.

8. Measure total depth of well (at least twice toconfirm measurement) and record in sitelogbook or on field data sheet.

9. Calculate the volume of water in the well andthe volume to be purged using thecalculations in Section 8.0.

10. Select the appropriate purging and samplingequipment.

11. If residual chlorine is suspected, use theHach Field Test Kit for chlorine to determineif there is residual chlorine in the water to besampled. If there is, treat the sample vialwith a crystal of sodium thiosulfate prior tosample collection.

7.3 Purging

The amount of flushing a well receives prior to samplecollection depends on the intent of the monitoringprogram as well as the hydrogeologic conditions.Programs where overall quality determination of waterresources are involved may require long pumpingperiods to obtain a sample that is representative of alarge volume of that aquifer. The pumped volume canbe determined prior to sampling so that the sample is

7

a collected after a known volume of the water is foreign materials.evacuated from the aquifer, or the well can be pumpeduntil the stabilization of parameters such as 3. Attach the line to the bailer and slowly lowertemperature, electrical conductance, pH, or turbidity until the bailer is completely submerged,has occurred. being careful not to drop the bailer to the

However, monitoring for defining a contaminant loss of volatile organic contaminants.plume requires a representative sample of a smallvolume of the aquifer. These circumstances require 4. Pull bailer out ensuring that the line eitherthat the well be pumped enough to remove the falls onto a clean area of plastic sheeting orstagnant water but not enough to induce flow from never touches the ground.other areas. Generally, three well volumes areconsidered effective, or calculations can be made to 5. Empty the bailer into a pail until full todetermine, on the basis of the aquifer parameters and determine the number of bails necessary towell dimensions, the appropriate volume to remove achieve the required purge volume.prior to sampling.

During purging, water level measurements may be and dispose of purge waters as specified intaken regularly at 15-30 second intervals. This data the site specific sampling plan.may be used to compute aquifer transmissivity andother hydraulic characteristics. The following wellevacuation devices are most commonly used. Otherevacuation devices are available, but have beenomitted in this discussion due to their limited use.

7.3.1 Bailers

Bailers are the simplest purging device used and have can be disassembled easily to allow surfaces contactedmany advantages. They generally consist of a rigid by contaminants to be cleaned, field decontaminationlength of tube, usually with a ball check-valve at the may be difficult and require solvents that can affectbottom. A line is used to lower the bailer into the sample analysis. The use of submersible pumps inwell and retrieve a volume of water. The three most multiple well-sampling programs, therefore, should becommon types of bailer are PVC, Teflon, and stainless carefully considered against other samplingsteel. mechanisms (bailers, bladder pumps). In most cases,

This manual method of purging is best suited to a submersible pump, however, submersible pumpsshallow or narrow diameter wells. For deep, larger may be the only practical sampling device fordiameter wells which require evacuation of large extremely deep wells (greater than 300 feet of water).volumes of water, other mechanical devices may be Under those conditions, dedicated pump systemsmore appropriate. should be installed to eliminate the potential for cross-

7.3.1.1 Operation

Equipment needed will include a cleandecontaminated bailer, Teflon or nylon line, a sharpknife, and plastic sheeting.

1. Determine the volume of water to be purgedas described in 8.0, calculations.

2. Lay plastic sheeting around the well toprevent contamination of the bailer line with

water, causing turbulence and the possible

6. Thereafter, pour the water into a container


The use of submersible pumps for sample collectionis permissible provided they are constructed ofsuitably noncontaminating materials. The chiefdrawback, however, is the difficulty avoiding cross-contamination between wells. Although some units

a sample can be collected by bailer after purging with

contamination of well samples.

Submersible pumps generally use one of two types ofpower supplies, either electric or compressed gas orair. Electric powered pumps can run off a 12 volt DCrechargeable battery, or a 110 or 220 volt AC powersupply. Those units powered by compressed airnormally use a small electric or gas-powered aircompressor. They may also utilize compressed gas(i.e., nitrogen) from bottles. Different size pumps areavailable for different depth or diameter monitoringwells.

8

7.3.2.1 Operation

1. Determine the volume of water to be purgedas described in 8.0 Calculations.

2. Lay plastic sheeting around the well toprevent contamination of pumps, hoses orlines with foreign materials.

3. Assemble pump, hoses and safety cable, and They include: centrifugal, peristaltic and diaphragm.lower the pump into the well. Make sure the Diaphragm pumps can be used for well evacuation atpump is deep enough so all the water is not a fast pumping rate and sampling at a low pumpingevacuated. (Running the pump without water rate. The peristaltic pump is a low volume pump thatmay cause damage.) uses rollers to squeeze the flexible tubing thereby

4. Attach flow meter to the outlet hose to well to prevent cross contamination. Peristalticmeasure the volume of water purged. pumps, however, require a power source.

5. Use a ground fault circuit interrupter (GFCI)or ground the generator to avoid possibleelectric shock.

6. Attach power supply, and purge the welluntil the specified volume of water has beenevacuated (or until field parameters, such astemperature, pH, conductivity, etc, havestabilized). Do not allow the pump to rundry. If the pumping rate exceeds the wellrecharge rate, lower the pump further into thewell, and continue pumping.

7. Collect and dispose of purge waters asspecified in the site specific sampling plan.


For this procedure, an all stainless-steel and TeflonMiddleburg-squeeze bladder pump (e.g., IEA,TIMCO, Well Wizard, Geoguard, and others) is usedto provide the least amount of material interference tothe sample (Barcelona, 1985). Water comes intocontact with the inside of the bladder (Teflon) and thesample tubing, also Teflon, that may be dedicated toeach well. Some wells may have permanentlyinstalled bladder pumps, (i.e., Well Wizard,Geoguard), that will be used to sample for allparameters.

7.3.3.1 Operation

1. Assemble Teflon tubing, pump and chargedcontrol box.

2. Procedure for purging with a bladder pump is

the same as for a submersible pump (Section7.3.2.1).

3. Be sure to adjust flow rate to prevent violentjolting of the hose as sample is drawn in.

7.3.4 Suction Pumps

There are many different types of suction pumps.

creating suction. This tubing can be dedicated to a

7.3.4.1 Operation

1. Assembly of the pump, tubing, and powersource if necessary.

2. Procedure for purging with a suction pump isexactly the same as for a submersible pump(Section 7.3.2.1).

7.3.5 Inertia Pumps

Inertia pumps such as the WaTerra pump and pistonpump, are manually operated. They are mostappropriate to use when wells are too deep to bail byhand, or too shallow or narrow (or inaccessible) towarrant an automatic (submersible, etc.) pump. Thesepumps are made of plastic and may be eitherdecontaminated or discarded.

7.3.5.1 Operation

1. Determine the volume of water to be purgedas described in 8.0, Calculations.

2. Lay plastic sheeting around the well toprevent contamination of pumps or hoseswith foreign materials.

3. Assemble pump and lower to the appropriatedepth in the well.

4. Begin pumping manually, discharging waterinto a 5 gallon bucket (or other graduatedvessel). Purge until specified volume ofwater has been evacuated (or until fieldparameters such as temperature, pH,

9

conductivity, etc. have stabilized). once at the surface, remove the bailer from

5. Collect and dispose of purge waters as and remove the vial. Begin slowly pouringspecified in the site specific project plan. from the bailer, and collect the duplicate

7.4 Sampling

Sample withdrawal methods require the use of pumps,compressed air, bailers, and samplers. Ideally,purging and sample withdrawal equipment should becompletely inert, economical to manufacture, easilycleaned, sterilized, reusable, able to operate at remotesites in the absence of power resources, and capable ofdelivering variable rates for sample collection.

There are several factors to take into considerationwhen choosing a sampling device. Care should betaken when reviewing the advantages or disadvantagesof any one device. It may be appropriate to use adifferent device to sample than that which was used topurge. The most common example of this is the useof a submersible pump to purge and a bailer tosample.

7.4.1 Bailers

The positive-displacement volatile sampling bailer isperhaps the most appropriate for collection of watersamples for volatile analysis. Other bailer types(messenger, bottom fill, etc.) are less desirable, butmay be mandated by cost and site conditions.

7.4.1.1 Operation

1. Surround the monitor well with clean plasticsheeting. If using the GPI bailer, insert a vialinto the claim and assemble the unit.

2. Attach a line to a clean decontaminatedbailer.

3. Lower the bailer slowly and gently into thewell, taking care not to shake the casingsides or to splash the bailer into the water.Stop lowering at a point adjacent to thescreen.

4. Allow bailer to fill and then slowly andgently retrieve the bailer from the wellavoiding contact with the casing, so as not toknock flakes of rust or other foreignmaterials into the bailer. If using the GPIbailer for collecting volatile organic samples,

the cable. Carefully open the GPI bailer unit

samples from the midstream sample.

5. Remove the cap from the sample containerand place it on the plastic sheet or in alocation where it won't becomecontaminated. See Section 7.7 for specialconsiderations on VOA samples.

6. Begin slowly pouring from the bailer.

7. Filter and preserve samples as required bysampling plan.

8. Cap the sample container tightly and placeprelabeled sample container in a carrier.

9. Replace the well cap.

10. Log all samples in the site logbook and onfield data sheets and label all samples.

11. Package samples and complete necessarypaperwork.

12. Transport sample to decontamination zonefor preparation for transport to analyticallaboratory.


Although it is recommended that samples not becollected with a submersible pump due to the reasonsstated in Section 4.4.2, there are some situationswhere they may be used.

7.4.2.1 Operation

1. Allow the monitor well to recharge afterpurging, keeping the pump just abovescreened section.

2. Attach gate valve to hose (if not alreadyfitted), and reduce flow of water to amanageable sampling rate.

3. Assemble the appropriate bottles.

4. If no gate valve is available, run the water

10

down the side of a clean jar and fill the prelabeled sample container in a carrier.sample bottles from the jar.

5. Cap the sample container tightly and placeprelabeled sample container in a carrier. 6. Log all samples in the site logbook and on


7. Log all samples in the site logbook and on paperwork.the field data sheets and label all samples.

8. Package samples and complete necessary for preparation for transport to analyticalpaperwork. laboratory.

9. Transport sample to decontamination zone 9. On completion, remove the tubing from thefor preparation for transport to the analytical well and either replace the Teflon tubing andlaboratory. bladder with new dedicated tubing and

10. Upon completion, remove pump and existing materials.assembly and fully decontaminate prior tosetting into the next sample well. Dedicate 10. Nonfiltered samples shall be collectedthe tubing to the hole. directly from the outlet tubing into the


The use of a non-contact gas positive displacementbladder pump is often mandated by the use ofdedicated pumps installed in wells. These pumps arealso suitable for shallow (less than 100 feet) wells.They are somewhat difficult to clean, but may be usedwith dedicated sample tubing to avoid cleaning.These pumps require a power supply and acompressed gas supply (or compressor). They may beoperated at variable flow and pressure rates makingthem ideal for both purging and sampling.

Barcelona (1984) and Nielsen (1985) report that the are not recommended for sampling purposes.non-contact gas positive displacement pumps causethe least amount of alteration in sample integrity ascompared to other sample retrieval methods.

7.4.3.1 Operation

1. Allow well to recharge after purging.


3. Turn pump on, increase the cycle time andreduce the pressure to the minimum that willallow the sample to come to the surface.

4. Cap the sample container tightly and place


field data sheets and label all samples.

7. Package samples and complete necessary

8. Transport sample to decontamination zone

bladder or rigorously decontaminate the

sample bottle.

11. For filtered samples, connect the pump outlettubing directly to the filter unit. The pumppressure should remain decreased so that thepressure build up on the filter does not blowout the pump bladder or displace the filter.For the Geotech barrel filter, no actualconnections are necessary so this is not aconcern.

7.4.4 Suction Pumps

In view of the limitations of these type pumps, they

7.4.5 Inertia Pumps

Inertia pumps may be used to collect samples. It ismore common, however, to purge with these pumpsand sample with a bailer (Section 7.4.1).

7.4.5.1 Operation

1. Following well evacuation, allow the well torecharge.


3. Since these pumps are manually operated,

11

the flow rate may be regulated by thesampler. The sample may be dischargedfrom the pump outlet directly into theappropriate sample container.





8. Transport sample to decontamination zonefor preparation for transport to the analyticallaboratory.

9. Upon completion, remove pump anddecontaminate or discard, as appropriate.

7.4.6. Sample Retrieval - Syringe

A limited number of commercial syringe typesamplers are available, (IEA, TIMCO, etc.) some arehomemade devices. These devices are claimed toprovide good quality samples for volatile analysis, butare severly limited in sample volume and are specificto sampling for volatiles. Essentially, they operatedwith an evacuated chamber that is lowered down thewell, and allowed to fill with the pressure of thewater. The entire mechanism is then brought to thesurface with the sample. The sample may then betransferred to a sample vial, or the entire unit may besent as the sample container.

1. Evacuate the syringe if necessary, and lowerthe sampling device to just below the wellscreen.

2. Remove the constriction from the device andallow the sample to fill the syringe, applyslight suction as necessary.

3. Bring unit to the surface. If necessary,transfer the sample to vials, as outlined insteps 2 through 7 above.

7.5 Filtering

For samples requiring filtering, such as total metalsanalysis, the filter must be decontaminated prior toand between uses. Filters work by two methods. Abarrel filter such as the "Geotech" filter works with abicycle pump, used to build up positive pressure in thechamber containing the sample which is then forcedthrough the filter paper (minimum size 0.45 µm) intoa jar placed underneath. The barrel itself is filledmanually from the bailer or directly via the hose of thesampling pump. The pressure must be maintained upto 30 lbs/in by periodic pumping.2

A vacuum type filter involves two chambers; theupper chamber contains the sample and a filter(minimum size 0.45 µm) divides the chambers. Usinga hand pump or a Gilian type pump, air is withdrawnfrom the lower chamber, creating a vacuum and thuscausing the sample to move through the filter into thelower chamber where it is drained into a sample jar.Repeated pumping may be required to drain all thesample into the lower chamber. If preservation of thesample is necessary, this should be done afterfiltering.

7.6 Post Operation

After all samples are collected and preserved, thesampling equipment should be decontaminated priorto sampling another well to preventcross-contamination of equipment and monitor wellsbetween locations.

1. Decontaminate all equipment.

2. Replace sampling equipment in storagecontainers.

3. Prepare and transport ground water samplesto the laboratory. Check sampledocumentation and make sure samples areproperly packed for shipment.

7.7 Special Considerations for VOASampling

The proper collection of a sample for volatile organicsrequires minimal disturbance of the sample to limitvolatilization and therefore a loss of volatiles from thesample.

Well volume '' nr 2h (cf) [Equation 1]

v(gal/ft) '' nr 2 (cf) [Equation 2]

vol/linear ft '' nr 2 (cf) [Equation 2]' 3.14 (1/12 ft)2 7.48 gal/ft 3

' 0.1632 gal/ft

12

Sample retrieval systems suitable for the valid where:collection of volatile organic samples are: positivedisplacement bladder pumps, gear driven submersiblepumps, syringe samplers and bailers (Barcelona, 1984;Nielsen, 1985). Field conditions and other constraintswill limit the choice of appropriate systems. Thefocus of concern must be to provide a valid sample foranalysis, one which has been subjected to the leastamount of turbulence possible.

The following procedures should be followed:

1. Open the vial, set cap in a clean place, andcollect the sample during the middle of thecycle. When collecting duplicates, collectboth samples at the same time.

2. Fill the vial to just overflowing. Do not rinsethe vial, nor excessively overflow it. Thereshould be a convex meniscus on the top ofthe vial.

3. Check that the cap has not beencontaminated (splashed) and carefully capthe vial. Place the cap directly over the topand screw down firmly. Do not overtightenand break the cap.

4. Invert the vial and tap gently. Observe vialfor at least ten (10) seconds. If an air bubbleappears, discard the sample and begin again.It is imperative that no entrapped air is in thesample vial.

5. Immediately place the vial in the protectivefoam sleeve and place into the cooler,oriented so that it is lying on its side, notstraight up.

6. The holding time for VOAs is seven days.Samples should be shipped or delivered tothe laboratory daily so as not to exceed theholding time. Ensure that the samplesremain at 4EC, but do not allow them tofreeze.

8.0 CALCULATIONS

If it is necessary to calculate the volume of the well,utilize the following equation:

n = pir = radius of monitoring well (feet)h = height of the water column (feet)

[This may be determined bysubtracting the depth to water fromthe total depth of the well asmeasured from the same referencepoint.]

cf = conversion factor (gal/ft ) = 7.483

gal/ft [In this equation, 7.48 gal/ft3 3

is the necessary conversion factor.]

Monitor well diameters are typically 2", 3", 4", or 6".Knowing the diameter of the monitor well, there area number of standard conversion factors which can beused to simplify the equation above.

The volume, in gallons per linear foot, for variousstandard monitor well diameters can be calculated asfollows:

where:

n = pir = radius of monitoring well (feet)cf = conversion factor (7.48 gal/ft )3

For a 2" diameter well, the volume per linear foot canbe calculated as follows:

Remember that if you have a 2" diameter well, youmust convert this to the radius in feet to be able to usethe equation.

The conversion factors for the common size monitorwells are as follows:

Well diameter 2" 3" 4" 6"Volume (gal/ft.) 0.1632 0.3672 0.6528 1.4688

If you utilize the conversion factors above, Equation

Well volume '' (h)(cf) [Equation 3]

13

1 should be modified as follows: must be implemented prior to sampling the first well.

where: such as minimizing contact with potentialcontaminants in both the vapor phase and liquid

h = height of water column (feet)cf = the conversion factor calculated

from Equation 2

The well volume is typically tripled to determine thevolume to be purged.


There are no specific quality assurance (QA) activitieswhich apply to the implementation of theseprocedures. However, the following general QAprocedures apply:

1. All data must be documented on field datasheets or within site logbooks.

2. All instrumentation must be operated inaccordance with operating instructions assupplied by the manufacturer, unlessotherwise specified in the work plan.Equipment checkout and calibrationactivities must occur prior tosampling/operation and they must bedocumented.

3. The collection of rinsate blanks isrecommended to evaluate potential for crosscontamination from the purging and/orsampling equipment.

4. Trip blanks are required if analyticalparameters include VOAs.




When working with potentially hazardous materials,follow U.S. EPA, OSHA or REAC health and safetyguidelines. More specifically, depending upon the sitespecific contaminants, various protective programs

The site health and safety plan should be reviewedwith specific emphasis placed on the protectionprogram planned for the well sampling tasks.Standard safe operating practices should be followed

matrix through the use of respirators and disposableclothing.

When working around volatile organic contaminants:

1. Avoid breathing constituents venting fromthe well.

2. Pre-survey the well head-space with anFID/PID prior to sampling.

3. If monitoring results indicate organicconstituents, sampling activities may beconducted in Level C protection. At aminimum, skin protection will be afforded bydisposable protective clothing.

Physical hazards associated with well sampling:

1. Lifting injuries associated with pump andbailers retrieval; moving equipment.

2. Use of pocket knives for cutting dischargehose.

3. Heat/cold stress as a result of exposure toextreme temperatures and protectiveclothing.

4. Slip, trip, fall conditions as a result of pumpdischarge.

5. Restricted mobility due to the wearing ofprotective clothing.

6. Electrical shock associated with use ofsubmersible pumps is possible. Use a GFCIor a copper grounding stake to avoid thisproblem.

12.0 REFERENCES

Barcelona, M.J., Helfrich, J.A., Garske, E.E., and J.P.Gibb, Spring 1984. "A Laboratory Evaluation ofGroundwater Sampling Mechanisms," Groundwater

14

Monitoring Review, 1984 pp. 32-41. Development. 1980, Ada, OK.

Barcelona, M.J., Helfrich, J.A., and Garske, E.E., Sisk, S.W. NEIC Manual for Ground/Surface"Sampling Tubing Effects on Groundwater Samples", Investigations at Hazardous Waste Sites,Analy. Chem., Vol. 57, 1985 pp. 460-463. EPA-330/9-81-002, 1981.

Driscoll, F.G., Groundwater and Wells (2nd ed.) U.S. Department of the Interior, National HandbookJohnson Division, UOP Inc., St. Paul, Minnesota, of Recommended Methods for Water-Data1986, 1089 pp. Acquisition, Reston, Virginia.

Gibb, J.P., R.M. Schuller, and R.A. Griffin,. U.S. Environmental Protection Agency, 1977.Monitoring Well Sampling and Preservation Procedures Manual for Groundwater Monitoring atTechniques, EPA-600/9-80-010, 1980. March, 1980. Solid Waste Disposal Facilities. EPA-530/SW-611.

Instrument Specialties Company, (January).Instruction Manual, Model 2100 Wastewater Sampler, U.S. Code of Federal Regulations, 49 CFR Parts 100Lincoln, Nebraska, 1980. to 177, Transportation revised November 1, 1985.

Keely, J.F. and Kwasi Boateng, Monitoring Well U.S. Environmental Protection Agency, 1982.Installation, Purging and Sampling Techniques - Part Handbook for Chemical and Sample Preservation ofI: Conceptualizations, Groundwater V25, No. 3, 1987 Water and Wastewater, EPA-600/4-82-029,pp. 300-313. Washington, D.C.

Keith, Lawrence H., Principles of Environmental U.S. Environmental Protection Agency, 1983.Sampling, American Chemical Society, 1988. Methods for Chemical Analysis of Water and Waste,

Korte, Nic, and Dennis Ealey,. Procedures for FieldChemical Analyses of Water Samples, U.S. U.S. Environmental Protection Agency, 1984. TestDepartment of Energy, GJ/TMC-07, Technical Methods for Evaluation of Solid Waste,Measurements Center, Grand Junction Project Office, EPA-SW-846, Second Edition, Washington, D.C.1983.

Korte, Nic, and Peter Kearl,. Procedures for the Manual of Groundwater Quality Sampling Procedures,Collection and Preservation of Groundwater and EPA-600/2-81-160, Washington, D.C.Surface Water Samples and for the Installation ofMonitoring Wells: Second Edition, U.S. Department U.S. Environmental Protection Agency, 1985.of Energy, GJ/TMC-08, Technical Measurements Practical Guide for Groundwater Sampling,Center, Grand Junction Projects Office, 1985. EPA-600/2-85/104, September, 1985.

National Council of the Paper Industry for Air and U.S. Environmental Protection Agency, 1986. RCRAStream Improvement, Inc.,. A Guide to Groundwater Groundwater Monitoring Technical EnforcementSampling, Technical Bulletin No. 362, Madison, New Guidance Document, OSWER-9950-1, September,York. January, 1982. 1986.

Nielsen, David M. and Yeates, Gillian L., Spring. "A Weston, 1987. Standard Operations Procedures forComparison of Sampling Mechanisms Available for Monitor Well Installation. MOUND IGMP/RIP.Small-Diameter Groundwater Monitoring Wells,"Groundwater Monitoring Review, 1985 pp. 83-99. U.S. Environmental Protection Agency, 1982.

Scalf, et al. (M.J. Scalf, McNabb, W. Dunlap, R. Water and Wastewater, EPA-600/4-82-029,Crosby, and J. Fryberger),. Manual for Groundwater Washington, D.C.Sampling Procedures. R.S. Kerr EnvironmentalResearch Laboratory, Office of Research and --- 1981. Manual of Groundwater Quality

August, 1977.

EPA-600/4-79-020, Washington, D.C.

U.S. Environmental Protection Agency, 1981.

Handbook for Sampling and Sample Preservation of

15

Sampling Procedures, EPA-600/2-81-160, WESTON, 1987. Standard Operating Procedures forWashington, D.C. Monitor Well Installation. MOUND IGMP/RIP

--- 1985. Practice Guide for Groundwater Barcelona, M.J. Helfrich, J.A., and Garske, E.E.,Sampling, EPA-600/2/85-104, September "Sampling Tubing Effects on Groundwater Samples".1985. 1985, Analy. Chem., Vol. 57, pp. 460-463.

Nielsen, David M. and Yeates, Gillian L., Spring1985. "A Comparison of Sampling MechanismsAvailable for Small-Diameter GroundwaterMonitoring Wells," Groundwater Monitoring Review,pp. 83-99.

1

SOP#: 2008DATE: 11/16/94

REV. #: 0.0

GENERAL AIRSAMPLING GUIDELINES


This Standard Operating Procedure (SOP) providesguidance in developing and implementing samplingplans to assess the impact of hazardous waste sites onambient air. It presents the United StatesEnvironmental Protection Agency/EnvironmentalResponse Team's (U.S. EPA/ERT's) approach to airsampling and monitoring and identifies equipmentrequirements. It is not within the scope of this SOP toprovide a generic air sampling plan. Experience,objectives, site characteristics, and chemicalcharacteristics will dictate sampling strategy. ThisSOP does not address indoor air sampling.

Two basic approaches can be used to assess ambientair (also referred to as air pathway assessments):modeling and measurements. The modeling approachinitially estimates or measures the overall siteemission rate(s) and pattern(s). These data are inputinto an appropriate air dispersion model, whichpredicts either the maximum or average airconcentrations at selected locations or distancesduring the time period of concern. This overallmodeling strategy is presented in the first threevolumes of the Air Superfund National TechnicalGuidance Series on Air Pathway Assessments .(1,2,3)

Specific applications of this strategy are presented inseveral additional Air Superfund Technical Guidancedocuments .(4)

The measurement approach involves actuallymeasuring the air impact at selected locations duringspecific time periods. These measurements can beused to document actual air impacts during specifictime intervals (i.e., during cleanup operations) or toextrapolate the probable "worst case" concentrationsat that and similar locations over a longer time periodthan was sampled.

This SOP addresses issues associated with this secondassessment strategy. This SOP also discusses theU.S. EPA/ERT's monitoring instruments, air sampling

kits, and approach to air sampling and monitoring athazardous waste sites.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, depending on site conditions, equipmentlimitations, or limitations imposed by the procedure.In all instances, the ultimate procedures employedshould be documented and associated with the finalreport.


2.0 METHOD SUMMARY

Air monitoring is defined as the use of direct-readinginstruments and other screening or monitoringequipment and techniques that provide instantaneous(real-time) data on the levels of airbornecontaminants. The U.S. EPA/ERT maintainsnumerous monitors for real-time measurements.Examples of air monitoring equipment are hand-heldphotoionization detectors (PID), flame ionizationdetectors (FID), oxygen/combustible gas detectors,and remote optical sensors.

Air sampling is defined as those sampling andanalytical techniques that require either off- or on-sitelaboratory analysis and therefore do not provideimmediate results. Typically, air sampling occursafter use of real-time air monitoring equipment hasnarrowed the number of possible contaminants andhas provided some qualitative measurement ofcontaminant concentration. Air sampling techniquesare used to more accurately detect, identify andquantify specific chemical compounds relative to themajority of air monitoring technologies.

In the Superfund Removal Program, On-SceneCoordinators (OSCs) may request the U.S. EPA/ERTto conduct air monitoring and sampling during the

2

following situations: emergency responses, site Disease Registry (ATSDR).assessments, and removal activities. Each of theseactivities has a related air monitoring/sampling The extent to which valid inferences can be drawnobjective that is used to determine the potential from air monitoring/sampling depends on the degreehazards to workers and/or the community. to which the monitoring/sampling effort conforms to

C Emergency Response objectives requires thorough planning of the

Emergency responses are immediate the most appropriate monitoring/sampling andresponses to a release or threatened release analytical procedures. These issues will be discussedof hazardous substances presenting an in this SOP.imminent danger to public health, welfare, orthe environment (i.e., chemical spills, fires,or chemical process failures resulting in acontrolled release of hazardous substances).Generally these situations require rapid on-site investigation and response. A major partof this investigation consists of assessing theair impact of these releases.

C Removal Site Assessment

Removal site assessments (referred to as siteassessments) are defined as any of severalactivities undertaken to determine the extentof contamination at a site and which help toformulate the appropriate response to arelease or threatened release of hazardoussubstances. These activities may include asite inspection, multimedia sampling, andother data collection.

C Removal Actions

Removal actions clean up or remove 4.0 INTERFERENCES ANDhazardous substances released into theenvironment. Removal actions include anyactivity conducted to abate, prevent,minimize, stabilize, or eliminate a threat topublic health or welfare, or to theenvironment.

Personal risk from airborne contaminants can bedetermined by comparing the results of on-sitemonitoring and sampling to health-based action levelssuch as the American Conference of GovernmentalIndustrial Hygienists (ACGIH) Threshold LimitValues (TLVs) and the Occupational Safety andHealth Administration (OSHA) Permissible ExposureLimits (PELs). Residential risk can be determined bycomparing the results of off-site monitoring orsampling to health-based action levels such as thosedeveloped by the Agency for Toxic Substance and

the objectives of the event. Meeting the project's

monitoring/sampling activities, and implementation of


Preservation, containers, handling and storage for airsamples are discussed in the specific SOPs for thetechnique selected. In addition, the analytical method(i.e., U.S. EPA, National Institute for OccupationalSafety and Health [NIOSH], and OSHA Methods)may be consulted for storage temperature, holdingtimes and packaging requirements. After samplecollection, the sampling media (i.e., cassettes ortubes) are immediately sealed. The samples are thenplaced into suitable containers (i.e., whirl bags,resealable bagsor culture tubes) which are then placedinto a shipping container.

Use bubble wrap or styrofoam peanuts when packingair samples for shipment. DO NOT USEVERMICULITE.

POTENTIAL PROBLEMS

Upwind sources can contribute to sampleconcentration. Natural sources, such as biologicalwaste, can produce hydrogen sulfide and methanewhich may contribute to the overall contaminant level.Extraneous anthropogenic contaminants (i.e., burningof fossil fuels; emissions from vehicular traffic,especially diesel; volatile compounds frompetrochemical facilities; and effluvium from smokestacks) may also contribute. Air sampling stationsshould be strategically placed to identify contributingsources.

Photoreactivity or reaction of the parameters ofconcern may occur with nonrelated compounds [i.e.,nitrogen compounds and polyaromatic hydrocarbons

3

(PAHs)]. Some sorbent media/samples should not beexposed to light during or after sampling due tophotochemical effects (i.e., PAHs).

Various environmental factors, including humidity,temperature and pressure, also impact the air samplingmethodology, collection efficiency and detectionlimit. Since the determination of air contaminants isspecifically dependent on the collection parametersand efficiencies, the collection procedure is an integralpart of the analytical method.

Detection limits depend on the contaminants beinginvestigated and the particular site situation. It isimportant to know why the data are needed and howthe data will be used. Care should be taken to ensurethe detection limits are adequate for the intended useof the final results.

Some equipment may be sensitive to humidity andtemperature extremes.


5.1 Direct Reading Instruments (AirMonitoring Instruments) C Clipboard

There are two general types of direct readinginstruments: portable screening devices andspecialized analytical instruments. Generally all thesetechniques involve acquiring, for a specific location orarea, continuous or sequential direct air concentrationsin either a real-time or semi-real-time mode. None ofthese instruments acquires true time-weighted averageconcentrations. In addition, these instruments are notcapable of acquiring simultaneous concentrationreadings at multiple locations, although several areable to sequentially analyze samples taken remotelyfrom different locations. The document, "Guide toPortable Instruments for Assessing AirbornePollutants Arising from Hazardous Waste Sites ,"(5)

provides additional information about air samplingand monitoring. The hazard levels for airbornecontaminants vary. See the ACGIH TLVs and theOSHA PELs for safe working levels. Commonscreening devices and analytical instruments aredescribed in Appendix A.

5.2 Air Sampling Equipment andMedia/Devices

The U.S. EPA/ERT uses the following analytical

methods for sampling: NIOSH Manual of AnalyticalMethods , American Society for Testing and(6)

Materials (ASTM) Methods , U.S. EPA Compendium(7)

of Methods for the Determination of Toxic OrganicCompounds in Ambient Air , and OSHA(8,9)

Methods . Additional air sampling references(10)

include Industrial Hygiene and Toxicology (3rdEd.) and Air Sampling Instruments for Evaluation(11)

of Atmospheric Contaminants . These methods(12)

typically specify equipment requirements forsampling. Since air sampling is such a diversetechnology, no single method or reference is best forall applications. Common sampling equipment andmedia/devices are described in Appendix B.

5.3 Tools/Material and EquipmentList

In addition to equipment and materials identified inAppendices A and B, the following equipment andmaterials may be required to conduct air sampling andmonitoring at hazardous waste sites:

C CameraC Site logbook

C Chain of custody recordsC Custody sealsC Air sampling worksheetsC Sample labelsC Small screwdriver setC Aluminum foilC Extension cordsC Glass crackerC Multiple plug outletC Whirl bags or culture tubesC Teflon tapeC Calibration devicesC Tygon and/or Teflon tubingR

C Surgical glovesC Lint-free glovesC IceC Sample container

Use the following additional equipment whendecontaminating glassware on site:

C Protective equipment (i.e., gloves, splashgoggles, etc.)

C Appropriate solvent(s)C Spray bottlesC Liquinox (soap)C Paper towels

4

C Distilled/deionized waterC Five-gallon bucketsC Scrub brushes and bottle brushes

6.0 REAGENTS

Impinger sampling involves using reagents contained lines and fences do not necessarily delineate the sitein a glass vial to absorb contaminants of concern (for boundary or area influenced by a release. Wheneverexample, NIOSH Method 3500 for formaldehyde uses possible, atmospheric hazards in the areas adjacent to1% sodium bisulfite solution). Impinger solutions the on-site zone should be monitored with direct-vary and are method-dependent. reading instruments. Monitoring at the fenceline or at

Reagents such as acetone and hexane are required to regarding pollutant migration. Three to four locationsdecontaminate glassware and some air sampling downwind of the source (i.e., plume) at breathing-equipment. Decontamination solutions are specified zone height, provide a basic fingerprint of the plume.in the Sampling Equipment Decontamination SOP. Negative instrument readings off site should not be7.0 PROCEDURES

7.1 Air Monitoring Design

7.1.1 Initial Surveys

In general, the initial survey is considered to be arelatively rapid screening process for collectingpreliminary data at hazardous waste sites. However,initial surveys may require many hours to completeand may consist of more than one entry.

Some information is generally known about the site;therefore, real-time instrumentation for specificcompounds (i.e., detector tubes and electrochemicalsensors) can be used to identify hot spots. Sufficientdata should be obtained with real-time instrumentsduring the initial entry to screen the site for variouscontaminants. When warranted, intrinsically safe orexplosion-proof instruments should be used. Anorganic vapor analyzer (OVA) is typically used duringthis survey. These gross measurements may be usedon a preliminary basis to (1) determine levels ofpersonal protection, (2) establish site work zones, and(3) map candidate areas for more thorough qualitativeand quantitative studies involving air sampling.

In some situations, the information obtained may besufficient to preclude additional monitoring.Materials detected during the initial survey may callfor a more comprehensive evaluation of hazards andanalyses for specific compounds. Since site activitiesand weather conditions change, a continuous programto monitor the ambient atmosphere must beestablished.

7.1.2 Off-Site Monitoring

Typically, perimeter monitoring with the sameinstruments employed for on-site monitoring isutilized to determine site boundaries. Because air isa dynamic matrix, physical boundaries like property

varying locations off site provides useful information

interpreted as the complete absence of airborne toxicsubstances; rather, they should be considered anotherpiece of information to assist in the preliminaryevaluation. The interpretation of negative readings isinstrument-dependent. The lack of instrumentreadings off site should not be interpreted as thecomplete absence of all airborne toxic substances;rather, it is possible that the particular compound orclass of compounds to which the monitoringinstrument responds is not present or that theconcentration of the compound(s) is below theinstrument's detection limit.

7.2 Air Sampling Design

7.2.1 Sampling Plan Design

The goal of air sampling is to accurately assess theimpact of a contaminant source(s) on ambient airquality. This impact is expressed in terms of overallaverage and/or maximum air concentrations for thetime period of concern and may be affected by thetransport and release of pollutants from both on- andoff-site sources. The location of these sources mustbe taken into account as they impact the selection ofsampling locations. Unlike soil and groundwaterconcentrations, air concentrations at points of interestcan easily vary by orders of magnitude over the periodof concern. This variability plays a major role indesigning an air sampling plan.

Downwind air concentration is determined by theamount of material being released from the site intothe air (the emission rate) and by the degree that thecontamination is diluted as it is transported. Local

5

meteorology and topography govern downwind associated with the site or with site activities? Indilution. Contaminant emission rates can also be addition, the assumptions associated with theheavily influenced by on-site meteorology and on-site sampling program must be defined. Theseactivities. All of these concerns must be incorporated assumptions include whether the sampling is to takeinto an air sampling plan. place under "typical," "worst case," or "one-time"

A sampling strategy can be simple or complex, sampling are different from those assumed during thedepending on the sampling program objectives. development of the sampling plan, then quality of thePrograms involving characterization of the pollutant data collected may be affected. The followingcontribution from a single point source tend to be definitions have been established:simple, whereas sampling programs investigating fateand transport characteristics of components from C Typical: routine daily sampling or routinediverse sources require a more complex sampling scheduled sampling at pre-establishedstrategy. In addition, resource constraints may affect locations.the complexity of the sampling design.

An optimal sampling strategy accounts for the worst meteorological and/or site conditionsfollowing site parameters: which would result in elevated ambient

C Location of stationary as well as mobilesources C One-time: only one chance is given to collect

C Analytes of concern a sample without regard to time orC Analytical detection limit to be achieved conditions.C Rate of release and transport of pollutants

from sources Qualitative data acquired under these conditions areC Availability of space and utilities for usually applicable only to the time period during

operating sampling equipment which the data were collected and may not provideC Meteorological monitoring data accurate information to be used in estimating theC Meteorological conditions in which sampling magnitude of an air impact during other periods or

is to be conducted over a long time interval.

The sampling strategy typically requires that the The sampling objectives also dictate the detectionconcentration of contaminants at the source or area of limits. Sampling methods for airborne contaminantsconcern as well as background contributions be will depend upon the nature and state (solid, liquid orquantified. It is important to establish background gas) of the contaminant. Gases and vapors may belevels of contaminants in order to develop a reference collected in aqueous media or adsorbents, inpoint from which to evaluate the source data. Field molecular sieves, or in suitable containers.blanks and lot blanks, as well as various other types of Particulates are collected by filters or impactors. TheQA/QC samples, can be utilized to determine other volume of sample to be collected is dependent uponsources. The impact of extraneous sources on an estimate of the contaminant concentration in thesampling results can frequently be accounted for by air, the sensitivity of the analytical method, and theplacing samplers upwind, downwind and crosswind standard or desired detection limit. A sufficientfrom the subject source. The analytical data from amount of sample must be collected to achieve thethese different sampling locations may be compared desired detection limit without interference from otherto determine statistical differences. contaminants. In addition, the selected method must

7.2.2 Sampling Objectives

The objectives of the sampling must be determinedprior to developing the sampling plan. Does thesampling plan verify adequate levels of protection foron-site personnel, or address potential off-site impacts

conditions. If the conditions present at the time of

C Worst case: sampling conducted under the

concentrations.

be able to detect the target compound(s).

7.2.3 Location and Number of IndividualSampling Points

Choose the number and location of sampling pointsaccording to the variability, or sensitivity, of the

6

sampling and analytical methods being utilized, the especially around major emission sources.variability of contaminant concentration over time atthe site, the level of precision required and A short-term monitoring program ranges from severalcostlimitations. In addition, determine the number of days to a few weeks and generally includes gatheringlocations and placement of samplers by considering data for site assessments, removal actions, and sourcethe nature of the response, local terrain, determination data (for further modeling). Activitiesmeteorological conditions, location of the site (with involved in a short-term sampling strategy must makerespect to other conflicting background sources), size the most of the limited possibilities for data collection.of the site, and the number, size, and relative Consider moving upwind/downwind locations dailyproximity of separate on-site emission sources and based on National Oceanic and Atmosphericupwind sources. The following are several Administration (NOAA) weather forecasts. Weatherconsiderations for sampler placement: monitoring becomes critical where complex terrain

C Location of potential on-site emission wind direction. Often, a number of alternatives cansources, as identified from the review of site fulfill the same objective.background information or from preliminaryon-site inspections. Prevailing winds running the length of a valley usually

C Location of potential off-site emission however, a complex valley may require more samplersources upwind of the sampling location(s). locations to account for the wide variety of winds.Review local wind patterns to determine the Ocean/lake effects may require a radical plan tolocation of off-site sources relative to wind collect enough samples to reach a low detection limit.direction. Two sets of samplers may be placed next to each

C Topographic features that affect the while the other set is turned off, and vice versa whendispersion and transport of airborne toxic there is no sea breeze. After the sampling event, theconstituents. respective upwind and downwind samples would be

Avoid natural obstructions when choosing air large body of water may be to use automatic, wind-sampling station locations, and account for vector-operated samplers, which turn the sampler onchannelization around those obstructions. only when the wind comes from a specified vector.

C Large water bodies, which affect valley and produce an upward fetch at the same time.atmospheric stability and the dispersion of Sampling locations may have to ring the site toair contaminants. measure the wind's impact.

C Roadways (dirt or paved), which may Off-site sources may affect on-site monitoring. In thisgenerate dust that could mask site case, on-site meteorological data, concurrent withcontaminants. sampling data, is essential to interpreting the acquired

C Vegetation, such as trees and shrubs, which needed to fully characterize ambient backgroundstabilizes soil and retards subsurface contaminant levels. Multiple off-site sources maycontaminants from becoming airborne. It require several monitoring locations, but if the sourcesalso affects air flow and scrubs some are at a sufficient distance, only one monitoringcontaminants from the air. Sometimes thick location is needed.vegetation can make an otherwise ideal airmonitoring location inaccessible. Topography and weather are not the only factors in

Consider the duration of sampling activities when from vandals and mishap. Secure all samplingchoosing the location and number of samples to be locations to maintain chain of custody, and to preventcollected. For example, if the sampling period is tampering with samples or loss of sampling units.limited to a few hours, one or two upwind and several High-volume sampling methods often require the usedownwind samples would typically be adequate, of 110 VAC electric power. When portable

and local meteorological effects frequently change

require a minimum number of sampler locations;

other: one set would be activated during the sea breeze

combined. Another alternative for sampling near a

At sites located on hillsides, wind will move down a

data. Also, additional upwind sampling sites may be

sampler location; the sampling sites must be secure

7

generators are used, the power quality may affect after the conclusion of daily cleanup activities. Forsampler operation. Also, be aware that the generators some sites, emissions are still a factor several hoursthemselves could be a potential pollution source if after daily site activities have been completed.their placement is not carefully considered. Because of the typically decreased downwind

Air quality dispersion models can be used to place concentrations than were present during daytime sitesamplers. The models incorporate source information, activities may be detected. For sites where this issurrounding topography, and meteorological data to possible, the sampling duration needs to be lengthenedpredict the general distance and directions of accordingly.maximum ambient concentrations. Modeling resultsshould be used to select sampling locations in areas of Sampling duration and flow rate dictate the volume ofmaximum pollutant concentrations. air collected, and to a major degree, the detection

7.2.4 Time, Duration and Frequency ofSampling Events

After choosing appropriate sampling or monitoringlocations, determine the sampling frequency and thenumber of samples to be collected. The time of day,duration and frequency of sampling events is governedby:

C The effects of site activities and meteorologyon emission rates

C The diurnal effect of the meteorology ondownwind dispersion

C The time period(s) of concern as defined bythe objective

C The variability in the impact from other non-site-related sources

C If defined, the degree of confidence neededfor either the mean or maximum downwindconcentrations observed

C The precision requirements for singlemeasurements

C Cost and other logistical considerations

The duration of the removal action and the number ofhours per day that site work is conducted determinethe time, duration, and frequency of samples. Short-term sampling programs may require daily sampling,while long-term programs may require 24-hoursampling every sixth or twelfth day. If the site will be A meteorological monitoring program is an integralundergoing removal activities 24 hours a day, part of site monitoring activities. Meteorological data,continuous air sampling may be warranted. However, which define local terrain impacts on air flow paths,if the site activities will be conducted for only eight are needed to interpret air concentration data.hours a day, and there are no emissions likely to occur Meteorological data may be available from an existingduring the remaining 16 hours, then sampling would station located near the site (i.e., at a local airport),be appropriate prior to the start of daily activities, otherwise a station should be set up at the site. Thiswould continue during operations, and end at the data will document the degree that samples actuallyconclusion of the daily activities. An off-peak sample were downwind and verify whether other worst-casecollection can ensure that emissions are not persisting assumptions were met. Meteorological parameters to

dispersion in the evening, higher downwind

limit. The analytical method selected will provide areference to flow rate and volume. Flow rates arelimited to the capacity of the pumps being employedand the contact time required by the collection media.

The duration or period of air sampling is commonlydivided into two categories (1) samples collected overa brief time period are referred to as "instantaneous"or "grab" samples and are usually collected in lessthan five minutes and (2) average or integratedsamples are collected over a significantly longerperiod of time. Integrated samples provide an averageconcentration over the entire sampling period.Integrated samples are not suited to determiningcyclical releases of contaminants because periodic orcyclical events are averaged out by the proportionallylong sampling duration.

Air quality dispersion models can predict themaximum air contaminant concentration expectedfrom a source. The meteorological and site conditionsexpected to cause the highest concentration are knownas worst-case conditions and can be identified byanalyzing the modeling results. Depending upon theobjective, one may sample when the model predictsworst-case conditions will exist.

7.2.5 M e t e o r o l o g i c a l a n dPhysical/Chemical Considerations

8

be monitored are, at a minimum, wind speed, wind the detection limit.direction, and sigma theta (which is the horizontalwind direction standard deviation and an indicator of C Atmospheric Pressureatmospheric stability). The remaining parametersprimarily affect the amount of a contaminant available Migration of landfill gases through thein the air. landfill surface and through surrounding soils

C Wind Speed pressure. Atmospheric pressure will

When the contaminant of concern is a contaminants from shallow aquifers into theparticulate, wind speed is critical in basements of overlying structures.determining whether the particulate willbecome airborne, the quantity of the In many cases, the transport and dispersionparticulate that becomes airborne, and the of air pollutants is complicated by localdistance the particulate will travel from the meteorology. Normal diurnal variations (i.e.,source. Wind speed also contributes to the temperature inversions) affect dispersion ofvolatilization of contaminants from liquid airborne contaminants. Terrain features cansources. enhance or create air inversions and can also

C Wind Direction complicating transport and dispersion

Wind direction highly influences the path ofairborne contaminants. In addition, The chemical characteristics of avariations in wind direction increase the contaminant (i.e., molecular weight, physicaldispersion of pollutants from a given source. state, vapor pressure, aerodynamic size,

C Atmospheric Stability photodegradation) affects its behavior and

Atmospheric stability refers to the degree to analyze it.which the atmosphere tends to dampenvertical and horizontal motion. Stableatmospheric conditions (i.e., evenings) resultin low dispersion, and unstable atmospheric

conditions (i.e., hot sunny days)result in higher dispersion.

C Temperature

Higher temperatures increase the rate ofvolatilization of organic and some inorganiccompounds and affect the initial rise ofgaseous or vapor contaminants. Therefore,worst-case emission of volatiles andsemivolatiles occurs at the hottest time ofday, or on the hottest day.

C Humidity

High humidity affects water-solublechemicals and particulates. Humidconditions may dictate the sampling mediaused to collect the air sample, or limit thevolume of air sampled and thereby increase

are governed by changes in atmospheric

influence upward migration of gaseous

influence the path and speed of air flow,

patterns.

temperature, reactive compounds, and

can influence the method used to sample and

8.0 CALCULATIONS

Volume is obtained by multiplying the sample time inminutes by the flow rate. Sample volume should beindicated on the chain of custody record. Adjustmentsfor temperature and pressure differences may berequired.

Results are usually provided in parts per million(ppm), parts per billion (ppb), milligrams per cubicmeter (mg/m ) or micrograms per cubic meter (µg/m ).3 3

Refer to the analytical method or regulatory guidelinesfor other applicable calculations.

9.0 QUALITYASSURANCE/QUALITY CONTROL

The manufacturer's instructions should be reviewedprior to instrument use. Instruments must be utilizedin accordance with manufacturer's instructions.Equipment checkout and calibration activities must

9

occur prior to and after monitoring and sampling and potentially explosive, flammable or acidicmust be documented. atmospheres. On rare occasions, the collection media

9.1 QA/QC Samples

QA/QC samples provide information on the variabilityand usability of environmental sample results.Various QA/QC samples may be collected to detecterror. QA/QC samples are submitted with the fieldsamples for analysis to aid in identifying the origin ofanalytical discrepancies; then a determination can bemade as to how the analytical results should be used.Collocated samples, background samples, fieldblanks, and lot blanks are the most commonlycollected QA/QC field samples. Performanceevaluation (PE) samples and matrix spikes provideadditional measures of data QA/QC control. QA/QCresults may suggest the need for modifying samplecollection, preparation, handling, or analyticalprocedures if the resultant data do not meet site-specific QA or data quality objectives.

9.2 Sample Documentation U.S. EPA. Air Superfund National

All sample and monitoring activities should bedocumented legibly, in ink. Any corrections orrevisions should be made by lining through theincorrect entry and by initialing the error. All samplesmust be recorded on an Air Sampling Worksheet. Achain of custody record must be maintained from thetime a sample is taken to the final deposition of thesample. Custody seals demonstrate that a samplecontainer has not been opened or tampered withduring transport or storage of samples.


Results for QA/QC samples should be evaluated forcontamination. This information should be utilized toqualify the environmental sample results accordinglywith data quality objectives. 11.0 HEALTH AND SAFETY

Personal protection equipment (PPE) requirementsidentified in federal and/or state regulations and 29Code of Federal Regulations (CFR) 1910.120 forhazardous waste site work must be followed.

The majority of physical precautions involved in airsampling are related to the contaminant sampled.Attention should be given when sampling in

may be hazardous; for example, in the instance wherean acidic or basic solution is utilized in an impinger.

When working with potentially hazardous materials,follow U.S. EPA, OSHA and corporate health andsafety procedures.

12.0 REFERENCES

U.S. EPA. Air Superfund National(1)

Technical Guidance Series. Volume I.Application of Air Pathway Analyses forSuperfund Activities. EPA/450/1-89/001.


Technical Guidance Series. Volume II.Estimation of Baseline Air Emissions atSuperfund Sites. EPA/450/1-89/002.

(3)

Technical Guidance Series. Volume III.Estimations of Air Emissions from CleanupActivities at Superfund Sites. EPA/450/1-89/003.


Technical Guidance Series. Volume IV.Procedures for Dispersion Air Modelingand Air Monitoring for Superfund AirPathway Analysis. EPA/450/1-89/004.

Guide to Portable Instruments for Assessing(5)

Airborne Pollutants Arising fromHazardous Wastes, InternationalOrganization of Legal Metrology (OIML)U.S. National Working Group (NWG) forOIML, American Conference ofGovernmental Industrial Hygienists,Cincinnati, OH

NIOSH. Manual of Analytical Methods,(6)

Second Edition. Volumes 1-7. U.S.Department of Health and Human ServicesPublication No. 84-100.

NIOSH. Manual of Analytical Methods,February 1984. U.S. Department of Healthand Human Services Publication No. 84-100.

10

Patty, F.A., Industrial Hygiene and(7)

Volume 11.03. Toxicology, Third Edition, John Wiley and

Riggin, R.M. Compendium of Methods for(8)

the Determination of Toxic OrganicCompounds in Ambient Air. EPA/600/4-84/041. Edition, 1989, American Conference of

Winberry, W.T. Supplement to U.S.(9)

EPA/600/4-84/041: Compendium ofMethods for the Determination of ToxicOrganic Compounds in Ambient Air.EPA/600/4-87/006.

OSHA. Analytical Methods Manual, Second(10)

Edition. Part 1, Organic Substances,January 1990. Part 2, Inorganic SubstancesAugust 1991.

ASTM. 1990. Annual Book of Standards, (11)

Sons, Inc., New York, NY.

Air Sampling Instruments for Evaluation of(12)

Atmospheric Contaminants, Seventh

Governmental Industrial Hygienists,Cincinnati, OH

BIBLIOGRAPHY

Removal Program Representative SamplingGuidance, Volume 2: Air, Environmental ResponseBranch, Emergency Response Division, Office ofEmergency and Remedial Response, Office of SolidWaste and Emergency Response, U.S. EnvironmentalProtection Agency, April 1992, Interim Final.

11

APPENDIX A

Portable Screening Devices and Specialized Analytical Instruments

PORTABLE SCREENING DEVICES

Where possible, a datalogger should be used tominimize the length of time required for site personnelto be in a potentially contaminated area. Dataloggercable is available from manufacturers for linear outputinstruments and some nonlinear output instruments.U.S. EPA ERT/REAC has output cables for organicvapor analyzers (i.e., HNU and OVA), toxic gasanalyzers (i.e., monitox) and real-time aerosolmonitors (i.e., RAM and miniram).

C Total Hydrocarbon Analyzers

Total hydrocarbon analyzers used to detect avariety of volatile organic compounds(VOCs) at hazardous waste sites principallyemploy either a photoionization detector(PID) or a flame ionization detector (FID).Compounds are ionized by a flame or anultraviolet lamp. PIDs depend on theionization potential of the compounds. PIDsare sensitive to aromatic and olefinic(unsaturated) compounds such as benzene,toluene, styrene, xylenes, and acetylene.Greater selectivity is possible by using low-voltage lamps. The ionization potential ofindividual compounds can be found in theNIOSH Pocket Guide to Chemical Hazards.These instruments are not compound-specificand are typically used as screeninginstruments. FIDs are sensitive to volatileorganic vapor compounds such as methane,propanol, benzene and toluene. Theyrespond poorly to organic compounds lackinghydrocarbon characteristics.

C Oxygen and Combustible Gas Indicators

Combustible Gas Indicators (CGIs) provideefficient and reliable methods to test forpotentially explosive atmospheres. CGImeters measure the concentration of aflammable vapor or gas in air and presentthese measurements as a percentage of the

lower explosive limit (LEL).

The measurements are temperature-dependent. Theproperty of the calibration gas determines sensitivity. LELs for individual compounds can be found in theNIOSH Pocket Guide to Chemical Hazards. Ifreadings approach or exceed 10% of the LEL, extremecaution should be exercised in continuing theinvestigation. If readings approach or exceed 25%LEL, personnel should be withdrawn immediately.

CGIs typically house an electrochemical sensor todetermine the oxygen concentration in ambient air.Normally, air contains approximately 20.9% oxygenby volume. Oxygen measurements are of particularimportance for work in enclosed spaces, low-lyingareas, or in the vicinity of accidents that haveproduced heavier-than-air vapors which could displaceambient air. The meters are calibrated for sea leveland may indicate a false negative (i.e, O content) at2

higher altitudes. Since the air has been displaced byother substances, these oxygen-deficient areas are alsoprime locations for taking additional organic vaporand combustible gas measurements. Oxygen-enrichedatmospheres increase the potential for fires by theirability to contribute to combustion or to chemicallyreact with flammable compounds and promote auto-ignition.

C Toxic Atmosphere Analyzers

The toxic atmosphere analyzer is acompound-specific instrument, designed andcalibrated to identify and quantify a specificcompound or class of compounds in eithergaseous or vapor form. Cross-sensitivity toair pollutants not of interest may be lead toerroneous results.

U.S. EPA/ERT has the following toxicatmosphere analyzers: carbon monoxide,phosgene, nitrous oxide, hydrogen cyanide,sulfur dioxide, hydrogen sulfide, and chlorinegas.

12

C Aerosol/Particulate Monitors C Gold Film (Hydrogen Sulfide and Mercury

A Real-Time Aerosol/Particulate Monitor(RAM) displays readings for total Hydrogen sulfide (H S) and Mercury (Hg)particulates. The instrument employs a pulse monitors operate on the principle that electriclight emitting diode which generates a resistivity increases across a gold film as anarrow band emission in conjunction with a function of H S and Hg concentration. Thephotovoltaic cell to detect light scattered monitors provide rapid and relatively lowfrom particulates. detection limits for H S and Hg in air. After

The U.S. EPA/ERT uses the RAM when the concentrations of H S and Hg, the gold filmcontaminant of concern is associated with must be heated to remove contamination andparticulates, and when responding to fires return the monitor to its original sensitivity.involving hazardous materials, to identifyplume levels. The instrument is very useful C Infrared Detectorsin determining the presence of a plume whenit is not visible. The U.S. EPA/ERT Infrared detectors such as the Miniaturetypically uses RAMs on tripods to obtain Infrared Analyzer (MIRAN) use infrared (IR)particulate concentrations at the breathing absorption as a function of specificzone level. Personal dataloggers are used compounds. MIRAN instruments apply towith the RAMs to document minimum, situations where the contaminants areaverage and maximum concentrations. This identified but concentrations are not.provides real-time data without requiring MIRAN instruments generally require ACthose in personal protective equipment to be power.constantly present in the plume.

C Chemical Detector Tubes (ColorimetricTubes)

A chemical detector tube is a hollow, tube-shaped, glass body containing one or morelayers of chemically impregnated inertmaterial. To use, the fused ends are brokenoff and a manufacturer-specified volume ofair is drawn through the tube with a pump toachieve a given detection limit. Thechemicals contained within the packingmaterial undergo a chemical reaction withthe airborne pollutant present, producing acolor change during the intake of each pumpstroke. The concentration of a pollutant isindicated by the length of discoloration on acalibrated scale printed on the detector tube.

C Radiation Meters

Radiation meters determine the presence andlevel of radiation. The meters use a gas orsolid ion detection media which becomesionized when radiation is present. Themeters are normally calibrated to one probe.Meters that detect alpha, beta, and gammaradiation are available.

Vapor) Monitors

2

2

2

extensive sampling periods or high2

SPECIALIZED ANALYTICALINSTRUMENTS

The continuous monitors described above providequalitative measurement of air contaminants.Quantitative measurements in the field can beobtained using more sophisticated instruments, suchas portable Gas Chromatographs, to analyze grabsamples.

C Direct Air Sampling Portable GasChromatographs (GCs)

Portable GCs use gas chromatography toidentify and quantify compounds. The timeit takes for a compound to move through achromatographic column is a function of thatspecific compound or group of compounds.A trained technician with knowledge of therange of expected concentrations ofcompounds can utilize a portable GC in thefield to analyze grab samples. GCs generallyrequire AC power and shelter to operate.This method is limited by its reliance on ashort-term grab sample to be representativeof the air quality at a site.

13

C Remote Optical Sensing C TAGA Direct Air Sampling Mass

This technique, also referred to as long-pathor open-path monitoring, involves The Trace Atmospheric Gas Analyzertransmitting either an infrared or ultraviolet (TAGA), which is operated by the U.S.light beam across a long open path and EPA/ERT, is capable of real-time detectionmeasuring the absorbance at specific of preselected organic compounds at lowwavelengths. The technique is capable of parts-per-billion concentrations. Theanalyzing any preselected organic or instrument has been successfully used by theinorganic volatile compound that can be U.S. EPA/ERT for isolating individualresolved from compounds naturally occurring emission plumes and tracking those plumesin ambient air. Current projected removal back to their sources.applications include perimeter monitoringduring site cleanups and measurement ofemission source strengths during siteassessments.

Spectrometer/Mass Spectrometer

14

APPENDIX B

Air Sampling Equipment and Media/Devices

AIR SAMPLING EQUIPMENT

C High-Volume, Total Suspended Particulate(TSP) Samplers

High-volume TSP samplers collect allsuspended particles by drawing air across an8- by 10-inch glass-quartz filter. The samplerate is adjusted to 40 cubic feet per minute(CFM), or 1134 liters per minute (L/min),and it is held constant by a flow controllerover the sample period. The mass of TSPscan be determined by weighing the filterbefore and after sampling. The compositionof the filter varies according to the analyticalmethod and the detection limit required.

C PM-10 Samplers

PM-10 samplers collect particulates with adiameter of 10 microns or less from ambientair. Particulates of this size represent therespirable fraction, and thus are of specialsignificance. PM-10 samplers can be high-volume or low-volume. The high-volumesampler operates in the same manner as theTSP sampler at a constant flow rate of 40CFM; it draws the sample through a specialimpactor head which collects particulates of10 microns or less. The particulate iscollected on an 8- by 10-inch filter. The low-volume sampler operates at a rate ofapproximately 17 L/min. The flow mustremain constant through the impactor head tomaintain the 10-micron cut-off point. Thelow-volume PM-10 collects the sample on37-mm Teflon filters.

C High-Volume PS-1 Samplers

High-volume PS-1 samplers draw a samplethrough polyurethane foam (PUF) or acombination foam and XAD-2 resin plug,and a glass quartz filter at a rate of 5-10CFM (144 to 282 L/min). This system is

excellent for measuring low concentrationsof semivolatiles, PCBs, pesticides, orchlorinated dioxins in ambient air.

C Area Sampling Pumps

These pumps provide flow-rate ranges of2-20 L/min and have a telescopic samplingmast with the sampling train. Because of thehigher volume, this pump is suitable forsampling low concentrations of airbornecontaminants (i.e., asbestos sampling).These pumps are also used for metals,pesticides and PAH sampling which requirelarge sample volumes.

C Personal Sampling Pumps

Personal sampling pumps are reliableportable sampling devices that draw airsamples through a number of sampling mediaincluding resin tubes, impingers, and filters.Flow rates are usually adjustable from 0.1 to4 L/min (or 0.01 to .75 L/min with arestrictive orifice) and can remain constantfor up to 8 hours on one battery charge orcontinuously with an AC charger/converter.

C Canister Samplers

Evacuated canister sampling systems use thepressure differential between the evacuatedcanister and ambient pressure to bleed airinto the canister. The sample is bled into thecanister at a constant rate over the samplingperiod using a critical orifice, a mechanicallycompensated regulator, or a mass flowcontroldevice until the canister is near atmosphericpressure.

Pressure canister sampling systems use apump to push air into the canister. Tomaintain a higher, more controlled flow, thepump typically controls the pressuredifferential across a critical orifice at the

15

inlet of the canister, resulting in a pressurized to collected compounds) are produced thancanister at the completion of sampling. with some other solid sorbents. PUF is used

AIR SAMPLING MEDIA/DEVICES

If possible, before employing a specific samplingmethod, consult the laboratory that will conduct theanalyses. Many of the methods can be modified toprovide better results or a wider range of results.

C Summa CanistersR

Summa canisters are highly polishedpassivated stainless steel cylinders. TheSumma polishing process brings chrome andnickel to the surface of the canisters, whichresults in an inert surface. This surfacerestricts adsorption or reactions that occur onthe canister's inner surface after collection.At the site, the canister is either placed in asampler to control sample collection rate, oropened to collect a grab sample. Samplescan be collected by allowing air to bleed intoor be pumped into the canister. U.S.EPA/ERT uses 6-liter Summa canisters forVOC and permanent gas analysis.

C Passive Dosimeters

Passive dosimeters are clip-on vapormonitors (samplers) in which the diffusedcontaminants are absorbed on speciallyprepared active surfaces. Industrialhygienists commonly use dosimeters toobtain time-weighted averages orconcentrations of chemical vapors, as theycan trap over 130 organic compounds.Selective dosimeters have also beendeveloped for a number of chemicalsincluding formaldehyde, ethylene oxide,hydrogen sulfide, mercury vapor, nitrogendioxide, sulfur dioxide, and ozone.Dosimeters must be sent to a laboratory foranalysis.

C Polyurethane Foam (PUF)

PUF is a sorbent used with a glass filter forthe collection of semivolatile organiccompounds such as pesticides, PCBs,chlorinated dioxins and furans, and PAHs.Fewer artifacts (chemical changes that occur

with the PS-1 sampler and U.S. EPA MethodTO13. PUF can also be used with personalsampling pumps when sampling for PAHsusing the Lewis/McCloud method.Breakthrough of the more volatile PCBs andPAHs may occur when using PUF.

C Sampling Bags (Tedlar )R

Sampling bags, like canisters, transport airsamples to the laboratory for analysis.Samples are generally pumped into the bags,but sometimes a lung system is used, inwhich a pump creates a vacuum around thebag in a vacuum box. Then the sample flowsfrom a source into the bag. This method isused for VOCs, fixed gases (CO , O and N )2 2, 2

and methane.

C Impingers

An impinger allows an air sample to bebubbled through a solution, which collects aspecific contaminant by either chemicalreaction or absorption. For long samplingperiods, the impinger may need to be kept inan ice bath to prevent the solution fromevaporating during sampling. The sample isdrawn through the impinger by using asampling pump or more elaborate samplingtrains with multiple impingers.

C Sorbent Tubes/Cartridges

A variety of sampling media are available insorbent tubes, which are used primarily forindustrial hygiene. A few examples arecarbon cartridges, carbon molecular sieves,Tenax tubes and tube containing the XAD-2polymer. Depending upon the sorbentmaterial, tubes can be analyzed using eithera solvent extraction or thermal desorption.The former technique uses standardlaboratory equipment and allows for multipleanalyses of the same sample. The lattertechnique requires special, but readilyavailable, laboratory equipment and allowsonly one analysis per sample. In addition,thermal desorption typically allows for lowerdetection limits by two or more orders ofmagnitude. Whenever sorbent tubes are

16

being used for thermal desorption, they carbonized molecular sieve. A potentialshould be certified as "clean" by the problem with mixed sorbent tubes is thelaboratory doing the analysis. breakthrough of a compound from an earlier

Thermally Desorbed Media cannot be desorbed.

During thermal desorption, high-temperature gas Solvent-Extracted Mediastreams are used to remove the compounds collectedon a sorbent medium. The gas stream is injected and Solvent-extracted media use the principle of chemicaloften cryofocused into an analytical instrument, such extraction to remove compounds collected on aas a GC, for compound analysis: sorbent media. The chemical solvent is injected into

C Tenax Tubes compounds. Examples of solvent-extracted media

Tenax tubes are made from commerciallyavailable polymer (p-phenylene oxide) C Chemically Treated Silica Gelpacked in glass or stainless steel tubesthrough which air samples are drawn or Silica gel is a sorbent which can be treatedsometimes pumped. These tubes are used in with various chemicals. The chemicallyU.S. EPA Method TO1 and VOST for treated silica gel can then be used to samplevolatile nonpolar organic, some polar for specific compounds in air. Examplesorganic, and some of the more volatile include the DNPH-coated silica gel cartridgesemivolatile organics. Tenax is not used with U.S. EPA Method TO11.appropriate for many of the highly volatileorganics (with vapor pressure greater than C XAD-2 Polymersapproximately 200 mm Hg).

C Carbonized Polymers custom-packed sandwich-style with

The carbonized molecular sieve (CMS), a U.S. EPA Method TO13 or the semi-VOSTcarbonized polymer, is a commercially method. The polymers are used for theavailable, carbon sorbent packed in stainless- collection of semivolatile polar and nonpolarsteel sampling tubes through which air organic compounds. The compoundssamples are drawn or sometimes pumped. collected on the XAD-2 polymer areThese are used in U.S. EPA Method TO2 for chemically extracted for analysis.highly volatile nonpolar compounds whichhave low-breakthrough volumes on other C Charcoal Cartridgessorbents. When high-thermal desorptiontemperatures are used with CMS, more Charcoal cartridges, consisting of primaryvariability in analysis may occur than with and backup sections, trap compounds byother sorbents. adsorption. Ambient air is drawn through

C Mixed Sorbent Tubes breakthrough of the analytes on the first

Sorbent tubes can contain two type of collection was therefore quantitative.sorbents. Combining the advantages of each Quantitative sample collection is evident bysorbent into one tube increases the possible the presence of target chemicals on the firsttypes of compounds to be sampled. The charcoal section and the absence on thecombination of two sorbents can also reduce second section. Next, the adsorbedthe chance that highly volatile compounds compounds must be eluted, usually with awill break through the sorbent media. An solvent extraction, and analyzed by GC withexample of a mixed sorbent tube is the a detector, such as a Mass Spectrometercombination of Tenax and charcoal with a (MS).

sorbent to a later sorbent from which it

an instrument, such as a GC, for analysis of

follow:

XAD-2 polymers usually are placed in tubes,

polyurethane foam, and prepared for use with

them so that the backup section verifies that

section did not occur, and the sample

17

C Tenax Tubes C Polyvinyl Chloride

Cartridges are used in OSHA and NIOSH Particulate filters with polyvinyl chloride aremethods in a manner similar to charcoal resistant to concentrated acids and alkalis.cartridges but typically for less volatile Their low moisture pickup and light tarecompounds. weight make them ideal for gravimetric

Particulate Filters

Particulate filters are used by having a sampling pumppass air through them. The filter collects the Teflon is manufactured fromparticulates present in the air and is then analyzed for polytetrafluorethylene (PTFE). Particulateparticulate mass or chemical or radiological filters with Teflon are easy to handle andcomposition. Particulate filters are made from exceptionally durable. Teflon filters are useddifferent materials which are described below. for metal collection.

C Mixed Cellulose Ester (MCE) C Silver

MCE is manufactured from mixed esters of Particulate filters manufactured from purecellulose which are a blend of nitro-cellulose silver have high collection efficiency andand cellulose acetate. MCE filters are used uniform pore size. These filters are used foroften for particulate sampling. mercury collection and analysis.

C Glass Fiber C Cellulose

Glass fiber is manufactured from glass fibers Particulate filters with cellulose contain lesswithout a binder. Particulate filters with than 0.01% ash. These filters are used toglass fiber provide high flow rates, wet collect particulates.strength, and high, solid holding capacity.Generally, the filters are used for gravimetricanalysis of particulates.

analysis.

C Teflon

1

SOP#: 2009DATE: 11/16/94

REV. #: 0.0 DRUM SAMPLING

1.0 SCOPE AND APPLICATION 3.0 SAMPLE PRESERVATION,

The purpose of this standard operating procedure(SOP) is to provide technical guidance onimplementing safe and cost-effective response actionsat hazardous waste sites containing drums withunknown contents. Container contents are sampledand characterized for disposal, bulking, recycling,segregation, and classification purposes.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent on site conditions, equipmentlimitations or limitations imposed by the procedure.In all instances, the ultimate procedures employedshould be documented and associated with the finalreport.


2.0 METHOD SUMMARY

Prior to sampling, drums must be excavated, (ifnecessary), inspected, staged, and opened. Drumexcavation must be performed by qualified personnel.Inspection involves the observation and recording ofvisual qualities of each drum and any characteristicspertinent to the classification of the drum's contents.Staging involves the physical grouping of drumsaccording to classifications established during thephysical inspection. Opening of closed drums can beperformed manually or remotely. Remote drumopening is recommended for worker safety. The mostwidely used method of sampling a drum involves theuse of a glass thief. This method is quick, simple,relatively inexpensive, and requires nodecontamination. The contents of a drum can befurther characterized by performing various field tests.

CONTAINERS, HANDLING,AND STORAGE

Samples collected from drums are considered wastesamples and as such, adding preservatives is notrequired due to the potential reaction of the samplewith the preservative. Samples should, however, becooled to 4 C and protected from sunlight in order too

minimize any potential reaction due to the lightsensitivity of the sample.

Sample bottles for collection of waste liquids, sludges,or solids are typically wide mouth amber jars withTeflon-lined screw caps. Actual volume required foranalysis should be determined in conjunction with thelaboratory performing the analysis.

Waste sample handling procedures should be asfollows:

1. Label the sample container with theappropriate sample label and complete theappropriate field data sheet(s). Place samplecontainer into two resealable plastic bags.

2. Place each bagged sample container into ashipping container which has been lined withplastic. Pack the container with enough non-combustible, absorbent, cushioning materialto minimize the possibility of containersbreaking, and to absorb any material whichmay leak.

Note: Depending on the nature and quantityof the material to be shipped, differentpackaging may be required. Thetransportation company or ashipping/receiving expert should beconsulted prior to packing the samples.

3. Complete a chain of custody record for eachshipping container, place into a resealable

2

plastic bag, and affix to the inside lid of the tube (3 meters long) is positioned at the vapor spaceshipping container. of the drum. A rigid, hooking device attached to the

4. Secure and custody seal the lid of the in place. The spear is inserted in the tube andshipping container. Label the shipping positioned against the drum wall. A sharp blow oncontainer appropriately and arrange for the the end of the spear drives the sharpened tip throughappropriate transportation mode consistent the drum and the gas vents along the grooves.with the type of hazardous waste involved. Venting should be done from behind a wall or


If buried drums are suspected, geophysicalinvestigation techniques such as magnetometry orground penetrating radar may be employed in anattempt to determine the location and depth of drums.During excavation, the soil must be removed withgreat caution to minimize the potential for drumrupture.

Until the contents are characterized, samplingpersonnel should assume that unlabelled drumscontain hazardous materials. Labelled drums arefrequently mislabelled, especially drums that arereused. Because a drum's label may not accuratelydescribe its contents, extreme caution must beexercised when working with or around drums.

If a drum which contains a liquid cannot be movedwithout rupture, its contents may be immediatelytransferred to a sound drum using an appropriatemethod of transfer based on the type of waste. In anycase, preparations should be made to contain the spill(i.e., spill pads, dike, etc.) should one occur.

If a drum is leaking, open, or deteriorated, then it mustbe placed immediately in overpack containers.

The practice of tapping drums to determine theircontents is neither safe nor effective and should not beused if the drums are visually overpressurized or ifshock-sensitive materials are suspected. A laserthermometer may be effective in order to determinethe level of the drum contents via surface temperaturedifferences.

Drums that have been overpressurized to the extentthat the head is swollen several inches above the levelof the chime should not be moved. A number ofdevices have been developed for venting criticallyswollen drums. One method that has proven to beeffective is a tube and spear device. A light aluminum

tube, goes over the chime and holds the tube securely

barricade. Once the pressure has been relieved, thebung can be removed and the drum sampled.

Because there is potential for accidents to occurduring handling, particularly initial handling, drumsshould only be handled if necessary. All personnelshould be warned of the hazards prior to handlingdrums. Overpack drums and an adequate volume ofabsorbent material should be kept near areas whereminor spills may occur. Where major spills mayoccur, a containment berm adequate to contain theentire volume of liquid in the drums should beconstructed before any handling takes place. If drumcontents spill, personnel trained in spill responseshould be used to isolate and contain the spill.


The following are standard materials and equipmentrequired for sampling:

C Personal protection equipmentC Wide-mouth amber glass jars with Teflon

cap liner, approximately 500 mL volumeC Other appropriate sample jarsC Uniquely numbered sample identification

labels with corresponding data sheetsC Drum/Tank Sampling Data Sheets and Field

Test Data Sheets for Drum/Tank SamplingC Chain of Custody recordsC Decontamination materialsC Glass thieving tubes or COLIWASAC Coring deviceC Stainless steel spatula or spoonsC Laser thermometerC Drum overpacksC Absorbent material for spillsC Drum opening devices

Bung Wrench

A common method for opening drumsmanually is using a universal bung wrench.These wrenches have fittings made to

3

remove nearly all commonly encountered Pneumatic Devicesbungs. They are usually constructed of anon-sparking metal alloy (i.e., brass, A pneumatic bung remover consists of abronze/manganese, aluminum, etc.) compressed air supply that is controlled by aformulated to reduce the likelihood of sparks. two-stage regulator. A high pressure air lineThe use of a "NON-SPARKING" wrench of desired length delivers compressed air todoes not completely eliminate the possibility a pneumatic drill, which is adapted to turnof a spark being produced. bung fitting selected to fit the bung to be

Drum Deheader has been designed to position and align the

One means by which a drum can be opened bracketing system must be attached to themanually when a bung is not removable with drum before the drill can be operated. Oncea bung wrench is by using a drum deheader. the bung has been loosened, the bracketingThis tool is constructed of forged steel with system must be removed before the drum canan alloy steel blade and is designed to cut the be sampled. This remote bung opener doeslid of a drum off or part way off by means of not permit the slow venting of the container,a scissors-like cutting action. A limitation of and therefore appropriate precautions mustthis device is that it can be attached only to be taken. It also requires the container to beclosed head drums. Drums with removable upright and relatively level. Bungs that areheads must be opened by other means. rusted shut cannot be removed with this

Hand Pick, Pickaxe, and Hand Spike

These tools are usually constructed of brassor a non-sparking alloy with a sharpenedpoint that can penetrate the drum lid or headwhen the tool is swung. The hand picks orpickaxes that are most commonly used arecommercially available; whereas, the spikesare generally uniquely fabricated four footlong poles with a pointed end.

Backhoe Spike

Another means used to open drums remotelyfor sampling is a metal spike attached orwelded to a backhoe bucket. This method isvery efficient and is often used in large-scaleoperations.

Hydraulic Drum Opener

Recently, remotely operated hydraulicdevices have been fabricated to open drums.This device uses hydraulic pressure to forcea non-sparking spike through the wall of adrum. It consists of a manually operatedpump which pressurizes fluid through alength of hydraulic line.

removed. An adjustable bracketing system

pneumatic drill over the bung. This

device.

6.0 REAGENTS

Reagents are not typically required for preservingdrum samples. However, reagents will be utilized fordecontamination of sampling equipment.

7.0 PROCEDURES

7.1 Preparation

1. Determine the extent of the sampling effort,the sampling methods to be employed, andthe types and amounts of equipment andsupplies needed.

2. Obtain necessary sampling and monitoringequipment.




4

6. Use stakes, flagging, or buoys to identify and 2. Symbols, words, or other markings on themark all sampling locations. If required the drum indicating hazards (i.e., explosive,proposed locations may be adjusted based on radioactive, toxic, flammable), or furthersite access, property boundaries, and surface identifying the drums.obstructions.

7.2 Drum Excavation

If it is presumed that buried drums are on-site andprior to beginning excavation activities, geophysicalinvestigation techniques should be utilized toapproximate the location and depth of the drums. Inaddition, it is important to ensure that all locationswhere excavation will occur are clear of utility lines,pipes and poles (subsurface as well as above surface).

Excavating, removing, and handling drums aregenerally accomplished with conventional heavyconstruction equipment. These activities should beperformed by an equipment operator who hasexperience in drum excavation. During excavationactivities, drums must be approached in a manner thatwill avoid digging directly into them.

The soil around the drum should be excavated withnon-sparking hand tools or other appropriate meansand as the drums are exposed, a visual inspectionshould be made to determine the condition of thedrums. Ambient air monitoring should be done todetermine the presence of unsafe levels of volatileorganics, explosives, or radioactive materials. Basedon this preliminary visual inspection, the appropriatemode of drum excavation and handling may bedetermined.

Drum identification and inventory should begin beforeexcavation. Information such as location, date ofremoval, drum identification number, overpack status,and any other identification marks should be recordedon the Drum/Tank Sampling Data Sheet (Attachment1, Appendix A).

7.3 Drum Inspection

Appropriate procedures for handling drums depend onthe contents. Thus, prior to any handling, drumsshould be visually inspected to gain as muchinformation as possible about their contents. Thedrums should be inspected for the following:

1. Drum condition, corrosion, rust, punctures,bungs, and leaking contents.

3. Signs that the drum is under pressure.

4. Shock sensitivity.

Monitoring should be conducted around the drumsusing instruments such as radiation meters, organicvapor analyzers (OVA) and combustible gasindicators (CGI).

Survey results can be used to classify the drums intocategories, for instance:

C RadioactiveC Leaking/deterioratingC BulgingC Lab packsC Explosive/shock sensitiveC Empty

All personnel should assume that unmarked drumscontain hazardous materials until their contents havebeen categorized. Once a drum has been visuallyinspected and any immediate hazard has beeneliminated by overpacking or transferring the drum'scontents, the drum is affixed with a numbered tag andtransferred to a staging area. Color-coded tags, labelsor bands should be used to identify the drum'scategory based on visual inspection. A description ofeach drum, its condition, any unusual markings, thelocation where it was buried or stored, and fieldmonitoring information are recorded on a Drum/TankSampling Data Sheet (Attachment 1, Appendix A).This data sheet becomes the principal record keepingtool for tracking the drum on-site.

7.4 Drum Staging

Prior to sampling, the drums should be staged to alloweasy access. Ideally, the staging area should belocated just far enough from the drum opening area toprevent a chain reaction if one drum should explode orcatch fire when opened.

During staging, the drums should be physicallyseparated into the following categories: thosecontaining liquids, those containing solids, thosecontaining lab packs, and those which are empty.

5

This is done because the strategy for sampling and drums are structurally sound (no evidence of bulginghandling drums/containers in each of these categories or deformation) and their contents are known to bewill be different. This may be achieved by visual non-shock sensitive, non-reactive, non-explosive orinspection of the drum and its labels, codes, etc. non-flammable. If opening the drum with bungSolids and sludges are typically disposed of in open wrenches is deemed safe, then certain procedurestop drums. Closed head drums with a bung opening should be implemented to minimize the hazard:generally contain liquid.

Where there is good reason to suspect that drums protective gear.contain radioactive, explosive, or shock-sensitive C Drums should be positioned upright with thematerials, these drums should be staged in a separate, bung up, or, for drums with bungs on theisolated area. Placement of explosives and shock- side, laid on their sides with the bung plugssensitive materials in diked and fenced areas will up.minimize the hazard and the adverse effects of any C The wrenching motion should be a slow,premature detonation of explosives. steady pull across the drum. If the length of

Where space allows, the drum opening area should be leverage for unscrewing the plug, a "cheaterphysically separated from the drum removal and drum bar" can be attached to the handle to improvestaging operations. Drums are moved from the leverage.staging area to the drum opening area one at a timeusing forklift trucks equipped with drum grabbers ora barrel grappler. In a large-scale drum handlingoperation, drums may be conveyed to the drumopening area using a roller conveyor. Drums may berestaged as necessary after opening and sampling.

7.5 Drum Opening

There are three basic techniques available for openingdrums at hazardous waste sites:

C Manual opening with non-sparking bungwrenches

C Drum deheadingC Remote drum puncturing or bung removal

The choice of drum opening techniques andaccessories depends on the number of drums to beopened, their waste contents, and physical condition.Remote drum opening equipment should always beconsidered in order to protect worker safety. UnderOSHA 1910.120, manual drum opening with bungwrenches or deheaders should be performed ONLYwith structurally sound drums and waste contents thatare known to be non-shock sensitive, non-reactive,non-explosive, and non-flammable.

7.5.1 Manual Drum Opening with a BungWrench 7.5.3 Manual Drum Opening with a Hand

Manual drum opening with bung wrenches (Figure 1,Appendix B) should not be performed unless the

C Field personnel should be fully outfitted with

the bung wrench handle provides inadequate

7.5.2 Manual Drum Opening with a DrumDeheader

Drums are opened with a drum deheader (Figure 2,Appendix B) by first positioning the cutting edge justinside the top chime and then tightening theadjustment screw so that the deheader is held againstthe side of the drum. Moving the handle of thedeheader up and down while sliding the deheaderalong the chime will enable the entire top to be rapidlycut off if so desired. If the top chime of a drum hasbeen damaged or badly dented it may not be possibleto cut the entire top off. Since there is always thepossibility that a drum may be under pressure, theinitial cut should be made very slowly to allow for thegradual release of any built-up pressure. A safertechnique would be to employ a remote method priorto using the deheader.

Self-propelled drum openers which are eitherelectrically or pneumatically driven are available andcan be used for quicker and more efficient deheading.

The drum deheader should be decontaminated, asnecessary, after each drum is opened to avoid crosscontamination and/or adverse chemical reactions fromincompatible materials.

Pick, Pickaxe, or Spike

When a drum must be opened and neither a bung

6

wrench nor a drum deheader is suitable, then it can beopened for sampling by using a hand pick, pickaxe, orspike (Figure 3, Appendix B). Often the drum lid orhead must be hit with a great deal of force in order topenetrate it. Because of this, the potential for splashor spraying is greater than with other opening methodsand therefore, this method of drum opening is notrecommended, particularly when opening drumscontaining liquids. Some spikes used have beenmodified by the addition of a circular splash plate nearthe penetrating end. This plate acts as a shield andreduces the amount of splash in the direction of theperson using the spike. Even with this shield, goodsplash gear is essential.

Since drums, some of which may be under pressure,cannot be opened slowly with these tools, spray fromdrums is common and appropriate safety measuresmust be taken. The pick or spike should bedecontaminated after each drum is opened to avoidcross contamination and/or adverse chemical reactionfrom incompatible materials.

7.5.4 Remote Drum Opening with aBackhoe Spike

Remotely operated drum opening tools are the safestavailable means of drum opening. Remote drumopening is slow, but provides a high degree of safetycompared to manual methods of opening.

In the opening area, drums should be placed in rowswith adequate aisle space to allow ease in backhoemaneuvering. Once staged, the drums can be quicklyopened by punching a hole in the drum head or lidwith the spike.

The spike (Figure 4, Appendix B) should bedecontaminated after each drum is opened to preventcross contamination and/or adverse reaction fromincompatible material. Even though some splash orspray may occur when this method is used, theoperator of the backhoe can be protected by mountinga large shatter-resistant shield in front of the operator'scage. This combined with the normal personalprotection gear should be sufficient to protect theoperator. Additional respiratory protection can beafforded by providing the operator with an on-boardairline system.

7.5.5 Remote Drum Opening withHydraulic Devices

A piercing device with a non-sparking, metal point isattached to the end of a hydraulic line and is pushedinto the drum by the hydraulic pressure (Figure 5,Appendix B). The piercing device can be attached sothat a hole for sampling can be made in either the sideor the head of the drum. Some of the metal piercersare hollow or tube-like so that they can be left in placeif desired and serve as a permanent tap or samplingport. The piercer is designed to establish a tight sealafter penetrating the container.

7.5.6 Remote Drum Opening withPneumatic Devices

Pneumatically-operated devices utilizing compressedair have been designed to remove drum bungsremotely (Figure 6, Appendix B). Prior to opening thedrum, a bung fitting must be selected to fit the bung tobe removed. The adjustable bracketing system is thenattached to the drum and the pneumatic drill is alignedover the bung. This must be done before the drill canbe operated. The operator then moves away from thedrum to operate the equipment. Once the bung hasbeen loosened, the bracketing system must beremoved before the drum can be sampled. Thisremote bung opener does not permit the slow ventingof the container, and therefore appropriate precautionsmust be taken. It also requires the container to beupright and relatively level. Bungs that are rustedshut cannot be removed with this device.

7.6 Drum Sampling

After the drum has been opened, preliminarymonitoring of headspace gases should be performedfirst with an explosimeter/oxygen meter. Afterwards,an OVA or other instruments should be used. Ifpossible, these instruments should be intrinsicallysafe. In most cases it is impossible to observe thecontents of these sealed or partially sealed drums.Since some layering or stratification is likely in anysolution left undisturbed, a sample that represents theentire depth of the drum must be taken.

When sampling a previously sealed drum, a checkshould be made for the presence of a bottom sludge.This is easily accomplished by measuring the depth toapparent bottom then comparing it to the knowninterior depth.

7

7.6.1 Glass Thief Sampler

The most widely used implement for sampling drumliquids is a glass tube commonly referred to as a glassthief (Figure 7, Appendix B). This tool is costeffective, quick, and disposable. Glass thieves aretypically 6mm to 16mm I.D. and 48 inches long.

Procedures for Use:

1. Remove the cover from the sample container.

2. Insert glass tubing almost to the bottom ofthe drum or until a solid layer is encountered.About one foot of tubing should extendabove the drum.

3. Allow the waste in the drum to reach its The Composite Liquid Waste Sampler (COLIWASA)natural level in the tube. and modifications thereof are equipment that collect

4. Cap the top of the sampling tube with a it in the transfer tube until delivery to the sampletapered stopper or thumb, ensuring liquid bottle. The COLIWASA (Figure 8, Appendix B) is adoes not come into contact with stopper. much cited sampler designed to permit representative

5. Carefully remove the capped tube from the containerized wastes. One configuration consists ofdrum and insert the uncapped end into the a 152 cm by 4 cm I.D. section of tubing with aappropriate sample container. neoprene stopper at one end attached by a rod running

6. Release stopper and allow the glass thief to other end. drain until the container is approximatelytwo-thirds full. Manipulation of the locking mechanism opens and

7. Remove tube from the sample container, neoprene stopper. One model of the COLIWASA isbreak it into pieces and place the pieces in shown in Appendix B; however, the design can bethe drum. modified and/or adapted somewhat to meet the needs

8. Cap the sample container tightly and label it.Place the sample container into a carrier. The major drawbacks associated with using a

9. Replace the bung or place plastic over the sampler is difficult to decontaminate in the field anddrum. its high cost in relation to alternative procedures (glass

10. Log all samples in the site logbook and on has applications, however, especially in instancesDrum/Tank Sampling Data Sheets. where a true representation of a multiphase waste is

11. Perform hazard categorization analyses ifincluded in the project scope. Procedures for Use

12. Transport the sample to the decontamination 1. Put the sampler in the open position byzone and package it for transport to the placing the stopper rod handle in the T-analytical laboratory, as necessary. position and pushing the rod down until theComplete chain of custody records. handle sits against the sampler's locking

In many instances a drum containing waste materialwill have a sludge layer on the bottom. Slow insertionof the sample tube into this layer; then a gradualwithdrawal will allow the sludge to act as a bottomplug to maintain the fluid in the tube. The plug can begently removed and placed into the sample containerby the use of a stainless steel lab spoon.

It should be noted that in some instances disposal ofthe tube by breaking it into the drum may interferewith eventual plans for the removal of its contents.The use of this technique should be cleared with theproject officer or other glass thief disposal techniquesshould be evaluated.

7.6.2 COLIWASA Sampler

a sample from the full depth of a drum and maintain

sampling of multiphase wastes from drums and other

the length of the tube to a locking mechanism at the

closes the sampler by raising and lowering the

of the sampler.

COLIWASA concern decontamination and costs. The

tubes) make it an impractical throwaway item. It still

absolutely necessary.

block.

8

2. Slowly lower the sampler into the liquid Procedures for use:waste. Lower the sampler at a rate thatpermits the levels of the liquid inside and 1. Assemble the sampling equipment.outside the sampler tube to be about thesame. If the level of the liquid in the sample 2. Remove the cover from the sample container.tube is lower than that outside the sampler,the sampling rate is too fast and will result in 3. Insert the sampling device to the bottom ofa non-representative sample. the drum. The extensions and the "T" handle

3. When the sampler stopper hits the bottom ofthe waste container, push the sampler tube 4. Rotate the sampling device to cut a core ofdownward against the stopper to close the material.sampler. Lock the sampler in the closedposition by turning the T-handle until it is 5. Slowly withdraw the sampling device so thatupright and one end rests tightly on the as much sample material as possible islocking block. retained within it.

4. Slowly withdraw the sample from the waste 6. Transfer the sample to the appropriatecontainer with one hand while wiping the sample container, and label it. A stainlesssampler tube with a disposable cloth or rag steel spoon or scoop may be used aswith the other hand. necessary.

5. Carefully discharge the sample into theappropriate sample container by slowly 7. Cap the sample container tightly and place itpulling the lower end of the T-handle away in a carrier.from the locking block while the lower endof the sampler is positioned in a sample 8. Replace the bung or place plastic over thecontainer. drum.

6. Cap the sample container tightly and label it. 9. Log all samples in the site log book and onPlace the sample container in a carrier. Drum/Tank Sampling Data Sheets.

7. Replace the bung or place plastic over the 10. Perform hazard categorization analyses ifdrum. included in the project scope.

8. Log all samples in the site logbook and on 11. Transport the sample to the decontaminationDrum/Tank Sampling Data Sheets. zone and package it for transport to the

9. Perform hazard categorization analyses if Complete chain of custody records.included in the project scope.

10. Transport the sample to the decontaminationzone and package for transport to theanalytical laboratory, as necessary.Complete the Chain of Custody records.

7.6.3 Coring Device

A coring device may be used to sample drum solids. regarding drum staging or restaging, bulking orSamples should be taken from different areas within compositing of the drum contents.the drum. This sampler consists of a series ofextensions, a T- handle, and the coring device.

should extend above the drum.

analytical laboratory, as necessary.

7.7 Hazard Categorization

The goal of characterizing or categorizing the contentsof drums is to obtain a quick, preliminary assessmentof the types and levels of pollutants contained in thedrums. These activities generally involve rapid, non-rigorous methods of analysis. The data obtained fromthese methods can be used to make decisions

9

As a first step in obtaining these data, standard tests 1. All data must be documented on Chain ofshould be used to classify the drum contents into Custody records, Drum/Tank Sampling Datageneral categories such as auto-reactives, water Sheets, Field Test Data Sheet for Drum/Tankreactives, inorganic acids, organic acids, heavy Sampling, or within site logbooks.metals, pesticides, cyanides, inorganic oxidizers, andorganic oxidizers. In some cases, further analyses 2. All instrumentation must be operated inshould be conducted to more precisely identify the accordance with operating instructions asdrum contents. supplied by the manufacturer, unless

There are several methods available to perform these Equipment checkout and calibrationtests: activities must occur prior to

C the HazCat chemical identification system documented.R

C the Chlor-N-Oil Test KitC Spill-fyter Chemical Classifier StripsC Setaflash (for ignitability)

These methods must be performed according to themanufacturers' instructions and the results must bedocumented on the Field Test Data Sheet forDrum/Tank Sampling (Attachment 2, Appendix A).

Other tests which may be performed include:

C Water ReactivityC Specific Gravity Test (compared to water)C Water Solubility TestC pH of Aqueous Solution

The tests must be performed in accordance with theinstructions on the Field Test Data Sheet forDrum/Tank Sampling and results of the tests must bedocumented on these data sheets.

The specific methods that will be used for hazardcategorization must be documented in the QualityAssurance Work Plan.

8.0 CALCULATIONS



The following general quality assurance proceduresapply:

otherwise specified in the work plan.

sampling/operation, and they must be




When working with potentially hazardous materials,follow U.S. EPA, OSHA, and corporate health andsafety procedures.

More specifically, the opening of closed containers isone of the most hazardous site activities. Maximumefforts should be made to ensure the safety of thesampling team. Proper protective equipment and ageneral awareness of the possible dangers willminimize the risk inherent to sampling operations.Employing proper drum opening techniques andequipment will also safeguard personnel. The use ofremote sampling equipment whenever feasible ishighly recommended.

12.0 REFERENCES

Guidance Document for Cleanup of Surface Tank andDrum Sites, OSWER Directive 9380.0-3.

Drum Handling Practices at Hazardous Waste Sites,EPA-600/2-86-013.

10

APPENDIX A

Attachments

ATTACHMENT 1. Drum/Tank Sampling Data Sheet

Samplers: Date:

Site Name: Work Order Number: 3347-040-001-

Container Number/Sample Number: REAC Task Leader:

SITE INFORMATION:

1. Terrain, drainage description:________________________________________________________________

2. Weather conditions (from observation):________________________________________________________

MET station on site: No Yes

CONTAINER INFORMATION:

1. Container type: Drum Tank Other:_________________________________________________

2. Container dimensions: Shape:________________________________________________________

Approximate size:_______________________________________________

3. Label present: NoYes:__________________________________________________________

Other Markings: ________________________________________________________________________________________________________________________________________________________________________________________________________________________

4. Spill or leak present: No Yes Dimensions:____________________________________________

5. Container location: (Circle one) N/A See Map Other: ____________________________________________________________________________________

________________________________________________________

11

APPENDIX A (Cont’d)

Attachments

ATTACHMENT 1. Drum/Tank Sampling Data Sheet (cont’d)

SAMPLE INFORMATION:

1. Description: _____ liquid _____ solid (_____ powder or _____ crystals) _____ sludge

2. Color: _________________________ Vapors:_____________________ Other:_____________________________________________________________________________________

3. Local effects present: (damage - environmental,material)_____________________________________________

FIELD MONITORING:

1. PID: ____________________ Background (clean zone)

____________________ Probe used/Model used

____________________ Reading from container opening

2. FID: ____________________ Background (clean zone)


3. Radiation Meter:

____________________ Model used

____________________ Background (clean zone)


4. Explosimeter/Oxygen Meter:

____________________ Oxygen level from container opening

____________________ LEL level from container opening

12


Attachments

ATTACHMENT 2. Field Test Data Sheet for Drum/Tank Sampling

Samplers: ______________________________ Date: ______________________

Site Name: _____________________________ Work Order Number: 3347-040-001-__________

Container Number/Sample Number: ______________ REAC Task Leader: ________________________

SAMPLE MONITORING INFORMATION:

1. PID: ____________________ Background (clean zone)

____________________ Probe used/Model used

____________________ Reading from sample

2. FID: ____________________ Background (clean zone)

____________________ Reading from sample

3. Radiation Meter: ________________ Model used

________________ Background (clean zone)

________________ Reading from sample

4. Explosimeter/Oxygen Meter: ____________ Oxygen level (sample)

____________ LEL level (sample)

SAMPLE DESCRIPTION:

________ Liquid ________ Solid ________ Sludge ________ Color ________ Vapors

WATER REACTIVITY:

1. Add small amount of sample to water: _____ bubbles _____ color change to _______________

_____ vapor formation _____ heat _____ No Change

SPECIFIC GRAVITY TEST (compared to water):

1. Add small amount of sample to water: _____ sinks _____ floats

2. If liquid sample sinks, screen for chlorinated compounds. If liquid sample floats and appears to be oily, screen for PCBs (Chlor-N-Oil kit).

13


Attachments

ATTACHMENT 2. Field Test Data Sheet for Drum/Tank Sampling (cont'd)

CHLOR N OIL TEST KIT INFORMATION:

1. Test kit used for this sample: Yes No

2. Results: _____ PCB not present _____ PCB present, less than 50 ppm

_____ PCB present, greater than 50 ppm _____ 100% PCB present

WATER SOLUBILITY TEST:

1. Add approximately one part sample to five parts water. You may need to stir and heat gently. [DO NOT HEAT IF WATER REACTIVE!] Results: ________ total ________ partial ________ no solubility

pH OF AQUEOUS SOLUTION:

1. Using 0-14 pH paper, check pH of water/sample solution: ___________________.

SPILL-FYTER CHEMICAL CLASSIFIER STRIPS:

1. Acid/Base Risk: (Circle one) Color Change

Strong acid (0) RED

Moderately acidic (1-3) ORANGE

Weak acid (5) YELLOW

Neutral (7) GREEN

Moderately basic (9-11) Dark GREEN

Strong Base (13-14) Dark BLUE

2. Oxidizer Risk: (Circle one)

Not Present WHITE

Present BLUE, RED, OR ANY DIVERGENCE FROMWHITE

3. Fluoride Risk: (Circle one)

Not Present PINK

Present YELLOW

14


Attachments


4. Petroleum Product, Organic Solvent Risk: (Circle one)

Not Present LIGHT BLUE

Present DARK BLUE

5. Iodine, Bromine, Chlorine Risk: (Circle one)

Not Present PEACH

Present WHITE OR YELLOW

SETAFLASH IGNITABILITY TEST:

140 F Ignitable: ________ Non-Ignitable ________ o

160 F Ignitable: ________ Non-Ignitable ________ o

______ Ignitable: ________ Non-Ignitable ________




Comments:________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________________

HAZCAT KIT TESTS:

1. Test: ____________________________________ Outcome:__________________________________

Comments:___________________________________________________________________________________

____________________________________________________________________________________________

2. Test: ____________________________________ Outcome:__________________________________

Comments:___________________________________________________________________________________

____________________________________________________________________________________________

15


Attachments


3. Test: ____________________________________ Outcome:__________________________________

Comments:___________________________________________________________________________________

____________________________________________________________________________________________

4. Test: ____________________________________ Outcome:__________________________________

Comments:___________________________________________________________________________________

____________________________________________________________________________________________

5. Test: ____________________________________ Outcome:__________________________________

Comments:___________________________________________________________________________________

____________________________________________________________________________________________

HAZCAT PESTICIDES KIT:

Present: ________________________________ Not Present: _______________________________________

Comments: __________________________________________________________________________________

____________________________________________________________________________________________

____________________________________________________________________________________________

16

APPENDIX B

Figures

Figure 1. Universal Bung Wrench

17

APPENDIX B (Cont’d)

Figures

Figure 2. Drum Deheader

18


Figures

Figure 3. Hand Pick, Pickaxe, and Hand Spike

19


Figures

Figure 4. Backhoe Spike

20


Figures

Figure 5. Hydraulic Drum Opener

21


Figures

Figure 6. Pneumatic Bung Remover

22


Figures

Figure 7. Glass Thief

23


Figures

Figure 8. COLIWASA

1

SOP#: 2010DATE: 11/16/94

REV. #: 0.0 TANK SAMPLING


The purpose of this standard operating procedure(SOP) is to provide technical guidance for theimplementation of sampling protocols for tanks andother confined spaces from outside the vessel.



2.0 METHOD SUMMARY

The safe collection of a representative sample shouldbe the criteria for selecting sample locations. Arepresentative sample can be collected usingtechniques or equipment that are designed forobtaining liquids or sludges from various depths. Thestructure and characteristics of storage tanks presentproblems with collection of samples from more thanone location; therefore, the selection of samplingdevices is an important consideration.

Depending on the type of vessel and characteristics ofthe material to be sampled, one can choose a baconbomb sampler, sludge judge, subsurface grab sampler,glass thief, bailer or Composite Liquid Waste Sampler(COLIWASA) to collect the sample. A sludge judge,bacon bomb or COLIWASA can be used to determineif the tank contents are stratified. Various othercustom-made samplers may be used depending on thespecific application.

All sample locations should be surveyed for airquality prior to sampling. At no time should sampling

continue with an LEL reading greater than 25%.


Samples collected from tanks are considered wastesamples and as such, addition of preservatives is notrequired due to the potential reaction of the samplewith the preservative. Samples should however, becooled to 4EC with ice and protected from sunlight inorder to minimize any potential reaction due to thelight sensitivity of the sample.

Sample bottles for collection of waste liquids, sludges,or solids are typically wide mouth amber jars withTeflon-lined screw caps. Actual volume required foranalysis should be determined in conjunction with thelaboratory performing the analysis.

Waste sample handling procedures should be asfollows:

1. Place sample container in two ziplock plasticbags.

2. Place each bagged container in a 1-galloncovered can containing absorbent packingmaterial. Place the lid on the can.

3. Mark the sample identification number onthe outside of the can.

4. Place the marked cans in a cooler, and fillremaining space with absorbent packingmaterial.

5. Fill out chain of custody record for eachcooler, place in plastic, and affix to inside lidof cooler.

6. Secure and custody seal the lid of cooler.

2

7. Arrange for the appropriate transportation C Chain of Custody recordsmode consistent with the type of hazardous C Flashlight (explosion proof)waste involved. C Coolers


Sampling a storage tank requires a great deal ofmanual dexterity, often requiring climbing to the topof the tank upon a narrow vertical or spiral stairway orladder while wearing protective clothing and carryingsampling equipment.

Before climbing onto the vessel, a structural surveyshould be performed. This will ensure appropriateconsideration of safety and accessibility prior toinitiation of any field activities.

As in all opening of containers, extreme cautionshould be taken to avoid ignition or combustion ofvolatile contents. All tools used must be constructedof a non-sparking material and electronic instrumentsmust be intrinsically safe.

All sample locations should be surveyed for airquality prior to sampling. At no time should samplingcontinue with a lower explosive limit (LEL) readinggreater than 25%.


Storage tank materials include liquids, sludges, still supplies needed.bottoms, and solids of various types. The type ofsampler chosen should be compatible with the waste. 2. Obtain necessary sampling and monitoringSamplers commonly used for tanks include: a bacon equipment.bomb sampler, sludge judge, glass thief, bailer,COLIWASA, and subsurface grab sampler. 3. Decontaminate or preclean equipment, and

Tank Sampling Equipment Checklist:

C Sampling plan clients, and regulatory agency, if appropriate.C Safety equipmentC Tape measure 5. Perform a general site survey prior to siteC Weighted tape line, measuring stick or entry in accordance with the site specific

equivalent Health and Safety Plan.C Camera/filmC Stainless steel bucket or bowl 6. Identify and mark all sampling locations.C Sample containersC Ziplock plastic bagsC LogbookC LabelsC Field data sheets

C IceC Decontamination suppliesC Bacon bomb samplerC Sludge judgeC Glass thievesC BailersC COLIWASAC Subsurface grab samplerC Water/oil level indicatorC OVA (organic vapor analyzer or equivalent)C Explosimeter/oxygen meterC High volume blower

6.0 REAGENTS

Reagents are not typically required for thepreservation of waste samples. However, reagentswill be utilized for decontamination of equipment.Decontamination solutions required are specified inthe Sampling Equipment Decontamination SOP.

7.0 PROCEDURE

7.1 Preparation

1. Determine the extent of the sampling effort,the sampling methods to be employed, andthe types and amounts of equipment and

ensure that it is in working order.

4. Prepare scheduling and coordinate with staff,

7.2 Preliminary Inspection

1. Inspect the external structural characteristicsof each tank and record in the site logbook.

3

Potential sampling points should be If sampling storage tanks, vacuum trucks, orevaluated for safety, accessibility and sample process vessels, collect at least one samplequality. from each compartment in the tank. Samples

2. Prior to opening a tank for internal opened hatch at the top of the tank. Valvesinspection, the tank sampling team shall: near the bottom should not be used, because

C Review safety procedures and If such a valve cannot be closed onceemergency contingency plans with opened, the entire tank contents may be lostthe Health and Safety Officer. to the ground surface. Also, individual strata

C Ensure that the tank is properly cannot be sampled separately through a valvegrounded. near the bottom.

C Remove all sources of ignition fromthe immediate area. 3. Compare the three samples for visual phase

3. Each tank should be mounted using systematic iterative sampling should beappropriate means. Remove manway covers performed. By halving the distance betweenusing non-sparking tools. two discrete sampling points, one can

4. Collect air quality measurements for eachpotential sample location using an 4. If another sampling port is available, sampleexplosimeter/oxygen meter for a lower as above to verify the phase information.explosive limit (LEL/O ) reading and an2

OVA/HNU for an organic vapor 5. Measure the inside diameter of the tank andconcentration. Both readings should be taken determine the volume of wastes using thefrom the tank headspace, above the sampling depth measurements (Appendix A).port, and in the breathing zone. Measuring the external diameter may be

5. Prior to commencing sampling, the tank have external supports that are covered.headspace should be cleared of any toxic orexplosive vapor concentration using a high 6. Sludges can be collected using a bacon bombvolume explosion proof blower. No work sampler, glass thief, or sludge judge.shall start if LEL readings exceed 25%. At10% LEL, work can continue but with 7. Record all information on the sample dataextreme caution. sheet or site logbook. Label the container

7.3 Sampling Procedure

1. Determine the depth of any and all liquid,solid, and liquid/solid interface, and depth ofsludge using a weighted tape measure, probeline, sludge judge, or equivalent.

2. Collect liquid samples from one (1) footbelow the surface, from mid-depth of liquid,and from one (1) foot above the bottomsludge layer. This can be accomplished witha subsurface grab sampler or bacon bomb.For liquids less than five (5) feet in depth,use a glass thief or COLIWASA to collectthe sample.

should always be collected through an

of their questionable or unknown integrity.

differences. If phase differences appear,

determine the depth of the phase change.

misleading as some tanks are insulated or

with the appropriate sample tag.

8. Decontaminate sampling equipment as perthe steps listed in the Sampling EquipmentDecontamination SOP.

7.4 Sampling Devices

7.4.1 Bacon Bomb Sampler

The bacon bomb sampler (Figure 1, Appendix B) isdesigned for the collection of material from variouslevels within a storage tank. It consists of acylindrical body, usually made of chrome-plated brassand bronze with an internal tapered plunger that actsas a valve to admit the sample. A line attached to thetop of the plunger opens and closes the valve. A line

4

is attached to the removable top cover which has a length of the sludge judge. The sampler consists oflocking mechanism to keep the plunger closed after 3/4" plastic pipe in 5-ft. sections, marked at 1-ft.sampling. increments, with screw-type fittings.

Procedures for Use: Procedures for Use:

1. Attach the sample line and the plunger line to 1. Lower the sludge judge to the bottom of thethe sampler. tank.

2. Measure and then mark the sampling line at 2. When the bottom has been reached, the pipethe desired depth. is allowed to fill to the surface level. This

3. Gradually lower the sampler by the sample column of material.line until the desire level is reached.

4. When the desired level is reached, pull up on tank liquid, the amount of sludge in thethe plunger line and allow the sampler to fill sample can be read using the one footbefore releasing the plunger line to seal off increments marked on the pipe sections.the sampler.

5. Retrieve the sampler by the sample line bottom section against a hard surface, thebeing careful not to pull up on the plunger material is released from the unit.line and thereby prevent accidental openingof the bottom valve. 5. Cap the sample container tightly and place

6. Rinse or wipe off the exterior of the samplerbody. 6. Replace the flange or manway or place

7. Position the sampler over the samplecontainer and release its contents by pulling 7. Log all samples in the site logbook and onup on the plunger line. field data sheets and label all samples.

8. Cap the sample container tightly and place 8. Package samples and complete necessaryprelabeled sample container in a carrier. paperwork.

9. Replace the flange or manway or place 9. Transport sample to decontamination zoneplastic over the tank. for preparation for transport to analytical



12. Transport sample to decontamination zonefor preparation for transport to analyticallaboratory.

7.4.2 Sludge Judge

A sludge judge (Figure 2, Appendix B) is used for 1. Screw the sample bottle onto the samplingobtaining an accurate reading of settleable solids in head.any liquid. The sampling depth is dependent upon the

will seat the check valve, trapping the

3. When the unit has been raised clear of the

4. By touching the pin extending from the

prelabeled sample container in a carrier.

plastic over the tank.

laboratory.

7.4.3 Subsurface Grab Sampler

Subsurface grab samplers (Figure 3, Appendix B) aredesigned to collect samples of liquids at variousdepths. The sampler is usually constructed ofaluminum or stainless steel tubing with apolypropylene or teflon head that attaches to a 1-litersample container.

Procedures for Use:

5

2. Lower the sampler to the desired depth. outside of the sample container.

3. Pull the ring at the top which opens the 6. Release stopper and allow the glass thief tospring-loaded plunger in the head assembly. drain until the container is approximately

4. When the bottle is full, release the ring, liftsampler, and remove sample bottle. 7. Remove tube from the sample container,

5. Cap the sample container tightly and place the tank.prelabeled sample container in a carrier.

6. Replace the flange or manway or place prelabeled sample container in a carrier.plastic over the tank.

7. Log all samples in the site logbook and on tank.field data sheets and label all samples.

8. Package samples and complete necessary field data sheets and label all samples.paperwork.

9. Transport sample to decontamination zone paperwork.for preparation for transport to analyticallaboratory. 12. Transport sample to decontamination zone

7.4.4 Glass Thief

The most widely used implement for sampling is aglass tube commonly referred to as a glass thief(Figure 4, Appendix B). This tool is simple, costeffective, quick, and collects a sample without havingto decontaminate. Glass thieves are typically 6mm to16mm I.D. and 48 inches long.

Procedures for Use:

1. Remove cover from sample container.

2. Insert glass tubing almost to the bottom of The positive-displacement volatile sampling bailerthe tank or until a solid layer is encountered. (Figure 5, Appendix B) (by GPI) is perhaps the mostAbout one foot of tubing should extend appropriate for collection of water samples for volatileabove the drum. analysis. Other bailer types (messenger, bottom fill,

3. Allow the waste in the tank to reach its and site conditions. Generally, bailers can provide annatural level in the tube. acceptable sample, providing that the sampling

4. Cap the top of the sampling tube with atapered stopper or thumb, ensuring liquid Operationdoes not come into contact with stopper.

5. Carefully remove the capped tube from the the tank.tank and insert the uncapped end in thesample container. Do not spill liquid on the 2. Attach a line to the bailer.

2/3 full.

break it into pieces and place the pieces in

8. Cap the sample container tightly and place

9. Replace the bung or place plastic over the

10. Log all samples in the site logbook and on

11. Package samples and complete necessary

for preparation for transport to analyticallaboratory.

In many instances a tank containing waste materialwill have a sludge layer on the bottom. Slow insertionof the sample tube down into this layer and then agradual withdrawal will allow the sludge to act as abottom plug to maintain the fluid in the tube. Theplug can be gently removed and placed into thesample container by the use of a stainless steel labspoon.

7.4.5 Bailer

etc.) are less desirable, but may be mandated by cost

personnel use extra care in the collection process.

1. Make sure clean plastic sheeting surrounds

6

3. Lower the bailer slowly and gently into the instances where a true representation of a multiphasetank so as not to splash the bailer into the waste is absolutely necessary.tank contents.

4. Allow the bailer to fill completely andretrieve the bailer from the tank. 1. Put the sampler in the open position by

5. Begin slowly pouring from the bailer. position and pushing the rod down until the

6. Cap the sample container tightly and place block.prelabeled sample container in a carrier.

7. Replace the flange or manway or place waste. Lower the sampler at a rate thatplastic over the tank. permits the levels of the liquid inside and

8. Log all samples in the site logbook and on same. If the level of the liquid in the samplefield data sheets and label all samples. tube is lower than that outside the sampler,

9. Package samples and complete necessary a non-representative sample.paperwork.

10. Transport sample to decontamination zone the waste container, push the sampler tubefor preparation for transport to analytical downward against the stopper to close thelaboratory. sampler. Lock the sampler in the closed

7.4.6 COLIWASA

Sampling devices are available that allow collectionof a sample from the full depth of a tank and maintainits integrity in the transfer tube until delivery to thesample bottle. The sampling device is known as aComposite Liquid Waste Sampler (COLIWASA)(Figure 6, Appendix B). The COLIWASA is a muchcited sampler designed to permit representativesampling of multiphase wastes from tanks and othercontainerized wastes.

One configuration consists of a 152 cm by 4 cm I.D.section of tubing with a neoprene stopper at one endattached by a rod running the length of the tube to alocking mechanism at the other end. Manipulation ofthe locking mechanism opens and closes the samplerby raising and lowering the neoprene stopper.

The major drawbacks associated with using aCOLIWASA concern decontamination and costs. Thesampler is difficult to decontaminate in the field, andits high cost in relation to alternative procedures (glasstubes) makes it an impractical throwaway item.Disposable COLIWASA's are a viable alternative.However, the COLIWASA is still the sampling deviceof choice for specific applications, especially in

Procedures for Use:

placing the stopper rod handle in the T-

handle sits against the sampler's locking

2. Slowly lower the sampler into the liquid

outside the sampler tube to be about the

the sampling rate is too fast and will result in

3. When the sampler stopper hits the bottom of

position by turning the T-handle until it isupright and one end rests tightly on thelocking block.

4. Slowly withdraw the sample from the wastecontainer with one hand while wiping thesampler tube with a disposable cloth or ragwith the other hand.

5. Carefully discharge the sample into asuitable sample container by slowly pullingthe lower end of the T-handle away from thelocking block while the lower end of thesampler is positioned in a sample container.


7. Replace the bung or place plastic over thetank.



7

10. Transport sample to decontamination zone illness, or death to the worker. Failure to recognizefor preparation for transport to analytical potential hazards of waste containers is the cause oflaboratory. most accidents. It should be assumed that the most

8.0 CALCULATIONS

There are no specific calculations for theseprocedures. Refer to Appendix A regardingcalculations utilized in determining tank volumes.


There are no specific quality assurance activitieswhich apply to the implementation of theseprocedures. However, the following general QAprocedures apply:






When working with potentially hazardous materials,follow U.S. EPA, OSHA, and corporate health andsafety procedures. More specifically, the hazardsassociated with tank sampling may cause bodilyinjury,

unfavorable conditions exist, and that the danger ofexplosion and poisoning will be present. Hazardsspecific to tank sampling are:

1. Hazardous atmospheres which are eitherflammable, toxic, asphyxiating, or corrosive.

2. If activation of electrical or mechanicalequipment would cause injury, each piece ofequipment should be manually isolated toprevent inadvertent activation while workersare occupied.

3. Communication is of utmost importancebetween the sampling worker and thestandby person to prevent distress or injurygoing unnoticed.

4. Proper procedures to evacuate a tank withforced air and grounding of equipment andtanks should be reviewed.

12.0 REFERENCES

Guidance Document for Cleanup of Surface Tank andDrum Sites, OSWER Directive 9380.0-3.

Drum Handling Practices at Hazardous Waste Sites,EPA-600/2-86-013.

8

APPENDIX A

Calculations

Various Volume Calculations

9


Calculations

Various Volume Calculations (Cont'd)

10

APPENDIX B

Figures

FIGURE 1. Bacon Bomb Sampler

11


Figures

FIGURE 2. Sludge Judge

12


Figures

FIGURE 3. Subsurface Grab Sampler

13


Figures

FIGURE 4. Glass Thief

14


Figures

FIGURE 5. Bailer

15


Figures

FIGURE 6. COLIWASA

SOP#: 2011DATE: 11/16/94

REV. #: 0.0CHIP, WIPE, AND

SWEEP SAMPLING


This standard operating procedure (SOP) outlines therecommended protocol and equipment for collectionof representative chip, wipe, and sweep samples tomonitor potential surficial contamination.

This method of sampling is appropriate for surfacescontaminated with non-volatile species of analytes(i.e., PCB, PCDD, PCDF, metals, cyanide, etc.)Detection limits are analyte specific. Sample sizeshould be determined based upon the detection limitdesired and the amount of sample requested by theanalytical laboratory. Typical sample area is onesquare foot. However, based upon sampling location,the sample size may need modification due to areaconfiguration.



2.0 METHOD SUMMARY

Since surface situations vary widely, no universalsampling method can be recommended. Rather, themethod and implements used must be tailored to suita specific sampling site. The sampling locationshould be selected based upon the potential forcontamination as a result of manufacturing processesor personnel practices.

Chip sampling is appropriate for porous surfaces andis generally accomplished with either a hammer andchisel, or an electric hammer. The sampling deviceshould be laboratory cleaned and wrapped in clean,autoclaved aluminum foil until ready for use. To

collect the sample, a measured and marked off area ischipped both horizontally and vertically to an evendepth of 1/8 inch. The sample is then transferred tothe proper sample container.

Wipe samples are collected from smooth surfaces toindicate surficial contamination; a sample location ismeasured and marked off. While wearing a new pairof surgical gloves, a sterile gauze pad is opened, andsoaked with solvent. The solvent used is dependenton the surface being sampled. This pad is thenstroked firmly over the sample surface, first vertically,then horizontally, to ensure complete coverage. Thepad is then transferred to the sample container.

Sweep sampling is an effective method for thecollection of dust or residue on porous or non-poroussurfaces. To collect such a sample, an appropriatearea is measured off. Then, while wearing a new pairof disposable surgical gloves, a dedicated brush isused to sweep material into a dedicated dust pan. Thesample is then transferred to the proper samplecontainer.

Samples collected by all three methods are then sentto the laboratory for analysis.


Samples should be stored out of direct sunlight toreduce photodegredation, cooled to 4 C and shipped too

the laboratory performing the analysis. Appropriatelysized laboratory cleaned, glass sample jars should beused for sample collection. The amount of samplerequired will be determined in concert with theanalytical laboratory.


This method has few significant interferences orproblems. Typical problems result from rough porous

surfaces which may be difficult to wipe, chip, or Health and Safety Plan.sweep.

5.0 EQUIPMENT

Equipment required for performing chip, wipe, orsweep sampling is as follows:

C Lab clean sample containers of proper sizeand composition

C Site logbookC Sample analysis request formsC Chain of Custody recordsC Custody seals C Field data sheetsC Sample labelsC Disposable surgical glovesC Sterile wrapped gauze pad (3 in. x 3 in.)C Appropriate pesticide (HPLC) grade solventC Medium sized laboratory cleaned paint brushC Medium sized laboratory cleaned chiselC Autoclaved aluminum foilC CameraC Hexane (pesticide/HPLC grade)C Iso-octaneC Distilled/deionized water

6.0 REAGENTS

Reagents are not required for preservation of chip,wipe or sweep samples. However, reagents will be 5. Chip the sample area horizontally, thenutilized for decontamination of sampling equipment. vertically to an even depth of approximately

7.0 PROCEDURES

7.1 Preparation





5. Perform a general site survey prior to siteentry in accordance with the site specific

6. Mark all sampling locations. If required theproposed locations may be adjusted based onsite access, property boundaries, and surfaceobstructions.

7.2 Chip Sample Collection

Sampling of porous surfaces is generallyaccomplished by using a chisel and hammer orelectric hammer. The sampling device should belaboratory cleaned or field decontaminated as per theSampling Equipment Decontamination SOP. It isthen wrapped in cleaned, autoclaved aluminum foil .The sampler should remain in this wrapping until it isneeded. Each sampling device should be used foronly one sample.

1. Choose appropriate sampling points; measureoff the designated area. Photodocumentation is optional.

2. Record surface area to be chipped.

3. Don a new pair of disposable surgical gloves.

4. Open a laboratory-cleaned chisel orequivalent sampling device.

1/8 inch.

6. Place the sample in an appropriately preparedsample container with a Teflon lined cap.

7. Cap the sample container, attach the labeland custody seal, and place in a plastic bag.Record all pertinent data in the site logbookand on field data sheets. Complete thesampling analysis request form and chain ofcustody record before taking the next sample.

8. Store samples out of direct sunlight and coolto 4EC.

9. Follow proper decontamination proceduresthen deliver sample(s) to the laboratory foranalysis.

7.3 Wipe Sample Collection

Wipe sampling is accomplished by using a sterile

gauze pad, adding a solvent in which the contaminant 3. Don new pair of disposable surgical gloves.is most soluble, then wiping a pre-determined, pre-measured area. The sample is packaged in an amber 4. Sweep the measured area using a dedicatedjar to prevent photodegradation and packed in coolers brush; collect the sample in a dedicated dustfor shipment to the lab. Each gauze pad is used for pan.only one wipe sample.

1. Choose appropriate sampling points; measure container.off the designated area. Photodocumentation is optional. 6. Cap the sample container, attach the label

2. Record surface area to be wiped. Record all pertinent data in the site log book

3. Don a new pair of disposable surgical gloves. sampling analysis request form and chain of

4. Open new sterile package of gauze pad.

5. Soak the pad with solvent of choice. to 4EC.

6. Wipe the marked surface area using firm 8. Leave contaminated sampling device in thestrokes. Wipe vertically, then horizontally to sample material, unless decontamination isinsure complete surface coverage. practical.

7. Place the gauze pad in an appropriately 9. Follow proper decontamination procedures,prepared sample container with a Teflon- then deliver sample(s) to the laboratory forlined cap. analysis.

8. Cap the sample container, attach the labeland custody seal, and place in a plastic bag.Record all pertinent data in the site logbookand on field data sheets. Complete thesampling analysis request form and chain ofcustody record before taking the next sample.

9. Store samples out of direct sunlight and coolto 4 C.o

10. Follow proper decontamination procedures,then deliver sample(s) to the laboratory foranalysis.

7.4 Sweep Sample Collection

Sweep sampling is appropriate for bulkcontamination. This procedure utilizes a dedicated,hand held sweeper brush to acquire a sample from apre-measured area.

1. Choose appropriate sampling points; measureoff the designated area. Photodocumentation is optional.

2. Record the surface area to be swept.

5. Transfer sample from dust pan to sample

and custody seal, and place in a plastic bag.

and on field data sheets. Complete the

custody record before taking the next sample.

7. Store samples out of direct sunlight and cool

8.0 CALCULATIONS

Results are usually provided in mg/g, µg/g, mass perunit area, or other appropriate measurement.Calculations are typically done by the laboratory.


The following general quality assurance proceduresapply:

1. All data must be documented on standardchain of custody forms, field data sheets orwithin the site logbook.

2. All instrumentation must be operated inaccordance with operating instructions assupplied by the manufacturer, unlessotherwise specified in the work plan.Equipment checkout and calibrationactivities must occur prior tosampling/operation, and they must bedocumented.

The following specific quality assurance activitiesapply to wipe samples:

For wipe samples, a blank should be collected foreach sampling event. This consists of a sterile gauzepad, wet with the appropriate solvent, and placed in aprepared sample container. The blank will helpidentify potential introduction of contaminants via thesampling methods, the pad, solvent or samplecontainer. Spiked wipe samples can also be collectedto better assess the data being generated. These areprepared by spiking a piece of foil of known area witha standard of the analyte of choice. The solventcontaining the standard is allowed to evaporate, andthe foil is wiped in a manner identical to the otherwipe samples.

Specific quality assurance activities for chip andsweep samples should be determined on a site specificbasis.


A review of the quality control samples will beconducted and the data utilized to qualify theenvironmental results.


When working with potentially hazardous materials ,follow EPA, OSHA and corporate health and safetyprocedures.

12.0 REFERENCES

U.S. EPA, A Compendium of Superfund FieldOperation Methods. EPA/540/5-87/001.

NJDEP Field Sampling Procedures Manual,February, 1988.

U. S. EPA ENVIRONMENTAL RESPONSE TEAM

STANDARD OPERATING PROCEDURESSOP: 2012

PAGE: 1 of 13REV: 0.0

DATE: 02/18/00SOIL SAMPLING

CONTENTS


2.0 METHOD SUMMARY

3.0 SAMPLE PRESERVATION, CONTAINERS, HANDLING, AND STORAGE

4.0 POTENTIAL PROBLEMS

5.0 EQUIPMENT

6.0 REAGENTS

7.0 PROCEDURES

7.1 Preparation7.2 Sample Collection

7.2.1 Surface Soil Samples7.2.2 Sampling at Depth with Augers and Thin Wall Tube Samplers7.2.3 Sampling at Depth with a Trier7.2.4 Sampling at Depth with a Split Spoon (Barrel) Sampler7.2.5 Test Pit/Trench Excavation

8.0 CALCULATIONS




12.0 REFERENCES

13.0 APPENDIX Figures

SUPERCEDES: SOP #2012; Revision 0.0; 11/16/94; U.S. EPA Contract 68-C4-0022.






The purpose of this standard operating procedure (SOP) is to describe the procedures for the collection ofrepresentative soil samples. Sampling depths are assumed to be those that can be reached without the useof a drill rig, direct-push, or other mechanized equipment (except for a back-hoe). Analysis of soil samplesmay determine whether concentrations of specific pollutants exceed established action levels, or if theconcentrations of pollutants present a risk to public health, welfare, or the environment.

These are standard (i.e., typically applicable) operating procedures which may be varied or changed asrequired, dependent upon site conditions, equipment limitations or limitations imposed by the procedure.In all instances, the actual procedures used should be documented and described in an appropriate sitereport.

Mention of trade names or commercial products does not constitute U.S. Environmental Protection Agency(EPA) endorsement or recommendation for use.

2.0 METHOD SUMMARY

Soil samples may be collected using a variety of methods and equipment depending on the depth of thedesired sample, the type of sample required (disturbed vs. undisturbed), and the soil type. Near-surfacesoils may be easily sampled using a spade, trowel, and scoop. Sampling at greater depths may beperformed using a hand auger, continuous flight auger, a trier, a split-spoon, or, if required, a backhoe.


Chemical preservation of solids is not generally recommended. Samples should, however, be cooled andprotected from sunlight to minimize any potential reaction. The amount of sample to be collected andproper sample container type are discussed in ERT/REAC SOP #2003 Rev. 0.0 08/11/94, Sample Storage,Preservation and Handling.

4.0 INTERFERENCES AND POTENTIAL PROBLEMS

There are two primary potential problems associated with soil sampling - cross contamination of samplesand improper sample collection. Cross contamination problems can be eliminated or minimized throughthe use of dedicated sampling equipment. If this is not possible or practical, then decontamination ofsampling equipment is necessary. Improper sample collection can involve using contaminated equipment,disturbance of the matrix resulting in compaction of the sample, or inadequate homogenization of thesamples where required, resulting in variable, non-representative results.

5.0 EQUIPMENT





Soil sampling equipment includes the following:

C Maps/plot planC Safety equipment, as specified in the site-specific Health and Safety PlanC Survey equipment or global positioning system (GPS) to locate sampling pointsC Tape measureC Survey stakes or flagsC Camera and filmC Stainless steel, plastic, or other appropriate homogenization bucket, bowl or panC Appropriate size sample containersC Ziplock plastic bagsC LogbookC LabelsC Chain of Custody records and custody sealsC Field data sheets and sample labelsC Cooler(s)C IceC VermiculiteC Decontamination supplies/equipmentC Canvas or plastic sheetC Spade or shovelC SpatulaC ScoopC Plastic or stainless steel spoonsC Trowel(s)C Continuous flight (screw) augerC Bucket augerC Post hole augerC Extension rodsC T-handleC Sampling trierC Thin wall tube samplerC Split spoonsC Vehimeyer soil sampler outfit

- Tubes- Points- Drive head- Drop hammer- Puller jack and grip

C Backhoe

6.0 REAGENTS





Reagents are not used for the preservation of soil samples. Decontamination solutions are specified inERT/REAC SOP #2006 Rev. 0.0 08/11/94, Sampling Equipment Decontamination, and the site specificwork plan.

7.0 PROCEDURES

7.1 Preparation

1. Determine the extent of the sampling effort, the sampling methods to be employed, and thetypes and amounts of equipment and supplies required.

2. Obtain necessary sampling and monitoring equipment.

3. Decontaminate or pre-clean equipment, and ensure that it is in working order.

4. Prepare schedules and coordinate with staff, client, and regulatory agencies, if appropriate.

5. Perform a general site survey prior to site entry in accordance with the site specific Healthand Safety Plan.

6. Use stakes, flagging, or buoys to identify and mark all sampling locations. Specific sitefactors, including extent and nature of contaminant, should be considered when selectingsample location. If required, the proposed locations may be adjusted based on site access,property boundaries, and surface obstructions. All staked locations should be utility-clearedby the property owner or the On-Scene-Coordinator (OSC) prior to soil sampling; andutility clearance should always be confirmed before beginning work.

7.2 Sample Collection

7.2.1 Surface Soil Samples

Collection of samples from near-surface soil can be accomplished with tools such asspades, shovels, trowels, and scoops. Surface material is removed to the requireddepth and a stainless steel or plastic scoop is then used to collect the sample.

This method can be used in most soil types but is limited to sampling at or near theground surface. Accurate, representative samples can be collected with this proceduredepending on the care and precision demonstrated by the sample team member. A flat,pointed mason trowel to cut a block of the desired soil is helpful when undisturbedprofiles are required. Tools plated with chrome or other materials should not be used.Plating is particularly common with garden implements such as potting trowels.

The following procedure is used to collect surface soil samples:





1. Carefully remove the top layer of soil or debris to the desired sample depthwith a pre-cleaned spade.

2. Using a pre-cleaned, stainless steel scoop, plastic spoon, or trowel, remove anddiscard a thin layer of soil from the area which came in contact with the spade.

3. If volatile organic analysis is to be performed, transfer the sample directly intoan appropriate, labeled sample container with a stainless steel lab spoon, orequivalent and secure the cap tightly. Place the remainder of the sample intoa stainless steel, plastic, or other appropriate homogenization container, andmix thoroughly to obtain a homogenous sample representative of the entiresampling interval. Then, either place the sample into appropriate, labeledcontainers and secure the caps tightly; or, if composite samples are to becollected, place a sample from another sampling interval or location into thehomogenization container and mix thoroughly. When compositing is complete,place the sample into appropriate, labeled containers and secure the capstightly.

7.2.2 Sampling at Depth with Augers and Thin Wall Tube Samplers

This system consists of an auger, or a thin-wall tube sampler, a series of extensions,and a "T" handle (Figure 1, Appendix A). The auger is used to bore a hole to adesired sampling depth, and is then withdrawn. The sample may be collected directlyfrom the auger. If a core sample is to be collected, the auger tip is then replaced witha thin wall tube sampler. The system is then lowered down the borehole, and driveninto the soil to the completion depth. The system is withdrawn and the core iscollected from the thin wall tube sampler.

Several types of augers are available; these include: bucket type, continuous flight(screw), and post-hole augers. Bucket type augers are better for direct samplerecovery because they provide a large volume of sample in a short time. Whencontinuous flight augers are used, the sample can be collected directly from theflights. The continuous flight augers are satisfactory when a composite of thecomplete soil column is desired. Post-hole augers have limited utility for samplecollection as they are designed to cut through fibrous, rooted, swampy soil and cannotbe used below a depth of approximately three feet.

The following procedure is used for collecting soil samples with the auger:

1. Attach the auger bit to a drill rod extension, and attach the "T" handle to thedrill rod.





2. Clear the area to be sampled of any surface debris (e.g., twigs, rocks, litter).It may be advisable to remove the first three to six inches of surface soil for anarea approximately six inches in radius around the drilling location.

3. Begin augering, periodically removing and depositing accumulated soils ontoa plastic sheet spread near the hole. This prevents accidental brushing of loosematerial back down the borehole when removing the auger or adding drill rods.It also facilitates refilling the hole, and avoids possible contamination of thesurrounding area.

4. After reaching the desired depth, slowly and carefully remove the auger fromthe hole. When sampling directly from the auger, collect the sample after theauger is removed from the hole and proceed to Step 10.

5. Remove auger tip from the extension rods and replace with a pre-cleaned thinwall tube sampler. Install the proper cutting tip.

6. Carefully lower the tube sampler down the borehole. Gradually force the tubesampler into the soil. Do not scrape the borehole sides. Avoid hammering therods as the vibrations may cause the boring walls to collapse.

7. Remove the tube sampler, and unscrew the drill rods.

8. Remove the cutting tip and the core from the device.

9. Discard the top of the core (approximately 1 inch), as this possibly representsmaterial collected before penetration of the layer of concern. Place theremaining core into the appropriate labeled sample container. Samplehomogenization is not required.

10. If volatile organic analysis is to be performed, transfer the sample into anappropriate, labeled sample container with a stainless steel lab spoon, orequivalent and secure the cap tightly. Place the remainder of the sample intoa stainless steel, plastic, or other appropriate homogenization container, andmix thoroughly to obtain a homogenous sample representative of the entiresampling interval. Then, either place the sample into appropriate, labeledcontainers and secure the caps tightly; or, if composite samples are to becollected, place a sample from another sampling interval into thehomogenization container and mix thoroughly.

When compositing is complete, place the sample into appropriate, labeledcontainers and secure the caps tightly.





11. If another sample is to be collected in the same hole, but at a greater depth,reattach the auger bit to the drill and assembly, and follow steps 3 through 11,making sure to decontaminate the auger and tube sampler between samples.

12. Abandon the hole according to applicable state regulations. Generally, shallowholes can simply be backfilled with the removed soil material.

7.2.3 Sampling with a Trier

The system consists of a trier, and a "T" handle. The auger is driven into the soil tobe sampled and used to extract a core sample from the appropriate depth.

The following procedure is used to collect soil samples with a sampling trier:

1. Insert the trier (Figure 2, Appendix A) into the material to be sampled at a 0o

to 45o angle from horizontal. This orientation minimizes the spillage ofsample.

2. Rotate the trier once or twice to cut a core of material.

3. Slowly withdraw the trier, making sure that the slot is facing upward.

4. If volatile organic analyses are required, transfer the sample into anappropriate, labeled sample container with a stainless steel lab spoon, orequivalent and secure the cap tightly. Place the remainder of the sample intoa stainless steel, plastic, or other appropriate homogenization container, andmix thoroughly to obtain a homogenous sample representative of the entiresampling interval. Then, either place the sample into appropriate, labeledcontainers and secure the caps tightly; or, if composite samples are to becollected, place a sample from another sampling interval into thehomogenization container and mix thoroughly. When compositing is complete,place the sample into appropriate, labeled containers and secure the capstightly.

7.2.4 Sampling at Depth with a Split Spoon (Barrel) Sampler

Split spoon sampling is generally used to collect undisturbed soil cores of 18 or 24inches in length. A series of consecutive cores may be extracted with a split spoonsampler to give a complete soil column profile, or an auger may be used to drill downto the desired depth for sampling. The split spoon is then driven to its sampling depththrough the bottom of the augured hole and the core extracted.

When split spoon sampling is performed to gain geologic information, all work should





be performed in accordance with ASTM D1586-98, “Standard Test Method forPenetration Test and Split-Barrel Sampling of Soils”.

The following procedures are used for collecting soil samples with a split spoon:

1. Assemble the sampler by aligning both sides of barrel and then screwing thedrive shoe on the bottom and the head piece on top.

2. Place the sampler in a perpendicular position on the sample material.

3. Using a well ring, drive the tube. Do not drive past the bottom of the headpiece or compression of the sample will result.

4. Record in the site logbook or on field data sheets the length of the tube used topenetrate the material being sampled, and the number of blows required toobtain this depth.

5. Withdraw the sampler, and open by unscrewing the bit and head and splittingthe barrel. The amount of recovery and soil type should be recorded on theboring log. If a split sample is desired, a cleaned, stainless steel knife shouldbe used to divide the tube contents in half, longitudinally. This sampler istypically available in 2 and 3 1/2 inch diameters. A larger barrel may benecessary to obtain the required sample volume.

6. Without disturbing the core, transfer it to appropriate labeled samplecontainer(s) and seal tightly.

7.2.5 Test Pit/Trench Excavation

A backhoe can be used to remove sections of soil, when detailed examination of soilcharacteristics are required. This is probably the most expensive sampling methodbecause of the relatively high cost of backhoe operation.

The following procedures are used for collecting soil samples from test pits ortrenches:

1. Prior to any excavation with a backhoe, it is important to ensure that allsampling locations are clear of overhead and buried utilities.

2. Review the site specific Health & Safety plan and ensure that all safetyprecautions including appropriate monitoring equipment are installed asrequired.





3. Using the backhoe, excavate a trench approximately three feet wide andapproximately one foot deep below the cleared sampling location. Placeexcavated soils on plastic sheets. Trenches greater than five feet deep must besloped or protected by a shoring system, as required by OSHA regulations.

4. A shovel is used to remove a one to two inch layer of soil from the vertical faceof the pit where sampling is to be done.

5. Samples are taken using a trowel, scoop, or coring device at the desiredintervals. Be sure to scrape the vertical face at the point of sampling to removeany soil that may have fallen from above, and to expose fresh soil for sampling.In many instances, samples can be collected directly from the backhoe bucket.

6. If volatile organic analyses are required, transfer the sample into anappropriate, labeled sample container with a stainless steel lab spoon, orequivalent and secure the cap tightly. Place the remainder of the sample intoa stainless steel, plastic, or other appropriate homogenization container, andmix thoroughly to obtain a homogenous sample representative of the entiresampling interval. Then, either place the sample into appropriate, labeledcontainers and secure the caps tightly; or, if composite samples are to becollected, place a sample from another sampling interval into thehomogenization container and mix thoroughly. When compositing is complete,place the sample into appropriate, labeled containers and secure the capstightly.

7. Abandon the pit or excavation according to applicable state regulations.Generally, shallow excavations can simply be backfilled with the removed soilmaterial.

8.0 CALCULATIONS



There are no specific quality assurance (QA) activities which apply to the implementation of theseprocedures. However, the following QA procedures apply:

1. All data must be documented on field data sheets or within site logbooks.

2. All instrumentation must be operated in accordance with operating instructions as supplied by themanufacturer, unless otherwise specified in the work plan. Equipment checkout and calibration





activities must occur prior to sampling/operation, and they must be documented.




When working with potentially hazardous materials, follow U.S. EPA, OHSA and corporate health andsafety procedures, in addition to the procedures specified in the site specific Health & Safety Plan..

12.0 REFERENCES

Mason, B.J. 1983. Preparation of Soil Sampling Protocol: Technique and Strategies. EPA-600/4-83-020.

Barth, D.S. and B.J. Mason. 1984. Soil Sampling Quality Assurance User's Guide. EPA-600/4-84-043.

U.S. Environmental Protection Agency. 1984 Characterization of Hazardous Waste Sites - A MethodsManual: Volume II. Available Sampling Methods, Second Edition. EPA-600/4-84-076.

de Vera, E.R., B.P. Simmons, R.D. Stephen, and D.L. Storm. 1980. Samplers and Sampling Proceduresfor Hazardous Waste Streams. EPA-600/2-80-018.

ASTM D 1586-98, ASTM Committee on Standards, Philadelphia, PA.





APPENDIX AFigures

SOP #2012February 2000





FIGURE 1. Sampling Augers





FIGURE 2. Sampling Trier

1

SOP#: 2013DATE: 11/17/94

REV. #: 0.0 SURFACE WATER SAMPLING


This standard operating procedure (SOP) is applicableto the collection of representative liquid samples, bothaqueous and non-aqueous from streams, rivers, lakes,ponds, lagoons, and surface impoundments. Itincludes samples collected from depth, as well assamples collected from the surface.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent upon site conditions,equipment limitations or limitations imposed by theprocedure or other procedure limitations. In allinstances, the ultimate procedures employed should bedocumented and associated with the final report.

Mention of trade names or commercial products doesnot constitute U.S. Environmental Protection Agency(EPA) endorsement or recommendation for use.

2.0 METHOD SUMMARY

Sampling situations vary widely, therefore, nouniversal sampling procedure can be recommended.However, sampling of both aqueous and non-aqueousliquids from the above mentioned sources is generallyaccomplished through the use of one of the followingsamplers or techniques:

C Kemmerer bottleC Bacon bomb samplerC Dip samplerC Direct method

These sampling techniques will allow for thecollection of representative samples from the majorityof surface waters and impoundments encountered.


Once samples have been collected, the followingprocedure should be followed:

1. Transfer the sample(s) into suitable, labeledsample containers.

2. Preserve the sample if appropriate, or usepre-preserved sample bottles. Do not overfillbottles if they are pre-preserved.

3. Cap the container, place in a ziploc plasticbag and cool to 4 C.o

4. Record all pertinent data in the site logbookand on field data sheets.

5. Complete the Chain of Custody record.

6. Attach custody seals to cooler prior toshipment.

7. Decontaminate all sampling equipment priorto the collection of additional samples withthat sampling device.


There are two primary interferences or potentialproblems with surface water sampling. These includecross contamination of samples and improper samplecollection.

2

1. Cross contamination problems can beeliminated or minimized through the use ofdedicated sampling equipment. If this is notpossible or practical, then decontamination ofsampling equipment is necessary. Refer tothe Sampling Equipment DecontaminationSOP.

2. Improper sample collection can involve usingcontaminated equipment, disturbance of thestream or impoundment substrate, andsampling in an obviously disturbed area.

Following proper decontamination procedures andminimizing disturbance of the sample site willeliminate these problems.


Equipment needed for collection of surface watersamples may include (depending on techniquechosen):

C Kemmerer bottlesC Bacon bomb samplerC Dip samplerC Line and messengersC Sample bottles/preservativesC Ziploc bagsC IceC CoolersC Chain of Custody records, custody sealsC Field data sheetsC Decontamination equipmentC Maps/plot planC Safety equipmentC CompassC Tape measureC Survey stakes, flags, or buoys and anchorsC Camera and filmC Logbook/waterproof penC Sample bottle labels

6.0 REAGENTS

Reagents will be utilized for preservation of samplesand for decontamination of sampling equipment. Thepreservatives required are specified by the analysis tobe performed.

7.0 PROCEDURES

7.1 Preparation


2. Obtain the necessary sampling andmonitoring equipment.

3. Decontaminate or pre-clean equipment, andensure that it is in working order.


5. Perform a general site survey prior to siteentry, in accordance with the site specificHealth and Safety Plan.

6. Use stakes, flagging, or buoys to identify andmark all sampling locations. If required theproposed locations may be adjusted based onsite access, property boundaries, and surfaceobstructions. If collecting sediment samples,this procedure may disturb the bottom.

7.2 Representative SamplingConsiderations

In order to collect a representative sample, thehydrology and morphometrics of a stream orimpoundment should be determined prior to sampling.This will aid in determining the presence of phases orlayers in lagoons, or impoundments, flow patterns instreams, and appropriate sample locations and depths.

Water quality data should be collected inimpoundments, and to determine if stratification ispresent. Measurements of dissolved oxygen, pH, andtemperature can indicate if strata exist which wouldeffect analytical results. Measurements should becollected at one-meter intervals from the substrate tothe surface using the appropriate instrument (i.e., aHydrolab or equivalent).

3

Water quality measurements such as dissolved 3. When the Kemmerer bottle is at the requiredoxygen, pH, temperature, conductivity, and oxidation- depth, send down the messenger, closing thereduction potential can assist in the interpretation of sampling device.analytical data and the selection of sampling sites anddepths when surface water samples are collected. 4. Retrieve the sampler and discharge from the

Generally, the deciding factors in the selection of a potential contamination of the valve.sampling device for sampling liquids in streams, Transfer the sample to the appropriaterivers, lakes, ponds, lagoons, and surface sample container.impoundments are:

1. Will the sample be collected from shore orfrom a boat?

2. What is the desired depth at which you wishto collect the sample?

3. What is the overall depth and flow directionof river or stream?

4. What type of sample will be collected (i.e.,water or lagoon liquids)?

7.2.1 Sampler Composition

The appropriate sampling device must be of a proper sampler.composition. Selection of samplers constructed ofglass, stainless steel, PVC or PFTE (Teflon) should be 3. Transfer the sample to the appropriatebased upon the analyses to be performed. sample container by pulling up on the trigger.


7.3.1 Kemmerer Bottle

A Kemmerer bottle (Figure 1, Appendix A) may beused in most situations where site access is from aboat or structure such as a bridge or pier, and wheresamples at depth are required. Sampling proceduresare as follows:

1. Use a properly decontaminated Kemmererbottle. Set the sampling device so that thesampling end pieces (upper and lowerstoppers) are pulled away from the samplingtube (body), allowing the substance to besampled to pass through this tube.

2. Lower the pre-set sampling device to thepredetermined depth. Avoid bottomdisturbance.

bottom drain the first 10-20 mL to clear any

7.3.2 Bacon Bomb Sampler

A bacon bomb sampler (Figure 2, Appendix A) maybe used in situations similar to those outlined for theKemmerer bottle. Sampling procedures are asfollows:

1. Lower the bacon bomb sampler carefully tothe desired depth, allowing the line for thetrigger to remain slack at all times. Whenthe desired depth is reached, pull the triggerline until taut. This will allow the sampler tofill.

2. Release the trigger line and retrieve the

7.3.3 Dip Sampler

A dip sampler (Figure 3, Appendix A) is useful insituations where a sample is to be recovered from anoutfall pipe or along a lagoon bank where directaccess is limited. The long handle on such a deviceallows access from a discrete location. Samplingprocedures are as follows:

1. Assemble the device in accordance with themanufacturer's instructions.

2. Extend the device to the sample location andcollect the sample by dipping the samplerinto the substance.

3. Retrieve the sampler and transfer the sampleto the appropriate sample container.

4

7.3.4 Direct Method

For streams, rivers, lakes, and other surface waters, This section is not applicable to this SOP.the direct method may be utilized to collect watersamples from the surface directly into the samplebottle. This method is not to be used for samplinglagoons or other impoundments where contact withcontaminants is a concern.

Using adequate protective clothing, access thesampling station by appropriate means. For shallowstream stations, collect the sample under the watersurface while pointing the sample container upstream;the container must be upstream of the collector.Avoid disturbing the substrate. For lakes and otherimpoundments, collect the sample under the watersurface avoiding surface debris and the boat wake.

When using the direct method, do not use pre-preserved sample bottles as the collection method maydilute the concentration of preservative necessary forproper sample preservation.

8.0 CALCULATIONS



There are no specific quality assurance (QA) activities U.S. Environmental Protection Agency. 1984.which apply to the implementation of these Characterization of Hazardous Waste Sites - Aprocedures. However, the following general QA Methods Manual: Volume II. Available Samplingprocedures apply: Methods, Second Edition. EPA/600/4-84-076.





When working with potentially hazardous materials,follow U.S. EPA, OSHA and corporate health andsafety procedures.

More specifically, when sampling lagoons or surfaceimpoundments containing known or suspectedhazardous substances, adequate precautions must betaken to ensure the safety of sampling personnel. Thesampling team member collecting the sample shouldnot get too close to the edge of the impoundment,where bank failure may cause him/her to lose his/herbalance. The person performing the sampling shouldbe on a lifeline and be wearing adequate protectiveequipment. When conducting sampling from a boat inan impoundment or flowing waters, appropriateboating safety procedures should be followed.

12.0 REFERENCES

U.S. Geological Survey. 1977. National Handbook orRecommended Methods for Water Data Acquisition.Office of Water Data Coordination Reston, Virginia.(Chapter Updates available).

5

APPENDIX A

Figures

FIGURE 1. Kemmerer Bottle

6


Figures

FIGURE 2. Bacon Bomb Sampler

7


Figures

FIGURE 3. Dip Sampler

1

SOP#: 2015DATE: 11/17/94

REV. #: 0.0 ASBESTOS SAMPLING


Asbestos has been used in many commercial productsincluding building materials such as flooring tiles andsheet goods, paints and coatings, insulation, androofing asphalts. These products and others may befound at hazardous waste sites hanging on overheadpipes, contained in drums, abandoned in piles, or aspart of a structure. Asbestos tailing piles from miningoperations can also be a source of ambient asbestosfibers. Asbestos is a known carcinogen and requiresair sampling to assess airborne exposure to humanhealth. This Standard Operating Procedure (SOP)provides procedures for asbestos air sampling bydrawing a known volume of air through a mixedcellulose ester (MCE) filter. The filter is then sent toa laboratory for analysis. The U.S. EnvironmentalProtection Agency/Environmental Response Team(U.S. EPA/ERT) uses one of four analytical methodsfor determining asbestos in air. These include: U.S.EPA's Environmental Asbestos Assessment Manual,Superfund Method for the Determination of Asbestosin Ambient Air for Transmission Electron Microscopy(TEM) ; U.S. EPA's Modified Yamate Method for(1)

TEM ; National Institute for Occupational Safety and(2)

Health (NIOSH) Method 7402 (direct method only)for TEM; and NIOSH Method 7400 for PhaseContrast Microscopy (PCM) . Each method has(3)

specific sampling and analytical requirements (i.e.,sample volume and flow rate) for determiningasbestos in air. The U.S. EPA/ERT typically follows proceduresoutlined in the TEM methods for determiningmineralogical types of asbestos in air and fordistinguishing asbestos from non-asbestos minerals.The Phase Contrast Microscopy (PCM) method isused by U.S. EPA/ERT as a screening tool since it isless costly than TEM. PCM cannot distinguishasbestos from non-asbestos fibers, therefore the TEMmethod may be necessary to confirm analyticalresults. For example, if an action level for thepresence of fibers has been set and PCM analysisindicates that the action level has been exceeded, then

TEM analysis can be used to quantify and identifyasbestos structures through examination of theirmorphology crystal structures (through electrondiffraction), and elemental composition (throughenergy dispersive X-ray analysis). In this instancesamples should be collected for both analyses in sideby side sampling trains (some laboratories are able toperform PCM and TEM analysis from the same filter).The Superfund method is designed specifically toprovide results suitable for supporting riskassessments at Superfund sites, it is applicable to awide range of ambient air situations at hazardouswaste sites. U.S. EPA's Modified Yamate Method forTEM is also used for ambient air sampling due to highvolume requirements. The PCM and TEM NIOSHanalytical methods require lower sample volumes andare typically used indoors; however, ERT willincrease the volume requirement for outdoorapplication.

Other Regulations pertaining to asbestos have beenpromulgated by U.S. EPA and OSHA. U.S. EPA'sNational Emission Standards for Hazardous AirPollutants (NESHAP) regulates asbestos-containingwaste materials. NESHAP establishes managementpractices and standards for the handling of asbestosand emissions from waste disposal operations (40CFR Part 61, Subparts A and M). U.S. EPA's 40 CFR763 (July 1, 1987) and its addendum 40 CFR 763(4)

(October 30, 1987) provide comprehensive rules for(4)

the asbestos abatement industry. State and localregulations on these issues vary and may be morestringent than federal requirements. The OSHAregulations in 29 CFR 1910.1001 and 29 CFR1926.58 specify work practices and safety equipmentsuch as respiratory protection and protective clothingwhen handling asbestos. The OSHA standard for an8-hour, time-weighted average (TWA) is 0.2fibers/cubic centimeters of air. This standard pertainsto fibers with a length-to-width ratio of 3 to 1 with afiber length >5 µm . An action level of 0.1 fiber/cc(5,6)

(one-half the OSHA standard) is the level U.S. EPAhas established in which employers must initiate suchactivities as air monitoring, employee training, and

2

medical surveillance . objectives should be carefully identified so as to select(5,6)

These are standard (i.e., typically applicable) some preparation (i.e., lot blanks results) prior to siteoperating procedures which may be varied or changed sampling may be required, these requirements areas required, dependent upon site conditions, specified in the analytical methods. equipment limitations or limitations imposed by theprocedure. In all instances, the ultimate proceduresemployed should be documented and associated withthe final report.


2.0 METHOD SUMMARY

Prior to sampling, the site should be characterized by Storage Proceduresidentifying on-site as well as off-site sources ofairborne asbestos. The array of sampling locationsand the schedule for sample collection, is critical tothe success of an investigation. Generally, samplingstrategies to characterize a single point source arefairly straightforward, while multiple point sourcesand area sources increase the complexity of thesampling strategy. It is not within the scope of thisSOP to provide a generic asbestos air sampling plan.Experience, objectives, and site characteristics willdictate the sampling strategy.

During a site investigation, sampling stations shouldbe arranged to distinguish spatial trends in airborneasbestos concentrations. Sampling schedules shouldbe fashioned to establish temporal trends. Thesampling strategy typically requires that theconcentration of asbestos at the source (worst case) orarea of concern (downwind), crosswind, as well asbackground (upwind) contributions be quantified. SeeTable 1 (Appendix A) for U.S. EPA/ERTrecommended sampling set up for ambient air. Indoorasbestos sampling requires a different type of strategywhich is identified in Table 2 (Appendix A). It isimportant to establish background levels ofcontaminants in order to develop a reference pointfrom which to evaluate the source data. Field blanksand lot blanks can be utilized to determine othersources.

Much information can be derived from each analyticalmethod previously mentioned. Each analyticalmethod has specific sampling requirements andproduce results which may or may not be applicableto a specific sampling effort. The site sampling

the most appropriate analytical method. Additionally,


3.1 Sample Preservation

No preservation is required for asbestos samples.

3.2 Sample Handling, Container and

1. Place a sample label on the cassetteindicating a unique sampling number. Donot put sampling cassettes in shirt or coatpockets as the filter can pick up fibers. Theoriginal cassette box is used to hold thesamples.

2. Wrap the cassette individually in a plasticsample bag. Each bag should be markedindicating sample identification number, totalvolume, and date.

3. The wrapped sampling cassettes should beplaced upright in a rigid container so that thecassette cap is on top and cassette base is onbottom. Use enough packing material toprevent jostling or damage. Do not usevermiculite as packing material for samples.If possible, hand carry to lab.

4. Provide appropriate documentation withsamples (i.e., chain of custody and requestedanalytical methodology).


Flow rates exceeding 16 liters/minute (L/min) whichcould result in filter destruction due to (a) failure of itsphysical support under force from the increasedpressure drop; (b) leakage of air around the filtermount so that the filter is bypassed, or (c) damage tothe asbestos structures due to increased impactvelocities.

3

4.1 U.S. EPA's Superfund Method

4.1.1 Direct-transfer TEM SpecimenPreparation Methods

Direct-Transfer TEM specimen preparation methodshave the following significant interferences:

C The achievable detection limit is restrictedby the particulate density on the filter, whichin turn is controlled by the sampled airvolume and the total suspended particulateconcentration in the atmosphere beingsampled.

C The precision of the result is dependent onthe uniformity of the deposit of asbestosstructures on the sample collection filter.

C Air samples must be collected so that theyhave particulate and fiber loadings withinnarrow ranges. If too high a particulateloading occurs on the filter, it is not possibleto prepare satisfactory TEM specimens by adirect-transfer method. If too high a fiberloading occurs on the filter, even ifsatisfactory TEM specimens can be prepared,accurate fiber counting will not be possible.

4.1.2 Indirect TEM Specimen PreparationMethods

Indirect TEM specimen preparation methods have thefollowing interferences:

C The size distribution of asbestos structures ismodified.

C There is increased opportunity for fiber lossor introduction of extraneous contamination.

C When sample collection filters are ashed, anyfiber contamination in the filter medium isconcentrated on the TEM specimen grid.

It can be argued that direct methods yield an under-estimate of the asbestos structure concentrationbecause many of the asbestos fibers present areconcealed by other particulate material with whichthey are associated. Conversely, indirect methods canbe considered to yield an over-estimate because sometypes of complex asbestos structures disintegrate

during the preparation, resulting in an increase in thenumbers of structures counted.

4.2 U.S. EPA's Modified YamateMethod for TEM

High concentrations of background dust interfere withfiber identification.

4.3 NIOSH Method for TEM

Other amphibole particles that have aspect ratiosgreater than 3:1 and elemental compositions similar tothe asbestos minerals may interfere in the TEManalysis. Some non-amphibole minerals may giveelectron diffraction patterns similar to amphiboles.High concentrations of background dust interfere withfiber identification.

4.4 NIOSH Method for PCM

PCM cannot distinguish asbestos from non-asbestosfibers; therefore, all particles meeting the countingcriteria are counted as total asbestos fibers. Fiber lessthan 0.25 um in length will not be detected by thismethod. High levels of non-fibrous dust particles mayobscure fibers in the field of view and increase thedetection limit.

5.0 EQUIPMENT/MATERIALS

5.1 Sampling Pump

The constant flow or critical orifice controlledsampling pump should be capable of a flow-rate andpumping time sufficient to achieve the desired volumeof air sampled.

The lower flow personal sampling pumps generallyprovide a flow rate of 20 cubic centimeters/minute(cc/min) to 4 L/min. These pumps are usually batterypowered. High flow pumps are utilized when flowrates between 2 L/min to 20 L/min are required. Highflow pumps are used for short sampling periods so asto obtain the desired sample volume. High flowpumps usually run on AC power and can be pluggedinto a nearby outlet. If an outlet is not available thena generator should be obtained. The generator shouldbe positioned downwind from the sampling pump.Additional voltage may be required if more than onepump is plugged into the same generator. Several

4

electrical extension cords may be required if sampling C Tools - small screw driverslocations are remote. C Container - to keep samples upright

The recommended volume for the Superfund method required)(Phase I) requires approximately 20 hours to collect. C Extension cords (may not be required) Such pumps typically draw 6 amps at full power so C Multiple plug outletthat 2 lead/acid batteries should provide sufficient C Sample labelspower to collect a full sample. The use of line C Air data sheetsvoltage, where available, eliminates the difficulties C Chain of Custody recordsassociated with transporting stored electrical energy.

A stand should be used to hold the filter cassette at thedesired height for sampling and the filter cassette shallbe isolated from the vibrations of the pump.

5.2 Filter Cassette

The cassettes are purchased with the required filters inposition, or can be assembled in a laminar flow hoodor clean area. When the filters are in position, ashrink cellulose band or adhesive tape should beapplied to cassette joints to prevent air leakage.

5.2.1 TEM Cassette Requirements

Commercially available field monitors, comprising25 mm diameter three-piece cassettes, withconductive extension cowls shall be used for samplecollection. The cassette must be new and notpreviously used. The cassette shall be loaded with anMCE filter of pore size 0.45 µm, and supplied from alot number which has been qualified as lowbackground for asbestos determination. The cowlsshould be constructed of electrically conductingmaterial to minimize electrostatic effects. The filtershall be backed by a 5 µm pore size MCE filter(Figure 1, Appendix B).

5.2.2 PCM Cassette Requirements

NIOSH Method 7400, PCM involves using a 0.8 to1.2 µm mixed cellulose ester membrane, 25 mmdiameter, 50 mm conductive cowl on cassette (Figure2, Appendix B). Some labs are able to perform PCMand TEM analysis on the same filter; however, thisshould be discussed with the laboratory prior tosampling.

5.3 Other Equipment

C Inert tubing with glass cyclone and hose barbC Whirlbags (plastic bags) for cassettes

C Generator or electrical outlet (may not be

6.0 REAGENTS

Reagents are not required for the preservation ofasbestos samples.

7.0 PROCEDURES

7.1 Air Volumes and Flow Rates

Sampling volumes are determined on the basis of howmany fibers need to be collected for reliablemeasurements. Therefore, one must estimate howmany airborne fibers may be in the sampling location.

Since the concentration of airborne aerosolcontaminants will have some effect on the sample, thefollowing is a suggested criteria to assist in selectinga flow rate based on real-time aerosol monitor (RAM)readings in milligrams/cubic meter (mg/m ).3

Concentration Flow RateC Low RAM readings: <6.0 mg/m 11-15. L/min3

C Medium RAM readings:>6.0 mg/m 7.5 L/min3

C High RAM readings: >10. mg/m 2.5 L/min3

In practice, pumps that are available for environmentalsampling at remote locations operate under amaximum load of approximately 12 L/min.

7.1.1 U.S. EPA's Superfund Method

The Superfund Method incorporates an indirectpreparation procedure to provide flexibility in theamount of deposit that be can be tolerated on thesample filter and to allow for the selectiveconcentration of asbestos prior to analysis. Tominimize contributions to background contaminationfrom asbestos present in the plastic matrices ofmembrane filters while allowing for sufficientquantities of asbestos to be collected, this method alsorequires the collection of a larger volume of air perunit area of filter than has traditionally been collected

5

for asbestos analysis. Due to the need to collect large of 560 L and a maximum volume of 3,800 L in ordervolumes of air, higher sampling flow rates are to obtain an analytical sensitivity of 0.005recommended in this method than have generally been structures/cc. The optimal volume for TEM is 1200employed for asbestos sampling in the past. As an L to 1800 L. These volumes are determined using aalternative, samples may be collected over longer time 200 mesh EM grid opening with a 25-mm filterintervals. However, this restricts the flexibility cassette. Changes in volume would be necessary if arequired to allow samples to be collected while 37-mm filter cassette is used since the effective areauniform meteorological conditions prevail. of a 25 mm (385 sq mm) and 37 mm (855 sq m)

The sampling rate and the period of sampling shouldbe selected to yield as high a sampled volume aspossible, which will minimize the influence of filtercontamination. Wherever possible, a volume of 15cubic meters (15,000 L) shall be sampled for thosesamples intended for analysis only by the indirectTEM preparation method (Phase 1 samples). Forthose samples to be prepared by both the indirect andthe direct specimen preparation methods (Phase 2samples), the volumes must be adjusted so as toprovide a suitably-loaded filter for the direct TEMpreparation method. One option is to collect filters atseveral loadings to bracket the estimated optimumloading for a particular site. Such filters can bescreened in the laboratory so that only those filtersclosest to optimal loading are analyzed. It has beenfound that the volume cannot normally exceed 5 cubicmeters (5000 L) in an urban or agricultural area, and10 cubic meters (10,000 L) in a rural area for samplescollected on a 25 mm filter and prepared by a direct-transfer technique.

An upper limit to the range of acceptable flow ratesfor this method is 15 L/min. At many locations, windpatterns exhibit strong diurnal variations. Therefore,intermittent sampling (sampling over a fixed timeinterval repeated over several days) may be necessaryto accumulate 20 hours of sampling time over constantwind conditions. Other sampling objectives also maynecessitate intermittent sampling. The objective is todesign a sampling schedule so that samples arecollected under uniform conditions throughout thesampling interval. This method provides for suchoptions. Air volumes collected on Phase I samplesare maximized (<16 L/min). Air volumes collectedon Phase 2 samples are limited to provide optimumloading for filters to be prepared by a direct-transferprocedure.

7.1.2 U.S. EPA's Modified YamateMethod for TEM

U.S. EPA's TEM method requires a minimum volume extension cowl marked "Calibration Cassette."

differ.

7.1.3 NIOSH Method for TEM and PCM

The minimum recommended volume for TEM andPCM is 400 L at 0.1 fiber/cc. Sampling time isadjusted to obtain optimum fiber loading on the filter.A sampling rate of 1 to 4 L/min for eight hours (700to 2800 L) is appropriate in non-dusty atmospherescontaining 0.1 fiber/cc. Dusty atmospheres i.e., areaswith high levels of asbestos, require smaller samplevolumes (<400 L) to obtain countable samples.

In such cases, take short, consecutive samples andaverage the results over the total collection time. Fordocumenting episodic exposures, use high flow rates(7 to 16 L/min) over shorter sampling times. Inrelatively clean atmospheres where targeted fiberconcentrations are much less than 0.1 fiber/cc, uselarger sample volumes (3,000 to 10,000 L) to achievequantifiable loadings. Take care, however, not tooverload the filter with background dust. If > 50% ofthe filter surface is covered with particles, the filtermay be too overloaded to count and will bias themeasured fiber concentration. Do not exceed 0.5 mgtotal dust loading on the filter.

7.2 Calibration Procedures

In order to determine if a sampling pump is measuringthe flow rate or volume of air correctly, it is necessaryto calibrate the instrument. Sampling pumps shouldbe calibrated immediately before and after each use.Preliminary calibration should be conducted using aprimary calibrator such as a soap bubble typecalibrator, (e.g., a Buck Calibrator, Gilibrator, orequivalent primary calibrator) with a representativefilter cassette installed between the pump and thecalibrator. The representative sampling cassette canbe reused for calibrating other pumps that will be usedfor asbestos sampling. The same cassette lot used forsampling should also be used for the calibration. Asticker should be affixed to the outside of the

6

A rotameter can be used provided it has been recently 6. Perform the calibration three times until theprecalibrated with a primary calibrator. Three desired flow rate of ± 5% is attained.separate constant flow calibration readings should beobtained both before sampling and after sampling.Should the flow rate change by more than 5% duringthe sampling period, the average of the pre- and post-calibration rates will be used to calculate the totalsample volume. The sampling pump used shallprovide a non-fluctuating air-flow through the filter,and shall maintain the initial volume flow-rate towithin ± 10% throughout the sampling period. Themean value of these flow-rate measurements shall beused to calculate the total air volume sampled. Aconstant flow or critical orifice controlled pump meetsthese requirements. If at any time the measurementindicates that the flow-rate has decreased by morethan 30%, the sampling shall be terminated. Flexibletubing is used to connect the filter cassette to thesampling pump.Sampling pumps can be calibratedprior to coming on-site so that time is saved whenperforming on-site calibration.

7.2.1 Calibrating a Personal SamplingPump with an Electronic Calibrator

1. See Manufacturer's manual for operational course, the flow rate is shown on the LEDinstructions. display.

2. Set up the calibration train as shown in 6. Turn the flow adjust screw or knob on the(Figure 3, Appendix B) using a sampling pump until the desired flow rate is attained.pump, electronic calibrator, and arepresentative filter cassette. The same lot 7. Record the electronic calibrator flow ratesampling cassette used for sampling should reading and the corresponding rotameteralso be used for calibrating. reading. Indicate these values on the

3. To set up the calibration train, attach one end able to work within the desired flow range.of the PVC tubing (approx. 2 foot) to the Readings can also be calibrated for 10 cmcassette base; attach the other end of the increments for Low Flow rotameters, 500tubing to the inlet plug on the pump. cm increments for medium flow rotametersAnother piece of tubing is attached from the and 1 liter increments for high flowcassette cap to the electronic calibrator. rotameters.

4. Turn the electronic calibrator and sampling 8. Perform the calibration three times until thepump on. Create a bubble at the bottom of desired flow rate of ± 5% is attained. Oncethe flow chamber by pressing the bubble on site, a secondary calibrator, i.e., rotameterinitiate button. The bubble should rise to the may be used to calibrate sampling pumps.top of the flow chamber. After the bubbleruns its course, the flow rate is shown on theLED display.

5. Turn the flow adjust screw or knob on thepump until the desired flow rate is attained.

7.2.2 Calibrating a Rotameter with anElectronic Calibrator

1. See manufacturer's manual for operationalinstructions.

2. Set up the calibration train as shown in(Figure 4, Appendix B) using a samplingpump, rotameter, and electronic calibrator.

3. Assemble the base of the flow meter with thescrew provided and tighten in place. Theflow meter should be mounted within 6o

vertical.

4. Turn the electronic calibrator and samplingpump on.

5. Create a bubble at the bottom of the flowchamber by pressing the bubble initiatebutton. The bubble should rise to the top ofthe flow chamber. After the bubble runs its

rotameter (sticker). The rotameter should be

3

3

7.2.3 Calibrating a Personal SamplingPump with a Rotameter

1. See manufacturer's manual for Rotameter'sOperational Instructions.

7

2. Set up the calibration train as shown in 3. Perform a general site survey prior to site(Figure 5, Appendix B) using a rotameter, entry in accordance with the site specificsampling pump, and a representative Health and Safety plan.sampling cassette.

3. To set up the calibration train, attach one end the clean zone. The calibration proceduresof the PVC tubing (approx. 2 ft) to the are listed in Section 7.2. cassette base; attach the other end of thetubing to the inlet plug on the pump. 5. After calibrating the sampling pump,Another piece of tubing is attached from the mobilize to the sampling location.cassette cap to the rotameter.

4. Assemble the base of the flow meter with thescrew provided and tighten in place. Theflow meter should be mounted within 6o

vertical.

5. Turn the sampling pump on.

6. Turn the flow adjust screw (or knob) on thepersonal sampling pump until the float ballon the rotameter is lined up with theprecalibrated flow rate value. A sticker onthe rotameter should indicate this value.

7. A verification of calibration is generallyperformed on-site in the clean zoneimmediately prior to the sampling.

7.3. Meteorology

It is recommended that a meteorological station be the cassette to face upward, place theestablished. If possible, sample after two to three cassette cap on the cassette, remove the inletdays of dry weather and when the wind conditions are plug from the cassette cap, attach a rotameterat 10 mph or greater. Record wind speed, wind to the inlet opening of the cassette cap todirection, temperature, and pressure in a field logbook. measure the flow rate, turn off the samplingWind direction is particularly important when pump, place the inlet plug into the inletmonitoring for asbestos downwind from a fixed opening on the cassette cap. To resumesource. sampling: remove the inlet plug, turn on the

7.4 Ambient Sampling Procedures

7.4.1 Pre-site Sampling Preparation


2. Obtain necessary sampling equipment andensure it is in working order and fullycharged (if necessary).

4. Once on-site the calibration is performed in

7.4.2 Site Sampling

1. To set up the sampling train, attach the airintake hose to the cassette base. Remove thecassette cap (Figure 6 and 7, Appendix B).The cassette should be positioned downward,perpendicular to the wind

2. If AC or DC electricity is required then turnit on. If used, the generator should be placed10 ft. downwind from the sampling pump.

3. Record the following in a field logbook:date, time, location, sample identificationnumber, pump number, flow rate, andcumulative time.

4. Turn the pump on. Should intermittentsampling be required, sampling filters mustbe covered between active periods ofsampling. To cover the sample filter: turn

sampling pump, attach a rotameter tomeasure the flow rate, remove the cassettecap, replace the inlet plug in the cassette capand invert the cassette, face downward andperpendicular to the wind.

5. Check the pump at sampling midpoint ifsampling is longer than 4 hours. Thegenerators may need to be regased dependingon tank size. If a filter darkens in appearanceor if loose dust is seen in the filter, a secondsample should be started.

8

6. At the end of the sampling period, orient the and 0.005 structures/cc or lower [TEM]). cassette up, turn the pump off.

7. Check the flow rate as shown in Section7.2.3. When sampling open-faced, thesampling cap should be replaced before postcalibrating. Use the same cassette used forsampling for post calibration (increasedust/fiber loading may have altered the flowrate.

8. Record the post flow rate.

9. Record the cumulative time or run.

10. Remove the tubing from the samplingcassette. Still holding the cassette upright,replace the inlet plug on the cassette cap andthe outlet plug on the cassette base.

7.4.3. Post Site Sampling

1. Follow handling procedures in Section 3.2, to initially dislodge fibers from surfaces.steps 1-4. This should take at least 5 minutes per 1000

2. Obtain an electronic or hard copy ofmeteorological data which occurred during 2. Place a 20-inch fan in the center of the room.the sampling event. Record weather: wind (Use one fan per 10,000 cubic feet of roomspeed, ambient temperature, wind direction, space.) Place the fan on slow speed andand precipitation. Obtaining weather data point it toward the ceiling.several days prior to the sampling event canalso be useful. 3. Follow procedures in Section 7.4.1 and 7.4.2

7.5 Indoor Sampling Procedures

PCM analysis is used for indoor air samples. Whenanalysis shows total fiber count above the OSHAaction level 0.1 f/cc then TEM (U.S. EPA's ModifiedYamate Method) is used to identify asbestos fromnon-asbestos fibers.

Sampling pumps should be placed four to five feet flow rate of the pump multiplied by the number ofabove ground level away from obstructions that may minutes the pump was running (volume = flow rate Xinfluence air flow. The pump can be placed on a table time in minutes). The sample volume should beor counter. Refer to Table 2 (Appendix A) for a submitted to the laboratory and identified on the chainsummary of indoor sampling locations and rationale of custody for each sample (zero for lot, field and tripfor selection. blanks).

Indoor sampling utilizes high flow rates to increased The concentration result is calculated using thesample volumes (2000 L for PCM and 2800 to 4200 L sample volume and the numbers of asbestos structuresfor TEM) in order to obtain lower detection limits reported after the application of the cluster and matrixbelow the standard, (i.e., 0.01 f/cc or lower [PCM] counting criteria.

7.5.1 Aggressive Sampling Procedures

Sampling equipment at fixed locations may fail todetect the presence of asbestos fibers. Due to limitedair movement, many fibers may settle out of the aironto the floor and other surfaces and may not becaptured on the filter. In the past, an 8-hour samplingperiod was recommended to cover various aircirculation conditions. A quicker and more effectiveway to capture asbestos fibers is to circulate the airartificially so that the fibers remain airborne duringsampling. The results from this sampling optiontypifies worst case condition. This is referred to asaggressive air sampling for asbestos. Refer to Table 2for sample station locations.

1. Before starting the sampling pumps, directforced air (such as a 1-horsepower leafblower or large fan) against walls, ceilings,floors, ledges, and other surfaces in the room

sq. ft. of floor.

(Turn off the pump and then the fan(s) whensampling is complete.).

4. Follow handling procedures in Section 3.2,steps 1-4.

8.0 CALCULATIONS

The sample volume is calculated from the average

9


Follow all QA/QC requirements from the laboratoriesas well as the analytical methods.

9.1 TEM Requirements

1. Examine lot blanks to determine thebackground asbestos structure concentration.

2. Examine field blanks to determine whetherthere is contamination by extraneousasbestos structures during specimenpreparation.

3. Examine of laboratory blanks to determine ifcontamination is being introduced duringcritical phases of the laboratory program.

4. To determine if the laboratory cansatisfactorily analyze samples of knownasbestos structure concentrations, referencefilters shall be examined. Reference filtersshould be maintained as part of thelaboratory's Quality Assurance program.

5. To minimize subjective effects, somespecimens should be recounted by a differentmicroscopist.

6. Asbestos laboratories shall be accredited bythe National Voluntary LaboratoryAccreditation Program.

7. At this time, performance evaluation samplesfor asbestos in air are not available forRemoval Program Activities.

9.2 PCM Requirements EPA's Report No. 68-02-3266, 1984, G.

1. Examine reference slides of knownconcentration to determine the analyst'sability to satisfactorily count fibers.Reference slides should be maintained aspart of the laboratory's quality assuranceprogram.

2. Examine field blanks to determine if there iscontamination by extraneous structuresduring sample handling.

3. Some samples should be relabeled thensubmitted for counting by the same analyst todetermine possible bias by the analyst.

4. Participation in a proficiency testing programsuch as the AIHA-NIOSH proficiencyanalytical testing (PAT) program.


Results of quality control samples will be evaluatedfor contamination. This information will be utilizedto qualify the environmental sample resultsaccordingly with the project's data quality objectives.


When working with potentially hazardous materials,follow U.S. EPA, OSHA, and corporate health andsafety procedures. More specifically, when enteringan unknown situation involving asbestos, a poweredair purifying respirator (PAPR) (full face-piece) isnecessary in conjunction with HEPA filter cartridges.See applicable regulations for action level, PEL, TLV,etc. If previous sampling indicates asbestosconcentrations are below personal health and safetylevels, then Level D personal protection is adequate.

12.0 REFERENCES

Environmental Asbestos Assessment(1)

Manual, Superfund Method for theDetermination of Asbestos in Ambient Air,Part 1: Method, EPA/540/2-90/005a, May1990, and Part 2: Technical BackgroundDocument, EPA/540/2-90/005b, May 1990.

Methodology for the Measurement of(2)

Airborne Asbestos by Electron Microscopy,

Yamate, S.C. Agarwal, and R. D. Gibbons.

National Institute for Occupational Safety(3)

and Health. NIOSH Manual of AnalyticalMethod. Third Edition. 1987.

U.S. Environmental Protection Agency.(4)

Code of Federal Regulations 40 CFR 763.July 1, 1987. Code of Federal Regulations40 CFR 763 Addendum. October 30, 1987.

10

Occupational Safety and Health(5)

Asbestos-Containing Materials in Schools; Administration. Code of Federal RegulationsFinal Rule and Notice. 52 FR 41826. 29 CFR 1910.1001. Washington, D.C.

U.S. Environmental Protection Agency. (6)

1987.

11

APPENDIX A

Tables

TABLE 1.

SAMPLE STATIONS FOR OUTDOOR SAMPLING

Sample Station Sample Numbers RationaleLocation

Upwind/Background Collect a minimum of two simultaneous Establishes background fiber levels.(1)

upwind/background samples 30 aparto

from the prevailing windlines.

Downwind Deploy a minimum of 3 sampling stations Indicates if asbestos is leaving thein a 180 degree arc downwind from the site.source.

Site Representative Obtain one site representative sample Verify and continually confirm andand/or Worst Case which shows average condition on-site or document selection of proper levels

obtain worst case sample (optional). of worker protection.

More than one background station may be required if the asbestos originates from different sources.(1)

12


Tables

TABLE 2

SAMPLE STATIONS FOR INDOOR SAMPLING

Sample Station Sample Numbers RationaleLocation

Indoor Sampling If a work site is a single room, disperse 5 Establishes representative samplessamplers throughout the room. from a homogeneous area.

If the work site contains up to 5 rooms, placeat least one sampler in each room.

If the work site contains more than 5 rooms,select a representative sample of the rooms.

Upwind/Background If outside sources are suspected, Establish whether indoor asbestosdeploy a minimum of two simultaneous concentrations are coming from anupwind/background samples 30 apart from outside source.o

the prevailing windlines.

Worst Case Obtain one worst case sample, i.e., Verify and continually confirm andaggressive sampling (optional). document selection of proper levels

of worker protection.

13

APPENDIX B

Figures

FIGURE 1. Transmission Electron Microscopy Filter Cassette

14


Figures

FIGURE 2. Phase Contrast Microscopy Filter Cassette

15


Figures

FIGURE 3. Calibrating a Personal Sampling Pump with a Bubble Meter

16


Figures

FIGURE 4. Calibrating a Rotameter with a Bubble Meter

17


Figures

FIGURE 5. Calibrating a Sampling Pump with a Rotameter

18


Figures

FIGURE 6. Personal Sampling Train for Asbestos

19


Figures

FIGURE 7. High Flow Sampling Train for Asbestos

1

SOP#: 2016DATE: 11/17/94

REV. #: 0.0 SEDIMENT SAMPLING


This standard operating procedure (SOP) is applicableto the collection of representative sediment samples.Analysis of sediment may be biological, chemical, orphysical in nature and may be used to determine thefollowing:

C toxicity;C biological availability and effects of

contaminants;C benthic biota;C extent and magnitude of contamination;C contaminant migration pathways and source;C fate of contaminants;C grain size distribution.

The methodologies discussed in this SOP areapplicable to the sampling of sediment in both flowingand standing water. They are generic in nature andmay be modified in whole or part to meet the handlingand analytical requirements of the contaminants ofconcern, as well as the constraints presented by siteconditions and equipment limitations. However, ifmodifications occur, they should be documented in asite or personal logbook and discussed in reportssummarizing field activities and analytical results.

For the purposes of this procedure, sediments arethose mineral and organic materials situated beneathan aqueous layer. The aqueous layer may be eitherstatic, as in lakes, ponds, and impoundments; orflowing, as in rivers and streams.


2.0 METHOD SUMMARY

Sediment samples may be collected using a variety ofmethods and equipment, depending on the depth of theaqueous layer, the portion of the sediment profile

required (surface vs. subsurface), the type of samplerequired (disturbed vs. undisturbed), contaminantspresent, and sediment type.

Sediment is collected from beneath an aqueous layereither directly, using a hand held device such as ashovel, trowel, or auger; or indirectly, using aremotely activated device such as an Ekman or Ponardredge. Following collection, sediment is transferredfrom the sampling device to a sample container ofappropriate size and construction for the analysesrequested. If composite sampling techniques areemployed, multiple grabs are placed into a containerconstructed of inert material, homogenized, andtransferred to sample containers appropriate for theanalyses requested. The homogenization procedureshould not be used if sample analysis includes volatileorganics; in this case, sediment, or multiple grabs ofsediment, should be transferred directly from thesample collection device or homogenization containerto the sample container.

3.0 SAMPLE PRESERVATION,CONTAINERS, HANDLING ANDSTORAGE

1. Chemical preservation of solids is generallynot recommended. Cooling to 4 C is usuallyo

the best approach, supplemented by theappropriate holding time for the analysesrequested.

2. Wide mouth glass containers with Teflonlined caps are utilized for sediment samples.The sample volume is a function of theanalytical requirements and will be specifiedin the Work Plan.

3. If analysis of sediment from a discrete depthor location is desired, sediment is transferreddirectly from the sampling device to alabeled sample container(s) of appropriatesize and construction for the analyses

2

requested. Transfer is accomplished with a can, therefore, greatly influence the analytical resultsstainless steel or plastic lab spoon or and should be justified and specified in the Workequivalent. Plan.

4. If composite sampling techniques or multiplegrabs are employed, equal portions ofsediment from each location are depositedinto a stainless steel, plastic, or otherappropriate composition (e.g., Teflon)containers. The sediment is homogenizedthoroughly to obtain a compositerepresentative of the area sampled. Thecomposite sediment sample is transferred toa labeled container(s) of appropriate size andconstruction for the analyses requested.Transfer of sediment is accomplished with astainless steel or plastic lab spoon orequivalent. Samples for volatile organicanalysis must be transferred directly from thesample collection device or pooled frommultiple areas in the homogenizationcontainer prior to mixing. This is done tominimize loss of contaminant due tovolatilization during homogenization.

5. All sampling devices should bedecontaminated, then wrapped in aluminumfoil. The sampling device should remain inthis wrapping until it is needed. Eachsampling device should be used for only onesample. Disposable sampling devices forsediment are generally impractical due tocost and the large number of sedimentsamples which may be required. Samplingdevices should be cleaned in the field usingthe decontamination procedure described inthe Sampling Equipment DecontaminationSOP.


Substrate particle size and organic matter content area direct consequence of the flow characteristics of awaterbody. Contaminants are more likely to be Reagents are not used for preservation of sedimentconcentrated in sediments typified by fine particle size samples. Decontamination solutions are specified inand a high organic matter content. This type of the Sampling Equipment Decontamination SOP.sediment is most likely to be collected fromdepositional zones. In contrast, coarse sediments withlow organic matter content do not typicallyconcentrate pollutants and are generally found inerosional zones. The selection of a sampling location


Equipment needed for collection of sediment samplesmay include:

C Maps/plot planC Safety equipmentC CompassC Tape measureC Survey stakes, flags, or buoys and anchorsC Camera and filmC Stainless steel, plastic, or other appropriate

composition bucketC 4-oz., 8-oz., and one-quart wide mouth jars

w/Teflon lined lidsC Ziploc plastic bagsC LogbookC Sample jar labelsC Chain of Custody records, field data sheetsC Cooler(s)C IceC Decontamination supplies/equipmentC Spade or shovelC SpatulaC ScoopC TrowelC Bucket augerC Tube augerC Extension rodsC "T" handleC Sediment coring device (tube, drive head,

eggshell check value, nosecone, acetate tube,extension rods, "T" handle)

C Ponar dredgeC Ekman dredgeC Nylon rope or steel cableC Messenger device

6.0 REAGENTS

3

7.0 PROCEDURES

7.1 Preparation

1. Determine the objective(s) and extent of thesampling effort. The sampling methods to beemployed, and the types and amounts ofequipment and supplies required will be afunction of site characteristics and objectivesof the study.

2. Obtain the necessary sampling andmonitoring equipment.

3. Prepare schedules, and coordinate with staff,client, and regulatory agencies, ifappropriate.



6. Use stakes, flagging, or buoys to identify andmark all sampling locations. Specific sitefactors including flow regime, basinmorphometry, sediment characteristics, depthof overlying aqueous layer, contaminantsource, and extent and nature ofcontamination should be considered whenselecting sample locations. If required, theproposed locations may be adjusted based onsite access, property boundaries, and surfaceobstructions.


Selection of a sampling device is most oftencontingent upon: (1) the depth of water at the For the purpose of this method, surface sediment issampling location, and (2) the physical characteristics considered to range from 0 to six inches in depth andof the sediment to be sampled. The following a shallow aqueous layer is considered to range from 0procedures may be utilized: to 24 inches in depth. Collection of surface sediment

7.2.1 Sampling Surface Sediment with aTrowel or Scoop from Beneath aShallow Aqueous Layer

For the purpose of this method, surface sediment isconsidered to range from 0 to six inches in depth and

a shallow aqueous layer is considered to range from 0to 12 inches in depth. Collection of surface sedimentfrom beneath a shallow aqueous layer can beaccomplished with tools such as spades, shovels,trowels, and scoops. Although this method can beused to collect both unconsolidated/consolidatedsediment, it is limited somewhat by the depth andmovement of the aqueous layer. Deep and rapidlyflowing water render this method less accurate thanothers discussed below. However, representativesamples can be collected with this procedure inshallow sluggish water provided care is demonstratedby the sample team member. A stainless steel orplastic sampling implement will suffice in mostapplications. Care should be exercised to avoid theuse of devices plated with chrome or other materials;plating is particularly common with garden trowels.

The following procedure will be used to collectsediment with a scoop, shovel, or trowel:

1. Using a decontaminated samplingimplement, remove the desired thickness andvolume of sediment from the sampling area.

2. Transfer the sample into an appropriatesample or homogenization container. Ensurethat non-dedicated containers have beenadequately decontaminated.

3. Surface water should be decanted from thesample or homogenization container prior tosealing or transfer; care should be taken toretain the fine sediment fraction during thisprocedure.

7.2.2 Sampling Surface Sediment with aBucket Auger or Tube Auger fromBeneath a Shallow Aqueous Layer

from beneath a shallow aqueous layer can beaccomplished with a system consisting of bucketauger or tube auger, a series of extensions, and a "T"handle (Figure 1, Appendix A). The use of additionalextensions in conjunction with a bucket auger canincrease the depth of water from which sediment canbe collected from 24 inches to 10 feet or more.However, sample handling and manipulation increases

4

in difficulty with increasing depth of water. The "T" handle. The use of additional extensions canbucket auger or tube auger is driven into the sediment increase the depth of water from which sediment canand used to extract a core. The various depths be collected from 24 inches to five feet or more.represented by the core are homogenized or a However, water clarity must be high enough to permitsubsample of the core is taken from the appropriate the sampler to directly observe the samplingdepth. operation. In addition, sample handling and

The following procedure will be used to collect depth of water. The bucket auger is used to bore asediment samples with a bucket auger or tube auger: hole to the upper range of the desired sampling depth

1. An acetate core may be inserted into the down the borehole, and driven into the sediment to thebucket auger or tube auger prior to sampling lower range of the desired sampling depth. The tubeif characteristics of the sediments or is then withdrawn and the sample recovered from thewaterbody warrant. By using this technique, tube. This method can be used to collect firmlyan intact core can be extracted. consolidated sediments, but is somewhat limited by

2. Attach the auger head to the required length initial borehole.of extensions, then attach the "T" handle tothe upper extension. The following procedure will be used to collect deep

3. Clear the area to be sampled of any surface auger:debris.

4. Insert the bucket auger or tube auger into the lengths of extensions, then attach the "T"sediment at a 0 to 20 angle from vertical. handle to the upper extension.o o

This orientation minimizes spillage of thesample from the sampler upon extraction 2. Clear the area to be sampled of any surfacefrom the sediment and water. debris.

5. Rotate the auger to cut a core of sediment. 3. Begin augering, periodically removing any

6. Slowly withdraw the auger; if using a tube the auger bucket. Cuttings should beauger, make sure that the slot is facing disposed of far enough from the samplingupward. area to minimize cross contamination of

7. Transfer the sample or a specified aliquot ofsample into an appropriate sample or 4. After reaching the upper range of the desiredhomogenization container. Ensure that non- depth, slowly and carefully remove bucketdedicated containers have been adequately auger from the boring.decontaminated.

7.2.3 Sampling Deep Sediment with aBucket Auger or Tube Auger fromBeneath a Shallow Aqueous Layer

For the purpose of this method, deep sediment isconsidered to range from six to greater than 18 inchesin depth and a shallow aqueous layer is considered torange from 0 to 24 inches. Collection of deepsediment from beneath a shallow aqueous layer can beaccomplished with a system consisting of a bucketauger, a tube auger, a series of extensions and a

manipulation increases in difficulty with increasing

and then withdrawn. The tube auger is then lowered

the depth of the aqueous layer, and the integrity of the

sediment samples with a bucket auger and a tube

1. Attach the bucket auger bit to the required

accumulated sediment (i.e., cuttings) from

various depths.

5. Attach the tube auger bit to the requiredlengths of extensions, then attach the "T"handle to the upper extension.

6. Carefully lower tube auger down boreholeusing care to avoid making contact with theborehole sides and, thus, cross contaminatingthe sample. Gradually force tube auger intosediment to the lower range of the desiredsampling depth. Hammering of the tubeauger to facilitate coring should be avoidedas the vibrations may cause the boring walls

5

to collapse. above the sediment surface.

7. Remove tube auger from the borehole, again 4. Drop the sampler to the sediment.taking care to avoid making contact with theborehole sides and, thus, cross contaminating 5. Trigger the jaw release mechanism bythe sample. lowering a messenger down the line, or by

8. Discard the top of core (approximately 1 extension handle.inch); as this represents material collected bythe tube auger before penetration to the layer 6. Raise the sampler and slowly decant any freeof concern. liquid through the top of the sampler. Care

9. Transfer sample into an appropriate sample fraction during this procedure.or homogenization container. Ensure thatnon-dedicated containers have been 7. Open the dredge jaws and transfer the sampleadequately decontaminated. into a stainless steel, plastic or other

7.2.4 Sampling Surface Sediment with anEkman or Ponar Dredge fromBeneath a Shallow or Deep AqueousLayer

For the purpose of this method, surface sediment isconsidered to range from 0 to six inches in depth.Collection of surface sediment can be accomplishedwith a system consisting of a remotely activateddevice (dredge) and a deployment system. Thistechnique consists of lowering a sampling device(dredge) to the surface of the sediment by use of arope, cable, or extended handle. The mechanism isactivated, and the device entraps sediment in springloaded or lever operated jaws.

An Ekman dredge is a lightweight sediment samplingdevice with spring activated jaws. It is used to collectmoderately consolidated, fine textured sediment. Thefollowing procedure will be used for collectingsediment with an Ekman dredge (Figure 2,Appendix A):

1. Attach a sturdy nylon rope or stainless steelcable through the hole on the top of thebracket, or secure the extension handle to thebracket with machine bolts.

2. Attach springs to both sides of the jaws. Fixthe jaws so that they are in open position byplacing trip cables over the release studs.Ensure that the hinged doors on the dredgetop are free to open.

3. Lower the sampler to a point 4 to 6 inches

depressing the button on the upper end of the

should be taken to retain the fine sediment

appropriate composition (e.g., Teflon)container. Ensure that non-dedicatedcontainers have been adequatelydecontaminated. If necessary, continue tocollect additional sediment grabs untilsufficient material has been secured to fulfillanalytical requirements. Thoroughlyhomogenize and then transfer sediment tosample containers appropriate for theanalyses requested. Samples for volatileorganic analysis must be collected directlyfrom the bucket before homogenization tominimize volatilization of contaminants.

A Ponar dredge is a heavyweight sediment samplingdevice with weighted jaws that are lever or springactivated. It is used to collect consolidated fine tocoarse textured sediment. The following procedurewill be used for collecting sediment with a Ponardredge (Figure 3, Appendix A):

1. Attach a sturdy nylon rope or steel cable tothe ring provided on top of the dredge.

2. Arrange the Ponar dredge with the jaws inthe open position, setting the trip bar so thesampler remains open when lifted from thetop. If the dredge is so equipped, place thespring loaded pin into the aligned holes in thetrip bar.

3. Slowly lower the sampler to a pointapproximately two inches above thesediment.

4. Drop the sampler to the sediment. Slack on

6

the line will release the trip bar or spring 2. Insert the "egg shell" check valve into theloaded pin; pull up sharply on the line lower end of the sampling tube with theclosing the dredge. convex surface positioned inside the acetate

5. Raise the dredge to the surface and slowlydecant any free liquid through the screens on 3. Screw the nosecone onto the lower end of thetop of the dredge. Care should be taken to sampling tube, securing the acetate tube andretain the fine sediment fraction during this eggshell check valve.operation.

6. Open the dredge and transfer the sediment to sampling tube and add extension rods asa stainless steel, plastic or other appropriate needed.composition (e.g., Teflon) container. Ensurethat non-dedicated containers have been 5. Place the sampler in a perpendicular positionadequately decontaminated. If necessary, on the sediment to be sampled.continue to collect additional sediment untilsufficient material has been secured to fulfill 6. If the "T" handle is used, place downwardanalytical requirements. Thoroughly pressure on the device until the desired depthhomogenized and then transfer sediment to is reached. After the desired depth issample containers appropriate for the reached, rotate the sampler to shear off theanalyses requested. Samples for volatile core at the bottom. Slowly withdraw theorganic analysis must be collected directly sampler from the sediment and proceed tofrom the bucket before homogenization to Step 15.minimize volatilization of contaminants.

7.2.5 Sampling Subsurface Sediment witha Coring Device from Beneath aShallow Aqueous Layer

For purposes of this method, subsurface sediment isconsidered to range from 6 to 24 inches in depth anda shallow aqueous layer is considered to range from 0to 24 inches in depth. Collection of subsurfacesediment from beneath a shallow aqueous layer can beaccomplished with a system consisting of a tubesampler, acetate tube, eggshell check valve, nosecone,extensions, and "T" handle, or drivehead. The use ofadditional extensions can increase the depth of waterfrom which sediment can be collected from 24 inchesto 10 feet or more. This sampler may be used witheither a drive hammer for firm sediment, or a "T"handle for soft sediment. However, sample handlingand manipulation increases in difficulty withincreasing depth of water.

The following procedure describes the use of a samplecoring device (Figure 4, Appendix A) used to collectsubsurface sediments.

1. Assemble the coring device by inserting theacetate core into the sampling tube.

core.

4. Screw the handle onto the upper end of the

7. If the drive hammer is selected, insert thetapered handle (drive head) of the drivehammer through the drive head.

8. Drive the sampler into the sediment to thedesired depth.

9. Record the length of the tube that penetratedthe sample material, and the number ofblows required to obtain this depth.

10. Remove the drive hammer and fit thekeyhole-like opening on the flat side of thehammer onto the drive head. In this position,the hammer serves as a handle for thesampler.

11. Rotate the sampler to shear off the core at thebottom.

12. Lower the sampler handle (hammer) until itjust clears the two ear-like protrusions on thedrive head, and rotate about 90 .o

13. Slowly withdraw the sampler from thesediment. If the drivehead was used, pull thehammer upwards and dislodge the samplerfrom the sediment.

7

14. Carefully remove the coring device from the 2. All instrumentation must be operated inwater. accordance with operating instructions as

15. Unscrew the nosecone and remove the otherwise specified in the work plan.eggshell check valve. Equipment checkout and calibration

16. Slide the acetate core out of the sampler sampling/operation, and they must betube. Decant surface water, using care to documented.retain the fine sediment fraction. If headspace is present in the upper end, a hacksawmay be used to shear the acetate tube off atthe sediment surface. The acetate core maythen be capped at both ends. Indicate on theacetate tube the appropriate orientation of thesediment core using a waterproof marker.The sample may be used in this fashion, orthe contents transferred to a sample orhomogenization container.

17. Open the acetate tube and transfer thesediment to a stainless steel, plastic or otherappropriate composition (e.g., Teflon)container. Ensure that non-dedicatedcontainers have been adequatelydecontaminated. If necessary, continue tocollect additional sediment until sufficientmaterial has been secured to fulfill analyticalrequirements. Thoroughly homogenize andthen transfer sediment to sample containersappropriate for the analyses requested.Samples for volatile organic analysis must becollected directly from the bucket beforehomogenization to minimize volatilization ofcontaminants.

8.0 CALCULATIONS



There are no specific quality assurance (QA) activities 600/4-84-076.which apply to the implementation of theseprocedures. However, the following QA procedures de Vera, E.R., B.P. Simmons, R.D. Stephen, and D.L.apply: Storm. Samplers and Sampling Procedures for


supplied by the manufacturer, unless

activities must occur prior to




When working with potentially hazardous materials ,follow U.S. EPA/OSHA and Corporate health andsafety procedures.

More specifically, when sampling sediment fromwaterbodies, physical hazards must be identified andadequate precautions must be taken to ensure thesafety of the sampling team. The team membercollecting the sample should not get too close to theedge of the waterbody, where bank failure may causeloss of balance. To prevent this, the personperforming the sampling should be on a lifeline, andbe wearing adequate protective equipment. Ifsampling from a vessel is determined to be necessary,appropriate protective measures must be implemented.

12.0 REFERENCES

Mason, B.J., Preparation of Soil Sampling Protocol:Technique and Strategies. 1983 EPA-600/4-83-020.

Barth, D.S. and B.J. Mason, Soil Sampling QualityAssurance User's Guide. 1984 EPA-600/4-84-043.

U.S. EPA. Characterization of Hazardous Waste Sites- A Methods Manual: Volume II. AvailableSampling Methods, Second Edition. 1984 EPA-

Hazardous Waste Streams. 1980 EPA-600/2-80-018.

8

APPENDIX A

Figures

FIGURE 1. Sampling Auger

9


Figures

FIGURE 2. Ekman Dredge

10


Figures

FIGURE 3. Ponar Dredge

11


Figures

FIGURE 4. Sample Coring Device

1

SOP#: 2017DATE: 11/17/94

REV. #: 0.0 WASTE PILE SAMPLING


The objective of this standard operating procedure(SOP) is to outline the equipment and methods used incollecting representative samples from waste piles,sludges or other solid or liquid waste mixed with soil.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent on site conditions, equipmentlimitations or other procedure limitations. In allinstances, the ultimate procedures employed should bedocumented and associated with the final report.


2.0 METHOD SUMMARY

Stainless steel shovels, trowels, or scoops should beused to clear away surface material before samples are Material to be sampled may be homogeneous orcollected. For depth samples, a decontaminated auger heterogeneous. Homogeneous material resulting frommay be required to advance the hole, then another known situations may not require an extensivedecontaminated auger used for sample collection. For sampling protocol. Heterogeneous and unknowna sample core, thin-wall tube samplers or grain wastes require more extensive sampling and analysissamplers may be used. Near surfaces, samples can be to ensure the different components (i.e. layers, strata)collected with a clean stainless steel spoon or trowel. are being represented.

All samples collected, except those for volatile The term "representative sample" is commonly usedorganic analysis, should be placed into a Teflon lined to denote a sample that has the properties andor stainless steel pail and mixed thoroughly before composition of the population from which it wastransfer to appropriate sample container. collected and in the same proportions as found in the


Chemical preservation of solids is generally notrecommended. Refrigeration to 4 C is usually the besto

approach, supplemented by a minimal holding time,depending on contaminants of concern.

Wide mouth glass containers with Teflon lined capsare typically used for waste pile samples. Samplevolume required is a function of the analyticalrequirements and should be specified in the work plan.


There are several variables involved in wastesampling, including shape and size of piles,compactness, and structure of the waste material.Shape and size of waste material or waste piles varygreatly in areal extent and height. Since state andfederal regulations often require a specified number ofsamples per volume of waste, the size and shape mustbe used to calculate volume and to plan for the correctnumber of samples. Shape must also be accounted forwhen planning physical access to the sampling pointand the equipment necessary to successfully collectthe sample at that location.

population. This can be misleading unless one isdealing with a homogenous waste from which onesample can represent the whole population.

The usual options for obtaining the most"representative sample" from waste piles are simplerandom sampling or stratified random sampling.Simple random sampling is the method of choiceunless: (1) there are known distinct strata; (2) onewants to prove or disprove that there are distinct

2

strata; or (3) one is limited in the number of samples C Canvas or plastic sheetand desires to statistically minimize the size of a "hot C Spade or shovelspot" that could go unsampled. If any of these C Spatulaconditions exist, stratified random sampling would be C Scoopthe better strategy. C Plastic or stainless steel spoons

Stratified random sampling can be employed only if C Continuous flight (screw) augersall points within the pile can be accessed. In such C Bucket augercases, the pile should be divided into a three- C Post hole augerdimensional grid system with, the grid cubes should C Extension rodsbe numbered, and the grid cubes to be sampled should C T-Handlebe chosen by random number tables or generators . C Thin-wall tube sampler with cutting tipsThe only exceptions to this are situations in which C Sampling trierrepresentative samples cannot be collected safely or C Grain samplerwhere the investigative team is trying to determineworst case conditions.

If sampling is limited to certain portions of the pile, astatistically based sample will be representative onlyof that portion, unless the waste is homogenous.


Waste pile solids include powdered, granular, or blockmaterials of various sizes, shapes, structure, andcompactness. The type of sampler chosen should becompatible with the waste. Samplers commonly usedfor waste piles include: stainless steel scoops,shovels, trowels, spoons, and stainless steel handaugers, sampling triers, and grain samplers.

Waste pile sampling equipment check list:

C Sampling planC Maps/plot planC Safety equipment, as specified in the Health

and Safety PlanC CompassC Tape measureC Survey stakes or flagsC Camera and filmC Stainless steel, plastic, or other appropriate

homogenization bucket or bowlC Appropriate size sample jarsC Ziplock plastic bagsC LogbookC LabelsC Chain of Custody records and sealsC Field data sheetsC Cooler(s)C IceC Decontamination supplies/equipment

C Trowel

6.0 REAGENTS

No chemical reagents are used for the preservation ofwaste pile samples; however, decontaminationsolutions may be required. If decontamination ofequipment is required, refer to the SamplingEquipment Decontamination SOP, and the sitespecific work plan.

7.0 PROCEDURES

7.1 Preparation

1. Review all information available on thewaste pile and expected or unknowncontaminants.

2. Determine the extent of the sampling effort,the sampling methods to be employed, andthe types and amounts of equipment andsupplies required.


4. Decontaminate or pre-clean equipment, andensure that it is in working order.

5. Prepare schedules, and coordinate with staff,client, and regulatory agencies, ifappropriate.


7. Use stakes or flagging to identify and mark

3

all sampling locations. Specific site factors, caps tightly; or, if composite samples are toincluding extent and nature of contaminant be collected, place a sample from anothershould be considered when selecting sample sampling interval into the homogenizationlocations. If required, the proposed locations container and mix thoroughly. Whenmay be adjusted based on site access, compositing is complete, place the sampleproperty boundaries, and surface into appropriate, labeled containers andobstructions. secure the caps tightly.


7.2.1 Sampling with Shovels and Scoops Thin-Wall Tube Samplers

Collection of samples from surface portions of the pile These samplers consist of a series of extensions, acan be accomplished with tools such as spades, "T" handle, and a bucket auger or thin-wall tubeshovels, and scoops. Surface material can be removed sampler (Appendix A, Figure 1). The auger is used toto the required depth with this equipment, then a bore a hole to a desired sampling depth, and is thenstainless steel or plastic scoop, or equivalent can be withdrawn. The sample may be collected directlyused to collect the sample. from the bucket auger. If a core sample is to be

Accurate, representative samples can be collected wall tube sampler. The sampler is then lowered downwith this procedure depending on the care and the borehole, and driven into the pile to theprecision demonstrated by sample team members. completion depth. The sampler is withdrawn and theUse of a flat, pointed mason trowel to cut a block of core collected from the thin-wall tube sampler.the desired material can be helpful when undisturbedprofiles are required. A stainless steel scoop, lab Several augers are available. These include: bucket,spoon, plastic spoon, or equivalent will suffice in most continuous flight (screw), and post hole augers.other applications. Care should be exercised to avoid Bucket augers are better for direct sample recoverythe use of devices plated with chrome or other since they provide a large volume of sample in a shortmaterials. Plating is particularly common with time. When continuous flight augers are used, theimplements such as garden trowels. sample can be collected directly from the flights,

The following procedure is used to collect the surface continuous flight augers are satisfactory for use whensamples: a composite of the complete waste pile column is

1. Carefully remove the top layer of material to sample collection as they are designed to cut throughthe desired sample depth with a pre-cleaned fibrous, rooted, swampy areas.spade.

2. Using a pre-cleaned stainless steel scoop, waste pile samples with the bucket augers and thin-plastic spoon, trowel, or equivalent remove wall tube samplers:and discard a thin layer of material from thearea which came in contact with the spade. 1. Attach the auger bit to a drill rod extension,

3. If volatile organic analysis is to beperformed, transfer the sample into an 2. Clear the area to be sampled of any surfaceappropriate, labeled sample container with a debris. It may be advisable to remove thestainless steel lab spoon, or equivalent, and first three to six inches of surface materialsecure the cap tightly. Place the remainder for an area approximately six inches in radiusof the sample into a stainless steel, plastic, or around the drilling location.other appropriate homogenization container,and mix thoroughly to obtain a homogenous 3. Begin augering, periodically removing andsample representative of the entire sampling depositing accumulated materials onto ainterval. Then, either place the sample into plastic sheet spread near the hole. Thisappropriate, labeled containers and secure the prevents accidental brushing of loose

7.2.2 Sampling with Bucket Augers and

collected, the auger tip is then replaced with a thin-

which are usually at five (5) foot intervals. The

desired. Post hole augers have limited utility for

The following procedure will be used for collecting

and attach the "T" handle to the drill rod.

4

material back down the borehole when container and mix thoroughly. Whenremoving the auger or adding drill rod compositing is complete, place the sampleextensions. It also facilitates refilling the into appropriate, labeled containers andhole, and avoids possible contamination of secure the caps tightly.the surrounding area.

4. After reaching the desired depth, slowly and same hole, but at a greater depth, reattach thecarefully remove the auger from the bucket auger to the drill and assembly, andborehole. When sampling directly from the follow steps 3 through 11, making sure toauger, collect the sample after the auger is decontaminate the bucket auger and thin-wallremoved from the borehole and proceed to tube sampler between samples.Step 10.

5. Remove auger tip from drill rods and replacewith a pre-cleaned thin-wall tube sampler.Install proper cutting tip.

6. Carefully lower the tube sampler down theborehole. Gradually force the tube samplerinto the pile. Care should be taken to avoidscraping the borehole sides. Avoidhammering the drill rod extensions tofacilitate coring as the vibrations may causethe borehole walls to collapse.

7. Remove the tube sampler, and unscrew thedrill rod extensions.

8. Remove the cutting tip and the thin-wall tubesampler.

9. Discard the top of the core (approximatelyone-inch), as this represents materialcollected before penetration of the layer ofconcern. Place the remaining core into theappropriate labeled sample container.Sample homogenization is not required.

10. If volatile organic analysis is to beperformed, transfer the sample into anappropriate, labeled sample container with astainless steel lab spoon, or equivalent andsecure the cap tightly. Place the remainderof the sample into a stainless steel, plastic, orother appropriate homogenization container,and mix thoroughly to obtain a homogenoussample representative of the entire samplinginterval. Then, either place the sample intoappropriate, labeled containers and secure thecaps tightly; or, if composite samples are tobe collected, place a sample from anothersampling interval into the homogenization

11. If another sample is to be collected in the

7.2.3 Sampling with a Trier

This sampling device consists of a trier, and a"T" handle. The trier is driven into the waste pile andused to extract a core sample from the appropriatedepth.

The following procedure will be used to collect wastepile samples with a sampling trier:

1. Insert the trier (Appendix A, Figure 2) intothe material to be sampled at a 0E to 45Eangle from horizontal. This orientationminimizes spillage of the sample. Extractionof the samples might require tilting of thesample containers.

2. Rotate the trier once or twice to cut a core ofmaterial.

3. Slowly withdraw the trier, making sure thatthe slot is facing upward.

4. If volatile organic analysis is to beperformed, transfer the sample into anappropriate, labeled sample container with astainless steel lab spoon, plastic lab spoon, orequivalent and secure the cap tightly. Placethe remainder of the sample into a stainlesssteel, plastic, or other appropriatehomogenization container, and mixthoroughly to obtain a homogenous samplerepresentative of the entire sampling interval.Then, either place the sample intoappropriate, labeled containers and secure thecaps tightly; or, if composite samples arebeing collected, place samples from the othersampling intervals into the homogenizationcontainer and mix thoroughly. Whencompositing is complete, place the sample

5

into appropriate, labeled containers and 7. If volatile organic analysis is to besecure the caps tightly. performed, transfer the sample into an

7.2.4 Sampling with a Grain Sampler

The grain sampler (Appendix A, Figure 3) is used forsampling powdered or granular wastes or materials inbags, fiber drums, sacks, similar containers or piles .This sampler is most useful when the solids are nogreater than 0.6 cm (1/4") in diameter.

This sampler consists of two slotted telescoping brassor stainless steel tubes. The outer tube has a conical,pointed tip at one end that permits the sampler topenetrate the material being sampled. The sampler isopened and closed by rotating the inner tube. Grainsamplers are generally 61 to 100 cm (24 to 40 in.)long by 1.27 to 2.54 cm (1/2 to 1 in.) in diameter andare commercially available at laboratory supplyhouses.

The following procedures will be used to collect wastepile samples with a grain sampler: This section is not applicable to this SOP.

1. With the sampler in the closed position,insert it into the granular or powderedmaterial or waste being sampled from a pointnear a top edge or corner, through the center,and to a point diagonally opposite the pointof entry.

2. Rotate the sampler inner tube into the openposition.

3. Wiggle the sampler a few times to allowmaterial to enter the open slots.

4. Place the sampler in the closed position andwithdraw from the material being sampled.

5. Place the sampler in a horizontal positionwith the slots facing upward.

6. Rotate the outer tube and slide it away fromthe inner tube.

appropriate, labeled sample container with astainless steel lab spoon, plastic lab spoon, orequivalent and secure the cap tightly. Placethe remainder of the sample into a stainlesssteel, plastic, or other appropriatehomogenization container, and mixthoroughly to obtain a homogenous samplerepresentative of the entire sampling interval.Then, either place the sample intoappropriate, labeled containers and secure thecaps tightly; or, if composite samples are tobe collected, place a sample from anothersampling interval into the homogenizationcontainer and mix thoroughly. Whencompositing is complete, place the sampleinto appropriate, labeled containers andsecure the caps tightly.

8.0 CALCULATIONS


There are no specific quality assurance activitieswhich apply to the implementation of theseprocedures. However, the following QA proceduresapply:


2. All instrumentation must be operated inaccordance with operating instructions assupplied by the manufacturer, unlessotherwise specified in the work plan.Equipment checkout and calibrationactivities must occur prior tosampling/operation, and they must bedocumented.

6

10.0 DATA VALIDATION 12.0 REFERENCES

This section is not applicable to this SOP. Test Methods for Evaluating Solids Waste (SW-846),


When working with potentially hazardous materials ,follow U.S. EPA/OSHA and corporate health andsafety procedures.

Third Edition, Vol. II Field Manual U.S. EPA Officeof Solid Waste and Emergency Response,Washington, D.C. November, 1986.

Engineering Support Branch Standard OperatingProcedures and Quality Assurance Manual, U.S.Environmental Protection Agency, Region IV, April1, 1986.

Field Sampling Procedures Manual, New JerseyDepartment of Environmental Protection, February,1988.

7

APPENDIX A

Figures

FIGURE 1. Sampling Augers

8


Figures

FIGURE 2. Sampling Trier

9


Figures

FIGURE 3. Grain Sampler




DATE: 09/06/01TEDLAR® BAG SAMPLING

CONTENTS

1.0 SCOPE AND APPLICATION*

2.0 METHOD SUMMARY*

3.0 SAMPLE PRESERVATION, CONTAINERS, HANDLING, AND STORAGE*

4.0 INTERFERENCES AND POTENTIAL PROBLEMS*

5.0 EQUIPMENT/APPARATUS*

6.0 REAGENTS

7.0 PROCEDURES

7.1 Field Preparation*7.2 Field Operations*

8.0 CALCULATIONS

9.0 QUALITY ASSURANCE/QUALITY CONTROL*



12.0 REFERENCES*

13.0 APPENDIX

A - Figure

* These sections affected by this revision.

SUPERCEDES: SOP #2102; Revision 0.0; 10/21/94; U.S. EPA Contract 68-C4-0022.






The purpose of this standard operating procedure (SOP) is to define the use of Tedlar® bags in collectinggaseous grab samples. Tedlar® bags are used to collect volatile organic compounds (VOCs) includinghalogenated and non-halogenated species. The sensitivity of the method is primarily dependent on theanalytical instrument and the compounds being investigated.

These are standard (i.e., typically applicable) operating procedures which may be varied or changed as required,dependent upon site conditions, equipment limitations or limitations imposed by the procedure. In allinstances, the ultimate procedures employed should be documented and associated with the final report.

Mention of trade names or commercial products does not constitute United States Environmental ProtectionAgency (U.S. EPA) endorsement or recommendation for use.

2.0 METHOD SUMMARY

When collecting gaseous samples for analysis it is often necessary to obtain a representative grab sample ofthe media in question. The Tedlar® bag collection system allows for this and consists of the following items:

C Tedlar® bag, complete with necessary fittingsC Vacuum boxC Vacuum pump(s)C Teflon® and Tygon® tubing

The Tedlar® bag is placed into the vacuum box and the fitting is attached to the sampling port and Teflon®tubing. The Teflon® tubing is the path through which the gaseous media will travel. The pump is attachedto the Tygon® tubing, which is connected to the vacuum fitting on the vacuum box. The pump evacuates theair in the vacuum box, creating a pressure differential that causes the sample to be drawn into the bag. Thesample introduced into the Tedlar® bag never passes through the pump. The flow rate for the pump must bedefined prior to sampling (usually 1 liters/minute [LPM] for bag sampling).


Tedlar® bags most commonly used for sampling have a 1-liter volume capacity. After sampling, the Tedlar®bags are stored in either a clean cooler or an opaque plastic bag at ambient temperature to preventphotodegradation. It is essential that sample analysis be undertaken within 24-48 hours following samplecollection since VOCs may escape or become altered.

4.0 INTERFERENCES AND POTENTIAL PROBLEMS

Contamination is a major concern since many of the compounds in question will be present in the parts per





billion range. In order to minimize the risk of cross contamination, the following factors should be considered:

1. Proximity of the bags to sources of potential contamination during transportation and storage. Thefurther away from the source(s) the bags are, the less likely the chances of external contamination.

2. Bags must be attached only to clean Teflon® tubing.

3. Once the bag has been collected, affix the sample label to the edge of the bag. Adhesives found inthe label may permeate the bag if placed on the body of the bag. Fill out labels with a ballpoint penas permanent markers contain volatile compounds that may contaminate the sample.

4. Due to the chemical structure of Tedlar®, highly polar compounds will adhere to the inner surface ofthe bag. Also, low molecular weight compounds may permeate the bag. Real-time monitors such asthe organic vapor analyzer (OVA), photoionization detector (HNu), and combustible gas indicator(CGI) may be used as screening devices prior to sampling. This information is documented on thesample label to assist individuals performing the sample analysis.

The Tedlar® bag sampling system is straightforward and easy to use. However, there are several things to beaware of when sampling.

1. The seal between the top half and the bottom half of the vacuum box must be air tight in order to allowthe system to work.

2. Check the O-ring gasket to see if it is in place with the proper fit. O-rings that have been stretched outwill not remain in place, thus requiring constant realignment.

3. Check that all the fittings associated with the vacuum joints are securely in place. The fittings can bepushed loose when inserting the valve stem into the Teflon tubing.

4. Occasionally, a corner of the Tedlar® bag will jut out between the two halves of the vacuum box, thusimpairing the seal. Since the bags will hold only a given volume, over-inflation will cause the bags toburst.


C Vacuum boxC Vacuum pumpsC Teflon® tubingC O-ringsC Tedlar® bagsC Chain of custody records and custody sealsC Sample collection documentation (sample labels, air sampling worksheets, logbooks)





C Large opaque plastic bagsC Ultra-zero air

6.0 REAGENTS


7.0 PROCEDURES

7.1 Preparation

1. Determine the extent of the sampling effort, the sampling methods to be employed, and thetypes and amounts of equipment and supplies needed.

2. Obtain necessary sampling and monitoring equipment.

3. Decontaminate or pre-clean equipment, and ensure that it is in working order.

4. Prepare scheduling and coordinate with staff, clients, and regulatory agency, if appropriate.

5. Perform a general site survey prior to site entry in accordance with the site specific Healthand Safety Plan. Prior to selecting sample locations, an underground utility search must becompleted. The local utility companies can be contacted to mark the locations of theunderground lines. Request the homeowner to mark any underground sprinklers, if present.

6. Use stakes or flagging to identify and mark all sampling locations. If required, the proposedlocations may be adjusted based on site access, property boundaries, and surfaceobstructions.

7.2 Field Operations

Tedlar® bags are stored in boxes of ten. The valve is in the open position when stored. Occasionally,a piece of debris will clog the valve, necessitating the closing of the valve stem to clear. The valvestem is closed by pulling the stem out. If the valve stem is difficult to pull, it helps to spin the valvestem simultaneously.

1. Remove the Tedlar® bag from the carton.

2. Insert the valve stem into the Teflon tube which runs through the vacuum box (Figure 1,Appendix A).

3. Place the Tedlar® bag in the vacuum box. Seal the vacuum box by applying pressure to the





top and bottom (ensure that the O-ring is in place and unobstructed).

4. Connect the sampling pump to the evacuation tube.

5. Connect the intake tube to the desired source or place the intake tube into the media ofconcern.

6. Turn on the sampling pump.

7. Allow the bag to fill (visual observation and sound of laboring pump).

8. Turn off the sampling pump and remove the evacuation tube from the pump.

9. Remove bag and pull the valve stem out.

10. Lock the valve stem.

11. Label the bag using either a tag or a sticker placed on the edge of the bag. Do not write onthe bag itself. Record the date, time, sample location and any instrument readings.

12. Place Tedlar® bag in a clean cooler or opaque trash bag to prevent photodegradation.

13. When transferring the Tedlar® bags, a chain of custody form must accompany the samples.Personnel should be aware that some of the compounds of concern will degrade within a fewhours of sampling.

8.0 CALCULATIONS



9.1 General QA Procedures

1. All data must be documented on field data sheets or within site logbooks.

2. All instrumentation must be operated in accordance with operating instruction as suppliedby the manufacturer, unless otherwise specified in the work plan. Equipment checkout andcalibration activities must occur prior to sampling/operation and must be documented.

3. Depending upon the Work Plan (WP) requirements, a background sample consisting ofupgradient/downgradient, beginning/ending of day or combination, may be collected. It may





also be desirable to change sample train tubing between sample locations.

9.2 Field Blanks

A field blank detects contamination during the handling and shipping process. The field blank mustbe associated with an actual sampling event. For each day of sampling not to exceed 20 samples, aTedlar® bag is filled with ultra-zero air at the beginning of the day. The field blank is handled in thesame manner as the samples.

9.3 Trip Blanks

Each cooler containing Tedlar® bag samples must contain one Tedlar® bag of ultra-zero air, actingas a trip blank, when samples are shipped to an outside laboratory. A chain of custody record mustaccompany each cooler of samples and should include the blank that is dedicated to that group ofsamples.

9.4 Lot Blanks

For each lot of Tedlar® bags, a minimum of one bag must be filled with ultra-zero air and analyzed forthe parameter(s) of interest. This procedure will ensure cleanliness prior to the start of he samplingeffort.

9.5 Duplicate Samples

A minimum of 5% should be collected in duplicate.


Results of the quality control samples (trip and lot blanks) will be evaluated for contamination. This informationwill be utilized to qualify the environmental sample results according to the project's data quality objectives.


When working with potentially hazardous materials, follow U.S. EPA, Occupational Safety and HealthAdministration (OSHA), and corporate health and safety procedures.

12.0 REFERENCES

Gilian Instrument Corporation. 1983. Instruction Manual for Hi Flow Sampler:HFS113, HFS113T, HFS113U,HFS113UT.





New Jersey Department of Environmental Protection. 1992. Field Sampling Procedures Manual. HazardousWaste Programs.

United States Environmental Protection Agency. 1995. Superfund Program Representative SamplingGuidance. Volume 2: Air (Short-Term Monitoring). EPA 540-R-95/140. Interim Final.

United States Environmental Protection Agency. 1984. Characterization of Hazardous Waste Sites - A MethodsManual: Volume II. Available Sampling Methods. 2nd ed. EPA-600/4-84-076.

13.0 APPENDICES

A - Figure





APPENDIX AFigure

SOP #2102September 2001





1

SOP#: 2103DATE: 10/24/94

REV. #: 0.0 CHARCOAL TUBE SAMPLING

IN AMBIENT AIR


The purpose of the Standard Operating Procedure(SOP) is to define the procedure for charcoal tubesampling which is utilized to identify specificcontaminants in ambient air. The greatest selectivityof activated charcoal is towards non-polar organicsolvent vapors, (e.g., carbon tetrachloride,chlorobenzene and toluene). Organic compounds thatare gaseous at room temperature, reactive, polar, oroxygenated (aldehyde alcohols and some ketones), areeither not adsorbed (relatively early breakthrough), orinefficiently desorbed.



2.0 METHOD SUMMARY

Charcoal tube sampling is performed by drawing a humidity may cause a decrease in the adsorptionknown volume of air through a charcoal adsorption capacity of activated carbon. Contaminants from thetube. As air is drawn through the tube during front portion of the tube may migrate to the backsampling, gases and vapors adsorb onto the surface of portion of the tube. Refrigeration may minimize thisthe charcoal. After sampling, the tubes are delivered migration.to the laboratory for analysis.

3.0 SAMPLE PRESERVATION,CONTAINERS, HANDLING, 5.1 Equipment ListAND STORAGE

Charcoal used for sampling is housed in a glass tubethat has been flame sealed. Charcoal tubes most oftenused contain 150 mg or 600 mg of charcoal. Thesmaller 150-mg tube is 7-cm long with a 4-mm inner

diameter (ID) and a 6-mm outer diameter (OD)containing two sections of 20/40 mesh activatedcharcoal separated by urethane foam. The adsorbingsection contains 100-mg of charcoal, the backupsection 50-mg of charcoal. The larger 600-mg tube is11-cm long with a 6-mm ID and a 8-mm ODcontaining two sections of 20/40 mesh activatedcharcoal separated by urethane foam. The adsorbingsection contains 400 mg of charcoal, the backupsection contains 200-mg of charcoal. A greatervolume of air can be drawn through the larger tubethereby providing a greater sensitivity.

To preserve and store samples:

1. Place plastic caps on the charcoal tube ends.2. Place the sample in a whirl bag. If

collocated samples have been collected,place both tubes in one whirl bag.

3. If the sample tube must be stored for morethan a week, refrigeration is recommended.Maximum recommended holding time is twoweeks.


Low sampling flow rates, and high temperature and

5.0 EQUIPMENT

C Personal Sampling PumpC Dowel RodsC Single or Dual Rotameter (with stand and

desired precalibrated flow rate)C Charcoal Tubes (600 mg or 150 mg)

2

C Tygon Tubing (for attaching the tube holder 6. Use stakes, flagging tape, or othersystem to the suction side of the pump) appropriate means to identify and mark all

C Sleeves (or support tubes to hold tubes in sampling locations. If required, the proposedplace) locations may be adjusted based on site

C Single or Dual Manifold Flow Controller access, property boundaries, and surfaceC Tube Holder End (to support and seal the obstructions.

sampling tube within the plastic housing)C Glass Tube CrackerC Resealable BagsC Whirl BagsC Plastic End CapsC Air Sampling Worksheets and Sample LabelsC Chain of Custody RecordsC Screwdriver Set

5.2 Equipment Source

Tubes are commercially available from SKC, Inc. and system (sleeve and tube holder end), and afrom Mine Safety Appliance Co., both of Pittsburgh, calibration tube. The calibration tube is aPennsylvania. representative tube from the same lot of

SKC: 1-800-752-8472Mine Safety Appliance Co.: 1-800-MSA-2222 2. Turn on the pump and adjust the flow using

6.0 REAGENTS


7.0 PROCEDURES

7.1 Preparation


2. Obtain and organize the necessary samplingand monitoring equipment.

3. Decontaminate or pre-clean equipment, andensure that it is in working order.Precalibrate sampling pumps as described inSection 7.2.

4. Prepare scheduling and coordinate with staff,client, and regulatory agency, if appropriate.

5. Perform a general site survey prior to siteentry, in accordance with the site specificHealth and Safety Plan.


To save time in the field, sampling pumps can beprecalibrated in the office prior to arriving at the site.The calibration must be checked in the field prior to,and upon completion of sampling.

1. Assemble the calibration train as shown inFigure 1 (Appendix A), using a rotameter,sampling pump, manifold (only if the desiredflow rate is below 750 cc/min), a tube holder

tubes that is used for sampling.

the flow adjust mechanism on the manifold(if used) or on the pump itself until the floatball on the rotameter is aligned with therotameter's precalibrated flow rate value. Asticker on the rotameter should indicate thisvalue.

3. Affix a sticker to the manifold (if used) andpump indicating the precalibrated flow rateand sampling media.

4. Remove the calibration tube from the sleeve.The pump and manifold (if used) arecalibrated as a unit and should not beseparated until the samples have beencollected.

7.3 Field Operation

1. Mobilize to the clean zone and calibrate theappropriate number of sampling pumps asdescribed in Section 7.2. If the pumps wereprecalibrated, the calibration should bechecked in the same manner. Fine tuning ofthe flow may be required.

2. Mobilize to the sampling location.

3. Crack the charcoal tube ends using a glasstube cracker.

3

4. Insert the charcoal tube in the sleeve with immediately after sampling. Never usearrow pointing in the direction of air flow rubber caps.(the smaller section is used for a backup andis positioned nearest the sampling pump). 4. Place the sample in a whirl bag labeled with

5. Screw the tip onto the sleeve so the charcoal analysis. If collocated samples have beentube is held in place. collected, place each tube in a separate whirl

6. Attach the sleeve(s) to a single or double tube.manifold. At higher flow rates (>750cc/min), charcoal tubes can run straight 5. Indicate all applicable information on the Airwithout a manifold. Sampling Worksheet (e.g., sample volume,

7. To set up the sampling train, attach one end parameters).of the Tygon tubing (approx. 2 foot) to the tipof the sleeve or manifold. Attach the other 6. If the sample tube must be stored for moreend of the tubing to the inlet plug on the than a week, refrigeration is recommended.pump, Figure 2 (Appendix A). Refer toFigures 3 and 4 (Appendix A), respectively, 7. Prepare samples, including QC samples, forfor illustrations of sampling trains without a transport by packing them in a shippingmanifold and with a dual manifold (for container with bubble wrap or styrofoamcollocated samples). pieces. Complete a Chain of Custody record

8. Adjust time on the pump to the required Custody Procedures.sample time.

9. Place the charcoal tube in a position free analysis of charcoal tubes: NIOSH Methods 1501,from obstruction on a dowel rod or stand. Aromatic Hydrocarbons; 1500, Hydrocarbons BP

10. Record weather data (e.g., ambient Other analytical parameters may be required. Thetemperature, barometric pressure, relative appropriate analytical methodology should behumidity, and wind direction) on the Air determined prior to field activities.Sampling Worksheet or in the logbook.

11. Turn on the pump.

12. After the pump has run the full time, checkthe fault button to determine if the pump ranfor the scheduled time.

13. Verify calibration by connecting a rotameterwith Tygon tubing and turning on the pump.Record the final flow rate on the AirSampling Worksheet.

7.4 Post Operation Procedures

1. Record the sampling time on the AirSampling Worksheet.

2. Remove the charcoal tube from the sleeve.

3. Cap charcoal tubes with plastic caps

sample ID#, total volume, and required

bag and assign a unique sample ID # to each

ID #, location, date, and weather

in accordance with appropriate Chain of

The following methods are typically used for the(1,2,3)

36E-126EC; and 1003, Halogenated Hydrocarbons.

8.0 CALCULATIONS

The total volume of a sample is calculated bymultiplying the total sample time by the flow rate.The total volume for each sample should be indicatedon the Chain of Custody record.


The following general QA procedures apply:

1. All data must be documented on AirSampling Worksheets or within sitelogbooks.

2. All instrumentation must be operated inaccordance with operating instructions as

4

supplied by the manufacturer, unlessotherwise specified in the work plan.Equipment checkout and calibrationactivities must occur prior tosampling/operation and they must bedocumented.

The following specific QC activities apply:

1. Provide one field blank per sampling event orper 20 samples, whichever is greater. Thefield blank should be handled in the samemanner as the sampling tube (break, seal, andtransport) except that no air is drawn throughit.

2. Collect one collocated sample per samplingevent or per 10 samples, whichever isgreater. Collocated samples are two samplescollected adjacent to each other during thesame time period at the same flow rates.

3. Include a minimum of one lot blank tube permanufacturer's lot of tube utilized persampling event. These tubes are takendirectly from the charcoal tube box. Do notbreak the ends.


Results of the quality control samples will beevaluated for contamination. This information will beutilized to qualify the environmental sample resultsaccordingly with the project's data quality objectives.


When working with potential hazardous materials,follow U.S. EPA, OSHA and corporate health andsafety procedures.

Specific hazards unique to charcoal tube samplinginclude:

1. Sharp edges associated with the tubes afterthey have been "cracked."

2. Walking and working surfaces, as well aspossible heights, associated with access tosampling locations.

12.0 REFERENCES

Eiler, Peter M., ed. NIOSH Method 1501,(1)

Aromatic Hydrocarbons. In: NIOSHManual of Analytical Methods, ThirdEdition, U.S. Gov.'t Printing Office,Washington, D.C., 1987. p. 1501-1.


Hydrocarbons, BP 36-126EC. In: NIOSHManual of Analytical Methods, ThirdEdition, U.S. Gov.'t Printing Office,Washington, D.C., 1987. p. 1500-1.


Halogenated Hydrocarbons. In: NIOSHManual of Analytical Methods, ThirdEdition, U.S. Gov.'t Printing Office,Washington, D.C., 1987. p. 1003-1.

5

APPENDIX A

Figures

FIGURE 1. Calibration Train

6


Figures

FIGURE 2. Charcoal Tube Sampling Train (Single Manifold)

7


Figures

FIGURE 3. Charcoal Tube Sampling Train (No Manifold)

8


Figures

FIGURE 4. Charcoal Tube Sampling Train (Dual Manifold for Collocated Sampling)

1

SOP#: 2104DATE: 10/19/94

REV. #: 0.0 TENAX/CMS TUBE SAMPLING


The purpose of this Standard Operating Procedure(SOP) is to define the procedure for air samplingusing Tenax/Carbonized Molecular Sieve (CMS)tubes which identify specific contaminants in air.Compounds that can be determined by Tenax are non-polar organics having boiling points in the range ofapproximately 80E-100EC. Compounds which can bedetermined by CMS are non-polar and non-reactiveorganics having boiling points in the range 15EC to120EC. However, not all compounds falling into thesecategories can be determined. Table 1 (Appendix A)lists many of the compounds which can be detectedusing Tenax/CMS. Analysis is performed by thermaldesorption into a gas chromatograph/massspectrometer (GC/MS).



2.0 METHOD SUMMARY

Tenax/CMS tube sampling is performed by drawing aknown volume of air through a Tenax absorbentfollowed by a CMS adsorbent. Volatile organiccompounds are captured on the adsorbent while majorinorganic atmospheric constituents pass through or areonly partially retained. After sampling, the tube isreturned to the laboratory for analysis using U.S. EPAMethods TO1 and TO2.


Tenax/CMS tubes contain a granular inert chemicalcompound with adsorbent properties. A flame-sealedouter glass tube protects the inner tube fromcontamination. This outer glass tube must be brokenand the Tenax/CMS tube must be removed prior tosampling. The Tenax/CMS tube is 6.0 mm outsidediameter (O.D.) and 4 mm inside diameter (I.D.)containing one section of 150-mg Tenax, 35/60 meshand one section of 150-mg CMS 60/80 mesh.

After sampling is complete, the Tenax/CMS tubes arestored in culture tubes. Therefore, prior to site work,the culture tubes should be cleaned and prepared usingthe following procedure:

1. A plug of precleaned glass wool (methanolrinsed, baked in an oven at 120EC) is placedin the bottom of each tube.

2. The culture tubes are placed in an oven for atleast two hours at 120EC. The Teflon linedcaps are not baked.

3. The culture tubes are removed from the ovenand allowed to cool.

4. The culture tubes are placed in a resealablebag or whirl bag.

Refrigerate the samples and keep out of sunlight.Storage for more than four weeks is notrecommended.


Contamination of the Tenax/CMS tubes with thecompound(s) of interest is a common problem. Tominimize this problem, the user must be extremely

2

careful in the preparation, storage, and handling of the supplies needed.tube throughout the sampling and analysis process.To avoid contamination from skin oils, a lint-free 2. Obtain and organize the necessary samplingglove must be used when handling Tenax/CMS tubes. and monitoring equipment.


5.1 Equipment List

C Calibrated personal sampling pumpC Dual rotameter with stand and precalibrated

flow rateC Tenax/CMS tubes, preferably of the same lot

numberC Flexible tygon tubing (for attaching the tube

holder system to the suction side of thepump)

C Universal tube holder system- Dual variable manifold flow controller- Tube holder end with rubber boot adaptor- Sleeves - clear plastic housings

C Glass crackerC Lint-free glovesC Glass woolC Teflon tapeC Culture tubesC ScrewdriversC Resealable bagsC Whirl bagsC Air Sampling WorksheetsC Chain of Custody records

5.2 Equipment Sources

Tenax/CMS tubes may be obtained from Supelco Inc.,Bellefonte, PA, at (800) 247-6628; Technical Service(814) 359-3441 and MSA, 1-800-MSA-2222.

6.0 REAGENTS

Methanol is used in the laboratory to clean the culturetubes which hold the Tenax/CMS samples. This isperformed prior to site work.

7.0 PROCEDURES

7.1 Preparation indicating the calibrated flow rate and media.

1. Determine the extent of the sampling effort,the sampling methods to be employed, andthe types and amounts of equipment and

3. Decontaminate or pre-clean equipment, andensure that it is in working order.Precalibrate sampling equipment, if possible.


5. Perform a general site survey prior to siteentry in accordance with the site-specificHealth and Safety Plan.

6. Use stakes, flagging tape, or otherappropriate means to mark all samplinglocations. If necessary, the proposedlocations may be adjusted based on siteaccess, property boundaries, and surfaceobstructions.


Assemble the calibration train as shown in Figure 1(Appendix B) using a dual rotameter, sampling pump,dual manifold, and representative Tenax/CMS tubes.The same lot number of Tenax/CMS tubes are usedfor both sampling and calibration.

1. Adjust the sampling pump to the low flowmode.

2. Remove the cap ends on the flow controllermanifold. To adjust the flow, turn the needlevalve with a small screwdriver(counter-clockwise to increase, clockwise todecrease).

3. Turn the flow adjust screw on each manifolduntil the float ball on the rotameter is linedup with the precalibrated flow rate value. Asticker on the rotameter should indicate thisvalue.

4. Affix a sticker to the manifold and pump

5. Remove the representative Tenax/CMS tubesfrom the sleeves.

3

The pump and manifold (including boots) arecalibrated as a unit and should not be separated untilthe samples have been collected. See Table 2(Appendix A) for recommended flow rates and samplevolumes.

7.3 Field Operation

1. Calibrate the appropriate number of pumps Sampling Worksheet.with manifolds as described in Section 7.2.If the pumps were precalibrated, the 3. Remove the Tenax/CMS tubes from sleevescalibration should be checked in the same using a lint-free cloth or gloves.manner. Fine tuning of the flow may berequired. 4. Place the Tenax/CMS tubes in a culture tube.

2. Crack the outer glass tubes using a glass from the same manifold and identical flowcracker. rates must be placed in the same culture tube.

3. Use a clean, lint-free cloth or gloves to 5. Place a sample sticker indicating sample ID#remove the Tenax/CMS tubes from the outer on the culture tube. Do not put a sampleglass housings. sticker on the Tenax/CMS tube itself as this

4. Insert the Tenax/CMS tubes into a boot, with will contaminate the tube.the CMS sections closest to the manifold.

5. Attach protective sleeves over the tubes. Do lid/tube interface with Teflon tape.not enclose the Tenax/CMS tube ends.

6. Set up the sampling train, by attaching one or a whirl bag.end of the Tygon tubing (approx. two feet) tothe manifold; and the other end to the inlet 8. Keep the samples refrigerated and out ofplug on the pump (Appendix B, Figure 2). sunlight. Storage for more than four weeks

7. Place the sampling tubes in the breathingzone. The pump and tubes can be placed on 9. Prepare the samples, including QC samples,a drum or hooked to a fence. A wooden for transport by packing them in shippingdowel rod can also be used. containers with bubble wrap or styrofoam

8. Place the tubes in either a vertical or in accordance with the appropriate Chain ofhorizontal position. Custody Procedures.

9. Adjust the pump time.

10. Turn on the pump.

11. Record weather data (e.g., ambienttemperature, barometric pressure, relativehumidity and wind direction) on the AirSampling Worksheet.

12. Check the pump at the midpoint of thesampling period if longer than four hours.

7.4 Post-Operation Procedures

1. At the end of the sampling period, record therun time on the Air Sampling Worksheet.

2. Check the flow rate by attaching a rotameterwith Tygon tubing and turning the pump on.Record the final flow rate on the Air

Pack with glass wool. Tenax/CMS tubes

6. Attach the culture tube lid and wrap the

7. Place the culture tubes into a resealable bag

is not recommended.

pieces. Complete a Chain of Custody record

8.0 CALCULATIONS

The total volume of a sample is calculated bymultiplying the total sample time by the flow rate.The total volume for each sample should be indicatedon the Chain of Custody record.


The following general QA procedures apply:

4




1. Provide one field blank per 20 samples. Thistube is handled in the same manner as asampling tube (break, seal, and transport),except that no air is drawn through this tube.

2. Provide a minimum of one lot blank tube persampling episode. These tubes are takendirectly from the Tenax/CMS tube box. Donot break the outer glass housing. Place in aresealable bag and keep with other samples.

3. All sample stations should have duplicatesample tubes.


Results of the quality control samples will beevaluated for contamination. This information will beutilized to qualify the environmental sample resultsaccordingly with the project's data quality objectives.


When working with potential hazardous materials,follow U.S. EPA, OSHA and corporate health andsafety procedures.

Specific hazards associated with Tenax/CMS tubesampling include:

1. Small pieces of glass flying during"cracking" of the tube.

2. Access to sampling locations.

3. Environmental contaminants being sampled.

12.0 REFERENCES

U.S. EPA, Compendium of Methods forDetermination of Toxic Organic Compounds inAmbient Air, EPA 600/4-84/041, December, 1984.

U.S. EPA, Characterization of Hazardous WasteSites - A Methods Summary: Volume II, AvailableSampling Methods, 2nd Edition, EPA 600/4-84/76,December, 1984.

5

APPENDIX A

Tables

TABLE 1. Air Analysis by GC/MS

Compound

Vinyl ChlorideTrichlorofluoromethane1,1-DichloroetheneMethylene ChlorideTrans-1,2-Dichloroethene1,1-DichloroethaneBromochloromethane(1)

1,1,1-TrichloroethaneCarbon TetrachlorideBenzene1,2-DichloroethaneTrichloroethyleneTolueneTetrachloroethyleneEthylbenzenem-Xyleneo-XyleneStyrenep-BromofluorobenzeneMeta-Ethyltoluene1,1,2,2-Tetrachloroethane1,1,2-TrichloroethaneDibromomethaneTrichloromethaneBromodichloromethaneChloroethaneChloromethane

Surrogate - Surrogates are injected into the Tenax/CMS tube to determine adsorption(1)

efficiencies.

6


Tables

TABLE 2. Recommended Flow Rates and Sample Volumes

Flow Rates

Maximum 50 cc/minOptimal 30-40 cc/minMinimum 10 cc/min

Volumes

Maximum 5 litersOptimal 2 litersMinimum 0.5 liters

7

APPENDIX B

Figures

FIGURE 1. Tenax/CMS Calibration Train

8


Figures

FIGURE 2. Tenax/CMS Sampling Train

1

SOP#: 2114DATE: 10/06/94

REV. #: 0.0 PHOTOIONIZATION

DETECTOR (PID) HNU


The purpose of this Standard Operating Procedure(SOP) is to describe the procedure for using aphotoionization detector (PID). The PID is a portable,nonspecific, vapor/gas detector employing theprinciple of photoionization to detect a variety ofchemical compounds, both organic and inorganic, inair. This procedure is applicable to the HNU PI-101,HNU ISPI-101, and HW-101 used for air monitoring.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, dependent on site conditions, equipmentlimitations or limitations imposed by the procedure.In all instances, the ultimate procedures employedshould be documented and associated with the finalreport.


2.0 METHOD SUMMARY

The PID is a useful general survey instrument athazardous waste sites. A PID is capable of detectingand measuring real-time concentrations of manyorganic and inorganic vapors in air. A PID is similarto a flame ionization detector (FID) in application;however, the PID has somewhat broader capabilitiesin that it can detect certain inorganic vapors.Conversely, the PID is unable to respond to certainlow molecular weight hydrocarbons, such as methaneand ethane, that are readily detected by FIDinstruments.

The PID employs the principle of photoionization.The analyzer will respond to most vapors that have anionization potential less than or equal to that suppliedby the ionization source, which is an ultraviolet (UV)lamp. Photoionization occurs when an atom ormolecule absorbs a photon of sufficient energy to

release an electron and form a positive ion. This willoccur when the ionization potential of the molecule inelectron volts (eV) is less than the energy of thephoton. The sensor is housed in a probe and consistsof a sealed ultraviolet light source that emits photonswith an energy level high enough to ionize many traceorganics, but not enough to ionize the majorcomponents of air (e.g., nitrogen, oxygen, carbondioxide). The ionization chamber exposed to the lightsource contains a pair of electrodes, one a biaselectrode, and the second the collector electrode.When a positive potential is applied to the biaselectrode, an electro-magnetic field is created in thechamber. Ions formed by the adsorption of photonsare driven to the collector electrode. The currentproduced is then measured and the correspondingconcentration displayed on a meter, directly, in unitsabove background. Several probes are available forthe PID, each having a different eV lamp and adifferent ionization potential. The selection of theappropriate probe is essential in obtaining useful fieldresults. Though it can be calibrated to a particularcompound, the instrument cannot distinguish betweendetectable compounds in a mixture of gases and,therefore, indicates an integrated response to themixture.

Three probes, each containing a different UV lightsource, are available for use with the HNU. Energiesare 9.5, 10.2, and 11.7 eV. All three detect manyaromatic and large molecular hydrocarbons. The 10.2eV and 11.7 eV probes, in addition, detect somesmaller organic molecules and some halogenatedhydrocarbons. The 10.2 eV probe is the most usefulfor environmental response work, as it is more durablethan the 11.7 eV probe and detects more compoundsthan the 9.5 eV probe.

Gases with ionization potentials near to or less thanthat of the lamp will be ionized. These gases will thusbe detected and measured by the analyzer. Gases withionization potentials higher than that of the lamp willnot be detected. Ionization potentials for variousatoms, molecules, and compounds are given in

2

Table 1 (Appendix A). The ionization potential of the 5. Certain models of PID instruments are notmajor components of air, oxygen, nitrogen, and carbon intrinsically safe. The HNU PI-101 anddioxide, range from about 12.0 eV to about 15.6 eV HW-101 are not designed for use inand are not ionized by any of the three lamps. potentially flammable or combustible

Table 2 (Appendix A) illustrates ionization should be used in conjunction with asensitivities for a large number of individual species Combustible Gas Indicator. The ISPI-101 iswhen exposed to photons from a 10.2 eV lamp. intrinsically safe, however.Applications of each probe are included in Table 3(Appendix A). 6. Electrical power lines or power transformers

While the primary use of the HNU is as a quantitative and thus cause measurement errors. Staticinstrument, it can also be used to detect certain voltage sources such as power lines, radiocontaminants, or at least to narrow the range of transmissions, or transformers may alsopossibilities. Noting instrument response to a interfere with measurements.contaminant source with different probes caneliminate some contaminants from consideration. For 7. High winds and high humidity will affectinstance, a compound's ionization potential may be measurement readings. The HNU maysuch that the 9.5 eV probe produces no response, but become unusable under foggy or humidthe 10.2 eV and 11.7 eV probes do elicit a response. conditions. An indication of this is the



4.0 INTERFERENCES ANDPOTENTIAL PROBLEMS about 1-2000 ppm, although the response is

4.1 PID Instrument Limitations

1. The PID is a nonspecific total vapor detector.It cannot be used to identify unknownsubstances; it can only roughly quantifythem.

2. The PID must be calibrated to a specificcompound.

3. The PID does not respond to certain lowmolecular weight hydrocarbons, such asmethane and ethane. In addition, the HNUdoes not detect a compound if the probe hasa lower energy than the compound'sionization potential.

4. Certain toxic gases and vapors, such ascarbon tetrachloride and hydrogen cyanide,have high ionization potentials and cannot bedetected with a PID.

atmospheres. Therefore, these models

may cause interference with the instrument

needle dropping below zero, or a slowconstant climb on the read-out dial.

8. The lamp window must be periodicallycleaned to ensure ionization of the newcompounds by the probe (i.e., new aircontaminants).

9. The HNU measures concentrations from

not linear over this entire range. Forexample, if calibrated to benzene, theresponse is linear from about 0-600 unitsabove background. This means the HNUreads a true concentration of benzene onlybetween 0 and 600. Greater concentrationsare detected at a lower level than the truevalue.

10. This instrument is not to be exposed toprecipitation (rain). The units are notdesigned for this service.

11. Do not use this instrument for head spaceanalysis where liquids can inadvertently bedrawn into the probe.

4.2 Regulatory Limitations

Transport of calibration gas cylinders by passengerand cargo aircraft must comply with International AirTransport Association (IATA) Dangerous Goods

3

Regulations or the U.S. Code of Federal Regulations,49 CFR Parts 100-177. A typical calibration gasincluded with a PID is isobutylene. It is classified asa non-flammable gas, UN #1556 and the propershipping name is Compressed Gas. It must be shippedby cargo aircraft only.


The following equipment is required for PIDoperation:

C PID (HNU)C Operating manualC Probes: 9.5 eV, 10.2 eV, or 11.7 eVC Battery charger for PIDC Spare batteriesC Jeweler's screwdriver for adjustmentsC Tygon tubingC NBS traceable calibration gasC "T" valve for calibrationC Field Data Sheets/Site LogbookC Intake assembly extensionC Strap for carrying PIDC Teflon tubing for downhole measurementsC Plastic bags for protecting the PID from

moisture and dirt

Note: Battery charge status - This instrument may bekept on continuous charge without battery damage.

6.0 REAGENTS

C Isobutylene standards for calibrationC Benzene reference standardC Methanol for cleaning ionization chamber

(GC grade)C Mild soap solution for cleaning unit surfacesC Specific gas standards when calibrating to a

specific compoundC Light source cleaning compound Cat. No.

PA101534-A1 (For use only with 9.5 and10.2 lamps)

The HNU is calibrated in accordance with theoperations manual using isobutylene as the calibrationstandard. The operations manual may also be referredto for alternate calibration to a specific compound.

7.0 PROCEDURES

7.1 Preparation

Check out and ensure the proper operation of the PID,as appropriate, using the equipment checklist providedin Sections 5.0 and 6.0 and the steps listed below.

7.2 Start-Up Procedures

1. Allow the temperature of the unit toequilibrate to its surrounding. This shouldtake about five minutes.

2. Attach the probe to the read-out unit. Matchthe alignment key, then twist the connectorclockwise until a distinct locking is felt.Make sure the microswitch (red button) isdepressed by the locking ring.

3. Turn the FUNCTION switch to the batterycheck position. Check to ensure that theindicator reads within or beyond the greenbattery arc on the scale plate. If the indicatoris below the green arc, or if the red LEDcomes on, the battery must be charged priorto using.

4. To zero the instrument, turn the FUNCTIONswitch to the STANDBY position and rotatethe ZERO POTENTIOMETER until themeter reads zero. Wait 15-20 seconds toensure that the zero adjustment is stable; ifnot, then readjust.

5. Check to see that the SPANPOTENTIOMETER is set at the appropriatesetting for the probe being used (i.e., 9.8 forthe 10.2 eV probe, 5.0 for the 11.7 eV probe,1 for the 9.5 eV probe. Note: The settingmay vary based on the intensity of the lightsource).

6. Set the FUNCTION switch to the desiredrange (i.e., 0-20, 0-200, 0-2000).

7. Listen for the fan operation to verify fanfunction.

4

8. Look for ultraviolet light source in the probe 6. Record the following information in the siteto verify function. Do not look at light logbook: the instrument ID number (U.S.source from closer than six inches with EPA decal or serial number if the instrumentunprotected eyes, observe only briefly. is a rental), the initial and final span settings,

9. Check instrument with an organic point calibration gas used, and the name of thesource, such as a magic marker, prior to person who field calibrated the instrument.survey to verify instrument function.

10. Routinely during the day, verify the useful calibrate properly, the instrument should notbattery life by turning the function switch to be used. Under no circumstances is workBATT and schedule the instrument's use requiring air monitoring with a PID to beaccordingly. done without a proper functioning

7.3 Field Operation

7.3.1 Field Calibration

1. Follow the start-up procedure in Section 7.2.

2. Set the FUNCTION switch to the rangesetting which includes the concentration ofthe calibration gas.

3. Attach a regulator to a disposable cylinder ofcalibration gas. Connect the regulator to theprobe of the HNU with a piece of cleantygon tubing. Open the valve on theregulator.

4. After 15 seconds, the meter reading shouldequal the response value as indicated on thecalibration gas cylinder used. If the readingis within ±15% of the response value, thenthe instrument can be field calibrated to theresponse value using the external SPANADJUSTMENT control. The SPANADJUSTMENT control should be adjustedto a lower setting until the correct readinghas been obtained. The lower the number onthe SPAN ADJUSTMENT conrol, thegreater the instrument sensitivity. If theSPAN ADJUSTMENT control has to beadjusted below a setting of 4.00, the unitshould be red-tagged and returned for repairs.

5. If the meter reading is greater than ±15% ofthe response value of the calibration gasused, then the instrument should be red-tagged and returned for re-calibration.

the date and time, concentration and type of

7. If the PID does not start up, check out, or

instrument.

8. In some field applications, with the exceptionof the probe's inlet and exhaust, the PIDshould be wrapped in clear plastic to preventit from becoming contaminated and toprevent water from getting inside in the eventof precipitation.

7.3.2 Operation

1. All readings are to be recorded in the sitelogbook. Readings should be recorded,following background readings, as "unitsabove background," not ppm.

2. As with any field instrument, accurate resultsdepend on the operator being completelyfamiliar with the operator's manual. Theinstructions in the operating manual shouldbe followed explicitly in order to obtainaccurate results.

3. Position the probe assembly close to the areato be monitored because the low samplingrate allows for only very localized readings.Under no circumstances should the probe tipassembly be immersed in fluid.

4. While taking care to prevent the PID frombeing exposed to excessive moisture, dirt, orcontamination, monitor the work activity asspecified in the site Health and Safety Plan.The PID survey should be conducted at aslow to moderate rate of speed and the intakeassembly (the probe) slowly swept from sideto side. There is a three to five second delayin read-out depending upon the instrumentssensitivity to the contaminant.

5

5. During drilling activities, PID monitoring is concentration, an internal calibration isperformed at regular intervals downhole, at necessary. Unlock the SPANthe headspace, and in the breathing zone. In POTENTIOMETER dial before adjusting it.addition, where elevated organic vapor levels Adjust the SPAN POTENTIOMETER to theare encountered, monitoring may be span setting recommended for the probeperformed in the breathing zone during actual being used (i.e., 9.8 for the 10.2 eV probe,drilling. When the activity being monitored 5.0 for the 11.7 eV probe, 1 for the 9.5 eVis other than drilling, readings should probe). To calibrate the instrument, unscrewemphasize breathing zone conditions. the bottom support screw and lift the

6. When the activity is completed or at the end the trimpot "R-32" (near the top of theof the day, carefully clean the outside of the printed circuit board) by inserting a smallPID with a damp disposable towel to remove screwdriver and gently turning. When theany visible dirt. instrument gives the correct reading for the

7.4 Post Operation

1. Turn FUNCTION Switch to OFF.

2. Return the PID to a secure area and check thecalibration (Section 7.3.1.) before charging.Connect the instrument to charger and plugin the charger. The probe must be connectedto the readout unit to charge the HNU.

3. Complete logbook entries, verifying theaccuracy of entries and signing/initialing allpages. Following completion of a series of"0" readings, verify the instrument isworking as in Section 7.3.1.

4. Check the equipment, repair or replacedamaged equipment, and charge thebatteries.

7.5 Equipment Calibration

1. Follow the start-up procedure in Section 7.2.

2. Set the FUNCTION switch to the rangesetting which includes the concentration ofthe calibration gas.

3. Attach a regulator to a cylinder of calibrationgas. Connect the regulator to the probe ofthe NHU with a piece of clean tygon tubing.Open the valve on the regulator.

4. After 15 seconds, the meter reading shouldequal the response value as indicated on thecalibration gas cylinder used. If the readingis greater than ±15% of the actual

instrument out of the case. Locate and adjust

calibration gas being used, reassemble it.

5. Record the following information in thecalibration logbook: the instrumentidentification number (U.S. EPA barcodenumber or serial number if the instrument isa rental), the initial and final span settings,the date and time, concentration and type ofcalibration gas used, and the name of theperson who calibrated the instrument. Affixa sticker to the instrument indicating theperson who performed the calibration, thedate of calibration, and the due date of thenext calibration.

6. Turn the FUNCTION switch to OFF andconnect the instrument to the charger. Theprobe must be connected to the readout unitto ensure that the unit accepts a charge.

8.0 CALCULATIONS

The HNU is a direct reading instrument. Readings areinterpreted as units above background rather thanppm.


There are no specific quality assurance activitieswhich apply to the implementation of theseprocedures. However, the following general QAprocedures apply:


2. All instrumentation must be operated in

6

accordance with operating instructions assupplied by the manufacturer, unlessotherwise specified in the work plan.Equipment checkout and calibrationactivities must occur prior tosampling/operation, and they must bedocumented.


This section is not applicable to this SOP. Methods Manual: Volume II, Available Sampling


When working with potentially hazardous materials,follow U.S. EPA, OSHA, or corporate health andsafety practices.

The HNU is certified by OSHA standards for use inClass 1, Division 2, Groups A, B, C, and D locations.

12.0 REFERENCES

HNU Systems, Inc. 1975. "Instruction Manual forModel PI-101 Photoionization Analyzer."

U.S. Code of Federal Regulations, 49 CFR Parts 100to 177, Transportation, revised November 1, 1985.

U.S. Environmental Protection Agency. 1984."Characterization of Hazardous Waste Sites - A

Methods, Second Edition", EPA-600/4-84-076,Environmental Monitoring Systems Laboratory,Office of Research and Development, Las Vegas,Nevada.

International Air Transport Association DangerousGoods Regulations

7

APPENDIX A

Tables

TABLE 1. Ionization Potentials

SOME ATOMS AND SIMPLE MOLECULES PARAFFINS AND CYCLOPARAFFINS

Molecule IP(Ev) Molecule IP (eV) Molecule IP (eV)

H 13.595 I 9.28 Methane 12.982

C 11.264 HF 15.77 Ethane 11.65N 14.54 HCl 12.74 Propane 11.07O 13.614 HBr 11.62 n-Butane 10.63Si 8.149 HI 10.38 I-Butane 10.57S 10.357 SO 12.34 n-Pentane 10.352

F 17.42 CO 13.79 ii-Pentane 10.322

Cl 13.01 COS 11.18 2,2-Dimethylpropane 10.35Br 11.84 CS 10.08 n-Hexane 10.182

I 10.48 N O 12.90 2-Methylpentane 10.122

H 15.426 NO 9.78 3-Methylpentane 10.082 2

N 15.580 O 12.80 2,2-Dimethylbutane 10.062 3

O 12.075 H O 12.59 2,3-Dimethylbutane 10.022 2

CO 14.01 H S 10.46 n-Heptane 10.082

CN 15.13 H Se 9.88 2,2,4-Trimethylpentane 9.862

NO 9.25 H Te 9.14 Cyclopropane 10.062

CH 11.1 HCN 13.91 Cyclopentane 10.53OH 13.18 C N 13.8 Cyclohexane 9.882 2

F 15.7 NH 10.15 Methylcyclohexane 9.852 3

Cl 11.48 CH 9.8402 3

Br 10.55 CH 12.982 4

8


Tables

TABLE 1. Ionization Potentials (Continued)

ALKYL HALIDES

Molecule IP (eV) Molecule IP (eV)

HCl 12.74 1-bromo-2-methylpropane 10.09Cl 11.48 2-bromo-2-methylpropane 9.892

CH 12.98 1-bromopentane 10.104

Methyl chloride 11.28 HI 10.38Dichloromethane 11.35 I 9.282

Trichloromethane 11.42 Methyl iodide 9.54Tetrachloromethane 11.47 Diiodomethane 9.34Ethyl chloride 10.98 Ethyl iodide 9.331,2-Dichloroethane 11.12 1-iodopropane 9.261,3-Dichloropropane 10.85 2-iodopropane 9.171-chlorobutane 10.67 1-iodobutane 9.212-chlorobutane 10.65 2-iodobutane 9.091-chloro-2-methylpropane 10.66 1-iodo-2-methylpropane 9.182-chloro-2-methylpropane 10.61 2-iodo-2-methylpropane 9.02HBr 11.62 1-iodopentane 9.19Br 10.55 F 15.72 2

Methyl bromide 10.53 HF 15.77Dibromomethane 10.49 CFCl (Freon 11) 11.773

Tribomomethane 10.51 CF Cl (Freon 12) 12.312 2

CH BrCl 10.77 CF Cl (Freon 13) 12.912 3

CHBr Cl 10.59 CHClF (Freon 22) 12.452 2

Ethyl bromide 10.29 CF Br 11.672 2

1,1-dibromoethane 10.19 CH CF Cl (Genetron 101) 11.983 2

1-bromo-2-chloroethane 10.63 CFCl CF Cl 11.992 2

1-bromopropane 10.18 CF CCl (Freon 113) 11.783 3

2-bromopropane 10.075 CFHBrCH Br 10.752

1,3-dibromopropane 10.07 CF BrCH Br 10.832 2

1-bromobutane 10.13 CF CH l 10.003 2

2-bromobutane 9.98 n-C F l 10.363 7

1-chloropropane 10.82 n-C F CH Cl 11.843 7 2

2-chloropropane 10.78 n-C F CH l 9.963 7 2

1,2-dichloropropane 10.87 CF Br 11.072 2

9


Tables


ALIPHATIC ALCOHOL, ETHER, THIOL, ALIPHATIC ALDEHYDES AND AND SULFIDES KETONES


Water 12.59 Carbon Dioxide 13.79Methyl alcohol 10.85 Formaldehyde 10.87Ethyl alcohol 10.48 Acetaldehyde 10.21n-propyl alcohol 10.20 Propionaldehyde 9.98i-propyl alcohol 10.16 n-butyraldehyde 9.86n-butyl alcohol 10.04 Isobutyraldehyde 9.74Dimethyl ether 10.00 n-valeraldehyde 9.82Diemthyl ether 9.53 Isovaleraldehyde 9.71n-propyl ether 9.27 Acrolein 10.10i-propyl ether 9.20 Crotonaldehyde 9.73Hydrogen Sulfide 10.46 Benzaldehyde 9.53Methanethiol 9.440 Acetone 9.69Ethanethiol 9.285 Methyl ethyl ketone 9.531-propanethiol 9.195 Methyl n-propyl ketone 9.391-butanethiol 9.14 Methyl i-propyl ketone 9.32Dimethyl sulfide 8.685 Diethyl ketone 9.32Ethyl methyl sulfide 8.55 Methyl n-butyl ketone 9.34Diethyl sulfide 8.430 Methyl i-butyl ketone 9.30di-n-propyl sulfide 8.30 3,3-dimethyl butanone 9.17

2-heptanone 9.33Cyclopentanone 9.26Cyclohexanone 9.142,3-butanedione 9.232,4-pentanedione 8.87

10


Tables


ALIPHATIC ACIDS AND ESTERS ALIPHATIC AMINES AND AMIDES


Carbon Dioxide 13.79 Ammonia 10.15Formic acid 11.05 Methyl amine 8.97Acetic acid 10.37 Ethyl amine 8.86Propionic acid 10.24 n-propyl amine 8.78n-butyric acid 10.16 i-propyl amine 8.72Isobutyric acid 10.02 n-butyl amine 8.71n-valeric acid 10.12 i-butyl amine 8.70Methyl formate 10.815 s-butyl amine 8.70Ethyl formate 10.61 t-butyl amine 8.64n-propyl formate 10.54 Dimethyl amine 8.24n-butyl formate 10.50 Diethyl amine 8.01Isobutyl formate 10.46 Di-n-propyl amine 7.84Methyl acetate 10.27 Di-i-propyl amine 7.73Ethyl acetate 10.11 Di-n-butyl amine 7.69n-propyl acetate 10.04 Trimethyl amine 7.82Isopropyl acetate 9.99 Triethyl amine 7.50n-butyl acetate 10.01 Tri-n-propyl amine 7.23Isobutyl acetate 9.97 Formamide 10.25Sec-butyl acetate 9.91 Acetamide 9.77Methyl propionate 10.15 N-methyl acetamide 8.90Ethyl propionate 10.00 N,N-dimethyl formamide 9.12Methyl n-butyrate 10.07 N,N-dimethyl acetamide 8.81Methyl isobutyrate 9.98 N,N-diethyl formamide 8.89

N,N-diethyl acetamide 8.60

11


Tables


OTHER ALIPHATIC MOLECULES WITH N ATOM OLEFINS, CYCLO-OLEFINS, ACETYLENES


Nitromethane 11.08 Ethylene 10.515Nitroethane 10.88 Propylene 9.731-nitropropane 10.81 1-butene 9.582-nitropropane 10.71 2-methylpropene 9.23HCN 13.91 Trans-2-butene 9.13Acetontrile 12.22 Cis-2-butene 9.13Propiontrile 11.84 1-pentene 9.50n-butyronitrile 11.67 2-methyl-1-butene 9.12Acrylonitrile 10.91 3-methyl-1-butene 9.513-butene-nitrile 10.39 3-methyl-2-butene 8.67Ethyl nitrate 11.22 1-hexene 9.46Methyl thiocyanate 10.065 1,3-butadiene 9.07Ethyl thiocyanate 9.89 Isoprene 8.845Methyl isothiocyanate 9.25 Cyclopentene 9.01Ethyl isothiocyanate 9.14 Cyclohexene 8.945

4-methylcyclohexene 8.914-cinylcylohexene 8.93Cyclo-octatetraene 7.99Acetylene 11.41Propyne 10.361-butyne 10.18

12


Tables


SOME DERIVATIVES OF OLEFINS HETEROCYCLIC MOLECULES


Vinyl chloride 9.995 Furan 8.89Cis-dichloroethylene 9.65 2-methyl furan 8.39Trans-dichloroethylene 9.66 2-furaldehyde 9.21Trichloroethylene 9.45 Tetrahydrofuran 9.54Tetrachloroethylene 9.32 Dihydropyran 8.34Vinyl bromide 9.80 Tetrahydropyran 9.261,2-dibromoethylene 9.45 Thiophene 8.860tribromoethylene 9.27 2-chlorothiophene 8.683-chloropropene 10.04 2-bromothiophene 8.632,3-dichloropropene 9.82 Pyrrole 8.201-bromopropene 9.30 Pyridine 9.323-bromopropene 9.7 2-picoline 9.02CF CCl=CClCF 10.36 3-picoline 9.043 3

n-C F CF=CF 10.48 4-picoline 9.045 11 2

Acrolein 10.10 2,3-lutidine 8.85Crotonaldehyde 9.73 2,4-lutidine 8.85Mesityl oxide 9.08 2,6-lutidine 8.85Vinyl methyl ether 8.93 Tribromoethylene 9.27Allyl alcohol 9.67Vinyl acetate 9.19

13


Tables


AROMATIC COMPOUNDS


Benzene 9.245 Phenyl isothiocyanate 8.520Toluene 8.82 Benzonitrile 9.705Ethyl benzene 3.76 Nitrobenzene 9.92n-propyl benzene 8.72 Aniline 7.70i-propyl benzene 8.69 Fluoro-benzene 9.195n-butyl benzene 8.69 Chloro-benzene 9.07s-butyl benzene 8.68 Bromo-benzene 8.98t-butyl benzene 8.68 Iodo-benzene 8.73o-xylene 8.56 o-dichlorobenzene 9.07m-xylene 8.56 m-dichlorobenzene 9.12p-xylene 8.445 p-dichlorobenzene 8.94Mesitylene 8.40 1-chloro-2-fluorobenzene 9.155Durene 8.025 1-chloro-3-fluorobenzene 9.21Styrene 8.47 1-bromo-4-fluorobenzene 8.99o-methyl styrene 8.35 o-fluorotoluene 8.915Ethynylbenzene 8.815 m-fluorotoluene 8.915Napthalene 8.12 p-fluorotoluene 8.7851-methylnapthalene 7.69 o-chlorotoluene 8.832-methylnapthalene 7.955 m-chlorotoluene 8.83Biphenyl 8.27 p-chlorotoluene 8.70Phenol 8.50 o-bromotoluene 8.79Anisole 8.22 m-bromotoluene 8.81Phenetole 8.13 p-bromotoluene 8.67Benzaldehyde 9.53 o-iodotoluene 8.62Acetophenone 9.27 m-iodotoluene 8.61Benzenethiol 8.33 p-iodotoluene 8.50Phenyl isocyanate 8.77 Benzotrifluoride 9.68

o-fluorophenol 8.66

14


Tables


MISCELLANEOUS MOLECULES

Molecule IP (eV)

Ethylene oxide 10.565Propylene oxide 10.22p-dioxane 9.13Dimethoxymethane 10.00Diethyoxymethane 9.701,1-dimethoxyethane 9.65Propiolactone 9.70Methyl disulfide 8.46Ethyl disulfide 8.27Diethyl sulfite 9.68Thiolacetic acid 10.00Acetyl chloride 11.02Acetyl bromide 10.55cyclo-C H CF 10.466 11 3

(n-C F )(CH )C=O 10.583 7 3

Trichlorovinylsilane 10.79(C F ) N 11.72 5 3

Isoprene 9.08Phosgene 11.77

15


Tables

TABLE 2. Relative Photoionization Sensitivities for Gases

Chemical Relative Sensitivity Examples

Aromatic 10 Benzene, Toluene, Styrene

Aliphatic Acid 10 Diethylamine

Chlorinated 5-9 Vinyl Chloride, VinylideneUnsaturated Chloride, Trichloroethylene

Carbonyl 7-9 MEK, MiBK, Acetone,Cyclohexanone

Unsaturated 3-5 A c r o l e i n , P r o p y l e n e ,Cyclohexanone, Allyl Alcohol

Sulfide 3-5 Hydrogen Sulfide, MethylMercaptan

Paraffin (C5-C7) 1-3 Pentane, Hexane, Heptane

Ammonia 0.3

Paraffin (C1-C4) 0 Methane, Ethane

NOTE: Relative sensitivity = meter reading when measuring 10 ppm of the listed gas with instrument with 10.2eV probe calibrated for 10 ppm of benzene, span pot setting = 9.8 for direct reading of benzene.

16


Tables

TABLE 3. Typical Applications of Interchangeable Probes

IonizationPotentials Relative Sensitivity

p-Xylene 8.44 0.10 0.104p-Chlorotoluene 8.70 0.09 0.112Toluene 8.82 0.09 0.112o-Chlorotoluene 8.83 0.075 0.112Ethyl Acetate 9.19 0.075 0.112

Benzene 9.24 0.10 0.10Methyl Mercaptan 9.24 0.10 0.072Pyridine 9.32 0.075 0.122Allyl Alcohol 9.67 0.10 0.111Crotonaldehyde 9.88 0.075 0.104

Amyl Alcohol 9.80 0.09 0.116Cyclohexane 9.88 0.075 0.104Vinyl Chloride 9.95 0.085 0.112Butanol 10.94 0.09 0.176Ammonia 10.15 0.06 0.160

Acetic Acid 10.37 0.04 0.560Ethylene 10.52 0.0 0.320Ethylene Oxide 10.56 0.0 0.298

Response with 9.5 or 11.7 eV probeRelative sensitivity =

Response with 10.2 eV probe

1

SOP#: 2119DATE: 10/07/94

REV. #: 0.0

AIR SAMPLING FOR METALS[NIOSH Method 7300, Elements]


The purpose of this standard operating procedure(SOP) is to define the proper sample collectiontechnique for air sampling for elements (metals), aswell as delineate the typical working range of themethod and indicate potential interferences. Elementscovered by this method include the metals listed inTable 1 (Appendix A).



2.0 METHOD SUMMARY

Air sampling for elements (metals) involves passinga known quantity of air across a mixed cellulose ester(MCE) filter. The particulate phase of the air, with anominal size of greater than or equal to 0.8 microns(µm), is trapped in the filter.

This method requires air sampling utilizing 37millimeter (mm), 3-stage cassettes loaded with 0.8 umMCE filters and support pads. The approximateminimum and maximum sample volumes required fordetection of the metals of interest are listed in Table1 (Appendix A).


No preservatives or special storage conditions arerequired. However, the samples should be stored with

the filter upright and transported at or near ambientconditions to prevent significant deterioration of thesamples. When transporting and handling thesamples, prevent impact and vibrations which woulddislodge particulates from the filters.


A potential problem with the sampling method isover-loading of the filter. This can disrupt flow,consequently producing falsely low analytical results.Periodic checking of the filter and pump can predictthis condition and sample cassettes can be changedduring the sampling period. The multiple filterswould be analyzed as one sample with the totalvolume indicated on the Chain of Custody record.


The following equipment is required for air samplingfor elements:

C Low or medium volume air pumpsC Tygon tubingC 0.8 µm MCE filters with support padsC 37 mm 3-stage cassettesC Hose-barb filter adaptersC Air flow calibration standard (calibrated

rotameter or bubble meter)C Screw driver setC Air Sampling Worksheets and sample labelsC Chain of Custody recordsC Particulate monitoring equipment (RAM)C Protective clothingC Whirl bags

6.0 REAGENTS


2

7.0 PROCEDURE

7.1 Preparation


2. Obtain and organize the necessary samplingand monitoring equipment.

3. Decontaminate or pre-clean equipment, andensure that it is in working order.Precalibrate sampling equipment, if possible.


5. Perform a general site survey prior to siteentry in accordance with the site-specificHealth and Safety Plan.

6. Use stakes, flagging tape, or otherappropriate means to mark all samplinglocations. If necessary, the proposedlocations may be adjusted based on siteaccess, property boundaries, and surfaceobstructions.

7. Make an estimate of the airborneconcentrations of the elements of concern. Itmay be possible to extrapolate theconcentration of particulates by assumingsimilar percentages of metals are present inthe airborne particulates as in the soils.However, it should be noted that this is onlya rough estimate. If estimation of theairborne concentration of metals is notpossible, then sample volumes should remainwithin the limits recommended in Table 1(Appendix A).

8. Arrange for sample analysis by anappropriately certified laboratory and checkwith the laboratory for any specialrequirements (e.g., additional lot blanks).

7.2 Calibration

Calibrate the required number of sampling pumps inthe following manner:

1. Assemble the calibration train as shown in

Figure 1 (Appendix A) using a representative37 mm, 3-stage filter cassette loaded with a0.8 µm MCE filter and support pad (outletplug removed), tygon tubing, a hose-barbfilter adapter, a rotameter, and an airsampling pump. Depending on the requiredflow rate, a low volume or a medium volumesampling pump may be required. Refer toFigure 2 (Appendix A) for an illustration ofthe components of the filter cassette.

2. Turn on the pump and adjust the flow usingthe flow adjust mechanism until the float ballon the rotameter is aligned with therotameter's precalibrated flow rate value. Asticker on the rotameter should indicate thisvalue.

3. Affix a sticker to the pump indicating flowrate and media.

7.3 Sampling

1. Assemble the sampling trains with cleanfilter cassettes (Figures 3 and 4, AppendixA).

2. Verify the pump calibration by removing theinlet plug from the cassette, attaching arotameter with Tygon tubing and turning onthe sampling pump. Ensure that allconnections are tight. Record the actual flowrate on the Air Sampling Worksheet.Replace the inlet plug until ready to sample.

3. Set the sampling pump timer (low volumepumps) for the appropriate sampling time asdetermined by the Work AssignmentManager, or record the elapsed timerreadings (medium volume pumps) on the AirSampling Worksheet. This will be dictatedby the type of sampling pump being utilized.

4. Deploy the sampling pumps as indicated inthe sampling plan, following site health andsafety procedures.

5. Remove the cassette cap or inlet plug fromthe cassette. Sampling for elements can beconducted with the cassettes open-faced(cassette cap removed) or closed-faced (onlyinlet port plug removed). Open-faced ispreferred because it permits an even loadingof the filter cassette and should be used

3

whenever high particulate concentrations are The following general QA procedures apply:expected. This allows greater particulateloading of the filter. However, either method 1. All data must be documented on Airis acceptable since the entire filter is used Sampling Worksheets or within siteduring sample analysis. Closed-faced logbooks.sampling is typically performed when thereis a possibility that the sample may be 2. All instrumentation must be operated inshaken and particulates may be lost. accordance with operating instructions as

6. Turn on the sampling pump and allow it to otherwise specified in the work plan.run for the sampling period determined by Equipment checkout and calibrationthe Work Assignment Manager. activities must occur prior to

7.4 Post Sampling

1. Verify the sampling period by reading thesample run time (low volume pumps) or bychecking the elapsed time on the counter(medium volume pumps). Record thesampling time on the Air SamplingWorksheet and turn off the pump.

2. Verify the pump calibration by attaching arotameter with Tygon tubing and turning onthe sampling pump. Record the actual flowrate on the Air Sampling Worksheet. Insertthe inlet plug.

3. Remove the sampling cassette from thesampling train and insert the outlet plug.

4. Complete the Air Sampling Worksheet andcalculate the sample volume.

5. Label the sample and place it in a whirl bagfor transport to the laboratory for analysis.

6. Prepare the samples (including QC samples)for transport by packing them in a shipping Results of the QA/QC samples will be evaluated forcontainer with bubble wrap or styrofoam contamination. This information will be utilized topieces. Complete a Chain of Custody record qualify the environmental sample results accordinglyin accordance with applicable Chain of with the project's data quality objectives.Custody Procedures.

8.0 CALCULATIONS

The total volume of a sample is calculated by follow U.S. EPA, OSHA, or corporate health andmultiplying the total sample time by the flow rate. safety procedures.The total volume for each sample must be indicatedon the Chain of Custody Record.


supplied by the manufacturer, unless

sampling/operation and they must bedocumented.


1. Provide one field blank per sampling event orper 20 samples, whichever is greater. Thefield blank should be handled in the samemanner as the sampling cassette(remove/replace cap and plug, and transport)except that no air is drawn through it.

2. Collect one collocated sample per samplingevent or per 10 samples, whichever isgreater. Collocated samples are two samplescollected adjacent to each other during thesame time period at the same flow rates.

3. Include a minimum of two lot blanks permanufacturer's lot of sampling cassettesutilized per sampling event. Consult with theanalytical laboratory to determine ifadditional lot blanks are required.



When working with potentially hazardous materials,

12.0 REFERENCES

NIOSH Manual of Analytical Methods, NIOSH(1)

Method 7300, Elements (ICP) (Issued 02/15/84).

4

APPENDIX A

Table

TABLE 1. Metal Concentrations are Anticipated to be at or Near the Threshold Limit Value (TLV)

Element Minimum Air Volume Maximum Air Volume(Symbol) to be collected - Liters to be collected - Liters

Silver (Ag) 250 2000Aluminum (Al) 5 100(1) (1)

Arsenic (As) 5 2000Beryllium (Be) 1250 2000Calcium (Ca) 5 200Cadmium (Cd) 13 2000Cobalt (Co) 25 2000Chromium (Cr) 5 1000Copper (Cu) 5 1000Iron (Fe) 5 100Lithium (Li) 100 2000Magnesium (Mg) 5 67Manganese (Mn) 5 200Molybdenum (Mo) 5 67Sodium (Na) 13 2000Nickel (Ni) 5 1000Phosphorus (P) 25 2000(1) (1)

Lead (Pb) 50 2000Platinum (Pt) 1250 2000Selenium (Se) 13 2000Tin (Sn) 5 500Tellurium (Te) 25 2000Titanium (Ti) 5 100Thallium (TI) 25 2000Vanadium (V) 5 2000Tungsten (W) 5 200(1) (1)

Yttrium (Y) 5 1000Zinc (Zn) 5 200Zirconium (Zr) 5 200

NOTE: Do not exceed a filter loading of approximately 2mg total dust.

Greater volumes may be required if the anticipated concentration is less than the ACGIH TLV.(1)

5

APPENDIX B

Figures

FIGURE 1. Calibration Train with Low Volume Sampling Pump

6


Figures

FIGURE 2. Filter Cassette Assembly

7


Figures

FIGURE 3. Medium Volume Sampling Train

8


Figures

FIGURE 4. Sampling Train with Low Volume Sampling Pump

1

SOP#: 2121DATE: 08/07/95

REV. #: 0.1

HIGH VOLUMEPOLYURETHANE FOAM

SAMPLING


The purpose of this Standard Operating Procedure(SOP) is to outline the protocol for collection of airsamples for organochlorine and organophosphatecompounds (i.e., dioxins and polychlorinatedbiphenyls) using the polyurethane foam (PUF)sampling medium. The PUF sampling system isdesigned to simultaneously collect suspended airborneparticulates and to trap airborne pesticide vapors.

These are standard (i.e., typically applicable)operating procedures which may be varied or changedas required, depending on site conditions, equipmentlimitations or limitations imposed by the procedure.In all instances, the ultimate procedures employedshould be documented and associated with the finalreport.


2.0 METHOD SUMMARY

Ambient air is drawn into a covered housing thenthrough a glass fiber filter and PUF plug by a high-flow-rate pump operating at approximately 250liters/minute (L/m) (approximately nine cubicfeet/minute [ft /m]). This allows total suspended3

particulates (TSP) to collect on the filter surface. ThePUF plug allows collection of vapor which might bestripped from the particulates on the filter.


Prior to sampling, determine whether pre- and post- Sample modulesfilter weighing is appropriate based on project needs Calibration orificeor client requirements. In addition, obtain pre-cleaned ManometerPUF plugs from the analytical laboratory. Plastic bags

After sampling, the PUF plug and filter should bestored in an 8-oz. glass jar. The PUF plug shouldoccupy the bottom portion of the jar and the filtershould be folded into quarters and placed on top of theplug. The jar is then wrapped with aluminum foil(shiny side out).


Humidity - Glass fiber filters are comparativelyinsensitive to changes in relative humidity; however,collected particulate matter can be hygroscopic.

Photosensitivity - PUF plugs are white and turnyellow upon exposure to light. They should be storedin a dark place (i.e., a black trash bag or a cooler)prior to and after sampling.


5.1 Sampling Media (Sorbents)

Polyurethane Foam - polyether-type polyurethanefoam (density No. 3014, 0.0225 grams/cm , or3

equivalent). This is the type of foam generally usedfor furniture upholstery, pillows, and mattresses(General Metals Work's part number GPS-116 isrecommended, three inch PUF plug, although one andtwo inch pieces are also available).

Glass Fiber Filter - 102-mm diameter.

5.2 Sampling Equipment

PS-1 PUF Samplers or Equivalent (platform,legs, motor, magnehelic panel, tubing,venturi, and ball valves)

Tweezers

2

Aluminum foil the types and amounts of equipment andHexane supplies needed.Surgical glovesSolvex gloves 2. Obtain and organize the necessary samplingSample jars and monitoring equipment.Trash bagsCalibration Worksheets 3. Decontaminate or pre-clean equipment andAir Sampling Worksheets (PUF) ensure that it is in working order.LogbookComputer or calculator to perform 4. Prepare scheduling and coordinate with staff,calculations client, and regulatory agency, if appropriate.Calibrated scale (if weighing is required)Source of electricity (AC/DC): an electrical 5. Perform a general site survey prior to sitesource of 100 volts, 15 amps is required entry, in accordance with the site specific

6.0 REAGENTS

Reagents are not used for the preservation of PUFsamples. Hexane is required for decontaminatingPUF glassware. No other decontamination solutionsare required.

7.0 PROCEDURES

7.1 Calibration of Elapsed-TimeMeters and Calibration Orifices

Elapsed-Time Meter

Every six months the elapsed-time meter should bechecked against a timepiece of known accuracy, eitheron site or in the laboratory. A gain or loss of >2min/24-hr period warrants adjustment or replacementof the indicator. The results of these checks should berecorded in the calibration logbook.

Calibration Orifices

Upon receipt and at one-year intervals, calibrationorifices should be certified with a positivedisplacement standard volume meter (such as aRootsmeter) traceable to the National Bureau ofStandards (NBS). This certification will be performedby the manufacturer. Calibration orifices should bevisually inspected for signs of damage before eachuse, and they should be recalibrated if the inspectionreveals any nicks or dents in the orifice.

7.2 General Preparation

1. Determine the extent of the sampling effort,the sampling methods to be employed, and

Health and Safety Plan.

6. Use stakes or flagging tape to identify andmark all sampling locations. If required, theproposed locations may be adjusted based onsite access, property boundaries, and surfaceobstructions.

7.3 Sample Module Preparation

1. Pre-clean all sampling equipment withhexane prior to use.

2. Check the lower canister to ensure that theupper and lower orange silicone gaskets arein place (Figure 1, Appendix A).

3. Using tweezers, load the glass cartridge witha pre-cleaned PUF plug, making sure thefoam is evenly distributed throughout thecartridge, and install in the lower canister.

4. Screw the filter holder support onto the lowercanister, after ensuring that the siliconerubber gasket is in place.

5. Screw the filter holder with support screenonto the filter holder support, after ensuringthat the silicone rubber gasket is in place.

6. Install the lower Teflon gasket in the filterholder.

7. Using tweezers to handle the filter, placeglass fiber filter (rough side up) into the filterholder.

8. Install the upper Teflon gasket.

3

9. Ensure that the silicone rubber gasket is 6. Connect the calibration orifice to the samplepresent and then install the filter retaining module (Figure 2, Appendix A). Ensure thatring and tighten the swing bolts. no

10. Ensure that all fittings are snug, yet notovertight (Overtightening will distort thegaskets.).

11. Cover the sample module with the metalcover and place in a cooler.

12. Assemble a field blank in the same mannerand store in the same cooler.

It is recommended that two sampling modules areprepared for each sampling system so that the filterand PUF plug exchange may take place in the cleanzone. The second set of modules is used for thesubsequent sampling round.

7.4 Field Calibration of the Sampler

Calibration of the PUF sampler is performed withouta PUF plug and without the glass fiber filter in thesampling module. However, the empty glass cartridgemust remain in the module to ensure a good sealthrough the module.

Calibration of the PUF sampler is performed prior tousing the sampling system in the field and after repairor replacement of major components of the samplingsystem (i.e., motor repair).

1. Assemble the sample module, as described inSection 7.2, without the PUF plug andwithout the glass fiber filter.

2. Assemble the sampling system by attachingthe legs and the magnehelic panel to theplatform. Connect the motor to the platform,making sure that the gasket is placedbetween the motor and the platform.

3. Plug the motor into the timer located on themagnehelic panel.

4. Connect the magnehelic to the venturi withtubing.

5. Place the sampling module into the quick-release fitting and engage by locking the twolevers down securely.

4

leaks exist between the orifice unit and thesampler.

7. Fill the manometer with colored water andconnect it to the calibration orifice pressuretap with tubing.

8. Set the manometer to "zero" as shown inFigure 3 (Appendix A). This is done bysliding the scale either up or down so the"zero" is level with the bottom of themeniscuses.

9. Connect the sampling system to the powersource and fully open the ball valve bypushing the red lever up to the "on" position.

10. Fully open the voltage variator by using ascrewdriver to turn the screw on themagnehelic gauge panel clockwise.

11. Operate the sampling system for at least 15minutes to establish thermal equilibriumprior to calibration.

12. Conduct a five point calibration in the rangeof the desired flow rate as follows:

a. Adjust the voltage variator (locatedon the magnehelic gauge panel)and/or the ball valve to obtain areading of 70 (arbitrary) inches onthe magnehelic gauge.

b. The magnehelic gauge number, 70,is pre-recorded on the FieldCalibration Work Sheet (Column#5, Attachment 1, Appendix B).Read and record (Column #4 on theField Calibration Work Sheet) thetotal distance between the twomeniscuses on the manometer(Figure 3, Appendix A). This is ameasure of the pressure drop acrossthe calibration orifice.

c. Move the ball valve (red lever) toadjust the magnehelic gauge downto 60 (arbitrary) inches. Let thesampler run for at least two minutesto re-establish the run temperatureconditions. Repeat step 12 b.

5

d. Using the above procedure (steps 12 direction from site, location, sample startb. and c.), adjust the ball valve for time, time/counter (start).readings at 50, 40, and 30 inches.

13. Measure the barometric pressure and ambienttemperature. 9. If necessary adjust the magnehelic gauge to

14. Record all data on the Field Calibration flow rate by turning the ball valve.Work Sheet (Attachment 1, Appendix B).Perform calculations as described in Sections 10. Wait approximately two minutes for the8.1, 8.2, 8.3, and 8.4 of this SOP and record magnehelic reading to stabilize.the appropriate results on the FieldCalibration Work Sheet. 11. Allow the sampling system to operate for the

15. Adjust the ball valve to the magnehelic Assignment Manager.reading required to achieve the targetvolumetric flow rate as requested by the 12. If the sampling system is to be in use for anWork Assignment Manager. extended period of time (i.e., the duration of

7.5 Sampling

1. Verify that the sampler has been calibratedas described in Section 7.4.

2. Transport the sampler to the desired location.The PUF sampler must be operated in thebreathing zone or it may be elevated. Thesampler should be located in an unobstructedarea, at a distance of twice the height of anyobstruction to air flow, if possible, but nocloser than two meters to the obstacle. In 7.6 Unit Shutdown and Sampleurban or congested areas, it is recommendedthat the sampler be placed on the roof of asingle story building.

3. If it is not already set up, assemble thesampling system as described in Section 7.4(Steps 2 to 4). Adjust the exhaust hose sothat it faces downwind of the sampler.

4. Put on clean surgical gloves.

5. Place the loaded sampling module into thequick release fitting and engage by lockingthe two levers down securely. Refer toFigure 4 (Appendix A) for the complete set-up of the sampling system.

6. Remove the metal cover.

7. Record the following information on the AirSampling Worksheet (Attachment 2,Appendix B): high volume pump number,

8. Plug in the unit.

the reading required to achieve the target

duration determined by the Work

sampling is greater than 24 hours), the initialcalibration should be audited every 24 hours.This audit is accomplished by checking onepoint in the calibration curve using the fieldcalibration procedure described in Section7.4 and using a fully assembled samplemodule with the PUF plug and glass fiberfilter installed. If the result of this check isgreater than ±7% of the initial calibrationvalue, the sampling system must berecalibrated.

Collection

1. Record the following information on the AirSampling Worksheet (Attachment 2,Appendix B): sample stop time, time/counter(stop), the ending magnehelic reading, andwhether or not there was a pump fault.Measure the ambient temperature andbarometric pressure at the end of thesampling period. This information and theending magnehelic gauge reading should berecorded on the Field Calibration WorkSheet.

2. Unplug the sampler and remove the samplemodule.

3. Cover the sample module with the metalcover. Keep the sample module in a verticalposition at all times.

6

4. Place the sample module in a cooler fortransport back to the command post. Thefield blank should also be stored in the samecooler.

5. If additional sampling is scheduled, performa field calibration audit as described inSection 7.5, #12. The unit must bedecontaminated with hexane and chem wipesprior to initiating additional samplingactivities. Install a new sampling moduleand begin sampling as described in Section7.5. If no additional sampling is scheduled,secure the unit.

6. Wearing surgical gloves and using tweezers,remove the PUF plug and place it in a clean8-oz. glass jar. Fold the glass fiber filter intoquarters and place it on top of the PUF plug.Label the jar appropriately and cover it withaluminum foil (shiny side out). Prepare thesample for transport to the laboratory foranalysis, as necessary.

7. Calculate the post-sampling flow rate, theaverage flow rate, and the total volumesampled (Sections 8.5 and 8.6).

8.0 CALCULATIONS

The total volumes calculated for each sampling unitare corrected to standard conditions (760 millimetersof mercury [mm Hg] and 298 kelvin [K]). This isnecessary for reporting the concentrations in a mannerconsistent with method requirements. The first step inthe calibration process is to determine the slope (m)and the y-axis intercept (b) from the FactoryCalibration Work Sheet. This is based on the formulay=mx+b. This is calculated either graphically (5-pointcalibration curve) or by a regression analysis of thedata provided on the Factory Calibration Work Sheet.Once the slope and intercept are calculated for thefactory calibration data, a calibration curve isdeveloped for each of the sampling units. Theimportant data elements needed to complete this taskare the pressure drop readings for each of the arbitraryvalues (I) (Section 7.4), ambient temperature andambient pressure. If the sampling unit calibrationresults will be provided in mm Hg instead of inchesof water, then Section 8.1 may be skipped becausethe manufacturer has already calculated the slope(m) and intercept (b) and provided them on theFactory Calibration Work Sheet. This information

should be recorded in the appropriate location onthe Field Calibration Work Sheet.

7

8.1 Determining the Slope (m) and Y-Axis Intercept (b) of the FactoryCalibration

1. Obtain the current Factory Calibration WorkSheet from manufacture's calibration kit orAir Team Calibration File. See Figure 5(Appendix A) for an example.

2. Copy columns #6 & #7 from the Q sectionstd

of the Factory Calibration Work Sheet tocolumn #1 & #2, respectively, on the FieldCalibration Work Sheet (Attachment 1,Appendix B). Record the ambienttemperature, ambient pressure at which thefactory orifice calibration was performed,and orifice serial number from the FactoryCalibration Work Sheet in the respectivelocations on the Field Calibration WorkSheet. Return the Factory Calibration WorkSheet to the calibration kit or the proper file.

3. Solve the following formula for everycalibration orifice static pressure found incolumn #1 of the Field Calibration WorkSheet. Record results in column #3 of theField Calibration Work Sheet. The units ofthe results are arbitrary. There should be atleast five computations.

Equation:

y-axis equation orifice =[ H(P /760)(298/T )]a a

1/2

Where:

H = Calibration orifice static pressure ininches of water ("H O) (Field2

Calibration Work Sheet, column#1).

P = Ambient pressure at which thea

factory orifice calibration wasperformed in mm Hg.

T = Ambient temperature at which thea

factory orifice calibration wasperformed in K.

8

Example: 2. Solve the y-axis equation using the formula

H = 2.0 "H O, P = 760.5mm Hg, T = 295 on the Field Calibration Work Sheet. Record2 a a

K the results in column #6 of the Field

y-axis equation orifice = [(2.0 results are arbitrary. There should be at least"H O)(760.5mm Hg/760 mm Hg)(298 K/295 five computations.2

K)]1/2

y-axis equation orifice = [2.02] Equation:1/2

y-axis equation orifice = 1.42 y-axis equation sampling unit =

4. Graph the results in column #2 of the FieldCalibration Work Sheet on the x-axis against Where:the data presented in column #3 of the FieldCalibration Work Sheet on the y-axis or H = Static pressure of the sampling unitperform a regression analysis of the data to in "H O (column #4 of the Fielddetermine the slope and (m) and the y-axis Calibration Work Sheet).intercept (b). Record in the appropriate P = Ambient pressure in mm Hg at timelocation on the Field Calibration Work Sheet. of unit calibration.

Example: Regression analysis from Lotus of unit calibration.123:

Regression Output:Constant - 0.03 H = 6.0 "H O, P = 756.92mm Hg, T = 295Std Err of Y Est 0.00246358 KR Squared 0.99999508No. of Observations 6 y-axis equation sampling unit =Degrees of Freedom 4 [(6.0 "H O)(756.92 mm Hg/760 mm Hg)(298

X Coefficient(s) 9.52Std Err of Coef. 0.01055231 y-axis equation sampling unit = [6.06]

Where: y-axis equation sampling unit = 2.46

Constant = y-Axis intercept (b) 3. Determine the volumetric flow rate (Q ) forX Coefficient(s) = Slope (m) each calibration point using the following

8.2 Determining the Slope (m) and aY-Axis Intercept (b) of the FieldCalibration

1. Obtain pressure drop readings from the watermanometer and the matching arbitrarymagnehelic values (I = 70, 60, 50, 40, 30)from Section 7.4 and record the data on aField Calibration Work Sheet in columns #4and #5, respectively. Record the ambienttemperature and ambient pressure at whicheach unit calibration was performed.

below and using the data found in column #4

Calibration Work Sheet. The units of the

[ H(P /760)(298/T )]a a1/2

2

a

T = Ambient temperature in K at timea

Example:

2 a a

2

K/295 K)]1/2

1/2

STD

equation. Record the results in column #7 ofthe Field Calibration Work Sheet.

Equation:

QSTD = 1/m [{ H(P /760)(298/T )} -b]a a1/2

Where:

m = Slope from the Factory CalibrationWork Sheet graph or regressionanalysis (Step #4, Section 8.1).

H = Pressure drop in "H O recorded on2

Field Calibration Work Sheet(column #4).

9

P = Ambient pressure in mm Hg at time the data presented in column #8 from thea

of field calibration. Field Calibration Work Sheet on the y-axisT = Ambient temperature in K at time or perform a regression analysis to determinea

of field calibration. the slope (m) and the y-axis intercept (b).b = y-Axis intercept from the Factory Record in the appropriate location on the

Calibration Work Sheet graph or Field Calibration Work Sheet.regression analysis (Step #4,Section 8.1). Example: Regression analysis from Lotus

Example:

m = 9.52, H = 6.0 "H O, P = Constant 1.642 a

756.92 mm Hg, T = 295 K, b = - 0.03 Std Err of Y Est 0.057770455a

Q = 1/9.52 [{6.0 "H O (756.92 mm No. of Observations 6STD 2

Hg/760 mm Hg)(298 K/295 K)} -(-0.03)] Degrees of Freedom 41/2

Q = 1/9.52 [2.46] X Coefficient(s) 25.66STD

Q = 0.26 m /minSTD 3

4. Determine the Y for each calibrationvalue

point. Record in column #8 on the Field Constant = y-axis intercept (b)Calibration Work Sheet. The units of the X Coefficient(s) = Slope (m)results are arbitrary.

Equation:

Y of each calibration point =value

[I(P /760)(298/T )]a a1/2

Where:

I = Arbitrary value located in column#5 on the Field Calibration WorkSheet.

P = Ambient pressure in mm Hg at timea

of unit field calibration.T = Ambient temperature in K at timea

of unit field calibration.

Example:

I = 70, P = 756.92 mm Hg, T = 295 Ka a

Y of each calibration point =value

[70(756.92mm Hg/760 mm Hg)(298 K/295K)]1/2

Y of each calibration point = 8.39value

5. Graph the results in column #7 of the FieldCalibration Work Sheet on the x-axis against

123:

Regression Output:

R Squared 0.998738313

Std Err of Coef. 0.45593301

Where:

8.3 Checking the Linearity of theCalibration

1. Calculate Y to determine if the calibrationcal

is within the limits of linearity (±5%) usingthe following formulas. Record the results incolumn #9 of the Field Calibration WorkSheet.

Equation: Y = mQ + bcal STD

Where:

m = Slope of the field calibration curvefrom the regression analysis ofcolumns #7 & #8.

Q = Volumetric flow rate calculated onSTD

the Field Calibration Work Sheet(column #7).

b = y-Axis intercept of the fieldcalibration curve from theregression analysis of columns #7and #8.

Example:

m = 25.66, Q = 0.26, b = 1.64STD

10

Y = [(25.66)(0.26)] + 1.64 curve graph or regression analysiscal

Y = 8.31cal

2. Calculate %-difference of the Y and Y .value cal

Record the results in column #10 of the Field I = 70, P = 756.92 mm Hg, T = 295 K, m =Calibration Work Sheet. If the results are not 25.66, b = 1.64with in ±5% recheck your calculations orrecalibrate. Q = (1/25.66)[{70(756.92mmEquation: Hg/760mmHg)(298 K/295 K)} -1.64]

%-difference = ((Y - Y )/Y )(100) Q = 0.26 m /minvalue cal cal

Where: 2. Determine the arbitrary set point for a target

Y = Y in column #8 of the Fieldvalue value

Calibration Work Sheet. a. Obtain the target volumetric flowY = Value from previous calculation rate in m /min from the Workcal

recorded in column #9 of the Field Assignment Manager.Calibration Work Sheet.

Example: pressure and the ambient

%-difference = ((8.39 - 8.31)/8.31)100 sampling event and record on the

%-difference = 0.96%

8.4 Determining Pre-SamplingVolumetric Flow Rate

1. Determine the volumetric flow rate at eachcalibration point using the following equationand recording the data in column #11 of theField Calibration Work Sheet.

Equation:

Q = (1/m)[{I(P /760)(298/T )} -b]a a1/2

Where:

I = Arbitrary magnehelic readingrecorded on Field Calibration WorkSheet (column #5).

P = Ambient pressure in mm Hg ata

which the sampling unit wascalibrated.

T = Ambient temperature in K at whicha

the sampling unit was calibrated.b = y-Axis intercept from the field

calibration graph or regressionanalysis of columns #7 & #8.

m = Slope from the field calibration

of columns #7 & #8.

Example:

a a

1/2

3

volumetric flow rate, as follows.

3

b. Obtain the ambient barometric

temperature at the start of the

Field Calibration Work Sheet.

c. Using the following equationcalculate your arbitrary set point foreach sampler. Record in theappropriate location on the FieldCalibration Work Sheet.

Equation:

I=[{(Q )(m)}+b] /[(P /760)(298/T )]target a a2

Where:

Q = Desired volumetric flow ratetarget

(m /min.)3

m = Slope of the field calibration asdetermined by the regressionof columns #7 & #8.

b = y-Axis intercept of the fieldcalibration as determined bythe regression of columns #7& #8.

P = Ambient pressure at which thea

sample is being taken (mm Hg)T = Ambient temperature at which thea

sample is being taken (K)

Example:

11

What is the magnehelic set point (I) for thetarget flow rate of 0.25 m /min.?3

m = 25.66, b = 1.64, P = 756.92 mm Hg, Ta a

= 295 K

I = [(0.25m /min.)(25.66)+1.64] /[(7563 2

.92/760)(298/295)]

I = 64.49

12

3. Determine the initial flow rate, as follows. volumetric flow rate.

a. Set the magnehelic set point (I) as Equation:determined by the previous step.

b. Use the following equation to checkthe set point to determine if is the Where:correct set point for the desired flowrate. Q = Volumetric flow rate at set point (I).

Equation: of the sampling event.

Q = (1/m)[{I(P /760)(298/T )} -b] sampling event.a a1/2

Where: end of the sampling event.

Q = Volumetric flow rate at set point (I). calibration graph or regressionI = Magnehelic set point (I). analysis of columns #7 & #8.P = Ambient pressure at the start of the m = Slope from the field calibrationa

sampling event. curve graph or regression analysisT = Ambient temperature in K at the of columns #7 & #8.a

start of the sampling event.b = y-Axis intercept from the field Example:

calibration graph or regressionanalysis of column #7 & #8. I = 50, P = 758.9 mm Hg, T = 299 K, m =

m = Slope from the field calibration 25.66, b = 1.64curve graph or regression analysisof column #7 & #8. Q = 1/25.66)[{50(758.9mmHg/760mm Hg)

Example:

I = 64.49, P = 756.9mm Hg, T = 295a a

K, m = 25.66, b = 1.64

Q = 1/25.66[{64.49(756.9mmHg/760mmHg)(298 K/295 K)} -1.64]1/2

Q = 0.25 m /min.3

8.5 Determining Post-SamplingVolumetric Flow Rate

1. Obtain the ambient barometric pressure andthe ambient temperature at the end of thesampling event and record on the FieldCalibration Work Sheet.

2. Obtain the set point (I) of the magnehelic atthe end of the sampling event and record onthe Field Calibration Work Sheet.

3. Use the following equation to determine the

Q = (1/m)[{I(P /760)(298/T )} -b]a a1/2

I = Magnehelic set point (I) at the end

P = Ambient pressure at the end of thea

T = Ambient temperature in K at thea

b = y-Axis intercept from the field

a a

(298 K/299 K)} -1.64]1/2

Q = 0.21 m /min.3

8.6 Determining Total Volume

Average the pre- and post-volumetric flow rates andmultiply by the time sampled to determine the volumesampled. Record all information on the FieldCalibration Work Sheet.

Example:

((0.25m /min + 0.21m /min)/2)480 min = 110.4 m3 3 3


Provide one field blank per sampling period or onefield blank for every 20 samples, whichever is greater.A field blank is treated exactly as a sample except thatair is not drawn through the media. PUF plugs shouldbe submitted to the laboratory for cleaning prior tofield sampling. If the PUF plugs were cleaned in

13

house, one or two clean plugs should be sent to thelaboratory which will be analyzing the samples.Sample spiking may be necessary for pesticide andPCB samples; consult with the Work AssignmentManager.


Results of the quality control samples will beevaluated for contamination. This information will beutilized to qualify the environmental sample results inaccordance with the data quality objectives.


When working with potentially hazardous materialsfollow U.S. EPA, OSHA, and corporate health andsafety practices.

12.0 REFERENCES

Method TO4, Determination of OrganochlorinePesticides and Polychlorinated Biphenyls in AmbientAir, Revision 1.0, April, 1984.

14

APPENDIX A

Figures

FIGURE 1. Sample Module

15


Figures

FIGURE 2. Calibration of the PUF Sampler

16


Figures

FIGURE 3. Manometer

17


Figures

FIGURE 4. PUF Sampler

18


Figures

FIGURE 5. Factory Calibration Work Sheet

19


Figures

FIGURE 5. Factory Calibration Work Sheet (Cont'd)

20

APPENDIX B

Attachments

ATTACHMENT 1. Field Calibration Work Sheet

21


Attachments

ATTACHMENT 2. Air Sampling Worksheet

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