General Counting Procedure

November 27, 2006 SLAC-I-7602A39C-004-R-01 Page 3

DISTRIBUTION LIST

To be filled out by Document Author or person requesting document deletion: Once approved, the new or revised document or the notice of deleted document(s) should be distributed to all persons identified below: ( ) All RP staff members ( X ) All holders of the following manual(s): SLAC Radioanalysis Laboratory Procedures

( ) The following individuals:

November 27, 2006 SLAC-I-7602A39C-004-R-01 Page 4

TABLE OF REVISIONS REVISION

# DATE SECTION(S) REASON FOR REVISION

001 June 2, 2005 All Update Data Entry procedures. Addition of Sample Analysis and Data Entry checklists.

General Sample Analysis Procedure

June 2, 2005 SLAC-I-7602A39C-004-R-01 Page 5

TABLE OF CONTENTS 1 PURPOSE ................................................................................................................................... 6

2 REFERENCES ........................................................................................................................... 6

3 RESPONSIBILITIES ................................................................................................................. 6 3.1 Rad Lab Operator.................................................................................................................. 6 3.2 REP Manager ........................................................................................................................ 6

4 PREREQUISITES ...................................................................................................................... 7

5 PROCEDURES .......................................................................................................................... 7

5.1 Sample Receiving ................................................................................................................. 7 5.2 Analysis Determination ........................................................................................................ 7 5.3 Perform Operational Check .................................................................................................. 7 5.4 Count the sample................................................................................................................... 8 5.5 Determine the results ............................................................................................................ 8 5.6 Data Entry and Distribution .................................................................................................. 8 5.7 Sample Disposal.................................................................................................................... 8

6 RECORDS................................................................................................................................... 9

7 ATTACHMENTS/FORMS......................................................................................................... 9 7.1 Attachment 1: Sample Analysis Flow chart........................................................................ 10 7.2 Attachment 2: General Sample Analysis Checklist ........................................................... 13 7.3 Attachment 3: Chain of Custody Form............................................................................... 18 7.4 Attachment 4: Radioactivity Analysis Form....................................................................... 19 7.5 Attachment 5: Data Entry and Reporting Checklist ........................................................... 20



1 PURPOSE

This procedure outlines the steps for general sample analysis. The procedure applies to anyone characterizing samples for the Radioanalysis Laboratory (Rad Lab). Following this procedure will ensure the completion of the necessary protocols and documentation. A flowchart (Attachment 1) is attached to provide an overview of the Sample analysis procedure. Sample Analysis checklist (Attachment 2) is attached to the appendix to provide detailed steps for routine analysis.

2 REFERENCES

2.1 SLAC Rad Lab Manual, Quality Assurance Plan 3 RESPONSIBILITIES

3.1 Rad Lab Operator

The Rad Lab Operator assigned to perform activities described in this chapter is responsible for:

• ensuring that prerequisites are met as required,

• maintenance of the laboratory equipment and performing daily quality control checks,

• reporting any problems or unexpected events to the Radiological Environmental Protection (REP) Manager,

• routine sample analysis counting,

• providing the data to the REP Manager for analysis and approval, and

• Performing other duties assigned by the REP Manager.

3.2 REP Manager

The REP Manager is responsible for:

• ensuring that the activities in this chapter are conducted in accordance with this written procedure,



• assigning the tasks in this procedure to a qualified Rad Lab Operator, and

• providing final approval or disapproval of all data and submittals.

4 PREREQUISITES

4.1 Must be familiar with Windows, Microsoft Access and Notepad. 4.2 Must be familiar with general laboratory equipment (pipettes, scales, etc.)

4.3 Must have a basic understanding of Liquid Scintillation Counting and Gamma

Spectroscopy theory 5 PROCEDURES

5.1 Sample Receiving

Samples may be received in person or they may be left in the sample drop off location in Room 185 of Building 24.

The person delivering the sample shall enter the sample number, date and time of delivery and a signature on the Chain of Custody Log Sheet (Attachment 3). A Radioactivity analysis form (Attachment 4) is also filled out by the customer. This form must accompany the sample. The Rad Lab Operator receiving the sample shall enter the date and time of sample receipt, sign the Chain of Custody Log Sheet, and enter the sample information into the Sample Database.

5.2 Analysis Determination

The customer should indicate which analysis he or she desires. The customer may not know which analysis is appropriate. In this case the procedure used shall be decided by the customer in consult with the Rad Lab Operator. If there is any question about the desired analysis, the Rad Lab Operator shall contact and assist the customer.

5.3 Perform Operational Check

Before analyzing samples, the Rad Lab Operator shall determine the status of the required periodic quality control checks. An operational source check should be performed on a system daily when in use. A source check procedure is outlined in the instrument system counting procedure. Follow the steps appropriate for the applicable instrument.



5.4 Count the sample

See the appropriate chapter for the desired analysis. To ensure integrity of the samples during the analysis process, samples shall be stored in an area with restricted access.

5.5 Determine the results

The Rad Lab Operator shall review all data for any discrepancies.

The following are examples of results that should be further investigated. They may be indications of a machine failure or inappropriate use of the software.

• Background measurements that are unusually high or low • Extreme departure from the expected result of the analysis • Isotopes that are not usually found at SLAC • Isotopes having relatively short half lives which should preclude

their presence in the sample

5.6 Data Entry and Distribution

The Rad Lab Operator shall enter the sample results into the Sample Database and print the results. The Rad Lab Operator shall prepare the analysis results for distribution. A Data Entry checklist is attached (Attachment 5) to provide the steps for routine data entry and file distribution.

The printed report should be reviewed for data entry errors by comparing it to the analysis printouts. When the accuracy of the report has been verified, the Rad Lab Operator shall sign the report, make a copy, and attach the original analyzer printouts and the Radioactivity Analysis Form to the report. The signed Radioactivity Analysis Form indicating release of the sample will be returned to the customer.

File a copy of the report, analyzer printout, and Analysis Form for each sample in the Rad Lab cabinet in Building 24.

5.7 Sample Disposal

Upon completion of analysis the sample, container, and release documentation are returned to the customer. Samples vials are to be placed in the appropriate Rad Lab waste container.



6 RECORDS

6.1 All analysis results generated from this procedure must be entered into the REP Rad Lab database on the network drive to ensure data access, security control, and backup.

6.2 All hardcopies of the Analysis reports generated from this procedure should

also be provided and stored in the Rad Lab archives. 7 ATTACHMENTS/FORMS

7.1 Attachment 1: Sample Analysis Flow chart

7.2 Attachment 2: General Sample Analysis Checklist

7.3 Attachment 3: Chain of Custody Form

7.4 Attachment 4: Radioactivity Analysis Form

7.5 Attachment 5: Data Entry and Reporting Checklist



7.1 Attachment 1: Sample Analysis Flow chart

Cited ProceduresSAC = Sample Analysis ChecklistRGS = Routine Gamma Spec

No ProcessRLSC = Routine Liquid Scintillation CountingDER = Data Entry & Reporting

Cited Forms/ReportsSIS = Sample Information Sheet

Yes (release authorization form)RA Report = Radioanalysis Report

Yes

No

No

Yes

Receive sample & SIS (info/release sheet)

[SAC Steps 1-4]

Determine radioactivity,

etc. [SAC 9-12]

LSC required for sample?[SAC Step 5]

Complete LSC analysis, vial

disposition [RLSC Steps 2 - 31]

REP or DOS personnel

complete GS analysis

[RGS Steps 2 - 28]

Gamma Spec required for

sample & not yet done?

[SAC 5]

Continue next page [A]

Is water or item release approval

needed?[SAC 22]

Continue next page [B]



Yes No

Yes No

Yes

No

Cited ProceduresSAC = Sample Analysis ChecklistRGS = Routine Gamma Spec ProcessRLSC = Routine Liquid Scintillation CountingDER = Data Entry & Reporting

Cited Forms/ReportsSIS = Sample Information Sheet (release authorization form)RA Report = Radioanalysis Report

[A]Does sample

contain radioactivity OR

any hazmat?

Sign SIS to authorize release

Notify requestor whether release approved or

disapproved (if approved, provide signed copy of

SIS.

REP mgr signs SIS if authorizing release of water (or FO, DREP &

DOS. Mgr )

Is request to release water

to sanitary sewer?

FO Mgr signs SIS if authorizing release of item (or REP, DREP or DOS Mgr)

[B]Enter results into database, print report, attach LSC or

GS print-out[DER 1 - 31]

DOS Mgr reviews RA Report & signs or

requests corrections (or REP, DREP or DOS Mgr)

Did sample analysis include

Gamma Spec?

REP Mgr reviews RA Report & signs or

requests corrections (or FO, DREP or DOS Mgr)

Continue next page [C]



Cited ProceduresSAC = Sample Analysis ChecklistRGS = Routine Gamma Spec ProcessRLSC = Routine Liquid Scintillation CountingDER = Data Entry & Reporting

Cited Forms/ReportsSIS = Sample Information Sheet (release authorization form)RA Report = Radioanalysis Report

[C]Distribute

RA Report (if appliacable). File RA Report & LSC/GS

print-out[SAC 26]

Assure sample handled per procedure (labeled, stored,

returned, disposed) per procedure

[SAC 27 - 28]



7.2 Attachment 2: General Sample Analysis Checklist

Done? Step

No. Item Additional Information

Sample Receiving

[ ] 1.

When picking up a sample for analysis from drop location (normally Room 185), check for sample no. on chain of custody log sheet. Sign sheet as “Receiving Person” & enter date & time. (If sample no. & other info not recorded in C-of-C Log, enter info immediately.)

SLAC-I-7602A39C-004 (general analysis procedure)

SLAC-I-7602A39C-014 (c-of-c log sheet)

[ ] 2. Confirm that a completed RP Analysis Form was submitted for the sample. Don’t proceed w/o a completed copy of this form. Verify that RP Analysis Form and Sample Label are in agreement. Contact the sample collector if the RP Analysis Form was not submitted, or if the information on the RP Analysis Form and Sample Label are inconsistent.

[ ] 3. Check sample with survey meter – notify REP or FO mgr if detect radiation.

[ ] 4.

If the RP Analysis From indicates a hazardous substance in the sample, label the sample bottle with the details.

Determine Analysis

[ ] 5.

Confirm type of analysis to be done. Consult person requesting analysis or REP mgr, if unclear. Also note that samples from EP, RAMSY, BDE, Storm water and wells EXW-4, MW-30, MW-81, & MW-94 must be analyzed using LSC & GS.


Perform Operational Check

[ ] 6. Confirm applicable QA checks have been completed (LSC: source check recorded completed w/in past 24 hrs in LSC log; GS: source check recorded completed w/in past 24 hrs in GS log]




Done? Step No.

Item Additional Information

[ ] 7.

If required source check(s) not completed, set up for check (source checks are required within 24 hours sample count – OK before or after).

See applicable procedure: Routine Liquid Scintillation Counting or Routine Gamma Spec Process

SLAC-I-7602A39C-008

SLAC-I-7602A39C-009

Count the Sample

[ ] 8.

Prepare & count sample per LSC &/or GS counting/analysis procedure.

See applicable procedure: Routine Liquid Scintillation Counting or Routine Gamma Spec Process

SLAC-I-7602A39C-008- R-002

SLAC-I-7602A39C-009

Determine the Results

[ ] 9. Determine the whether radioactivity was detected in the sample:

a. For GS, a sample is “NDA” if the only radioactivity detected was naturally-occurring & in concentrations normal for the material.

b. For LSC (H-3) swipes, a swipe is “NDA” if <1000 DPM

c. For LSC environmental samples counted on Protocol 13, a sample is “NDA” if the calculated H-3 concentration is < 500 pCi/L

d. For all other LSC samples counted on Protocol 1 or 13, a sample is “NDA” if the calculated H-3 concentration is < 1000 pCi/L

[ ] 10. If the sample is not “NDA” put a rad mat’l label on sample bottle & mark radionuclide(s) detected.



Done? Step No.


[ ] 11. If the sample is one that was run on the GS only, proceed to Step 16; otherwise continue with Step 12.

[ ] 12. If the sample was determined to be “NDA” in Step 9, mark the LSC print-out to clearly indicate this.

[ ] 13. Determine whether sample is one that may require GS analysis in addition to LSC. Review:

• Steps 25 & 26 of Routine Liquid Scintillation Counting procedure, and

• List in Step 5 of this procedure.

[ ] 14. If GS analysis is required & hasn’t been completed, attach the LSC print-out to the sample bottle & place it on the top shelf of the bookcase by the door to the GS lab. DON’T DO DATA ENTRY UNTIL ALL ANALYSES ARE COMPLETE!

[ ] 15. Proceed to Step 18.

[ ] 16. Determine whether this sample is one that requires LSC in addition to GS (generally all water samples).

[ ] 17. If LSC is required & hasn’t been completed, attach the GS print-out & RP Analysis Form to the sample bottle & place it in the bin for incoming samples in Room 185.

[ ] 18. Double-check to assure that all required LSC (correct protocol) & GS analyses have been completed. Make sure all results are clearly stated. (For GS results, list any nuclides detected & their activities. Normally, positive GS results should be converted to pCi & be listed on paperwork with units “pCi – GS”.)

[ ] 19. Put sample bottle in holding location until all data entry for the sample is completed.

[ ] 20.

Wash hands!



Done? Step No.


Data Entry

[ ] 21. Either continue with Step 22 or turn over all sample paperwork (RP Analysis Form, SC &/or GS reports) to person responsible for data entry.

[ ] 22.

Proceed with entering results into database (see Data Entry checklist). Print report of results using sample database. Check that report(s) matches analysis print-outs.

See procedure Data Entry & Reporting


Prepare for Distribution

[ ] 23. If the sample was submitted requesting RP approval for the release of the material (e.g. approval to release water to the sanitary sewer, resin for off-site treatment, or a sample or item for shipment), proceed to Step 24, otherwise skip to Step 25.

[ ] 24. If the sample contains a hazardous substance OR if it contains radioactivity (per Step 9), one of the following must sign (or disapprove) the Sample Log Sheet to authorize the release: the REP mgr, the FO mgr, or the DREP mgr.

SLAC-I-760-2A39Z-001 (REP water release policy – draft as of 7/04)

SBSA permit

SLAC-I-760-xxxx-00x (FO resin procedure)

SLAC-I-760-2A39Z-001 (FO release criteria)

[ ] 25. If the sample contains no hazardous substances and no radioactivity (per Step 9), the person who did the radioanalysis may sign RP Analysis Form to authorize the release.

[ ] 26.

Notify person/group requesting approval to release of outcome – if approval has been refused, follow-up as necessary (e.g. notify RP, SEM mgmt. of circumstances & alternatives).

[ ] 27. Obtain signature the REP mgr, the FO mgr, or the DREP mgr on radioanalysis report.




Done? Step No.


[ ] 28.

File the Radioanalysis report, LSC/& or Gamma Spec printout, and a copy of the RP Analysis Form in the Rad Lab file cabinet. Return the RP Analysis Form to the sample requestor.


Sample Disposal

[ ] 29. For the following types of samples, alert the responsible employees to retrieve the sample:

• solid samples (including resins)

• samples containing a hazardous material

• samples that are unusually radioactive

[ ] 30.

If water sample has not been returned (Step 29), assure it is labeled per Step 10. Store it in location specified by REP or FO mgr.

[ ] 31. Dispose of the sample vial in the appropriate Rad Lab waste drum.



7.3 Attachment 3: Chain of Custody Form



7.4 Attachment 4: Radioactivity Analysis Form



7.5 Attachment 5: Data Entry and Reporting Checklist Done? Step

No. Item

[ ] 1 Open the Microsoft Access database: V:\ESH\OHP\REP\Rad Lab\sample.mdb

[ ] 2. Opening this database should bring you to a gray start-up form labeled “Slac Environmental” & showing six buttons. (If this screen does not appear, move the cursor to the left sidebar. Under “Objects” click on [Forms] & then double click on the icon for the form named “StartUp”).

[ ] 3.

Before entering the results of counting, you must enter information on the sample. Proceed to Step 13 if you have already done that & want to enter LSC &/or Gamma Spec results or to Step 26 if you want to view or print out an analysis report for a known sample number.

Initial Data Entry

[ ] 4. Click on the button labeled “Data Entry for Taken Sample”. This will bring you to the “Taken Samples” screen. Do not enter any information if data is displayed in any field.

[ ] 5. Move the cursor to the bottom left corner of the display. To the right of the box showing that you are at record 1, click on the >* button. This moves you to an empty record at the end of the table.

[ ] 6. Click on the “Sample Id” box & enter the sample ID that is in the upper right corner of the sample label & on the RP Analysis Form. Swipes, resin, and liquid samples should to be labeled with an ID that starts with L; solids start with S0 (S-zero).

[ ] 7. Use the Tab-key to get to the “Taken Date” box. Enter the date the sample was collected (listed on the sample label & on the RP Analysis Form using the form mmddyy.

[ ] 8. Tab to the “Sample Type” box & select the appropriate sample description from the drop-down menu. For water samples submitted with paperwork asking approval for release of water to the sanitary sewer, select “Water (sewer)” – do this even if the water is storm water or LCW. For water samples from any well, select “Water (well)”. Otherwise, select the most appropriate description.



Done? Step No.

Item

[ ] 9. Tab to the “System Name” box &, based on the sample label (& RP Analysis Form), select the appropriate description from the drop-down menu – there are many choices, take a moment to select the most appropriate. Note that the wells EXW-4, MW-94, MW-30, & MW-81 are individually listed – please be sure to identify samples from them correctly! (Samples from any other wells should be identified as “GROUND H2O WELLS”.)

[ ] 10. Tab to the “Taken by” box &, based on the sample label (or accompanying paperwork), select the appropriate name from the drop-down menu.

[ ] 11. Tab to the “Sample Description and Comments” box & enter any further description that might help identify the sample. For the wells EXW-4, MW-94, MW-30, & MW-81, enter the measured distance to the top of the water, if that information appears on the sample label or RP Analysis Form.

[ ] 12.

To save the entered record for the sample, move the cursor to the bottom left corner of the display. To the right of the box showing the record number, click on the >* button. To do initial data entry for additional samples, repeat Steps 6 – 12.

Entering Analysis Results

[ ] 13. Before proceeding, assure that all analyses have been completed & have results available for entry. If not, don’t start entering results.

Note: There are some samples for which both LSC & Gamma Spec analysis are required (e.g. samples from EXW-4, MW-94, MW-30, & MW-81, BDE LCW, BDE sump, storm water, etc.).

[ ] 14. If necessary to report the specific activity (pCi/g or pCi/L) from Gamma Spec (GS) analysis, determine the sample weight or volume and calculate the specific activity from the activity determined by GS before proceeding with data entry.

[Note: The output from GS provides radionuclide identities and activities. The activities reported by the GS system assume the sample had the same volume, shape, composition, density, counting geometry, etc. as the applicable standard did at the time the calibration was done. The accuracy of the activity reported by the system for a sample will decrease if this is not the case.]



Done? Step No.

Item

[ ] 15. In the start-up screen, click on the button labeled “Data Entry for Released Sample”. If you are in another screen (e.g. the “Taken Sample” screen), move to a blank record, then use the innermost “x” in the upper right corner of the display to close that window – this should bring you to the start-up screen. (If elsewhere in the database, move the cursor to the left sidebar. Under “Objects” click on [Forms] & then click on the icon for the form named “StartUp”).

[ ] 16. Before entering any data, move the cursor to the bottom left corner of the display. To the right of the box showing that you are at record 1, click on the >* button. This moves you to an empty record at the end of the table (>4600 as of July 2004).

[ ] 17. Enter the sample ID in the box labeled “SAMPLE ID #”.

[ ] 18. Tab to the “Released_Date” box and enter the date the sample was analyzed, using the form mmddyy.

[ ] 19. Proceed to Step 22 unless the sample is water.

[ ] 20. If the sample is from water that is to be released to the sanitary sewer, tab to the “Amount” box and enter the volume for release (in gallons). In most cases, this volume will be listed on the RP Analysis Form. Water from the four wells EXW-4, MW-94, MW-30, or MW-81 (unlike all other wells at SLAC) is always released to the sewer, but if you have no information on the volume that will go to the sewer, enter 1 (gallon) – this will be noted & corrected later.

[ ] 21. If the sample is from water that is to be released to the sanitary sewer, tab to the “To” box & select “SS sanitary sewer” from the drop down menu.

[ ] 22. Using the cursor, move to field labeled “Nuclide”. If no radioactivity was detected using the Liquid Scintillation counter, press the “*” key. If no radioactivity was detected using the Gamma Spectrometer, use the “.” key. This will fill-in the field with *NDA or .NDA, indicating no detected activity. Otherwise start typing the radionuclide symbol &/or select from the choices on the drop-down menu.

[ ] 23. If radioactivity was detected, enter the applicable activity or specific activity (by volume or weight), in the field labeled “Concentration”. Note that for all liquid samples, results are normally recorded as a concentration (pCi/L); for solids, they are recorded as a sample activity (pCi), unless there is a specific request.



Done? Step No.

Item

[ ] 24. Select the units that apply to the info entered in the “Concentration” field, even if the sample is NDA:

For LSC For GS For swipes

pCi/Liter pCi – GS pCi/Swipe

pCi/Gram - LS pCi/Gram - GS DPM/swipe

Qualitative

pCi/Liter - GS

[ ] 25. If more than one radionuclide was detected for this sample, use the >* button at the bottom of the dark gray box to move to add a record to the table of radionuclides. Repeat Steps 22 – 26 until all detected radionuclides and quantities have been entered for this sample.

[ ] 26.

To save the entered information for the sample, move the cursor to the bottom left corner of the display. To the right of the box showing the record number, click on the >* button. To record results for additional samples, repeat Steps 13 – 26.

Print the Analysis Report

[ ] 27. Viewing or printing an analysis report: before proceeding, assure you have the sample ID(s) for the sample(s) of interest.

[ ] 28. In the start-up screen, click on one of the buttons labeled “Analysis Report”. (See instructions in Step 15 if you are in another screen.)

[ ] 29. Enter the sample ID of interest & [OK].

[ ] 30. Before printing the report, make sure it has the relevant info report may be blank if the sample ID is not in the database.

[ ] 31. Follow steps in procedure Sample Analysis Checklist for signatures, distribution, & filing of the report(s).

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General Counting Procedure