LABORATORY DATA QUALITY ASSESSMENT AND … 5-9-17/1-DQA2017... · LABORATORY DATA QUALITY ASSESSMENT AND DATA USABILITY EVALUATION FOR ENVIRONMENTAL ... Metals By SW-846 Method 6020

LABORATORY DATA QUALITY ASSESSMENT AND DATA USABILITY EVALUATION FOR ENVIRONMENTAL INVESTIGATION AND REMEDIATION PROJECTS

Schedule

9:00 9:20 AM (20 minutes): Introduction and overview of training Peter Hill Nora Conlon

9:20 9:50 AM (30 minutes): Introduction and overview of the RCPs

Paul Clark

9:50 10:10 AM (30 minutes): Roles and Responsibilities for DQA/DUE Process and Documentation Lisandro Suarez Allison Forrest-Laiuppa

10:10 10:30 AM (20 minutes): Pop Quiz

Rebecca Mertz 10:30 10:45 AM (15 minute): Break 10:45 12:15 PM (1.5 hours): Data Quality Assessment Jim Occhialini 12:15-1:00 PM (45 minutes): Lunch 1:00 3:15 PM (2.25 hours): DQA/DUE Issues and Solutions with Interactive Case Studies

Presenters: Mike Ainsworth, Christina Clemmey, Dr. Gail Batchelder, and William Flick Assistants for Case Studies: Tamara Burke Devine, P.E., LEP, Nora Conlon, and David Clymer (maybe)

3:15 3:45 PM (30 minutes): DEEP/LEP Panel Discussion Moderator: Nora Conlon Panelist: Peter Hill, Jim Occhialini, Mike Ainsworth, William Flick, Christina Clemmey, and Nicole Leja

3:45 4:00 PM (15 minutes): Training wrap up and questions

Allison Forrest-Laiuppa and the QA/QC Workgroup

Laboratory Data Quality Assessment and Data Usability Evaluation For Environmental Investigation and Remediation Projects

Acronym List

% R Percent Recovery 6010 Determination of Trace Metals By SW-846 Method 6010 Inductively Coupled Plasma-

Atomic Emission Spectrometry 6020 Determination of Trace Metals By SW-846 Method 6020 Inductively Coupled Plasma-

Mass Spectrometry 8081 Pesticides by Method 8081, SW-846 8260 EPA SW-846 Method 8260 for determination of volatile organic compounds 8270 EPA SW-846 Method 8270 for determination of semivolatile organic compounds APH Air-Phase Petroleum Hydrocarbons BAA Benzo(a)anthracene BAP Benzo(a)pyrene BCEE Bis 2-chloroethylether BEHP Bis(2-ethylhexyl) phthalate BLK Blank BKF Benzo(k)fluoranthene BRL Below Reporting Limit BTEX Benzene, Toluene, Ethylbenzene, and Xylenes C Degrees Celsius CERCLA Comprehensive Environmental Response, Compensation, and Liability Act, CC Continuing Calibration CCAL Continuing Calibration CCV Continuing Calibration Verification CFR Code of Federal Regulations CLP Contractor laboratory program COC Constituent of Concern or Chain of Custody Cmpd Compound Cr Chromium CSM Conceptual Site Model DDT Dichloro-Diphenyl-Trichloroethane DEC Direct Exposure Criteria DEEP Connecticut Department of Environmental Protection DMP Dimethylphenol DPH State of Connecticut Department of Public Health DQA Data Quality Assessment DQO Data Quality Objective DUE Data Usability Evaluation EA Endrin Aldehyde EDB Ethylene Dibromide EK Endrin Ketone ELCP Environmental Laboratory Certification Program ELUR Environmental Land Use Restriction EP Environmental Professional EPA United States Environmental Protection Agency

EPC Jims slide #73 EPH Extractable Petroleum Hydrocarbons EPOC Environmental Professionals Organization of Connecticut EPTH Extractable Total Petroleum Hydrocarbons ESA Environmental Site Assessment FD Field Duplicate GA PMC Pollutant Mobility Criteria for Class GA Groundwater GB PMC Pollutant Mobility Criteria for Class GB Groundwater GC/MS Gas Chromatography/Mass Spectrometry GWPC Groundwater Protection Criteria Hg Mercury ICAL Initial Calibration IDEC Industrial Commercial/Residential Direct Exposure Criteria IDOC Initial Demonstration of Capability ID(s) Sample Identification Number(s) LEP Licensed Environmental Professional LCL Lower Control Limit LCF Reasonable Confidence Protocol Laboratory Certification Form LCS Laboratory Control Sample LCSD Laboratory Control Sample Duplicate LFB Laboratory Fortified Blank MEK Methyl Ethyl Ketone MEOH Methanol MIBK 4-Methyl-2-petanone g/kg Micrograms per Kilogram g/l Micrograms per Liter mg/kg Milligrams per Kilogram MRL Method Reporting Limit MS/MSD Matrix Spike/Matrix Spike Duplicate ND Not Detected ORP Oxidation Reduction Potential PAHs Polycyclic Aromatic Hydrocarbons, also known as Polynuclear Aromatic Hydrocarbons PARCCS Precision, accuracy, representativeness, comparability, completeness, and sensitivity PCBs Polychlorinated Biphenyls PCE Tetrachloroethene, also known as Tetrachloroethylene or Perchloroethylene Pest Pesticides PP Priority Pollutants as defined by the Clean Water Act ppb Part Per Billion ppm Part Per Million QA Quality Assurance QA/QC Quality Assurance/Quality Control QAP Quality Assurance Plan QAPP Quality Assurance Project Plan QC Quality Control RCP(s) Reasonable Confidence Protocol(s) RCP Guidance Laboratory Quality Assurance and Quality Control Reasonable Confidence

Protocols, effective November 17, 2007 RPD Relative Percent Difference

RCSA Regulations of Connecticut State Agencies RCRA Resource Conservation and Recovery Act RDEC Residential Direct Exposure Criteria RF Response Factors RL Reporting Limit RPD Relative Percent Difference RRF Relative Response Factor RSR Criteria Numeric criteria presented in the Remediation Standard Regulations of the

Regulations of Connecticut State Agencies, Sections 22a-133k-1 through 22a-133-3, inclusive.

RSRs Remediation Standard Regulations of the Regulations of Connecticut State Agencies, Sections 22a-133k-1 through 22a-133-3, inclusive

Soil Guidance CTDEP's Guidance for Collecting and Preserving Soil and Sediment Samples Preservation for Laboratory Determination of Volatile Organic Compounds, effective March 1, 2006 Guidance SCGD Site Characterization Guidance Document, effective September 2007, Connecticut

Department of Environmental Protection SOP Standard Operating Procedure SPLP Synthetic Precipitation Leaching Procedure SVOCs Semi Volatile Organic Compounds SWPC Surface Water Protection Criteria SW-846 Test Methods for Evaluating Solid Wastes, Physical /Chemical Methods, EPA

Publication SW-846, United State Environmental Protection Agency TAT Turn-Around Time TCA Trichloroethane TCE Trichloroethene TCLP Toxicity Characteristic Leaching Procedure TICs Tentatively Identified Compounds TPH Total Petroleum Hydrocarbons UCL Upper Control Limit VOA Volatile Organic Analysis VOCs Volatile Organic Compounds VPH Volatile Petroleum Hydrocarbons YR Year

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ConnecticutDepartmentofEnergyandEnvironmentalProtection

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LaboratoryDataQualityAssessmentandDataUsabilityEvaluationForEnvironmentalInvestigationandRemediationProjects

May2017PresentedbytheDEEPQA/QCWorkgroup

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ConnecticutDepartmentofEnergyandEnvironmentalProtectionConnecticutDepartmentofEnergyandEnvironmentalProtection

Overviewoftodaystraining OverviewofSeminar,IntroductiontoRCPs,DQAandDUE RolesandresponsibilityforDQA/DUEprocess QuizTime Break(15minutes) ReviewofDQA Break(Lunch) DQA/DUEissuesandsolutionswithInteractiveCaseStudies

DQA/DUEPaneldiscussion Summary

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ImportanceofReasonableConfidenceProtocols,DataQualityAssessmentandDataUsabilityEvaluation

[email protected]

[email protected]

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WorkgroupMembers DEEP

RemediationDivision MaterialManagementandComplianceAssuranceDivision

DPH EPA LEPs/Consultants/EnvironmentalProfessionals DataValidators Laboratorypersonnel

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BigPicture

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ToHelpEnvironmentalProfessionals

ReasonableConfidenceProtocols(RCPs)forcommonlyusedanalyticalmethodswerepublished(Nov.2007)

SeveralofGuidanceDocumentsonRCPsandontheDQA/DUEprocesshavebeenpublished

DEEPandEPOCheldtrainingsessionsonQA/QCandRCPsin2005andDQA/DUEin2009andtoday

TheCTDEEPRemediationDivisionLaboratoryQA/QCWorkgroupwasformedin2004

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ForsamplescollectedonorafterSeptember1,2007,theDEEPexpectsthatallanalyticaldatausedtosupportremediationprojectsbegeneratedusingtheRCPs(ormethodologiesthatcontainalevelofqualitycontrolanddocumentationadequatetoevaluatethePARCCSparameters).

CTDEEPExpectationsRegardingAnalyticalDataQuality

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AnalyticalDataQuality

Analyticaldatausedforenvironmentalinvestigationandremediationprojectsmustbeofaknownanddocumentedquality.

Theenvironmentalprofessionalhastheresponsibilitytoevaluatewhetheranalyticaldataareofsufficientqualitytobeusablefortheintendedpurpose.

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BriefOverviewoftheReasonableConfidenceProtocolsandtheDQA/DUEProcess

[email protected]

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PARCCS DataQualityIndicators

Precision Accuracy Representativeness Comparability Completeness Sensitivity

PARCCSparameterscanbeusedtoexaminethequalityofmeasurementsandsamplingefforts

Source: Ohio EPA

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WhyWeretheRCPsDeveloped?

SW846methodsallowforflexibilitywithrespecttoQA/QCrequirements.

QA/QCpracticesvarywidelybylaboratory UndocumentedQA/QCpractices. InconsistencyinQA/QCdeliverables. Inconsistencyinlaboratoryperformance.

RCPsbasedonMassachusettsCompendiumofAnalyticalMethods.

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ReasonableConfidenceProtocolsKeyConcepts

RCPsweredevelopedtostandardizespecificperformancecriteriaforSW846Methodsandtostandardizedeliverablesfromlaboratoryanalysis

RCPmethodsprovideanalyticaldataofknownquality

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RCPKeyConcepts

IfReasonableConfidenceisachieved,theenvironmentalprofessionalcanhaveReasonableConfidencethatthelaboratoryhasfollowedtheenhancedQA/QCproceduresforanalyticalmethodsandreportingandhasdescribednonconformances.

ReasonableConfidencewillformthebasisforthereviewoftheanalyticaldatabytheenvironmentalprofessionaltodetermineifthedataisacceptablefortheintendedpurpose.

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ReasonableConfidenceProtocols

Purpose DataofKnownQuality

LEPsMUSTdetermineifthatdataofknownqualitymeetstheirprojectobjectives(Usable)

Alone,reasonableconfidenceisnotenough

RCPsreportnonconformancesthatareevaluatedaspartoftheDUE

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DataQualityAssessmentandDataUsabilityEvaluation

TheDQA/DUEprocess: Providesconfidencethatthelaboratoryanalyticaldataisofsufficientqualitytosupportthedecisionsbeingmade

Providesanaccurateandconsistentmeanstoassessenvironmentalimpactstoland,waterandhumanhealth

Reducesuncertaintyandtherisk(humanhealth,financial,environmental)

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OverviewoftheDQAandDUEProcess

Twostepprocess: 1ststepisDataQualityAssessment(DQA) identifyandsummarizeQCnonconformances.

2ndstepisDataUsabilityEvaluation(DUE) determinewhetherornotthequalityofthedataissufficientfortheintendedpurpose.

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DataQualityAssessment

TheDQAwillidentifyandsummarizeanyqualitycontrolproblemsthatoccurredduringlaboratoryanalysis.

TheDQAshouldbeperformedthroughoutthecourseoftheproject.

TheDQAmustbeperformedpriortotheDUE

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DataUsabilityEvaluation

TheDUEisanevaluationbytheenvironmentalprofessionaloftheresultsoftheDQAtodetermineiftheanalyticaldataareofsufficientquality,andareusablefortheintendedpurpose.

AprimarypurposeoftheDUEistodetermineifanybiasintheanalyticalresultsaffectsusability.

TheaffectofthebiascanbeevaluatedbyconsideringdifferenttypesoflaboratoryQCinformation(multiplelinesofevidence).

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DataUsabilityEvaluationTheenvironmentalprofessionalwillalsousetheresultsoftheDQAtoevaluatetheusabilityoftheanalyticaldatawithinthecontextoftheprojectspecificobjectivesandtheconceptualsitemodel(CSM).

Thisincludesconsidering: volumeofdataavailableforthesite

screeningleveldata fieldobservations

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TypesofAnalyticalDataTypeofData Description DataQualityAssessment

RCPData AnalyticaldatageneratedusingtheRCPs.Evaluateprecision,accuracy,andsensitivity.

NonRCPData

AnalyticaldatageneratedfromsamplescollectedafterSeptember1,2007usinganonRCPmethodwherethereisanexistingRCPmethod(useReasonableConfidenceEquivalencyDeterminationForm);OR,

DemonstrateequivalencywiththeReasonableConfidenceProtocols RCPEquivalencyDeterminationRequestFormrequired.Evaluateprecision,accuracy,andsensitivity.

AnalyticaldatageneratedfromsamplescollectedafterSeptember1,2007whennoRCPmethodispublished.

Evaluateprecision,accuracy,andsensitivityusingQCdataequivalenttoasimilarRCPmethod.

PreRCPDataAnalyticaldatageneratedpriortoSeptember1,2007thatwerenotgeneratedusinganRCPmethod.

UseexistingQCdatatoevaluateprecision,accuracy,andsensitivity.IfprecisionandaccuracyQCdataarenotavailable,evaluatesensitivity.

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DQAandDUEFlowChart

CSM

SamplingPlan,FieldQA/QC,andMethod

Selection

AnalyticalData,FieldObservations,

HydrogeologicalandPhysicalData

CollectAdditionalLaborFieldData

Modify/ExpandInvestigation/Remediate

CollectAdditionalLaborFieldDataModify/Expand

Investigation

RepresentativenessEvaluation

DoestheInformation/DataRepresenttheSiteandSupporttheCSM?

DUE AretheAnalyticalDataAdequatefortheIntendedPurpose

BasedonaReviewofQCNonconformances

andInformation?

DataisRepresentativeandofAdequateQualitytoSupportEnvironmentalProfessionalsOpinion

NO

YES

YES

DQA IdentifyNonConformances

NO

Start

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Questions

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DetailedlookatTheReasonableConfidenceProtocols

[email protected]

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WhatsIntheRCPs? Performancecriteriaforlaboratoriesregardingcalibration,

qualitycontrol,andreporting.

Guidanceonwhatthelaboratoryshoulddoifanalyticalproblemsareencountered.

Uniformtargetcompoundlists.

Requiredlaboratorydeliverables.

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GeneralDescriptionoftheRCPs

OverviewofMethod: Reportingtolowestcalibrationstandard. GeneralQCperformancecriteria.

SamplePreparationRequirements.

AnalysisDescription.

Interferences.

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DetailsofRCPs

Analyte List: Allcompoundscalibratedandreportedunlessdirecteddifferentlybytheenvironmentalprofessional.

ReportingSpecifications: BatchMS/MSDnotreported. ResultsbelowRLreportedasND,NoJflags. Specificlistofreportdeliverables. Soils/Sedimentsondryweightbasis.

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DetailsoftheRCPs

HoldingTimes.

Preservation.

SampleContainerTypes.

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ImportanceofTable1A

EachRCPmethodhasaTable1a SummarizestheQCperformancecriteria

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RCPLaboratoryCertificationForm

PerformancecriteriaforlabstocertifythedatameetsRCPswithexceptionsnotedinnarrative. 7questions Requiressignature Cantbealtered

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LaboratoryNarrative

Allreportsmusthaveanarrative.

Describeindetailallnonconformances.

Provideallsamplesandanalytes effected.

Narrativesshouldbesamplespecific,asappropriate.

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LaboratoryCommunication Oftenlaboratorydatadoesnotmeetintendedusedueto

wrongcompoundlist,incorrectmethodemployed,reportinglimitstoohigh,etc.

Problemscanbeavoidedbylistingprojectdatarequirementsbeforesampling,forexampleinaprojectQAPPorworkplan.

AND

Communicatingtherequirementstothelaboratory. TheProjectCommunicationForm,orothersimilardocument,canbeusedforthispurpose.

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WhatMethodsCurrentlyHaveRCPs?

8260 VolatileOrganics 8270 Semivolatile Organics 8081 Pesticides 8082 PolychlorinatedBiphenyls(PCBs) 8151 ChlorinatedHerbicides 8021 VolatileOrganics 1311 ToxicityCharacteristicLeachingProcedure(TCLP) 1312 SyntheticPrecipitationLeachingProcedure(SPLP) 7196 DeterminationofHexavalentChromium ETPH ExtractableTotalPetroleumHydrocarbons

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WhatMethodsCurrentlyHaveRCPs? 6010 InductivelyCoupledPlasmaAtomic

EmissionSpectrometry 6020 DeterminationofTraceMetals 7470/7471 DeterminationofMercury 7000 SeriesDeterminationofMetals 9010/9012/9014 DeterminationofTotalCyanide T013A PAHs TO15 VolatileOrganics TO17 VolatileOrganics VPH VolatilePetroleumHydrocarbons EPH ExtractablePetroleumHydrocarbons APH AirPhasePetroleumHydrocarbons

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Questions

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RolesandresponsibilitiesforDQA/DUE

[email protected]

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GuidanceDocument:DQA/DUECommunication

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EnvironmentalProfessionalsResponsibilityDuringProjectSetup:

QAPP/RCPs ProjectObjectivesandCSM

Sourceandnumberofsamples Samplingmethods,samplehandling&QCrequirements

Communicatewithlaboratory Requestappropriatesamplingcontainers,preservation,holdingtimes,andarchivingofsamples

Requestappropriatereportinglimits&RCPmethod ProvideaChainofCustodyandproperlypreservedsampleswithinholdingtimes

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LaboratorysResponsibility

TheLabprovidestheEnvironmentalProfessionalandotherswith: Samplecontainerswithpreservative

SignoffonChainofCustody LaboratoryDatawithQA/QCinformation

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LaboratorysResponsibility

TheLabprovidestheEnvironmentalProfessionalandotherswith: LaboratoryAnalysisQA/QCCertificationForm

7questionswithsignature Narrativeofnonconformances

Answerquestionswhenasked

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EnvironmentalProfessionalsResponsibility UponReceivingDataPackage:

ReviewLaboratoryDataPackageforcompletenessinatimelymanner

ReviewRCPCertificationForm ReviewNarrativeandChainofCustodyandlookforanyQA/QCissues

Communicatewithlaboratoryifthereareanyissueswiththepackage

Reviewandevaluatethelaboratorydataandnonconformancesinatimelymanner

Communicatewithlaboratoryifthereareanyquestions

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EnvironmentalProfessionalsResponsibility Perform/DocumentDQA/DUEProcess ReviewQA/QC

Lookbeyondnarrativeandreviewlaboratorydata

Assessthequalityofthedata Evaluatetheusabilityofthedata Demonstrateanddocumentanunderstandingofthequalityandusabilityofthedataforreportingpurposes

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Questions

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DocumentingtheDQA/DUEProcess

[email protected]

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Commonproblemswithdocumentation

DQA/DUEisnotdoneatall DQA/DUEisnotwelldocumented

Isnotsuccinct Doesnotshowreviewbeyondlabnarratives

Incorrectuseofmethoddetectionlimitinsteadofreportinglimit

RCPmethodLaboratorynarrativeclutteredwithextras,notjustnonconformances

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ConceptsofGoodDQA/DUEDocumentation

WelldocumentedDQA/DUE Understandingandappropriatenesstotheprojectobjectives Screening CharacterizationCompliance Verification?

RegulatoryCriteria

UnderstandingoftheConceptualSiteModel Historyofsiteandpreviousenvironmentaldata Representativenessanduniformityofsamplescollected

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Discussesessentialnonconformances Evaluatesprecision,accuracy,andsensitivityofthedataandhowtheymayimpacttheusabilityofthedata

Considersmultiplelinesofevidence

ConceptsofGoodDQA/DUEDocumentation

IncludesreviewofChainofCustody Explainspossibleimpactstodataoutsideoflaboratoryanalysis

Isconcise

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ExampleofDQAWorksheet

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ExampleofDUEWorksheet(page1)

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ExampleofDUEWorksheet(page1,continued)

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ExampleofDUEWorksheet(page2)

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ExampleofaDQA/DUETextSummaryOnesoilwascollectedattheCleanerspropertyat967Breadbaker Lane,NowhereCTandsubmittedtoastatecertifiedanalyticallaboratoryforvolatileorganiccompounds(VOCs)usingtheReasonableConfidenceProtocol(RCP)Method8260.ThissamplewascollectedtoconfirmtheresultsofapreviousinvestigationthatconcludedthataPCEreleaseareaislocatednearalocationusedfordrycleaningfilterstorage.Thesitewasusedadrycleanersforatleast40yearsfrom1950to1990.

AdataqualityassessmentanddatausabilityevaluationwasperformedfordatageneratedinaccordancewithCTDEEPguidanceandnotedthefollowingqualitycontrolnonconformances.

MethylenechloridewasfoundinalaboratoryblankandinasampleataconcentrationlessthantheclassGAGroundwaterProtectionCriteria(GAPMC)asaresultoflaboratorycontamination.

ContinuingCalibration,LaboratoryControlSamples,andMatrixSpike/MatrixSpikeDuplicatesexhibitedbiasforpoorperformingcompoundsandseveralothercompoundsthatarenotconstituentsofconcernatthereleasearea.

Thesamplewasnotfrozenwithin48hoursofcollectionandexhibitslowbiasforVOCs.Tetrachloroethene detectedinsampleat400g/kgwellaboveGAPMCof100ug/kg.

GroundwaterdataindicatesthataPCEreleasehasoccurredatthesite.BasedontheabovefindingsfromtheDQAandDUE,theanalyticaldataisadequatequalityandofsufficientaccuracy,precision,andsensitivitytoconfirmthatremediationofthisreleaseareaisrequired.Furtherinvestigationwillbeconductedtocharacterizetheextentthisreleasearea.DQAandDUEworksheetsareincludedintheappendixtothisdocument.

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Reportsshouldinclude

Discussionofyoursitedecisionanddatausabilitystatement

LaboratoryDataandNarratives RCPAnalysisandRCPQA/QCCertificationForm

ChainofCustody

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Reportsshouldinclude

DQA/DUEWorksheetsordocumentationofthoughtprocess

SummaryoftheevaluationallQA/QCissuesandlaboratorynonconformances

Anyotherpertinentinformation

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Questions

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MultipleChoiceA.YesB.NoC.ItDepends

RebeccaMerzEurofinsSpectrumAnalytical,[email protected]

QuizTime

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DoesthelaboratoryneedtoknowthatyourprojectfallsundertheCTRCPprogramandthisformshouldbeincludedwithyourreport?

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SurrogatesOutsideCriteriaLEPJoesubmittedtwo1Lambersfor8270analysisforstandardTATandnotesSWPCcriterianeedstobeachieved.AcenaphtheneistheCOC(SWPC=0.3ug/L).

Whenyoureceiveyourlabreportthenarrativestatesthatthesurrogaterecoveryforthissampleisoutsideofestablishedcontrollimitsduetoasamplematrixeffect.Thelabhasreextractedandconfirmedmatrixinterference,however,thereextractionwasperformedoutsideholdingtime.

Acenaphthenereportableconcentration(original)0.26ug/L(reextract)0.29ug/L

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ChainofCustody101Doesyourchainneedtomatchyourlabelsforthefollowing? sampleID,collection,date,time,andprojectname/site

location?Doyouneedtobespecificwithyourmethods? Metals

Ifusingcontainercapstowriteinformationshouldthesame

informationmustbeonthelabel?

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CASENARRATIVE:

SW8466020AArsenicThemethodblankcontainsanalyteataconcentrationabovetheMRL;however,concentrationislessthan10%ofthesampleresult,whichisnegligibleaccordingtomethodcriteria.

Table1ASpecificQA/QCRequirementsandPerformanceStandardsforMethod6020

LaboratoryBlankContaminationassociatedtoMetalssamples

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TheresultreportedforPCEisflagged"E"orestimatedbecausetheresultwasabovethecalibrationrangeoftheinstrument.Thelabperformedadilution.

Shouldbothsetsofdatabeincludedinthelabreport?

WhichresultshouldbeusedforNDconcentrations?

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LCS/LCSDLowBiasBariumpercentrecoveries(83/79)areoutsideindividualacceptancecriteria85115.Resultsofthefollowingsamplesareconsideredtohaveapotentiallylowbias. GiventheexamplebelowwhataresomeDUE

considerations?

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WhatiswrongwiththisVOCSample?Whatpotentialissuesmightthelabhaveduringanalysis?

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15MinuteBreak

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DataQualityAssessment(DQA)

[email protected]

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Topics for Discussion

Overview

Quality

Data Quality Assessment (DQA) Data Usability Evaluation (DUE) Data Management

Lab Report Review

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WhyisDataUsabilityImportant??

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Its all about managing uncertainty

and incorporating that uncertainty into your decision making

risk of wrong decisionCERTAINTY

RiskTolerance

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Relationship Between Risk Tolerance & Uncertainty

Do you evaluate all your data the same way? Final clean up verification samples

vs. initial site screening?

Level of scrutiny applied to laboratory data commensurate with what it will be used for Risk assessment? Locate hot spots?

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Field/Sampling

contaminantdistribution/homogeneity

samplelocationrationale

samplingmethod

preservation&handling

calibrationpreparationperformanceQAprogram

Lab+ =

TotalUncertainty

QUALITATIVE+

QUANTITATIVE

Sources of Uncertainty

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EPA Program wide approach

CERCLA (superfund) Contractor laboratory program (CLP) - PRESCRIPTIVE

Project specific approach RCRA

SW-846 GUIDANCE Quality Assurance Project Plans (QAPPs)

Data Quality Objectives (DQOs) for RI/FS ~1984 States

Program wide approach CT Reasonable Confidence Protocols (RCP) ~2006

RCP DQA/DUE MA Compendium of Analytical Methods (CAM) ~2003

MCP REDUA 2007 NJ DEP Technical Guidance 4/2014

Regulatory Approaches to Managing Uncertainty

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WaitaminutearentlabsCERTIFIED?

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ConnecticutDepartmentofEnergyandEnvironmentalProtectionConnecticutDepartmentofEnergyandEnvironmentalProtection73

CERTIFIEDMEANS:

YES,yourequalified

Certification is provided through a formal process of application, audit and approval of a laboratories' quality system. Certification must be renewed annually

Comprehensive, well thought-out process, based on approval of a laboratories quality system

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...solabcertificationmeanseverythingisinplacetoproduce

dataofknownquality

Doesntmeanthatalldatageneratedbythelabisof

knownqualityorthedatainyourreport

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LABORATORY

QA/QC

OVERVIEW

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QA&QCSeparateFunctions

QualityControl (2components)1. QCinfrastructure2. Continuingmonitoring/documentingdataquality

1. Internallabsystemcontrol&project specificDQIinfo

QualityAssurance Assures theQCisperformed,enforcer Systematic&performanceaudits

Doesthelabperforminternalaudits? Followuponcorrectiveactions?

QualitySystem

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Reasonable Confidence Process

DataQualityAssessment(DQA) Identifynonconformances

Data Usability Evaluation (DUE) Impact of non-conformances on your useofthedata

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79

sowhatdowemeanbydataquality?

Thedegreeofqualitative&quantitativeuncertaintythatexistsinthedataset

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How Do You Evaluate Data Quality?

Precision ExpressionofVariability,howreproducibleisthedata?

Accuracy ExpressionofBias,observedversustruevalue

Representativeness Doesthedataprovideatruereflectionoftheactualsite

conditions?

Completeness doIhaveenoughusabledatatosupportdecisionmaking?Valid

dataforidentifiedcriticalsamples?

Comparability applestoapplesAremultipledatasetsvalidcomparisons?

Sensitivity dothereportinglimitssupportregulatorycriteria?

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PARCCS

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Whatisdataofknownquality???

Known PARCCs

From the laboratory perspective The accuracy, precision and

sensitivity is ascertainable

Whatitisntnecessarily


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How Do You Get Data of Known Quality

LevelofuncertaintyisknownHOW?

1. Datagenerated&reportedinaccordancewithanRCPprotocol

2. Datagenerated&reportedwithafulldatadeliverablespackage

IncorporatingacomprehensiveQAPP&completedatavalidation

3.LabfollowedSPECIFIC,WELLDOCUMENTEDmethodsWithdetailedperformance,QCrequirementsandcorrectiveactions

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RCP compliant data and QUESTION 4 Were all QA/QC performance criteria specified in the

DEEP Reasonable Confidence Protocol documents achieved? YES

Further data quality assessment may not be necessary LEP should still review the data Known quality data, WITH NO NON-CONFORMANCES

Data usable as is for all applications Still need to review reporting limits versus regulatory criteria

DataQualityAssessment

Unfortunately

StartingtheProcess

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There are usually some non-conformances

Documentthemaspart

oftheDQA

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Data Quality Assessment Where do I start?

LAB NARRATIVE (list of non-conformances) Includes all issues of significance to data user: method

performance problems, QA/QC outliers, etc. Lab report BATCH QC summary data section Lab report SAMPLE SPECIFIC QC data pages

What do I need to know? Data quality indicators (info for usability purposes)

Accuracy Precision Sensitivity (reporting limits)

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Is there bias? Lab measurement system

in control? Sample - specific

interferences?

Dataqualityindicatorsmeasurementtool:

blanks&spikes%Rcanindicatepositiveornegativebias

MV

TV X100=%R

WhereMV=MeasuredValue&TV=Truevalue

Spike recovery:

Accuracy Evaluation of Bias that Exists in the Measurement System

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Accuracy LabDataQualityIndicatorsLab Batch QC

Lab control sample (LCS) if done in duplicate (LCS / LCSD) Baseline accuracy determination, entire target analyte list Potential POSITIVE or NEGATIVE bias

Matrix spike/matrix spike duplicate (MS/MSD) Same as LCS/LCSD w/spike added to actual sample

Laboratory method blank False positive indicator, potential POSITIVE bias

Sample Specific QC

Surrogate Spikes Chemically similar subset of analytes

Added to every sample (organics analysis) 24

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Sample Specific QC Surrogate Spikes

Chemically similar subset of analytes

Hold times (sample & parameter specific QC element) False negative indicator, potential NEGATIVE bias

Field QC Matrix spike/matrix spike duplicate (MS/MSD) *

Same as LCS/LCSD w/spike added to actual sample

Field, trip, and/or equipment blank (field QC samples) False positive indicator, potential POSITIVE bias

Accuracy Additional Data Quality Indicators

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Evaluating Accuracy

%R used for surrogates, LCS/LCSD & MS/MSD Dont do the math!

Example %R

Example Acceptance Criteria Recommendation

55 70 - 130 Negative bias

147 70 - 130 Positive bias

Wheredoesthecriteriacomefrom?Whatsinyourreport?

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InterpretingAccuracyBias

result spike%R actionlevel acceptancecriteria

50 22% 55 75 110%

50 47% 1 75 110%

Interpretation:

Positive/negativebiasvs.

Relationshipofdatapointtotheactionlevelvs.

Specificuseofthedata

27


VOC Surrogate Spike Data

Reported for each sample at the end of the target compound list

Surrogate %R does not automatically indicate that a QC issue exists for a specific compound MS can be used to evaluate performance of a

specific compound

report data page

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Precision Expression of Reproducibility & Variability

How reproducible is the lab measurement system?

Sample homogeneity?

Precisionmeasurementtool:replicateanalyses

Evaluated using relative percent difference (RPD)

|R1 R2|

(R1 +R2) /2X100=%RPD

% RPD = the absolute value of the range divided by the mean times 100

29


Precision ExpressionofReproducibility&Variability

Laboratory generated precision information:

(LCS / LCSD) Two analyses > results compared (%RPD) for precision

Laboratory batch duplicates

Field generated precision information: Field duplicates, co-located samples, MS/MSD

Submit blind, calculate RPD

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Evaluating Precision

%RPD acceptance criteria represents an upper limit Greater the RPD, more variability (less precision)

%RPD used for LCS/LCSD, MS/MSD, lab/field duplicates

Example RPD

Example Acceptance Criteria (%RPD Upper Limit)

Recommendation

14 25 Precision withinacceptable range

35 25 Precision outsideacceptable range

31


InterpretingPrecisionInformation

Sources of variability1. measurement system performance (lab & field)

reproducibility issues2. sample non-homogeneity, media variability (field)

representativeness issues

Evaluating replicate non-agreement Field / lab duplicate samples (conservative, use > result)

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97

VOC LCS / LCSD Data

33


3 4 5 6 7 8 9 10 11 12 13Reported result - 9

Highest allowable variability (25% RPD) of associated LCS/LCSD

If LCS/LCSD RPD was 43%

IF LCS %R indicated LOW BIAS

precision

accuracy (biased low)

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ReportingLimit

SampleConcentration:

17PPM

SampleResponse:17500

MDL

Sensitivity(LaboratoryReportingLimits)

Whatactionlevelsdoyouneedtomeet?

Maynotbeattainablewithroutinemethods

MDL*

ElevatedRLsduetodilutions: Hightarget(ornontarget) compoundconcentration Difficultsamplematrix,spikesdilutedout?

lowestcal std

SampleExtraction winnowingdownprocess

isolate(extract)&concentrate exploitsolubilitydifference

primarysourceofmethodsensitivityandmethodperformanceproblems

extraction

concentration

1000 mLaqueoussample

300 mLorganicsolvent

1 mLorganicsolventextract

1 mg/L (instrument RL)1000x concentration factor= 1 ug/L method sensitivity

PreparativeAnalysis

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So Youve Documented the Non-Cons

DotheDUEIsthedatausable?

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Data Collection Process

Objective:CollectDataofKnownQualitySuitableforitsIntendedUse

Planning projectsetup Involvealldatausers Fieldstaging/labsetup

Execution Collect&analyzesamples

Datamanagementprojectfollowup DQA/DUE Meetmyneeds?Isitusable?

39


YouveCompletedtheDQAAretheDataUsable?

Why did the report get a NO on Question 4 (RCP) ? What else did your DQA find?

Isolate analysis Isolate analytes

This is the data that needs to be evaluated

Everything else is OK to use as is Still need sensitivity evaluation

Focus

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DataUsabilityEvaluationProcess CompletedDQA

Summaryofnonconformances

Evaluaterelevancy Contaminantofconcern?Samplelocation?Significance?

Bias:+, orindeterminate? Relationshipofresulttoregulatorycriteria

Incorporateuncertaintyintodecisionmaking Doesthisnonconformanceimpactmyuseofthedata? RISKTOLERANCE

DUE whatdoesitmeanformyproject?

41


DUE:Additional Considerations

Multiple lines of evidence Batch QC DQIs / sample specific DQIs

Additive or contradictory effect?

Bring in info beyond current lab report Historical data, field data, other samples, CSM, etc.

Trade offs Non-conformance severity (17% R or 70% R)

Importance of this data point / risk tolerance?

Is the non-conformance tempered by facts? (dilution, co-elution, obvious sample matrix issues)

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EvaluatingSignificantQA/QCVariances

ExcessiveQCnonconformances

Rejecteddata Intendeduse&risktolerancedependent

Wouldrequiresubstantialjustification

43


SoIs the Data Usable?

Canyoujustifyit?Canyoumakethecaseforusingqualifiedresults

foryourprojectapplication?

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Managing Usability Information Summarize your data qualifications

Table summary (Exception Report NON-CONFORMANCES?)

Integrate into project data base

Use data usability -qualified data for all decision making

Reminder you really should have an understanding of

data limitations ongoing as decisions are made

45


I 2

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Data Usability Table

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www.epa.gov/superfund/programs/clp/download/somnfg.pdf

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www.epa.gov/oswer/riskassessment/datause/pdf/datauseparta.pdf

53


Laboratory Report Review

YouaretheLEPofrecord Sitehistory Currentlytruckmaintenancefacility Postremediationanalyticaldata

DQA/DUEtosupportdecisionmaking

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55


DQA DUE Data

Review RCP certification form Review non-conformance narratives

& QC information Accuracy, Precision & Sensitivity

Results,reportinglimitsCOCs,Reg Criteria

QCnoncons Datause

goodfit?

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Whatarewelookingfor? NoanswersonQuestionnaire Narrativecomments QCoutliers

QCsummarysections DatapagesforsamplespecificQC

CONCEPT

DQA:FindnonconformancesDUE:Evaluateimpactofnonconformances

Triage whatsimportant? COCornot? Samplelocationsignificant? Otherprojectspecificdriver

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RCPSummaryQuestionnaire

Any Nos?

QUESTION 4: NOQUESTION 5b: NO

59


Werethesereportinglimitsmet?NO

WhytheNOanswer?Checkthenarrative,usedatatable

1,2Dibromo3chloropropaneRunbyMethod8260(RL2.5ug/L)

AlternativePollutingSubstanceCriteria0.2ug/L

Alternativemethodsnotrequested Notcontaminantofconcernatthissite

Question5b:

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WereallQA/QCperformancecriteriaspecifiedintheDEEPReasonableConfidenceProtocoldocumentsachieved?

NO(notabigsurprise) Formostprojects,youshouldnotexpectaYEStothisquestion

Proceedtonarrative

Question4:

61


(page14)SamplespecificQC

(onlyappliestoSampleL170484802)

VOCSurrogateSpike%RNonConformance

Surrogate spikeCompound

% Recovery Acceptance Criteria (%R)

1,2-dichloroethane-d4 57% 70 130%

Samplewasrerun(pages15 17)similarsurrogateperformance(54%R)

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VOCSampleL170484802

Datausabilityimpact? Negativebias

Actualresultscouldbegreaterthanreportedvalue Datareportedcouldbelessconservative

Implications Thissampleonly,appliestoentireTCL Rerunconfirmssamplespecificmatrixeffect BTEXhits,restofTCLND(bothruns)

SERIOUSISSUE,BTEXCOCsw/negativebiasindicated DUEimplications

LowSurrogate%R

63


VOC LCS / LCSD Non-Conformances

LCS / LCSD (over-recoveries - compound specific) Analytical Batch QC (applies to all samples run in this batch)

Compound LCS %R LCSD %R Acceptance Criteria %R

4-methyl-2-pentanone 155 155 70 - 130

2-butanone 153 153 70 - 130

2-hexanone 154 154 70 -130

(Pages 24 - 27)

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VOCLCS/LCSDNonConformances(overrecoveries) Datausabilityimpact?

BatchQC:Appliestoallsamplesruninthisbatch Positivebiasscenario

Actualresultcouldbelessthanreportedvalue Dataforthesecompoundsismoreconservative

Implications? NDreportedforeachcompound,w/positivebias Cmpds arenotcontaminantsofconcern Cmpds areconsideredpoorperformers

NOISSUE,noDUEimplications

65


VOCLCS/LCSDNonConformances(underrecoveries compoundspecific)

AnalyticalBatchQC(appliestoallsamplesruninthisbatch)

Compound LCS %R LCSD %R AcceptanceCriteria

Benzene 47 98RPD 70%70 130RPD 20%

(Page24)

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LCS/LCSDRecoveries(benzeneunderrecovery) Datausabilityimpact?

BatchQC:Appliestoallsamplesruninthisbatch Negativebias

Actualresultcouldbegreaterthanreportedvalue Datareportedcouldbelessconservative

Implications? Cmpd isacontaminateofconcern Multiplelinesofevidencesupportingnegativebiasforsample02Benzeneresult{surrogate&LCS}

SERIOUSISSUE,BenzeneaCOCw/negativebiasindicated DUEimplications

67

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VOCDQANonConformancesofConcernSample ID or QC element

CMPD Initial Re-Analysis

Decision / rationale

LCS %R Benzene 47% NA Benzene low bias, applies to both samplesL1704848-021,2-DCA d4Surrogate

All cmpds 57% 54% Low %RAll TCL

Probable low biasL1704848-01 Benzene

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SVOCNonConformances (Page5051)LCS/LCSDRecoveriesandRPDsDQAReview

AnalyticalBatchQC(appliestoallsamplesruninthisbatch)

Compound LCS%R

LCSD%R

%RPD %R Acceptance

Criteria

RPDCriteria

Benzo(a)anthracene 33 41 22 40 140 30%

2,4-Dimethylphenol 33 27 20 30 130 30%

Benzo(a)pyrene 30 40 29 40 -140 30%

71


SVOCLCS/LCSDRecoveriesDUEThought Process



Implications? All3cmpds slightlybelowacceptable%Rrange

SERIOUSISSUE(?),COCsw/negativebiasindicated DUEimplications

Needtoevaluateresultsinrelationtoactionlevels

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SVOCDUEThoughtProcessMLE PAHs benzo(a)anthracene,benzo(a)pyrene

OUT:Lowbias(LCS) Impactsall3samples

IN:LCSD,MS/MSD,surrogates,blankacceptable&FD Sample03ND(

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SVOCMS/MSDNonConformances(DQAsummary)

AnalyticalBatchQC(butappliestosample01only) (Page55 58)

Compound MS%R

MSD%R

%RPD %R Acceptance

Criteria

RPDCriteria

Bis(2chloroethyl)ether 38 48 23 40 140 30%

Benzo(k)fluoranthene 38 48 23 40 140 30%

Pentachlorophenol 20 32 46 30 -130 30%

75


SVOCMS/MSD DataDUEThoughtProcessAction?



Implications? SimilarsituationaswithLCSdata

COCsw/negativebiasindicated,DUEimplications Needtoevaluateresultsinrelationtoactionlevels

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SVOCDataUsabilityEvaluationSummary(DUEmultiplelinesofevidence)

PAHs Benzo(k)fluoranthene OUT:Lowbias(MS/MSD,justout) IN:LCS/LCSD,surrogates,blankacceptable&FD

03ND(

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Pentachlorophenol OUT:Lowbias(MS/MSD,wayout),FD%RPD IN:LCS/LCSD,surrogates,blankacceptable

#03:

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EPHNonConformances(pages62 63) EPHCODextractionsurrogate

SamplespecificQC(L170484803)

Surrogate spikeCompound

% Recovery (%R)

Acceptance Criteria (%R)

Chloro-octadecane 248% 40 140%

81


Extractionsurrogatehigh seriousness? Chlorooctadecane monitorsextractionperformance ofaliphaticextractiononly

Positivebias Actualresultscouldbelessthanreportedvalue Datareportedcouldbemoreconservative

WHYISTHESURROGATERECOVERYSOHIGH?

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Chromatographicinterference,coelution?

COD Surrogate

Chromatogramshouldbeincludedwithreport

83


EPH OUT:CODsurrogatehighbias(coelution) IN:LCS/LCSD,OTPsurrogate,MS/MSD,&blank

Fieldduplicate 57%RPD

TPH(sample03):10,14,9rangehits(20mg/Kgcriteria) Ifanybiaspresent,itwouldbehighbias

Actualresultlessthanreportedvalue

OK?

EPHDUESummary(multiplelinesofevidence)

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PCBNonConformances(Page74)Sample 03TCMXsurrogate

Sample specific QC

Surrogate Col 1% R

Col 2% R

% R Acceptance

Criteria2,4,5,6-tetrachloro-

m-xylene 8 9 30 150

Decachlorobiphenyl 33 37 30 150

85


Sample03,contradictoryMLE OUT:TCMXsurrogate IN:LCS/LCSD,MS/MSD,DCBsurrogate

Guidance:MS%Rcanoverrulesurrogate%R Samplespecific Alwaysajudgmentcall

Butinthiscasewithsurrogate%R

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Surrogaterecovery

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PCBDataUsabilityEvaluationSummary

Sample ID or QC element

Result Criteria Bias / Qualifier

Decision / rationale

L1425103-03

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Lunch45Minutes


Laboratory Case Narratives

MichaelAinsworthHRPAssociates,[email protected]

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Laboratory Case Narratives

1


Laboratory Case Narrative

StateswhetherdatameetsRCPstandards.

Listsnonconformancesandissuesrelatedtomatrixinterferences,sampling,labanalyses,qualitycontrol,etc.

Providesadditionalinformationregardingthesamplesandanalyticalresults.

Keycomponentoflab EPcommunication:

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Case Narrative ExamplesGeneraltopics/categories:

MatrixInterferences ReportingLimits Analyte Issues PhysicalCharacteristicsofSample SamplingProcedures LabMethodIssues LabQualityControl/AcceptanceCriteria/Surrogates LackofRCPCriteria

3


Case Narrative Examples

Therewerenoanomaliesassociatedwiththereporteddata.

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Case Narrative ExamplesPhysicalCharacteristics

TheVOAvialspreservedwithdeionized waterwerereceivedfrozenuponcustodytransfertolaboratoryrepresentative.

Sampleisvalidaslongas:

Sealisnotbroken Vialisnotcracked Vialwasfrozenbytheclientorlabwithin48hrs Holdingtimeshavenotbeenexceeded

ReviewtheCOCfortimeofcollectionandfreezing

5


Case Narrative ExamplesSamplingIssues

ThemethanolVOAvialwascracked.Wehaveextractedinhouse.

Highresultsmaybeusableforscreening Usewithmultiplelinesofevidence

Dependsonstageofinvestigation

Resampleifmoreaccurateresultsarerequired

RCPswerenot met.

Isthedatausable?

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Case Narrative ExamplesSamplingIssues

TheMeOH vialcontainedalargeamountofsoilascomparedtotheextractant (greaterthanthe1:1ratioreferencedinEPAMethod5035).Theresultsreportedfromthedilutedaliquotarethereforebasedonthesampleasreceived.

Result:datadidnot meetRCPcriteria Lowbias Isthedatausable?

Stageofinvestigation Levelsdetected CSM

7


Case Narrative ExamplesMatrixInterferences

Duetomatrixinterferences,selectedsampleswereanalyzedforcertainanalysesonadilutedbasis.Insuchcases,thereportinglevelshavebeenraisedaccordingly.

Arecontaminantsofconcerninvolved?

AresamplesbeingusedtomeetRSRcriteria?

Canthelabcleanupandrerunthesamplewithinholdingtime?

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Case Narrative ExamplesSampleDilution

Sampledilutionwasrequiredforhighconcentrationsoftargetanalytes tobewithintheinstrumentcalibrationrange.

Sampledilutionisoftenrequired

AreraisedReportingLevelsoverRSRcriteria?

Reviewdilutedandundilutedresults mayhelp

9


Case Narrative ExamplesEstimatedValues

TheresultreportedforTCEisanestimatedvalue(E)becauseitwasgreaterthanthehighestcalibrationstandardanalyzed.

Candatabeusedforquantitativepurposes?

Iftherearetwosetsofdataduetodilution,arebothoutofcalibrationrange?

Resultsareonlyaccuratewithinthecalibrationrangeandlimitationsoftheequipmentandmethod.

ResultsmeetRCPs

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Case Narrative ExamplesQA/QCBlanks

Analyte isfoundintheassociatedblankaswellasinthesample.

Whichblankwasitfoundin(lab,trip,orfieldblank)?

Whatsubstanceandconcentration?10Xrule.

Significancedependson:

Contaminantofconcern?

Certaincompoundsarecommonlaboratorycontaminants: Methylene chloride Acetone MEK

11


Case Narrative ExamplesPotentiallyDifficultCompounds

AccordingtoCTDEEPRCPQualityAssuranceandQualityControlRequirementsforVOCsbyMethod8260,Table1A,recoveryforsomeVOCanalytes hasbeendeemedpotentiallydifficult.

RCPslistanycompoundsthatarepotentiallydifficulttoquantify.

Methods8260and8270

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EPAMethod8260Acetone

BromomethaneChloroethane

DichlorodifluoromethaneDibromochloromethaneHexachlorobutadiene2butanone(MEK)

Trichlorofluoromethane4methyl2pentanone

13



EPAMethod8270

Dimethyl phthalate4nitrophenol

Phenol4methylphenol2methylphenol2,4dinitrophenolPentachlorophenol4chloroaniline

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Case Narrative ExamplesAnalyticalMethodIssues

ThissamplewasanalyzedforVOCsoutsidetheEPArecommendedholdingtimeof14daysperclientrequest.

Howlongafter?1day?10days?

Datacouldpossiblybeusedforscreeningorwithmultiplelinesofevidence.

NotusableforRSRcompliance

PCBslesspronetodegradationafter14days

15


Case Narrative ExamplesLaboratoryCalibrationIssues

Thefollowinganalytes donotmeetRCPcriteriaintheSVOCinitialcalibration(ICAL) withResponseFactorsof

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ForMethod6010,onlyRCRA8metalswererequestedandreported.

SimilarforPAHs(partofMethod8270)oranyothermethods.

LabMethodIssues

17



MethodAcceptanceCriteria

Benzidine percentrecovery(30%)isoutsideindividualacceptancecriteria(40140%),butwithinoverallmethodallowances.Resultsofthefollowingsamplesareconsideredtohaveapotentiallylow bias.

Chloroethane percentrecovery(138%)isoutsideindividualacceptancecriteria(70130%),butwithinoverallmethodallowances.Resultsareconsideredtohaveapotentiallyhighbias.

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MethodAcceptanceCriteria

20%oftotalnumberofcompoundscanbeoutsideofacceptancecriteriaformethod compliance

Contaminantsofconcern? Useofresults? RSRcriteria?

19


Case Narrative ExamplesSurrogates SVOCs

Acidsurrogaterecoveryoutsideofcontrollimits.Thedatawasacceptedbasedonvalidrecoveryofremainingtwoacidsurrogates.

SurrogaterecoveryforSVOCanalysis

2,4,6 Tribromophenol

Surrogate %Recovery WithinLimits?

Terphenyld14

PhenolD5

11%

86%

78%

AcceptableLimitsare30% 130%

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Case Narrative ExamplesSurrogates VOCs

Surrogaterecoveryoutsideofcontrollimits.Thedatawasacceptedbasedonvalidrecoveryoftheremainingsurrogateswiththreerequiredbyprogrammethods.

SurrogateRecoveryforVOCanalysis

Dibromofluoromethane

Constituent SurrogateRecovery

62%

WithinLimits?

AcceptableLimitsare70% 130%

1,2 Dichloroethane d4

106%Toluene d8

112%

4 Bromofluorobenzene 101%

21


Case Narrative ExamplesAcceptanceLimitsforDuplicates

RPDTheRelativePercentDifference(RPD)ofthesampleduplicateexceededtheQCcontrollimitof20%;howeverprecisionisdemonstratedwithacceptableRPDvaluesforMS/MSD.

Nickel

Constituent Duplicate

Lead

21

57

MS/MSD5

4

RPDwithinlimit?

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Case Narrative ExamplesNoRCPCriteria

TherearecurrentlynoRCPcriteriaforoneormoreanalytes ormethodsrequested,howeverQCdatahasbeenreportedandmeetstherequirementsofeachnonRCPmethod.

RequestadditionalQA/QCinformationisnecessary

Ifanylistedanalytes areimportanttotheSite:

DocumentthatequivalentQA/QCwasperformed

Informationstatement

Somemetals,wastecharacterizationtests,etc.

UnderstandyourprojectsobjectivesandlaboratorySOPs

23



ThiscompoundwasovertheinstrumentcalibrationrangeandwasnotreanalyzedfromtheMethanolvialbecauseaminimum50xdilutionfactorisrequired.ThedilutionfactorcombinedwithreportinglimitwouldmeanthefinalconcentrationwouldbeBRL.

Ifacommentisunclear,

Contactthelab!

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CaseStudy#1

TinaM.ClemmeyEnsafe [email protected]

GailL.Batchelder,Ph.D.,P.G.,L.E.P.HRPAssociates,[email protected]

1

CaseStudy#1Objectives

ProvideanopportunitytogothroughtheDQA/DUEprocessforaspecificsite.ThefocusonthiscasestudyistheDQA.

TheDQAwillbeguided

TheDUEwillbepresented

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CaseStudy#1Scenario

Releasefromaningroundwastewatertreatmentsump.

Releaseinvestigatedandremediated. Evaluategroundwaterdatatodetermineifremediationwassuccessful.

Forpurposesofthisexercise,theanalyticalresultswillbecomparedtotheGWPC.

3

DQA/DUEProcess

DQAIdentifynonconformancesandsummarize.

DUEEvaluatetheeffectsofnonconformances onusabilityofsampledatainrelationtotheintendedpurposeoralternativedecisionmakingpurposes.

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Step1:PerformtheDQA

Reminder:AppendixCoftheDQA/DUEGuidanceliststheinformationtobereviewedduringaDQA.

Summarizenonconformances onaDQAWorksheet.

5

GuidedDQA Reviewlaboratoryreport

Isthereportcomplete?(Thereportforthiscasestudyiscomplete)

LaboratoryAnalysisRCPQA/QCCertificationForm. ChainofCustodyForm. CaseNarrativeReport. AnalyticalResults. QCResults.

Crossreferencebatchnumberswithsamplenumbers.

CompleteaDQAWorksheet Notenonconformances only.

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AboutDQAWorksheets Exampleworksheetsmaybemodified. TheexampleworksheetsprovidedincludeRSRcriteria,results,andpreliminaryDUEfindings; thismayworkforsmallerprojects,butcouldbetoocumbersomeforlargeprojects.

Completeasyougothroughcasenarrative,labQCinformation,otherDQAtasks

7

ExampleDQAWorksheet

Electronicversions,databases,orspreadsheetsmaybeused.

ContactyourlabtoseeiftheycanprovideaDQAoriftheyhaveaportalthatallowsyoutopullandcompilethedataalongwiththerespectiveQCsamples.

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ExampleDQAWorksheet

Forthepurposeofthistraining,wewillgothroughtheDQAprocessMANUALLY

9

CASE STUDY 1RCP DQA

Laboratory: JGBTSDG: 08R-2469.0Date Samples Collected: 4/17/2008RCP Certification Form Included: YesLaboratory Case Narrative Included: Yes

Sample # Lab # Location # Compound QC Outlier

% Rec.

Rel. %

Diff.

Results(ug/L)

GWPC Comments

ExampleDQAWorksheet

Thispartcanbeenteredinadvance Thispartisenteredasyoufindissues 10

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BecomeFamiliarwithyourDataPackage

DataPackageReview

CASESTUDY1 DATADELIVERABLES

RCPCertificationForm page1of54

CaseNarrative page2and3of54

SampleSummary page4of54

LabReports page5through33of54

QCReport page34through50of54

BatchAssociation page51and52of54

MethodSummary page53and54of54

ChainofCustodyForm Lastpageofdatapackage

DataDeliverables

JGBTEnvironmental

Inc.

11

ReviewofLaboratoryReportPackage

ReviewLaboratoryAnalysisRCPCertificationForm(LCF):

AreallthequestionsintheLCFanswered? NotewhichquestionsareansweredNO.

AretheseNOresponsesfullyexplainedintheCaseNarrativeReport?

LaboratoryshouldnothavemadeanychangestoForm

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RCPCertificationForm

Typeequationhere.

Case Study 1 Data PackagePage 1 of 54

13

RCPCertificationForm IstheLCFsigned?


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ChainofCustody ReviewChainofCustodytoensureformiscompleteandcorrect.

Correctanyerrorswithasingleline,initial,andnotereasonforcorrection.

Note:theChainofCustodyshouldbealsoreviewedatthetimeofsamplingtoo.

Weresamplesappropriatelypreserved/refrigerated/iced?

Contactthelaboratoryforhelporclarificationifneeded.

Wereallanalysesperformed?

15

ChainofCustodyEvaluation

RSRcriteriawerenotnotedonChainofCustody. Inthiscase,GWPC.

AreviewoftheanalyticalresultswillshowthattwosampleswerenotanalyzedforETPHasrequestedontheChainofCustody.

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Onlypage1presentedhere

CaseStudy1 Datapackage Lastpage 17

REPORTONLABORATORYEXAMINATIONS

LaboratoryNo.: LS08003507 ClientSampleID:MW4SampleMatrix: Groundwater ReceivedDate:Thursday,April17,2008CollectedBy: ENVIROBIZ,INC. CollectDate:Thursday,April17,2008Source: KRRGPlating,BigCity,CTSampleID: MonitoringWellSample

AnalysisMethod: SW8468260BReporting Analysis

Test Result Units: Dil: Limit Analyst Date Batch#LS08003507 Acetone ND ug/L 1 10.0 MS 4/30/2016 45165LS08003507 Acrylonitrile ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 Benzene ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 Bromobenzene ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 nButylbenzene ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 secButylbenzene ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 tertButylbenzene ND ug/L 1 0.5 MS 4/30/2008 45165LS08003507 Bromodichloromethane ND ug/L 1 0.5 MS 4/30/2008 45165

IfETPHanalysiswasperformeditshouldbehere

SampleID

Note:thesamplefromMW7isalsomissingtheETPHanalyticalresults.

Case Study 1 Data PackageMW-4 - Page 14 of 54 and

MW-7 - Page 22 of 5418

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DQAWorksheet

InitialinformationinthesecolumnswasalreadyenteredinadvancetospeedupprocessduringtheDQA.

Informationinthesecolumnsisenteredasissuesareidentified.

SAMPLE#

LAB #

LOCATION ID # COMPOUND

QCOUTLIER %R RPD BIAS COMMENTS

LS08003507 LS08003507 MW-4 ETPH No resultreported

ETPH analysis not performed

LS08003510 LS08003510 MW-7 ETPH No result Reported

ETPH analysis not performed

19

LaboratoryNarrative Reviewthenarrativeforfindings(i.e.,QCnonconformances)andrequestadditionalinformationfromthelaboratory,ifapplicable.

Checkthatholdingtimesandpreservationrequirementshavebeenmet.

Notenonconformances onDQAworksheet.

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DQAWorksheet

SAMPLE#

LAB #

LOCATION ID # COMPOUND

QCOUTLIER %Rec.

Rel. %

Diff. BIAS COMMENTS

LS08003513 LS08003513 MW-2m CadmiumMS

MSD50.9156.47

LowLow

Low Recovery

Note:MS/MSDRCPLimitsforMetals%R:75125%

SincetheSample#andLab#arethesameinthisdeliverableexample,theLaboratory#hasbeendroppedonthepresentationslidestosavespace.

21

CaseNarrative

MetalsBatch45066

Zincwasdetectedinthemethodblank at0.01mg/L.

BatchappliestosamplesMW1mthroughMW6m,butnotMW7m.


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Batch AssociationAnalysis Method: CT ETPH

Lab # Client ID# Analysis Batch # Prep Batch #

LS08003504 MW-1 45137 5801LS08003505 MW-2 45137 5801LS08003506 MW-3 45137 5801LS08003508 MW-5 45137 5801LS08003509 MW-6 45137 5801LS08003511 MW-8 45137 5801

Analysis Method: SW-846 6010BLab # Client ID# Analysis Batch # Prep Batch #

LS08003512 MW-1m 45066 5795LS08003513 MW-2m 45066 5795LS08003514 MW-3m 45066 5795LS08003515 MW-4m 45066 5795LS08003516 MW-5m 45066 5795LS08003517 MW-6m 45066 5795LS08003518 MW-7m 45085 5797

Anaysis Method: SW-846 7010Lab # Client ID# Analysis Batch # Prep Batch #


Method

Case Study 1 Data PackagePage QC 51 of 54 23

QCReport


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DQAWorksheetSAMPLE

#LOCATION

ID COMPOUNDQC

OUTLIER

%Rec. or

Blank Contamination

Resultmg/L

Comments

LS08003512 MW-1m Zinc Method Blank

0.01 mg/l detected in blank

ND

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BatchAssociationAnalysis Method: CT ETPH

Lab # Client ID# Analysis Batch # Prep Batch #

LS08003504 MW-1 45137 5801LS08003505 MW-2 45137 5801LS08003506 MW-3 45137 5801LS08003508 MW-5 45137 5801LS08003509 MW-6 45137 5801LS08003511 MW-8 45137 5801

Analysis Method: SW-846 6010BLab # Client ID# Analysis Batch # Prep Batch #


Anaysis Method: SW-846 7010Lab # Client ID# Analysis Batch # Prep Batch #


Method


QCReport


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DQAWorksheet

SAMPLE # LOCATION ID COMPOUNDQC

OUTLIER %R RPD BIAS COMMENTSLS08003518 MW-7m Cadmium Lab. Control

Sample57.47 low LCS not

reanalyzed by laboratory

LS08003518 MW-7m Copper Lab. Control Sample

60.93 low LCS notreanalyzed by

laboratory

Note:LaboratoryControlSampleRCPLimitsforMetals%Recovery:85115%

ThereisonlyonesampleinPrepBatch5797.

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SAMPLE #LOCATION

ID COMPOUNDQC

OUTLIER %Rec.Rel. % Diff. BIAS COMMENTS

LS08003504 MW-1 ETPHSurrogate:

n-Pentacosane 153 High

DQAWorksheet

Note:LaboratoryControlSampleRCPSurrogateLimitsforCTETPH

%R:50150%

Onlyonesampleisaffected.

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CaseNarrative

CTETPHBatch45137

Ahighpercentrecovery(153%)forsurrogatenpentacosane wasreportedforSampleLS08003504.


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CaseNarrativeReport

QC Number Test QC Type % R Prep# Narrative Explanation

LS08003504R n-Pentacosane Surrogate 153 Recovery is high which may indicate high bias

Batch#45137AnalysisMethod:ETPH

Surrogatesaresamplespecific,notbatchQC.

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QCReport


LaboratoryAnalyticalDataReview

ArethereportinglimitslistedandaretheylessthanregulatorycriteriarequestedontheChainofCustody?

WasanythingreportedabovelaboratoryReportingLimits?

Checkdilutionfactortoseeifadilutionwasperformed.DilutionfactorsresultinelevatedReportingLimits(RLs).

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LaboratoryReportDataReview

AnalyticalResults: OnlyconcentrationsgreaterthanReportingLimitsshouldbereported,noJflags.

Bflagstobeusedforresultswithcontaminationinablank.

Soilandsedimentsresultsreportedonadryweightbasis.

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EvaluationofSampleResults

PartiallistofRCPMethodmetalsanalyzed,asrequestedintheChainofCustody.

Requestedlistcoversconstituentsofconcern. ReportingLimitsachievedarelessthanorequaltotheGWPC.

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LaboratoryQCReport

ReviewQCresultstobecomefamiliarwiththedata.Theseresultsinclude:methodblanks,fieldblanks,LaboratoryControlSamples,surrogates,etc.

MatrixSpike/MatrixSpikeDuplicate(MS/MSD)wasrequestedforthiscasestudy.

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FinalDQAWorksheet RelatesallQCnonconformances

tosamplesandsamplelocations. DQAworksheets(spreadsheets)canbesortedby:

Sample Samplelocation Constituentofconcern QCOutlier

DQAspreadsheetsforindividualSampleDeliveryGroups(SDGs)canbecombinedtoassessoverallevaluationofdataandtrends.

FormsthebasisoftheDataUsabilityEvaluation.

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FinalDQAWorksheetGroundwaterMonitoring Round1RCP DQA Worksheet

Laboratory: JGBTSDG: 08R-2469.0Date Samples Collected: 4/17/2008RCP Certification Form Included: Yes CASE STUDY #1Laboratory Case Narrative Included: Yes

Note 1: Bias High: reported result may be lower than reported, RLs are accepted as reported.Bias Low: reported result may be higher than reported, RLs may be higher

Note 2: RCP VOC list analyzed for total xylenes, not isomersRCP Metal list did not analyze full RCP metal list

SAMPLE # LAB # LOCATION ID# COMPOUND QC OUTLIER

%R orMethod Blank Contamination RPD COMMENTS

LS08003504 LS08003504 MW-1 ETPH Surrogate: n-Pentacosane 153 high

1,1,2,2-tetrachloroethane LCS 60 low RCP poorly performing compound

LS08003505 LS08003505 MW-2 1,1,2,2-tetrachloroethane LCS 60 low RCP poorly performing compound



ETPH No result reported ETPH analysis not performed



LS08003510 LS08003510 MW-7 1,1,2,2-tetrachloroethane LCS 60 Low RCP poorly performing compound

ETPH No result reported ETPH analysis not performed

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FinalDQAWorksheet

SAMPLE # LAB # LOCATION ID# COMPOUND QC OUTLIER

%R orMethod Blank Contamination RPD COMMENTS

LS08003511 LS08003511 MW-8 1,1,2,2-tetrachloroethane LCS 60 low RCP poorly performing compound1,1-dichloroethylene MS/MSD 34.85 non-directional2-hexanone MS/MSD 54.6 non-directional RCP poorly performing compoundAcetone MS/MSD 35.73 non-directional RCP poorly performing compoundAcrylonitrile MS/MSD 41.92 non-directionalcis-1,2-dichloroethylene MS/MSD 131.51 / 134.15 highDichlorodifluoromethane MS/MSD 24.95 non-directional RCP poorly performing compoundTetrachloroethylene MS/MSD 68.49 / 69.06 LowToluene MS/MSD 21.64 non-directionalTrans-1,2-dichloroethylene MS/MSD 21.58 non-directional

Trichloroethylene MS/MSD 62.08 / 62.45 low

LS08003512 LS08003512 MW-1m ZincMethod Blank Contamination

0.01 mg/l detected in blank Common laboratory contaminant



Common laboratory contaminant

Cadmium MS/MSD 50.91 / 56.47 low






Common laboratory contaminant5X Action Level (AL)= 0.05 mg/LResult is less than 10X AL.






Common laboratory contaminant5X Action Level (AL)= 0.05 mg/LResult is less than 5X AL.

LS08003518 LS08003518 MW-7m Cadmium LCS 57.47 low LCS not reanalyzed by laboratoryCopper LCS 60.93 low LCS not reanalyzed by laboratory

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DataUsabilityEvaluation

TheDQAworksheetsummarizesnonconformances thatneedtobeevaluatedduringtheDUE.

OntheDUEWorksheetprovided,Page1shouldbefilledinfirst Criticalreminderonlythenonconformances needtobenoted,

butsupplementalinformationcanbeaddedtohelpexplainitemsforPage2.

Hownonconformances affectusabilityonthespecificprojectarethenindicatedonPage2oftheDUEworksheet.

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DUEWorksheet

Thisisintendedtobeasuccinct summaryofnonconformances tohelpstarttheDUE.42

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DUEWorksheet

ReasonableConfidence QuestionNo.1onRCPForm No,becauseLCSforcadmiumandcoppernotreanalyzed.

ChainofCustodyEvaluation NoETPHanalysisrunforMW4andMW7.

SampleResultEvaluation Partiallistofmetalsanalyzed,asrequestedonChainofCustody.

Page1

43

Blanks Zincinmethodblankataconcentrationof0.01mg/Lor10g/L.Zincisacommonlaboratorycontaminant.ApplyEPA10timesrule.

LaboratoryControlSamples MW7 copperandcadmiumlowbias Forallsamples 1,1,2,2tetrachloroethanelowbias

Surrogates ETPH NPentacosane highbiasforMW1only

DUEWorksheetPage1

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MatrixSpikeandMatrixSpikeDuplicatesMS/MSDfromMW8 PCE,TCElowbiasappliestoallGWsamples Cis1,2DCEhighbiasappliestoallGWsamples HighRPDfor1,1DCE;2hexanone*;acetone*;acrylonitrile;dichlorodifluoromethane*;toluene;andtrans1,2DCE

MS/MSDfromMW2 lowbiasforcadmium

*=poorlyperformingcompounds

DUEWorksheetPage1

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SummaryofDetectedResultsandQA/QCDeficiencies

CaseStudy#1 SummaryofDetectedResultsandQA/QCDeficiencies

Samples

ConstituentDetected RSRGWPCMW1MW1m

MW2MW2m

MW3MW3m

MW4MW4m

MW5MW5m

MW6MW6m

MW7MW7m MW8

ETPH 250g/L 120g/L4 Noresult Noresultcis1,2Dichloroethylene 70g/L 88g/L5 66g/L5 76g/L5 61g/L5

Trichloroethylene 5g/L 4.4g/L1 1.5ug/L1 4.0g/L1 2.6g/L1

Toluene 1,000ug/L 0.6g/L

Barium 1mg/L 0.011mg/L 0.023mg/L 0.017mg/L 0.020mg/L 0.011mg/L 0.037mg/LCadmium 0.005mg/L 0.004mg/L1 0.004mg/L1 0.005mg/L1,3Nickel 1mg/L 0.037mg/LZinc 5mg/L 0.029mg/L2 0.018mg/L2

Copper 1.3mg/L 0.045mg/L 0.047mg/L3

QAQCDeficiency:1 LowbiasforMS/MSD2 MethodBlankContamination3 LCSlowbias4 Surrogatehighbias5MS/MSDhighbias

Note:QA/QCdeficiencyfor1,1,2,2tetrachloroethanealso(lowbiasduetoLCS),butallresultswereND.

PotentialUsabilityissueshighlightedinred.

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DUEWorksheetPage2

APPENDIX I-2 (CONTINUED)

DATA USABILITY EVALUATION WORKSHEET

Provide a summary statement describing how the analytical data set relied upon is of adequate quality and of sufficient accuracy, precision, and sensitivity for the intended purpose. These results will used as the first quarter of four quarters of groundwater sampling to demonstrate compliance with the RSRs and evaluate effectiveness of remediation. Reasonable Confidence not achieved. Question 1 answered No on RCP Certification Form LCS lower than acceptance criteria for cadmium and copper, did not reanalyze, as required by RCPs. See MS/MSDs summary below. No impact to usability from LCS. RLs not noted on Chain of Custody, but RLs achieved are appropriate for a GA Area. Partial list of RCP Method metals analyzed, as requested on the Chain of Custody form. Requested list covers constituents of concern. No impact to data usability. ETPH analyses were not performed on samples from MW-4 and MW-7, since containers broken in transit to lab. Additional samples from MW-4 and MW-7 necessary. No data to evaluate for usability. Zinc was found in the method blank at 10 g/L. Zinc is a common laboratory contaminant. Appli