USR UNITED STATES ENVIRONMENTAL PROTECTION AGENCYREGION 111

CENTRAL REGIONAL LABORATORY-'••- '" 839 BESTGATE ROAD 301-224-2740

ANNAPOLIS, MARYLAND 21401 FTS-922-3752

DATE :0uly10,1985 -

SUBJECT: Revised C & R Battery QA Review /&-..."*•

FROM -Patricia J.' DPOQA

TO .Darius Ostrauskas (3HW23)'Environmental Scientist

Enclosed you will find the revised C & R Battery report. I apologize forthe delay but I got hit with the flu and that set things back a little. .As you can see, I decided to stick with the regular format and amsimultaneously sending the report to FIT. The data review was/btfsed onthe S.O.P., our discussions, and my own analytical experience.' I believethe coding (semantics aside) accurately reflects the useability of thedata. In general, I only rejected data when I felt the results wereextremely suspect and considered results "estimated" when one or more QCcriteria cast suspicion on the result but did not prohibit using it fordecision-making. Let me know if you have any questions.

cc: Etl Skernolisv/Butch ByerGarth GlennDick Brunker

7

Site Name: C & R BatteryTOD No.: F3-8503-29

6.2.2 Inorganic Data Lab Case 4265

6.2.2.1 Introduction

The findings offered in this report are based upon a review of all availablesample data, blank results, matrix spike and duplicate analysis results, ICPinterference QC, calibration data, and quality assurance documentation.

6.2.2.2 Qualifiers " " - - - - - - - ------

It is recommended that this data package be utilized only with the followingqualifier statements:

0 The results which may be qualitatively questionable are listed below:

Constituent Samples With Questionable Results

Aluminum MCB311, MCB244, MCB246, MCB248, MCB249, MCB228

Iron - MCB311, MCB244, MCB226, MCB228, MCB246, MCB248

Zinc MCB311, MCB244, MCB226, MCB228, MCB246, MCB248,MCB249

The aforementioned results were designated questionable since there isevidence to doubt the presence of these constituents at any concentrationless than or equal to the levels reported. However, it can be assumedthat concentrations significantly greater than the levels reported forthese samples cannot be present.

Low level results for lead in aqueous samples should be considered highlyquestionable (Code R). The high level reported for MCB227 should beconsidered an estimate of the true amount present (code J).

Actual detection limits for arsenir, cobalt, and manganese in the aqueousmatrix may be slightly higher than reported. Reported results may bebiased low for arsenic (25-45%), cobalt (25-35%), and manganese (25-35%)in the aqueous matrix. Values have been coded J to reflect the quantitativeuncertainty of the results.

Actual detection limits for tin in the aqueous matrix may be significantlyhigher than reported (30 ug/L). In fact, the reported detection limit forMCB227 is 300 ug/L.

The reported results "for antimony, cadmium, lead, silver, tin, and zincin solid sample MCB233 may not accurately reflect the average concentrationfor these .constituents in this sample or others of a similar matrix.

100108

Site Name: C & R BatteryTDD No.: F3-8503-29

The reported results or antimony, cadmium, copper, magnesium, nickel,potassium, sodium, tin, and cyanide in field duplicate samples MCB238/239(solid) may not accurately reflect the average concentrations of theseconstituents in these samples or others of a similar matrix.

Actual detection limits for arsenic and selenium in the solid matrix may bebiased slightly higher than reported. Reported results may be biased lowfor arsenic (30-50%) in the solid matrix.

Reported results may be biased high for barium (40-60%), beryllium (40-60%), cadmium (60-80%), chromium (30-50%), copper (35-55%), manganese(20-40%), mercury (30-50%), nickel (25-45%), tin (300-450%), vanadium(40-50%), and zinc (25-45%) in the solid matrix.

The impact, on solid sample results, of the poor field and lab precisionand poor spike recovery is as follows:

antimony — data rejected—extreme precision problems

arsenic -^ values considered valid estimates (J) except for MCB239 (reviewof the raw data suggests, that 103 is an anomaly and should berejected).

barium — values considered estimates due to recovery problemsberyllium ....-..--.-..chromiummanganese .. ~ • .mercurynickelvanadium

cadmium ~ estimated due to precision (field and lab) and recovery problem

copper ~ estimated due to precision (field and lab) and recovery problemzinccyanide

silver — data "rejected—extreme recovery problems

tin — data rejected—extreme precision and accuracy problems

Data has been coded 0 or R to reflect these qualifiers.

The presence/absence of cyanide in MCB234, MCB237, and HCB239 could notbe determined. ....: .._ .- ... - —---.--.:-~. .—--.-7 .-

Mercury results for all aqueous samples could not be validated.

100109

Site Name: C & R BatteryTDD No.: F3-8503-29

6.2.2.3 Findings ...

0 Field blank analysis revealed the presence of aluminum, iron, and zinc atlevels sufficient to question the aforementioned results for theseparameters.

0 Aqueous field duplicate (MCB244/311 and MCB226/228) analysis for leadexhibited unusually large relative percent differences for groundwater-type samples. That fact, along with failure to recover lead in the matrixspike, suggests that the reliability of the aqueous lead results isseverely compromised and the results should be rejected. The levelreported in MCB227, however, is sufficiently large that it can be consideredan indicator, not only of the presence of lead, but also the relativeorder of magnitude. Due to the problems discussed above, however, thevalue should be considered an estimate of the true concentration.

0 Low matrix spike recovery was reported for arsenic (65%), cobalt (70%),and manganese (70%) in the aqueous matrix.

0 Extremely Tow matrix spike recovery was reported for lead (0%) and tin(0%) in the aqueous sample MCB244. Lead values have been coded to reflectthe poor recovery. False negatives for tin cannot be ruled out.

0 Duplicate laboratory analysis of solid samples MCB233 revealed poorprecision for antimohy,~clTdmium, lead, silver, tin, and zinc.

0 Solid field duplicate results for antimony, arsenic, cadmium, copper,magnesium, nickel, potassium, solium, tin, zinc, and cyanide exhibitedhigh relative percent differences. This variability is normally associatedwith poor sample homogeneity.

0 Low matrix spike recovery was reported for arsenic (60%) and selenium(60%) in the solid matrix.

0 High matrix spike recovery was reported for barium (141%), beryllium(152%), cadmium (172%), chromium (138%), copper (144%), manganese (131%),mercury (142%), nickel (136%), tin (376%), vanadium (147%), and zinc(135%) in the solid matrix.

0 The laboratory reported that interference problems precluded a quantitativedetermination of cyanide in MCB234, MCB237, and MCB239.

0 Laboratory failed to analyze matrix spike and duplicate samples formercury in the aqueous samples.

0 Review of method of standard addition analysis by furnace"raw data forMCB238/239 revealed an analytical anomaly. The 103 ug/L value should berejected. . . . . _ . - _ - _ • •

6.2.2.4 Summary

This Quality Assurance Review has identified the following areas of concern;field blank contamination, sample non-homogeneity and poor precision, poormatrix spike results, and matrix interferences.

Please see the accompanying support documentation appendix for specifics onthis Quality Assurance Review.

Report prepared by Steve L. Markham:£

PPatricia 0. Krantz:^3rrTo^J-> Pate:-(301)224-2740, FTS 922-3752

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PR03ECT NAME; £"# ft AafJefY_____ EPA SITE NO,TDD NO; }~Jt~~&3oZ -& ? ~ REGION:

QUALITY ASSURANCE REVIEW OFINORGANIC ANALYTICAL DATA PACKAGE

Case No.: fygJ& T' -'-- "-' —"---.- _ Applicable Sample No's.:ContractContract Laboratory: ^'?g^w^CW» W - - " : -•Mchad'>;Mei?Z8 ,/*c& Z2o,M& £%.**>Applicable IFB No.:Reviewer:Review Date: _____________________ A*iA5tZ9;'/.icfi3y3.#ir&"~~ " " - - - - - — - ~ _ / -^ ~

The inorganic analytical data for this case has been reviewed. The quality assurance evaluation issummarized in the following table:

Revi ewer's E vai uati on*

'\cceptable\cceptable withexception(s,M|stiorableCTTTacceptabie

FractionTASK I

ECP or AAMETALS

0)

TASK II' FURNACE AAMETALS

TASK IIICOLD VAPOR AAMERCURY

TASK IIICYANIDE

* Definitions of the evaluation score categories are listed on next page.

This evaluation was based upon an analysis of the review items indicated below:

• DATA COMPLETENESS • INITIAL CALIBRATION VERIFICATION• BLANK ANALYSIS RESULTS • CONTINUING CALIBRATION VERIFICATION• MATRIX SPIKE RESULTS @ INTERFERENCE QC RESULTS• DUPLICATE ANALYSIS RESULTS • DETECTION LIMITS RESULTSO STANDARD ADDITIONS RESULTS • INSTRUMENT SENSITIVITY REPORTS• QUANTITATIVE CALCULATIONS

Data review forms are attached for each of the review items indicated above.^=No errors noted, no form attached.9 Spot Check performed.

Comments; H)&

DATA EVALUATION SCORE CATEGORIES

ACCEPTABLE; Data is within established control limits, orthe- data which is outside established control

• ' '; limits does no£ affect the validity of theanalytical results. •

ACCEPTABLE WITH EXCEPTION CS); Data is not completely within 'established control limits. The deficiences are .identified and specific data is still valid,•given certain qualifications which are listed below.

QtlESTIONABIEt Data is not within established control limits.———————:——The deficiences bring the validity of the entire

data set into question. However, the data validityis neither proved nor disproved by the availableinformation.

UNACCEPTABLE; Data is not within established control limits.—————————The deficiences imply the results are not meaningful.

DATACOMPLETENESS

FIELD QC

TASK 1 ;ICAPOR AA:METALS

TASK 11 :FURNACEAA:METALS

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TASK in:CYANIDE

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TRAFFICREPORT **LAB 1.0. **

BLANK

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TAB. RESULTS

TAB, D.L.'s

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100118

DATAicoMPcereMEs

7 FIELD QC

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TRAFFICREPORT *LAB I.D. «

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BLANK ANALYSIS RESULTSTASK

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LABORATORY REPORTED FIELD BLANK DATA IS COMPARED WITH THE SAMPLE DATA IN A TABULATION FORM WITHlfSAMPLE ANALYTICAL DATA SUMMARY.

COMMENTS:(1) RESULT REPORTED BY LABORATORY AND CONFIRMED BY REVIEWER.

(2) RESULT INFERRED FROM RAW DATA

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100120

C43Duplicate Analysis Results

rne applicable duplicate pairs are:

sample no.

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The relative percent difference (RPD) for each parameter group wasduplicate analysis RPD acceptance criteria should be:

maximum acceptable

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evaluated. The

T itf— Percent Difference

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The RPD's exceeding the maximum acceptable percent difference were:

W£"0?iX Compound - Actual RPD CA W- SampleA® JTAJA/ C*°iS"ff ~ ft/ W J /,-3,/

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Duplicate Analysis Results

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sample no.

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The relative percent difference (RPD) for each parameter group was evaluated. Theduplicate analysis RPD acceptance criteria should be:

maximum acceptableMftri?^ Percent Difference

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» S & U ' ± V f t %•The RPD's exceeding the maximum acceptable percent difference were:

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-MATRIX SPIKE RECOVERIES

/ ..... . . . . . . . .__.Sample No. **Field Spike

OftfGLab Spike I/ VMatrix AQCone. LevelMethodStd.

All matrix spike recoveries were within the established control ranges specified in;FB WAS -A , Exhibit E, Table 2. " .. -._. - . . . . Yes

Except! on{s):

ParameterAcceptedRanse (96)

Actual% Rec

SampleNumber

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Comments:

100123

MATRIX SPIKE "RECOYER^S

Sample No.Field SpikeLab SpikeMatrixCone. LevelMethodStd.

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All matrix spike recoveries were within the established control ranges specified in; . /EFB WAS -A , Exhibit E, fable 2. . . . . . . . . .. . .. . Yes ^No

Except: on Cs):

Parameter' /3o

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Comments:

100124

STANDARD ADDITION RESULTS

^^umentation indicates a standard addition correction was performed•|all spiked samples for parameters having recoveries outside ofcontrol limits: Yes____ No____

For the parameters having poor recoveries in the spiked sample (s),standard additions were also performed on all other samples wherethe following conditions were met:

(1) The sample matrix was similar to the matrix of the samplewhich was spiked; and

(2) The parameters in question were detected with postive results.No

The parameters with poor spike recoveries are listed "below, alongwith the type of standard addition performed (none, 1, 2, or 3 point).The results for these parameters in other samples which have a similarmatrix are also listed below s

ranrale

*description of .matrix

•"NV\XN

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parameter

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recovery,

,

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type of std. add.

Comments:

Initial Calibration Verification and Continuing Calibration Verification

Documentation indicates calibrations were performed and checked every ten samples: Yes'Exceptions:

Calibrations and verifications were all within the control limits

Outliers are listed beiov

Parameter

/:AcceptableRange (%)

•

CalibrationIdentifier

%ofTrue Value

\

Qp. - ———————— -specified in ''"'M/

/ Yes _ /_ Nc

Comments

Interference QC Results - , - - - ... .-. - ., _ ... z,-;.--- -™ . "."1".!L— „- . -... . •• •Documentation indicates interference QC samples were run before and after every ten samples: Yes __ Nc

**"\ i t

Interference QC results were all within the control limits specified" in— V /: EFA Cite *nr tf\vnl>cl/N*&^ ©JT— nw A Yes*/ No

Exceptions:

Parameter

»

AcceptableRange (%)

CalibrationIdentifier

96 ofTrue Value Comments

lOOiiib

--•QUANTITATIVE CALCULATIONSERRORS AND CORRECTED RESULTS "ARE LISTED BELOW

10012 I-

Detection Limits Results

Detection limits were reported for all samples analyzed: Yes t/ No

Exceptions:_________;__________-__ __

Detection limits were less than or equal to the required detection limitsspecified in c>^ *v/< V; ....: 7~ ' - -...._ Yes No

Exceptions:____________________________________

"'^Instrument Sensitivity Reports

Instrument sensitivity reports were documented for all parameters:

Yes No

Comments:

Other Remarks Concernina this Case:

There are currently no established control ranges for ICP interference checkstandards. However, although not a contractual requirement, 85% - 1152J is c'.i""here as a tentative guideline for evaluation. Outliers of this tentative -control ranoe, if any, are tabulated on the bottom of the preceeding page.

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