Post on 16-Jun-2018
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DeltaRegionalMonitoringProgram
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QualityAssuranceProgramPlan
Preparedby
ThomasJabusch,DonYee,andAmyFranz
SanFranciscoEstuaryInstitute-AquaticScienceCenter
Version2.2
July29,2016
SanFranciscoEstuaryInstitute-AquaticScienceCenter
4911CentralAvenue
Richmond,CA94804
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TitleandApproval
For
PROJECTNAME: DeltaRegionalMonitoringProgram
Date: August1,2016
NAMEOFRESPONSIBLEORGANIZATION: SanFranciscoEstuaryInstitute–AquaticScienceCenter(SFEI-ASC)
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TableofContents
TitleandApproval...........................................................................................................................2TableofContents.............................................................................................................................4
ListofTables.......................................................................................................................................6ListofFigures......................................................................................................................................6
0. DistributionList........................................................................................................................71. ProjectTask/Organization.......................................................................................................10
1.1. Roles.......................................................................................................................................101.2. PersonsResponsibleforQAPPUpdateandMaintenance......................................................12
2. ProblemDefinition/Background.............................................................................................123. ProgramTasksDescription......................................................................................................13
3.1. WorkStatementandProducts...............................................................................................133.2. EvaluationofMonitoringData...............................................................................................143.3. BeneficalUsesandWaterQualityGoals................................................................................153.4. ConstituentstobeMonitoredandReported.........................................................................243.5. GeographicalandTemporalSetting.......................................................................................303.6. Constraints..............................................................................................................................32
4. DataQualityObjectivesandIndicators,Criteria,andControlProceduresforMeasurementData 36
4.1. FieldQCProcedures...............................................................................................................384.2. LaboratoryPerformanceMeasurementsforChemicalAnalyses...........................................404.3. LaboratoryQualityControlProceduresforChemicalAnalyses..............................................454.4. DataQualityIndicatorsandTestAcceptabilityCriteriaforToxicityTestingandAssociatedWaterQualityMeasurements..........................................................................................................564.5. Performance-basedmethodconceptforthedeterminationofLT2pathogens(CryptosporidiumandGiardia)........................................................................................................66
5. SpecialTrainingNeedsandCertification.................................................................................695.1. SpecializedTrainingorCertifications......................................................................................695.2. TrainingCertificationandDocumentation.............................................................................705.3. TrainingPersonnel..................................................................................................................70
6. DocumentsandRecords.........................................................................................................706.1. ReportPackageInformation...................................................................................................716.2. DataReportingRequirements................................................................................................776.3. DataStorage/Database...........................................................................................................78
7. SamplingProcessDesign.........................................................................................................787.1. StudyAreaandPeriod............................................................................................................787.2. SamplingSites.........................................................................................................................79
8. SamplingMethods..................................................................................................................808.1. FieldEquipmentandSupplies................................................................................................808.2. FieldSampleCollectionandQualityAssuranceProcedures...................................................818.3. CorrectiveAction....................................................................................................................86
9. SampleHandlingandCustody.................................................................................................899.1. FieldSampleHandlingandShippingProcedures...................................................................89
10. AnalyticalMethods...............................................................................................................9210.1. FieldAnalytical/MeasurementMethods..............................................................................92
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10.2. LaboratoryMethods.............................................................................................................9310.3. SampleArchiveandDisposal................................................................................................95
11. Instrument/Equipment/Supplies..........................................................................................9512. Non-directMeasurements(ExistingData).............................................................................9713. DataManagement................................................................................................................9714. AssessmentandResponseActions........................................................................................9915. ReportstoManagement.......................................................................................................9916. DataReview,Verification,andValidation...........................................................................10017. VerificationandValidationMethods...................................................................................10018. ReconciliationwithUserRequirements...............................................................................10419. References..........................................................................................................................10420. Appendices.........................................................................................................................107
20.1. AppendixA.ManagementQuestions.................................................................................10720.2. AppendixB.AssessmentQuestions....................................................................................10820.3. AppendixC.DeltaRMPMonitoringElements....................................................................11220.4. AppendixD.ListofSOPs.....................................................................................................11320.5. AppendixE.ExampleFieldSheets......................................................................................11620.1. AppendixF.ExampleforChainofCustodyForm...............................................................120
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ListofTables
Table0.1.DistributionList............................................................................................................................................7Table1.1.Analyticallaboratories...............................................................................................................................11Table3.1.DeltaRMPreportingcycle.........................................................................................................................14Table3.2.BeneficialUsesassociatedwithDeltaRMPmonitoringelements.............................................................16Table3.3.EPAOfficeofWater(OW)AmbientWaterQualityCriteria,EPAOfficeofPesticidePrograms(OPP)
AquaticLifeCriteria,andWaterQualityObjectivesfortargetanalytesofCUPmonitoring............................17Table3.4.Waterqualitybenchmarksformercury.....................................................................................................24Table3.5.BinclassificationforPublicWaterSystems................................................................................................24Table3.6.DeltaRMPtargetparametersandreportingunits....................................................................................25Table3.7.ListofsitetypesamplingfrequenciesandassociatedparametergroupsforCUPmonitoring.................31Table4.1.PurposesoffieldandlaboratoryQCsampletypesanddataqualityindicatorsapplicabletotheDelta
RMP...................................................................................................................................................................36Table4.2.Acceptancecriteriaforfieldmeasurements..............................................................................................39Table4.3.Chemical-analyticalQC..............................................................................................................................42Table4.4.SummaryofReportingLimits(RL)andMethodDetectionLimits(MDL)ofDeltaRMPconstituents........48Table4.5.Summaryofinstrumentrangesandresolutionforlaboratorymeters.....................................................54Table4.6.Recoverysurrogatestandardsusedforpesticideanalysesandassociatedmeasurementquality
objectives..........................................................................................................................................................56Table4.7.Measurementqualityobjectivesfortoxicitytestingandassociatedwaterqualitymeasurements.........57Table4.8.Summaryoftestacceptabilitycriteria.......................................................................................................57Table4.9.QualityControlMeasuresfortoxicitytesting............................................................................................61Table4.10.MeasurementQualityObjectivesfortoxicitytesting..............................................................................63Table4.11.QCrequirementsandacceptancecriteriafordeterminationofCryptosporidiumandGiardiainaqueous
matrices(EPAMethod1623)............................................................................................................................67Table4.12.QCrequirementsandacceptancecriteriafordeterminationofCryptosporidiumandGiardiainaqueous
matrices(EPAMethod1623.1).........................................................................................................................68Table6.1.CEDENcontrolledvocabularyforresultqualifiers.....................................................................................74Table6.2.CommonCEDENQAcodes........................................................................................................................75Table7.1.Samplingsitesandschedule......................................................................................................................79Table8.1.Samplingeventtriggersforpesticideeventssampling.............................................................................82Table8.2.Samplecontainertypeandvolumeusedforeachparametergroupforcollectionofwatersamples.....85Table8.3.Targetspecies,numberofindividuals,andsizerangesforcollectionoffishtissuesamples....................86Table9.1.Storageandholdtimerequirementsforeachparametergroup..............................................................90Table10.1.Summaryofanalyticalmethodsandinstruments...................................................................................93Table10.2.Correctiveactionsproceduresforanalyticallaboratories.......................................................................94Table17.1.ComplianceCodes..................................................................................................................................103Table17.2.BatchVerificationCodes........................................................................................................................103
ListofFigures
Figure1.1.ProjectOrganizationChart.......................................................................................................................10Figure3.1.FY2014-17PesticideWaterSamplingSites..............................................................................................33Figure3.2.FY2016-17MercuryMonitoringSites......................................................................................................34Figure3.3.FY2014-17AmbientPathogenMonitoringSites......................................................................................35
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0. Distribution List
Table0.1.DistributionList.
Name Affiliation Title Phone EmailAddress No.ofCopies
RichardDanielson
BioVirLaboratoryDirector
(800)442-7342 red@biovir.com 1
JamesTruscott
BioVir QAOfficer (800)442-7342 jrt@biovir.com 1
ElbaMoran BioVir ClientRep (800)442-7342 elba.moran@biovir.com 1
SelinaCole CVRWQCBDeltaRMPStaff
(916)464-4683 Selina.Cole@waterboards.ca.gov 1
PatrickMorris
CVRWQCB ASCContractManager
(916)464-4621 Patrick.Morris@waterboards.ca.gov 1
AlishaWenzel
CVRWQCB
SWAMPRegion5ContractManager
(916)464-4712 awenzel@waterboards.ca.gov 1
MagnoliaBusse
EurofinsAnalyticalServicesManager
(916)605-3387 MagnoliaBusse@eurofinsus.com 1
NildaCox Eurofins QAOfficer (626)3861170 nildacox@eurofinsus.com 1
BrianLaurenson
LWA
DeltaRMPPathogenStudyLiaison
(530)753-6400ext.230
brianl@lwa.com 1
WesHeim
MPSL
PI/ProjectManager
(831)771-4459 wheim@mlml.calstate.edu 1
AutumnBonnema
MPSL
ProjectCoordinator/QAOfficer
831-771-4175 bonnema@mlml.calstate.edu 1
TravisBrown
MWQISampleCollectionTeamLead
(916)375-6809 travis.brown@water.ca.gov 1
ArinConner
MWQISampleCollectionTeamLead
(916)371-3121 arin.conner@water.c.agov 1
JeremyDelCid
MWQISampleCollectionTeamLead
(916)371-3118 Jeremy.delcid@water.ca.gov 1
StevenSanJulian
MWQIMWQIFieldSectionSupervisor
(916)371-2284 steven.sanjulian@water.ca.gov 1
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Name Affiliation Title Phone EmailAddress No.ofCopies
AdamLaputz
SCRepresentative–Regulatory(State)
(916)464-4848 Adam.laputz@waterboards.ca.gov 1
GregGearheart
SCRepresentative–Regulatory(State)
(916)341-5892 Greg.Gearheart@waterboards.ca.gov 1
TerryFleming
SCRepresentative–Regulatory(Federal)
(415)972-3462 fleming.terrence@epa.gov 1
GreggErickson
SCRepresentative–CoordinatedMonitoring
(209)942-6071 gerickson@dfg.ca.gov 1
DaveTamayo
SCRepresentative–Stormwater,PhaseI
(916)874-8024 tamayod@saccounty.net 1
BrendanFerry
SCRepresentative–Stormwater,PhaseII
(530)573-7905 Brendan.ferry@edcgov.us 1
StephanieReyna-Hiestand
SCRepresentative–Stormwater,PhaseII
(209)831-4333 Stephanie.hiestand@ci.tracy.ca.us 1
LindaDorn SC Representative–POTWs
(916)876-6030 dornl@sacsewer.com 1
DeedeeAntypas
SCRepresentative–POTWs
(205)937-7425 deedee.antypas@stocktonca.gov 1
JosieTellers
SCRepresentative–POTWs
(530)747-8291 jtellers@cityofdavis.org 1
DavidCory SC Representative–Agriculture
(209)658-5854 farmeratlaw@comcast.net 1
MikeWackman
SCRepresentative–Agriculture
(209)472-7127ext.125
michaelkw@msn.com 1
ValConnor SCRepresentative–WaterSupply
(530)219-9295 valerieconnor@att.net 1
MelanieOkoro
SCRepresentative–ResourceAgencies
(916)930-3728 Melanie.Okoro@noaa.gov 1
ReneeSpears
StateWaterBoard
QAofficer (916)341-5583 renee.spears@waterboards.ca.gov 1
MelissaMorris
SWAMP QAofficer (916)-341-5868 melissa.morris@waterboards.ca.gov 1
MarieStillway
UCD-AHPLLaboratoryManager/QAOfficer
(530)754-6772 mariestillway@gmail.com 1
SweeTeh UCD-AHPL PI (530)754-8183 sjteh@ucdavis.edu 1
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Name Affiliation Title Phone EmailAddress No.ofCopies
GregBrewster
USGSSamplingCoordinator
(916)278-1332 gdbrews@usgs.gov 1
JosephDomagalski
USGSNAWQALeadScientist
(916)278-3077 joed@usgs.gov 1
MichelleHladik
USGS Co-PI (916)278-3183 mhladik@usgs.gov 1
MeganMcWayne
USGSLaboratoryManager
(916)278-3127Lab:(916)278-3208
mmcwayne@usgs.gov 1
JimOrlando
USGS Co-PI(916)278-3271Cell(530)218-7198
jorlando@usgs.gov 1
AmandaEgler
USGS QA/QCOfficer 916-278-3210 alegler@usgs.gov 1
CoreySanders
USGS DataManager (916)278-3289 csanders@usgs.gov 1
PhilTrowbridge
SFEI-ASCProgramManager
(510)746-7345 philt@sfei.org 1
ThomasJabusch
SFEI-ASCProjectManager
(510)746-7340 thomas@sfei.org 1
AmyFranz SFEI-ASC DataManager (510)746-7394 amy@sfei.org 1
DonYee SFEI-ASC QAOfficer (510)746-7369 donald@sfei.org 1
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1. Project Task/Organization
1.1. RolesAnorganizationalchart,withmonitoringresponsibilitiesnoted,isprovidedinFigure1-1.
Figure1.1.ProjectOrganizationChart.
UnderthedirectionoftheDeltaRegionalMonitoringProgram(DeltaRMP)SteeringCommittee,theTechnicalAdvisoryCommittee(TAC)providestechnicaloversightoftheDeltaRMPandSanFranciscoEstuaryInstitute–AquaticScienceCenter(SFEI-ASC)managesandoperatestheprogramastheimplementingentity.
TheSFEI-ASCProjectManagerisresponsibleforcoordinatingallaspectsofmonitoringcomponentsofthisprojectincludingtheorganizationoffieldsampling,schedulingofsamplingdays,andinteractionswiththecontractlaboratories.TheSFEI-ASCProjectManagerworksincloseconsultationwiththeSFEI-ASCProgramManager.SFEI-ASCProgramManagerandSFEI-
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ASCProjectManagerreportdirectlytotheDeltaRMPSteeringCommittee.Projectplansaretobereviewedannually.
TheSFEI-ASCRegionalDataCenterManagerwillensurethatdatasubmittedbysubcontractorlabsaretimely,complete,andproperlyincorporatedintotheRegionalDataCenterdatabase,forusebystatewidecompilationsofdata,suchasCEDENorMyWaterQualityEstuaryPortal.
SFEI-ASC’sQualityAssuranceOfficer(QAO)roleistoestablishandoverseethequalityassuranceandqualitycontrol(QA/QC)proceduresfoundinthisQAPP,whichincludefieldandlaboratoryactivities.TheSFEIQAOwillworkwiththeQualityAssuranceOfficersforcontractedanalyticallaboratories,reviewingandcommunicatingallQA/QCissuescontainedinthisQAPPtothelaboratories.ContactinformationforkeystaffislistedinTable0.1.
LaboratoriescontractedbySFEI-ASCprovidehighqualityanalyticalservices.TheanalyticallaboratorieswillactasatechnicalresourcetoSFEI-ASCstaffandmanagement.TheresponsiblepersonnelandcontactinformationarelistedaboveinTable0.1.
Table1.1.Analyticallaboratories.
Analyticallaboratory Lababbrev. Matrix Analytical
Services
ELAP/NELAPAccreditation
NumberLabQAManualLink
BioVirLaboratories BioVir WaterCryptosporidium/
Giardia
ELAP
CertificateNo.1795
QualitySystemPlanforEnvironmentalHealth,
Inc.,D/B/ABiovirLaboratories
Eurofins Eurofins WaterCryptosporidium/
Giardia
ELAPCertificateNo.2944/NELAPID:4034
LT2-Giardia/CryptoQAPP
MarinePollutionStudiesLab,MossLandingMarineLabs
MPSLTissue,Water
Fishattributes,mercury,
suspendedsolids
N/A
MPSLLaboratoryQAP,Revision5.February,
20061CADepartmentofFishandWildlife-WaterPollutionControlLab2
WPCL Water
Chlorophylla,dissolvedorganic
carbon
ELAPCertificateNo.1795
N/A3
U.S.GeologicalSurveyOrganicChemistryResearchLaboratory
USGS-OCRL
WaterField
Measurements,Pesticides
N/A N/A4
U.S.GeologicalSurveyNationalWaterQuality
USGS-NWQL
WaterCopper
(dissolved),
QualityAssuranceandQualityControl
1 ContactMPSLLaboratoryQAO(Table0.1)toobtainacopy. 2 PerformsspecificanalyticalservicesonbehalfofMPSL. 3TheWPCLlabQAmanualiscurrentlybeingupdated.Itwillbemadeavailablewhentheupdatesarecomplete.4USGS-OCRLcurrentlyhasnostandalonedocumentdescribinggeneralQAprocedures.TheexistingQAprocedureshavebeenincorporatedintotheDeltaRMPQAPP,asappropriate,andarealsodocumentedinSOPs.
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Analyticallaboratory Lababbrev. Matrix Analytical
Services
ELAP/NELAPAccreditation
NumberLabQAManualLink
Laboratory dissolvedandparticulate
organiccarbon
N/A
UniversityofCaliforniaDavis-AquaticHealthProgramLaboratory
UCD-AHPL
Water
Toxicity,TIEs,alkalinity,ammonia,hardness
ELAPCertificateNo.2243
UCDAHPLQAM
1.2. PersonsResponsibleforQAPPUpdateandMaintenance
ChangesandupdatestothisQAPPmaybemadeafterareviewoftheevidenceforchangebySFEI-ASC’sProjectManagerandQAO,andwiththeconcurrenceoftheDeltaRMPTechnicalAdvisoryCommittee.SFEI-ASC’sQAOwillberesponsibleformakingthechanges,submittingdraftsforreview,preparingafinalcopy,andsubmittingthefinalforsignatures.ChangesareexpectedyeartoyearintheearlyyearsofDeltaRMPimplementation.
2. Problem Definition/Background
TheDeltaRMPwasinitiatedin2008bytheCentralValleyRegionalWaterQualityControlBoard(RegionalWaterBoard)withtheprimarygoaloftrackinganddocumentingtheeffectivenessofbeneficialuseprotectionandrestorationeffortsthroughcomprehensivemonitoringofwaterqualityconstituentsandtheireffectsintheDelta.ThedevelopmentoftheDeltaRMPwasinitiallypromptedbythecollapseofthepopulationsofseveralspeciesoffishintheearly2000s,aneventthattriggerednewinquiriesintothepotentialroleofcontaminantsinwhatisnowtermedthePelagicOrganismDecline(POD).However,theseinquirieshighlightedshortcomingsofexistingmonitoringeffortstoaddressquestionsatthescaleoftheDelta.Therecognitionthatdatafromcurrentmonitoringprogramswereinadequateincoverage,couldnoteasilybecombined,andwerenotadequatetosupportarigorousanalysisoftheroleofcontaminantsinthePODpersuadedregulatoryagenciestoimprovecoordinationacrossmultiplemonitoringprograms.
Inaddition,theDeltaRMPreflectsanincreasingdesireamongwaterqualityandresourcemanagersthroughoutthestateformoreintegratedinformationaboutpatternsandtrendsinambientconditionsacrosswatershedsandregions.Manystressorsonbeneficialusesareinterrelatedandmustbeaddressedmoreholistically.TheDeltaRMPcomplementsexistinglarger-scalecollaborativemonitoringeffortsthroughoutthestatethatattempttoaddressquestionsandconcernsaboutregionalconditionsandtrends(e.g.,SanFranciscoBayRMP,SouthernCaliforniaBightMonitoringProgram,SurfaceWaterAmbientMonitoringProgram).
TheDeltaRMPSteeringCommitteeisthedecision-makingbodyoftheDeltaRMP.TheSteeringCommitteeisresponsibleforestablishingtheDeltaRMP’sstrategicdirectionandthepolicies
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andproceduresthatgovernitsoperation.TheSteeringCommitteemaydirectDeltaRMPstaffandadvisorycommitteestoassistinmeetingtheobjectivesandmaydelegateday-to-dayfunctionsoftheDeltaRMPtotheDeltaRMP’simplementingentity.
TheSteeringCommitteeauthorizestheimplementationofagreementsamongtheparticipatingmembersand,specifically:
1. Directsthefiscal/operatingagenttorequestandreceivefederal,state,local,andprivatefundsfromanysourceandtoexpendthosemoneystoaccomplishtheDeltaRMP’sgoals
2. Approvesbudgetsandexpenditures
3. Directsthefiscal/operatingagenttoenterintopartnerships,contracts,andotherlegalagreementsonbehalfoftheDeltaRMP,asnecessarytofulfilltheDeltaRMP’smission
4. ApprovesDeltaRMPworkproductsandanyotherplans,products,orresolutionsoftheDeltaRMP
5. SetsprioritiesandoverseetheactivitiesoftheTechnicalAdvisoryCommittees
6. Establishesandoverseestheimplementationofpoliciesandproceduresnecessarytotheday-to-dayfunctioningoftheDeltaRMP
TheDeltaRMPSteeringCommitteedecidedthattheinitialDeltaRMPwouldfocusonmercury,nutrients,pathogens,andpesticides.ManagementquestionstobeansweredbythemonitoringweredevelopedandprovidedtotheTACtodesignamonitoringprogramthatwouldanswerthemanagementquestionsposedbytheSteeringCommittee.ThisQAPPisaddressingmercury,pathogens,andpesticides.TheDeltaRMPnutrientmonitoringisstillbeingdeveloped.Whenthenutrientmonitoringhasbeendeveloped,thisQAPPwillbeupdatedtoincludenutrientandnutrient-associatedconstituents.
3. Program Tasks Description
3.1. WorkStatementandProducts
Toaddressthemanagementquestionsposed(AppendixA),theDeltaRMPwillconductsamplingforpesticides(monthly),mercury(quarterlyforunfilteredmethylmercuryandassociatedconstituentsinwaterandannuallyforfish),andpathogens(monthly).ThisworkisplannedandperformedundertheguidanceoftheDeltaRMPSteeringCommitteewithtechnicaladviceonmonitoringdesignfromtheTechnicalAdvisoryCommittees,whicharecomposedofstateandfederalregulators,permittees,watersupply,andcoordinatedmonitoringprogramrepresentatives.
DatafromStatusandTrendsmonitoringeffortswillbemadeavailableannuallyfordownloadviatheSFEI-ASCContaminantData,DisplayandDownloadtool(CD3)(http://cd3.sfei.org)andsubsequentlyincorporatedintotheCaliforniaEnvironmentalDataExchangeNetwork(CEDEN)andtheCaliforniaEstuarieswebportal.DatawillbereportedinanAnnualMonitoringReport,
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andaninterpretivemainreport(ThePulseofTheDelta)thatwillbepublishedinintervalsdecidedbytheSteeringCommitteetosummarizemonitoringresultsandsynthesizetheinformationtheyprovideinthecontextoftheassessmentandmanagementquestionsthatprovidetheframeworkforthemonitoringprogram.
Table3.1providesasummaryofkeyproductsoftheDeltaRMP.ThePulseoftheDeltawillbethemaininterpretivereportingvehicleforDeltaRMPresults.Theaudienceofthisreportwillbelocal,state,andfederaldecision-makersandtheinterestedpublic.ThedatawillbeinterpretedtoanswerDeltaRMPmanagementandassessmentquestions,basedonthemostappropriatestatisticalanalysestobeusedforevaluatingthedatainrelationtoaquestion,asguidedbytheTAC.BoththeTACandtheSCwillprovidereviewofthePulseoftheDelta.PriortoreleaseofthePulseoftheDelta,SFEI-ASCwillprovidebasicannualdatareports(AnnualMonitoringResultsReport)forreviewbytheTACandSC.Monitoringresultswillbeoneofthemaindecisionfactorsforadaptivechangestothemonitoringprogram.AnannualSCplanningmeeting/workshopwillidentifyadaptationsneededtothemonitoringprogramandwillbeinformedbymonitoringresults.Inaddition,theTACwillhaveaccesstopreliminarydatathroughtheTACwebsiteandthepassword-protecteddata-sharingworkspaceoftheCaliforniaEstuarieswebportal.
Table3.1.DeltaRMPreportingcycle.
Deliverable Frequency Releasedate
Datauploads
Provisionaldata(availabletoTACmembers)
Variable Variable
CD3 Annually1 March1
CEDEN Annually March1
CaliforniaEstuarieswebportal Annually March1
Reports
AnnualMonitoringReports(includingQAreport) Annually March1
TechnicalReports Variable Variable
PulseoftheDelta Variable Fall1Timeperiodofdataforannualreporting:pesticides(15months:July1throughSeptember30ofthefollowingyear),mercury(July1–June30),pathogens(April1–March31).
3.2. EvaluationofMonitoringData
Theprogram’smissionistoinformdecisionsonhowtoprotectandrestorebeneficialusesofwaterintheDelta,byproducingobjectiveandcost-effectivescientificinformationcriticaltounderstandingregionalwaterqualityconditionsandtrends.Dataanalysesandinterpretationin
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theDeltaRMPprovideanswerstotheassessmentquestions,andultimately,themanagementquestions.
Programparticipantsdeveloptheinterpretationcollectivelyinascience-basedandcollaborativeprocess.TheDeltaRMPSteeringCommitteehastheleadroleinmakingstatementsaboutthecoremanagementquestions.WithoversightbytheTAC,programstaffandcontractedindependentscientistsconducttherelevantanalysesbyevaluatingthedataagainstthespecificmonitoringquestionsandanystatedbenchmarksorperformancetargets.Asolidreviewprocessensuresthatinformationgeneratedbytheprogramishighquality,objective,andrelevant.
TheDeltaRMPprovidesdecision-makersandresourcemanagerswithinformationtofocusonwaterqualityproblems,todeterminewhatisandwhatisnotaproblemandfacilitateinformeddecisions.However,decisionsbasedonthedataaboutwhetherthereisimpairmentorwhetherandwhattypesofactionsaretobetakenaremadeoutsideoftheprogram.Regulatorydecisions,suchas303(d)listings,willbemadebytheWaterBoardusingitsownprocess.Therefore,theDeltaRMPdoesnothaveadetailedassessmentframeworkfordatainterpretationandfollow-up.
3.3. BeneficalUsesandWaterQualityGoals
ThecoremanagementquestionsandassessmentquestionscurrentlyencompassthefollowingbeneficialusesintheCentralValleyRegionBasinPlan(BasinPlan,CentralValleyRegionalWaterBoard2011)andtheBay-DeltaWaterQualityControlPlan(Bay-DeltaPlan,StateWaterBoard2006):
• ColdFreshwaterHabitat(COLD)
• CommercialandSportFishing(COMM)
• EstuarineHabitat(EST)
• FishMigration(MIGR)
• MunicipalandDomesticWaterSupply(MUN)
• PreservationofRare,Threatened,orEndangeredSpecies(RARE)
• WaterContactRecreation(REC1)
• NoncontactWaterRecreation(REC2)
• ShellfishHarvesting(SHELL)
• FishSpawning(SPWN)
• WarmFreshwaterHabitat(WARM)
• WildlifeHabitat(WILD)
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Table3.2providesanoverviewofbeneficialusesthatarerelevanttotheprioritizedassessmentquestions(AppendixB)ofeachoftheindividualmonitoringelements.Table3.3summarizesexistingnumericwaterqualitycriteriaandaquaticlifebenchmarksfortargetanalytesofpesticidemonitoring.Chemicalspecificnumericcriteriadonotexistforalltargetanalytes.Table3.4liststheregulatorytargetsformethylmercurythatwillbeusedinevaluationsofDeltaRMPdata.Table3.5providesinformationonLT2Rulebinlevelclassificationofsourcewater,basedonCryptosporidiumconcentrations.Binlevelsareusedintriggerexceedanceassessmentsofpathogenmonitoringdata.
Table3.2.BeneficialUsesassociatedwithDeltaRMPmonitoringelements.
BeneficialUse Pesticides Mercury Nutrients1 Pathogens
COLD X X X
COMM X X
EST X X X
MIGR X X
MUN X X
RARE X X X
REC1 X
REC2 X
SHELL X X
SPWN X X
WARM X X X
WILD X X X 1Plannedforfutureimplementation.
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Table3.3.EPAOfficeofWater(OW)AquaticLifeAmbientWaterQualityCriteria,EPAOfficeofPesticidePrograms(OPP)AquaticLifeBenchmarks5,andWaterQualityObjectivesfortargetanalytesofpesticidemonitoring(CentralValleyWaterBoard1998,2007;EPA2000,2015a,2015b)(concentrationsinμg/L).
Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteTraceElements
Copper(dissolved) 10 — 13 9 CalculatedusingtheBioticLigandModel 15.7 9.01 2.05 1.11 3.1 2300 —
DegradatesChlorpyrifosOA — — — — — — — — — — — — —Dichlorophenyl-3-methylUrea,3,4- — — — — — — — — — — — — —
DDD(p,p’) — — — — — — — — — — — — —DDE(p,p’) — — — — — — — — — — — — —Dichloroaniline,3,4- — — — — — — — — — — — — —Dichloroaniline,3,5- — — — — — — — — — — — — —DichlorophenylUrea,3,4- — — — — — — — — — — — — —Diazoxon — — — — — — — — — — — — —FipronilDesulfinyl — — — — — — 10 0.59 100 10.3 140 >100 —FipronilDesulfinylAmide — — — — — — — — — — — — —FipronilSulfide — — — — — — 41.5 6.6 1.065 0.11 140 >100 —FipronilSulfone — — — — — — 12.5 0.67 0.36 0.037 140 >100 —Malaoxon — — — — 0.065 0.013 — — — — — — —
5EPA.2015a.AquaticLifeBenchmarksforPesticideRegistration.URL:http://www2.epa.gov/pesticide-science-and-assessing-pesticide-risks/aquatic-life-benchmarks-pesticide-registration#benchmarks.AccessedonJuly8,2016.
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteTebupirimfosoxon — — — — — — — — — — — — —FungicidesAcibenzolar-S-methyl — — — — — — — — — — — — —Azoxystrobin — — — — — — 235 147 130 44 49 3400 —Boscalid — — — — — — 1350 116 >2665 790 1340 >3900 —Captan — — — — — — 13.1 16.5 4200 560 320 >12700 —Carbendazim — — — — — — 190 — 150 — 7700 — 75Chlorothalonil — — — — — — 5.25 3 1.8 0.6 6.8 630 —Cyazofamid — — — — — — >53.5 90.1 >650 <87 — >1220 —Cymoxanil — — — — — — 29000 — 27000 — 254 — 254Cyproconazole — — — — — — — — — — — — —Cyprodinil — — — — — — 1205 230 16 8 2250 — —Desthio-Prothioconazole — — — — — — — — — — — — —Difenoconazole — — — — — — 405 8.7 385 5.6 98 1900 —Dimethomorph — — — — — — 3100 <341 >5300 110 — — —Ethaboxam — — — — — — — — — — — — —Famoxadone — — — — — — 11 — 12 — 22 — 5.5Fenamidone — — — — — — 370 4.7 24.5 12.5 70 >880 —Fenarimol — — — — — — 450 180 3400 113 100 — —Fenbuconazole — — — — — — 1500 — 2300 — 330 — 330Fenhexamide — — — — — — 670 101 >9400 1000 4820 >2300 —Fluazinam — — — — — — 18 0.69 90 68 1.1 — —Fludioxonil — — — — — — 235 19 450 <19 70 >1000 —Fluopicolide — — — — — — 174.5 151 >850 190 <1.4 >3200 —Fluoxastrobin — — — — — — 435 — 480 — 350 — 217.5
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteFlusilazole — — — — — — — — — — — — —Flutolanil — — — — — — 1250 233 >3400 530 8010 8010 —Flutriafol — — — — — — 16500 4800 33550 310 460 780 —Fluxapyroxad — — — — — — — — — — — — —Imazalil — — — — — — 1480 — 3500 — 870 — 740Ipconazole — — — — — — 765 0.18 850 — — — —Iprodione — — — — — — — 260 120 — >130 >12640 —Kresoxim-methyl — — — — — — 95 87 166 55 29.2 >301 —Mandipropamid — — — — — — — 220 3550 — >2500 >7400 —Metalaxyl — — — — — — 65000 9100 14000 100 140000 92000 —Metconazole — — — — — — 2100 — 4200 — 1700 — 1050Myclobutanil — — — — — — 1200 980 5500 — 830 — —Paclobutrazol — — — — — — 7950 49 120 9 40800 8 —PCNB — — — — — — 50 13 385 18 — — —Picoxystrobin — — — — — — 32.5 36 12 1 4 210 —Propiconazole — — — — — — 425 95 650 260 21 4828 —Pyraclostrobin — — — — — — 3.1 2.35 7.85 4 1.5 1720 —Pyrimethanil — — — — — — 5050 20 1500 1000 1800 7800 —Quinoxyfen — — — — — — — — — — — — —Sedaxane — — — — — — — — — — — — —Tebuconazole — — — — — — 1135 12 1440 120 1450 151.5 —Tetraconazole — — — — — — 1925 300 1315 190 — 310 —Thiabendazole — — — — — — 280 110 155 42 3060 2320 —Triadimefon — — — — — — 2050 41 800 52 17000 — —Triadimenol — — — — — — — — — — — — —
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteTrifloxystrobin — — — — — — 7.15 4.3 12.65 2.76 37.1 >1930 —Triflumizole — — — — — — 290 33 700 67 140 720 —Triticonazole — — — — — — — — — — — — —Zoxamide — — — — — — 78 3.48 >390 39 10 19 —HerbicidesAlachlor — — — — — — 900 187 1250 110 1.64 2.3 —Atrazine — — — — — — 2650 — 360 60 <1 0.001 —Benfluralin — — — — — — — — — — — — —Butralin — — — — — — — — — — — — —Butylate — — — — — — 105 — 5950 — — — —Clomazone — — — — — — 1450 350 2700 2200 167 30200 —Cycloate — — — — — — 2250 — 1300 — — — —Cyhalofop-butyl — — — — — — 790 — 2700 — 960 — 395Dacthal — — — — — — 15000 — 13500 — >11000 >11000 —Dithiopyr — — — — — — — — — — — — —Diuron — — — — — — 200 26.4 80 200 2.4 15 —EPTC — — — — — — 7000 — 3250 800 1,400 5600 —Ethalfluralin — — — — — — 16 0.4 30 24 25 — —Flufenacet — — — — — — — — — — — — —Fluridone — — — — — — 2800 480 680 — — — —Hexazinone — — — — — — 137000 17000 75800 20000 7 37.4 —Metolachlor — — — — — — 1600 30 550 1 8 21 —Molinate — — — — — — 105 390 170 340 220 3300 —Napropamide — — — — — — 3200 1100 7150 1100 3400 — —Novaluron — — — — — — >490 6.16 0.075 0.03 3549 >75.4 —
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteOryzalin — — — — — — 1440 220 750 358 42 >15.4 —Oxadiazon — — — — — — 600 33 1090 33 5.2 41 —Oxyfluorfen — — — — — — 100 1.3 750 13 1.1 0.33 —Pebulate — — — — — — 3150 — 3,315 — 230 1800 —Pendimethalin — — — — — — 69 6.3 140 14.5 5.2 12.5 —Penoxsulam — — — — — — >51000 10200 >49250 2950 92 3 —Prodiamine — — — — — — >6.5 — >6.5 1.5 — — —Prometon — — — — — — 6000 19700 12850 3450 98 — —Prometryn — — — — — — 1455 620 4850 1000 1.04 11.9 —Propanil — — — — — — 1150 9.1 600 86 16 110 —Pronamide — — — — — — 36000 7700 >2800 600 >4000 1180 —Simazine — — — — — — 3200 — 500 — 2.24 140 —Thiazopyr — — — — — — 3400 — 6100 — 40 — 40Thiobencarb — — — — — — 220 21 50.6 1.0 17 770 —Triallate — — — — — — 600 38 45.5 14 21 2400 —TributhylPhosphorotrithioate,S,S,S-
— — — — — — 122.5 3.5 3.4 1.56 148 1100 —
Trifluralin — — — — — — 20.5 1.14 280 2.4 7.52 43.5 —InsecticidesAcetamiprid — — — — — — >50000 19200 10.5 2.1 >1000 >1000 —Allethrin — — — — — — — — 1.05 — — — —AzinphosMethyl — — — — — — 0.18 0.055 0.08 0.036 — — —Bifenthrin — — — — — — 0.075 0.04 0.8 0.013 — — —Carbaryl — — 2.1 2.1 2.1 2.1 110 6 0.85 0.5 660 1500 —
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteCarbofuran — — — — — — 44 5.7 1.115 0.75 — — —Chlorantraniliprole — — — — — — >600 110 4.9 4.5 1800 2000 —Chlorpyrifos 0.025 0.015 — — 0.083 0.041 0.9 0.57 0.05 0.04 140 — 0.025Clothianidin — — — — — — >50750 9700 11 11 64000 121000 —Coumaphos — — — — — — 140 11.7 0.037 0.0337 — — —Cyantranilipole — — — — — — >5000 10700 10.2 6.56 >10000 12100 —Cyfluthrin,Total — — — — — — 0.034 0.01 0.0125 0.0074 >181 — —Cyhalothrin,Total — — — — — — — — — — — — —Cypermethrin,Total — — — — — — 0.195 0.14 0.21 0.069 — — —DDT(p,p') — — 1.1 0.001 1.1 0.001 — — — — — — —Deltamethrin — — — — — — 0.29 0.017 0.055 0.0041 — — —Diazinon 0.16 0.1 — — 0.17 0.17 45 <0.55 0.105 0.17 3700 — 0.16Dinotefuran — — — — — — >49550 >6360 >484150 >95300 >97600 >110000 —Esfenvalerate — — — — — — 0.035 0.035 0.025 0.017 — — —Ethofenprox — — — — — — 1.35 23 0.4 0.17 >18.8 >26 —Fenpropathrin — — — — — — 1.1 0.091 0.265 0.064 — — —Fenpyroximate — — — — — — 0.22 0.11 0.8 0.56 1.9 >190 —Fenthion — — — — — — 415 7.5 2.6 0.013 400 >2800 —Fipronil — — — — — — 41.5 6.6 0.11 0.011 140 >100 —Flonicamid — — — — — — 100000 — 100000 — 3300 — 3300Imidacloprid — — — — — — >41500 1200 34.5 1.05 >10000 — —Indoxacarb — — — — — — 145 150 300 75 >110 >84 —Malathion — — — — — 0.1 16.5 8.6 0.295 0.035 2400 >9630 —Methidathion — — — — 0.065 0.013 1.1 6.3 1.5 0.66 — — —Methoprene — — — — — — 380 48 165 51 — — —
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Pesticide
WaterQualityObjectives
WaterQualityObjectives
OWAquaticLifeCriteria
OPPAquaticLifeBenchmarks(italicized:OPPbenchmarkequivalents,Luoetal.2013)
OPPBenchmarkEquivalents
R5-Delta CAToxicsRule Fish Invertebrates Nonvascularplants
Vascularplants
Lowestreported
Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Chronic Acute Acute AcuteMethoxyfenozide — — — — — — >2100 530 25 6.3 >3400 — —Parathion,Methyl — — — — — — 925 <10 0.485 0.25 15000 18000 —Pentachloroanisole — — — — — — 28 — 150 — — — —Permethrin,Total — — — — — — 0.395 0.0515 0.0106 0.0014 68 — —Phenothrin — — — — — — — — — — — — —Phosmet — — — — — — 35 3.2 1 0.8 — — —Propargite — — — — — — 59 16 37 9 66.2 75000 —Pyridaben — — — — — — — — — — — — —Resmethrin — — — — — — 0.14 0.35 1.55 — — — —Tebupirimfos — — — — — — 44.5 130 0.039 0.011 630 8800 —Tefluthrin — — — — — — 0.03 0.004 0.035 0.008 — — —Tetradifon — — — — — — — — — — — — —Tetramethrin — — — — — — 1.85 — 22.5 — — — —T-Fluvalinate — — — — — — — — — — — — —Thiacloprid — — — — — — 12600 918 18.9 0.97 45000 >95400 —Thiamethoxam — — — — — — >50000 20000 17.5 — >97000 >90000 —Tolfenpyrad — — — — — — — — — — — — —PlantGrowthRegulatorsFlumetralin — — — — — — — — — — — — —SynergistsPiperonylButoxide — — — — — — 950 40 255 30 — — —
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Table3.4.Waterqualitybenchmarksformercury(CentralValleyWaterBoard2011).
Constituent
WaterQualityObjectives
CentralValleyBasinPlan/
Sacramento-SanJoaquinDeltaandYoloBypasswaterways
Muscletissueoftrophiclevel4fish
(mg/kg,wetweight)
Water(unfiltered)
TMDLimplementationgoal
(ng/L)
Mercury,Methyl 0.246 0.06
Table3.5.BinclassificationforPublicWaterSystems(EPA2013).
Cryptosporidiumbinconcentration
(oocysts/L)
Binclassification
<0.075 Bin1
>0.075,<1 Bin2
>1,<3 Bin3
>3 Bin4
3.4. ConstituentstobeMonitoredandReported
DeltaRMPmonitoringwillincludethecollection,measurement,andreportingofmany
parameters.Thefollowinginformationwillbeincludedwitheachsamplecollection:
• Sitelocation(latitudeandlongitude)(Tables7.1)
• Sitesamplingdateandtime(Tables7.1)
• Matrixsampled(e.g.,water)
• Parametermeasurements(Table3.6)
• Collectionandanalyticalmethods(Table4.4)
• Qualifiersandcomments(appliedbyanalyticallabsorbyDeltaRMPstaffindata
review)(Table6.1)
ThecurrentimplementationoftheDeltaRMPincludesmonitoringforpesticides,mercury,and
pathogens.Thus,theQAPPonlyaddressesthepesticides,mercury,andpathogensmonitoring
6Totalmercuryconcentrationsareusedasasurrogateformercury,methylconcentrationsinfishtissue.
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elements.Thepesticidesmonitoringelementincludeschemicalanalysesandtoxicitytesting.
Thechemicalanalytegroupsforthismonitoringelementincludeseveralpesticidegroups,
dissolvedcopper,andancillaryparameterssuchasdissolved/particulateorganiccarbonand
hardness.Themercurymonitoringelementincludestheanalysisofsamplesfromwaterand
fish.Table3.6providesacompletelistoftargetparametersforthecurrentimplementationof
theDeltaRMP.
Table3.6.DeltaRMPtargetparametersandreportingunits.Allparameterslistedunder
pesticidesamplingwillbeanalyzedforeachpesticidesamplingsiteateachpesticidesampling
event.Mercuryfishtissueparameterswillbeanalyzedannuallyandmercurywatersampling
parameterswillbeanalyzedquarterly.Pathogenmonitoringparameterswillbeanalyzedfor
eachpathogenmonitoringsiteateachmonthlysamplingevent.
PesticideSampling
Constituent ReportingGroup Matrix Unit
Oxygen,Dissolved FieldMeasurements Water mg/L
Oxygen,Dissolved FieldMeasurements Water %saturation
pH FieldMeasurements Water pH
SpecificConductivity FieldMeasurements Water μS/cm
Temperature FieldMeasurements Water °CTurbidity FieldMeasurements Water FNU
PesticideSampling–ToxicityTestingLaboratoryAnalysis
Constituent ReportingGroup Matrix Unit
HardnessasCaCO3 Conventional Water mg/L
Ceriodaphniadubia(Reproduction) WaterColumnToxicity Wateryoung/originalorganisms
exposed
Ceriodaphniadubia(Survival) WaterColumnToxicity Water %
Hyalellaazteca(Survival)7 WaterColumnToxicity Water %
Pimephalespromelas(Larvalbiomass)
WaterColumnToxicity Watermg/originalorganisms
exposed
Pimephalespromelas(Larvalsurvival) WaterColumnToxicity Water %
Selenastrumcapricornutum(Growth) WaterColumnToxicity Water cells/mL
PesticideSampling–ChemicalAnalysisLaboratory
Constituent ReportingGroup Matrix Unit
DissolvedOrganicCarbon(DOC) Conventional Water mg/L
PesticideSampling–ChemicalAnalysisLaboratory
Constituent ReportingGroup Matrix Unit
ParticulateOrganicCarbon(POC) Conventional Water mg/L
TotalSuspendedSolids(TSS) Conventional Water mg/L
Copper(dissolved) TraceMetals Water ug/L
7InclusionofHyalellawatertoxicitytestingispendingafinaldecisionbytheSC.
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ChlorpyrifosOxon Degradates Water ng/L
Dichlorophenyl-3-methylUrea,3,4- Degradates Water ng/L
DDD(p,p') Degradates Water ng/L
DDE(p,p') Degradates Water ng/L
Diazoxon Degradates Water ng/L
Dichlorobenzenamine,3,4- Degradates Water ng/L
Dichloroaniline,3,5- Degradates Water ng/L
DichlorophenylUrea,3,4- Degradates Water ng/L
FipronilDesulfinyl Degradates Water ng/L
FipronilDesulfinylAmide Degradates Water ng/L
FipronilSulfide Degradates Water ng/L
FipronilSulfone Degradates Water ng/L
Malaoxon Degradates Water ng/L
Tebupirimfosoxon Degradates Water ng/L
Acibenzolar-S-methyl Fungicides Water ng/L
Azoxystrobin Fungicides Water ng/L
Boscalid Fungicides Water ng/L
Captan Fungicides Water ng/L
Carbendazim Fungicides Water ng/L
Chlorothalonil Fungicides Water ng/L
Cyazofamid Fungicides Water ng/L
Cymoxanil Fungicides Water ng/L
Cyproconazole Fungicides Water ng/L
Cyprodinil Fungicides Water ng/L
Dimethomorph Fungicides Water ng/L
Desthio-Prothioconazole Fungicides Water ng/L
Difenoconazole Fungicides Water ng/L
Ethaboxam Fungicides Water ng/L
Famoxadone Fungicides Water ng/L
Fenamidone Fungicides Water ng/L
Fenarimol Fungicides Water ng/L
Fenbuconazole Fungicides Water ng/L
Fenhexamid Fungicides Water ng/L
Fluazinam Fungicides Water ng/L
Fludioxonil Fungicides Water ng/L
Fluopicolide Fungicides Water ng/L
Fluoxastrobin Fungicides Water ng/L
PesticideSampling–ChemicalAnalysisLaboratory
Constituent ReportingGroup Matrix Unit
Flusilazole Fungicides Water ng/L
Flutolanil Fungicides Water ng/L
Flutriafol Fungicides Water ng/L
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Fluxapyroxad Fungicides Water ng/L
Imazalil Fungicides Water ng/L
Ipconazole Fungicides Water ng/L
Iprodione Fungicides Water ng/L
Kresoxim-methyl Fungicides Water ng/L
Mandipropamid Fungicides Water ng/L
Metalaxyl Fungicides Water ng/L
Metconazole Fungicides Water ng/L
Myclobutanil Fungicides Water ng/L
Paclobutrazol Fungicides Water ng/L
PCNB Fungicides Water ng/L
Picoxystrobin Fungicides Water ng/L
Propiconazole Fungicides Water ng/L
Pyraclostrobin Fungicides Water ng/L
Pyrimethanil Fungicides Water ng/L
Quinoxyfen Fungicides Water ng/L
Sedaxane Fungicides Water ng/L
Tebuconazole Fungicides Water ng/L
Tetraconazole Fungicides Water ng/L
Thiabendazole Fungicides Water ng/L
Triadimefon Fungicides Water ng/L
Triadimenol Fungicides Water ng/L
Trifloxystrobin Fungicides Water ng/L
Triflumizole Fungicides Water ng/L
Triticonazole Fungicides Water ng/L
Zoxamide Fungicides Water ng/L
Alachlor Herbicides Water ng/L
Atrazine Herbicides Water ng/L
Benfluralin Herbicides Water ng/L
Butralin Herbicides Water ng/L
Butylate Herbicides Water ng/L
Clomazone Herbicides Water ng/L
Cycloate Herbicides Water ng/L
Cyhalofop-butyl Herbicides Water ng/L
Dacthal Herbicides Water ng/L
Dithiopyr Herbicides Water ng/L
Diuron Herbicides Water ng/L
PesticideSampling–ChemicalAnalysisLaboratory
Constituent ReportingGroup Matrix Unit
EPTC Herbicides Water ng/L
Ethalfluralin Herbicides Water ng/L
Flufenacet Herbicides Water ng/L
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Fluridone Herbicides Water ng/L
Hexazinone Herbicides Water ng/L
Metolachlor Herbicides Water ng/L
Molinate Herbicides Water ng/L
Napropamide Herbicides Water ng/L
Novaluron Herbicides Water ng/L
Oryzalin Herbicides Water ng/L
Oxadiazon Herbicides Water ng/L
Oxyfluorfen Herbicides Water ng/L
Pebulate Herbicides Water ng/L
Pendimethalin Herbicides Water ng/L
Penoxsulam Herbicides Water ng/L
Prodiamine Herbicides Water ng/L
Prometon Herbicides Water ng/L
Prometryn Herbicides Water ng/L
Propanil Herbicides Water ng/L
Pronamide Herbicides Water ng/L
Simazine Herbicides Water ng/L
Thiazopyr Herbicides Water ng/L
Thiobencarb Herbicides Water ng/L
Triallate Herbicides Water ng/L
TributylPhosphorotrithioate,S,S,S- Herbicides Water ng/L
Trifluralin Herbicides Water ng/L
Acetamiprid Insecticides Water ng/L
Allethrin Insecticides Water ng/L
AzinphosMethyl Insecticides Water ng/L
Bifenthrin Insecticides Water ng/L
Carbaryl Insecticides Water ng/L
Carbofuran Insecticides Water ng/L
Chlorantraniliprole Insecticides Water ng/L
Chlorpyrifos Insecticides Water ng/L
Clothianidin Insecticides Water ng/L
Coumaphos Insecticides Water ng/L
Cyantraniliprole Insecticides Water ng/L
Cyfluthrin,Total Insecticides Water ng/L
Cyhalothrin Insecticides Water ng/L
Cypermethrin,Total Insecticides Water ng/L
PesticideSampling–ChemicalAnalysisLaboratory
Constituent ReportingGroup Matrix Unit
DDT(p,p') Insecticides Water ng/L
Deltamethrin Insecticides Water ng/L
Diazinon Insecticides Water ng/L
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Dinotefuran Insecticides Water ng/L
Esfenvalerate Insecticides Water ng/L
Ethofenprox Insecticides Water ng/L
Fenpropathrin Insecticides Water ng/L
Fenpyroximate Insecticides Water ng/L
Fenthion Insecticides Water ng/L
Fipronil Insecticides Water ng/L
Flonicamid Insecticides Water ng/L
Imidacloprid Insecticides Water ng/L
Indoxacarb Insecticides Water ng/L
Malathion Insecticides Water ng/L
Methidathion Insecticides Water ng/L
Methoprene Insecticides Water ng/L
Methoxyfenozide Insecticides Water ng/L
Parathion,Methyl Insecticides Water ng/L
Pentachloroanisole Insecticides Water ng/L
Permethrin,Total Insecticides Water ng/L
Phenothrin Insecticides Water ng/L
Phosmet Insecticides Water ng/L
Propargite Insecticides Water ng/L
Pyridaben Insecticides Water ng/L
Resmethrin Insecticides Water ng/L
Tebupirimfos Insecticides Water ng/L
Tefluthrin Insecticides Water ng/L
Tetradifon Insecticides Water ng/L
Tetramethrin Insecticides Water ng/L
T-Fluvalinate Insecticides Water ng/L
Thiacloprid Insecticides Water ng/L
Thiamethoxam Insecticides Water ng/L
Tolfenpyrad Insecticides Water ng/L
Flumetralin PlantGrowthRegulators Water ng/L
PiperonylButoxide Synergists Water ng/L
Mercury–FishSampling
Constituent/Measurement ReportingGroup Matrix Unit
Mercury TraceMetalsTissue
(filletmuscle)μg/gww
TotalLength FishAttributes Tissue mm
Mercury–FishSampling
Constituent/Measurement ReportingGroup Matrix Unit
ForkLength FishAttributes Tissue mm
Weight FishAttributes Tissue g
Sex FishAttributes Tissue male/female
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Moisture FishAttributes Tissue %
Mercury-WaterSampling
Constituent/Measurement ReportingGroup Matrix Unit
Mercury,Methyl,total(unfiltered) TraceMetals Water ng/L
Mercury,Methyl,(filtered) TraceMetals Water ng/L
Mercury(unfiltered) TraceMetals Water ng/L
Mercury(filtered) TraceMetals Water ng/L
Chlorophylla Conventional Water μg/L
DissolvedOrganicCarbon(DOC) Conventional Water mg/L
TotalSuspendedSolids(TSS) Conventional Water mg/L
TSS(volatile) Conventional Water mg/L
Oxygen,Dissolved FieldMeasurements Water mg/L
Oxygen,Dissolved FieldMeasurements Water %saturation
pH FieldMeasurements Water pH
SpecificConductivity FieldMeasurements Water μS/cm
PathogenMonitoring
Constituent ReportingGroup Matrix Unit
Cryptosporidium Pathogens Water oocysts/L
Giardia Pathogens Water cysts/L
3.5. GeographicalandTemporalSetting
ThegeographicscopeoftheDeltaRMPencompassesthelegalDelta(asdefinedbysection
12220oftheWaterCode),includingwaterbodiesthatdirectlydrainintotheDelta,Yolo
Bypass,andSuisunBay.Inaddition,thebasemonitoringandspecialstudiesoftheDeltaRMP
mayextendupstreamordownstream,ifrequiredtoaddressspecificmanagementquestions.
Monitoringsitesforpesticides8,mercury,andpathogensaredescribedinthissection.
Additionalinformationfornutrientsmonitoringsiteswillbeaddedlater.
3.5.1. Pesticides
Thesurfacewatersamplesforpesticideanalysesarecollectedfromfixedsitesrepresentingkey
inflowstotheDeltathatarevisitedmonthly.Targetedeventsamplinginanygivenmonthmay
beconductedinlieuofscheduledmonthlysampling.Targetedeventsincludetwowetevents
(1stseasonalflush,2ndsignificantstorminwinter)andthreedryevents(earlyspring,irrigation
seasonsamplinglatespring/earlysummer,irrigationseasonsamplinglatesummer).
Figures3.1showsthecurrentwatersamplingsitesandTable3.7providesanoverviewofthe
samplingscheduleforpesticides.Thepesticidesmonitoringelementincludeschemicalanalyses
8Pesticidemonitoringincludeschemicalpesticideanalysis,toxicitytesting,andtheanalysisofdissolvedcopperandrelevantfieldand
conventionalwaterqualityparametersatallsites.
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andtoxicitytesting.Theparametersanalyzedforthismonitoringelementincludeseveral
pesticidereportinggroups,dissolvedcopper,fieldparameters,and“conventional”parameters
(ancillaryparametersmeasuredinthelaboratory,suchasdissolved/particulateorganiccarbon
andhardness).
Table3.7.Listofsitetypesamplingfrequenciesandassociatedparametergroupsforpesticides
monitoring.
ParameterGroup Baselinesitesamplingfrequency Matrix
Conventionalparameters Monthly Water
Fieldparameters Monthly Water
Metals(dissolvedCopperonly) Monthly Water
Pesticides Monthly Water
Watercolumntoxicity Monthly Water
3.5.2. Mercury
Thesurfacewatersamplesformercuryanalysesarecollectedquarterlyfromfixedsitesthat
alignwithsportfishmonitoringsites.
Thesportfishsamplesformercuryanalysesarecollectedannuallyfromfixedsitesthat
representdifferentsubareasoftheDelta.
Figure3.2showsthemercurysamplingsites.Themercurymonitoringelementincludesfishand
watersampling.Thechemicalanalytegroupsforthismonitoringelementincludemercuryand
methylmercuryandancillaryparameterssuchaschlorophylla,DOC,totalsuspendedsolids,andvolatilesuspendedsolids.
3.5.3. Pathogens
Ambientpathogenmonitoringsitesareco-locatedwithexistingsitesoftheMunicipalWater
QualityInvestigations(MWQI)program(Figure3.3).Someofthesesitesareupstreamofthe
Delta,butcouldinfluencewaterqualityatthedrinkingwaterintakesorarerepresentativeof
largerareaswiththesamelanduses.AdditionalsampleswillbecollectedatvariousDelta
watersupplyintakes(7drinkingwaterintakesiteswithasinglesource,plus2facilitieswith
blendingfrom4drinkingwaterintakes)incoordinationwiththeseambientsites.
TheDeltaRMPPathogenStudyDesignspecifiesmonthlyambientmonitoringsamplecollection
fortwoyearsbeginninginApril2015tomatchtheLongTerm2EnhancedSurfaceWater
TreatmentRule(LT2)-requiredwatersupplyintakesamplecollection.MWQIwillcollectgrab
samplesateachofthelocationsshowninTableA-1duringthefirstweekofeachmonthonthe
site-specificday.
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3.6. Constraints
Theabilitytomeasuresomeofthetargetcompoundsattheultra-tracelevelsfoundinthe
ambientenvironmentmaybeconstrainedbythedetectionlimitsroutinelyachievableby
analyticallaboratories.Targetdetectionlimitsinthisdocumentrepresentthoseachievedby
laboratoriescontractedbytheDeltaRMPorlevelsneededtoobtainquantitative
measurementsofambientconcentrationsinamajorityofsamples.
Anotherconstraintisthatdiscretesamplesrepresentonlyamomentintimeandmaytherefore
notalwaysrepresentconditionsduringothertimeperiods.
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Figure3.1.FY2014-17PesticideWaterSamplingSites9.
9 Pesticidemonitoringincludeschemicalpesticideanalysis,toxicitytesting,andtheanalysisofdissolvedcopperandrelevantfieldand
conventionalwaterqualityparametersatallsites.
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Figure3.2.FY2016-17MercuryMonitoringSites.
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Figure3.3.FY2014-17AmbientPathogenMonitoringSites.
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4. Data Quality Objectives and Indicators, Criteria, and Control Procedures for Measurement Data
DataQualityObjectives(DQOs)aimtosupportdefensibleconclusionsthataddressthe
managementquestionsandassessmentquestionsinAppendicesAandB.Dataquality
indicators(DQIs)forfieldandlaboratorymeasurementsevaluatethefollowing:
• Fieldmeasurements–sensitivity,precision,accuracy,completeness
• Laboratorychemicalanalyses–sensitivity,precision,accuracy,completeness,
contamination
• Toxicitytesting–precision,completeness,representativeness
Thediscussioninthissectionreviewsthemeasurementsandproceduresexpectedto
demonstratethequalityofreporteddata.Table4.1providesanoverviewofqualitycontrol
(QC)sampletypesandtheirpurpose.Thequalityassessmentprocessthatisusedafterthedata
havebeencollectedtoevaluatewhethertheDataQualityObjectives(DQOs)havebeen
satisfiedisdescribedandillustratedinSection17,VerificationandValidationMethods.
Table4.1.PurposesoffieldandlaboratoryQCsampletypesanddataqualityindicators
applicabletotheDeltaRMP
QCSampleType DataQualityIndicator/Purpose
CalibrationAccuracyofmeasurement(fieldparameters,laboratorychemical
analysis).
CalibrationCheck Accuracyofcalibration(fieldparameters,laboratorychemicalanalysis).
LaboratoryBlanks-
MethodBlanks
Contamination/confirmtheabsenceofanalytesintroducedinthelab
(laboratorychemicalanalysis).
LaboratoryBlanks-
InstrumentBlanks
Contamination/Assessthepresenceorabsenceofinstrument
contamination(laboratorychemicalanalysis).
CRM(Reference
Material)
Accuracyofmeasurement(primarily);precision/mostrobustindicatorof
measurementaccuracy;mayalsobeusedtoevaluatereplicateprecision
andrecoverywhereaveragevaluesforfieldsamplesareexpected(based
onhistoricalorliteratureresults)tofallinanon-quantitativerange
(laboratorychemicalanalysis).
LaboratoryDuplicates-
MatrixSpikes
(MS)/MatrixSpike
Duplicates(MSD)
Accuracyandprecision/evaluatetheeffectofthesamplematrixonthe
recoveryofthecompound(s)ofinterestandprovidinganestimateof
analyticalprecisionwhenmeasuredinduplicate(laboratorychemical
analysis).
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QCSampleType DataQualityIndicator/Purpose
LaboratoryDuplicates-
MatrixDuplicates
Precisionofintra-laboratoryanalyticalprocess(laboratorychemical
analysis)
SurrogateSpikesAccuracyofanalyticalmethod/assesstheefficiencyoftheextraction
methodfororganicanalytes(laboratorychemicalanalysis).
InternalStandards
Accuracyofanalyticalmethod/enableoptimalquantitation,particularly
ofcomplexextractssubjecttoretentiontimeshiftsorinstrument
interferencesrelativetotheanalysisofstandards.Internalstandardscan
alsobeusedtodetectandcorrectforproblemsintheinjectionportor
otherpartsoftheinstrument(laboratorychemicalanalysis).
FieldBlanks
Contamination/Tocheckcross-contaminationduringsamplecollection,
fieldsampleprocessing,andshipment.Alsotochecksamplecontainers
(laboratorychemicalanalysis).Fieldcrewswillneedtoincludefiltrationin
processingblanksforapplicablesampletypes.
Field
Duplicate/Replicate
Precision/Checkreproducibilityoffieldprocedures.Toindicatenon-
homogeneity.(FieldDuplicate:n=2;FieldReplicate:n>2).Thissampleis
tobecollectedinthefieldintandemwitharegularenvironmental
sample.Tobepreserved,handledandprocessedasauniquesample.Lab
precisioniscoveredbelow(laboratorychemicalanalysis).
InstrumentReplicates Precisionofinstrument(laboratorychemicalanalysis).
Travel/bottleblanks
Contamination/Toaccountforcontaminantsintroducedduringthe
transportprocessbetweenthelaboratoryandfieldsite,inadditiontoany
contaminationfromthesourcesolutionandcontainer(laboratory
chemicalanalysis).
NegativeControlToevaluatetestperformanceandthehealthandsensitivityofthe
specificbatchoforganisms(laboratorytoxicitytesting).
Referencetoxicant
testing
Sensitivity,precisionandaccuracyoftoxicitytestsperformedinthe
laboratory/Determinethesensitivityofthetestorganismsovertime;
assesscomparabilitywithinandbetweenlaboratorytestresults;identify
potentialsourcesofvariability,suchastestorganismhealth,differences
amongbatchesoforganisms,changesinlaboratorywaterorfoodquality,
andperformancebylaboratoryanalysts(laboratorytoxicitytesting).
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4.1. FieldQCProcedures
4.1.1. FieldPerformanceMeasurements
Sensitivityistheabilityofameasurementtodetectsmallquantitiesofthemeasured
component.Thesensitivityoffieldmeasurementsisgenerallydeterminedbytheoutputofthe
analyticalinstrument.Appropriateinstrumentsand/orinstrumentsettingsshouldbechosen
thatgenerallyallowdifferencesbetweensitesorwithinasiteatdifferenttimesbeingreported.
Resolutionontheorderofapproximately1%ofthemaximumorrangeofmeasurementslikely
tobeencounteredisdesired.
Precisionoffieldmeasurementsisdeterminedbyrepeatedmeasurementofthesame
parameterwithinasinglesample,orsamplestakeninrapidsuccession(onlywhenconditions
arenotdynamicallyvariable).Approximately10%ofmeasurements,aminimumofone
measurementperevent,shouldberepeatedforallmeasuredparameters.Repeated
measurementmayalsobeaccomplishedbycontinuousloggingofinsituprobesormeters.
Accuracyoffieldmeasurementsisestablishedbyperiodicmeasurementofknownstandardsor
byrecalibrationtoknownstandards.Instrumentrecalibrationshouldbeperformedpriorto
eachsamplingdayoreventforuser-calibratedinstruments(e.g.dailyforhandheldfield
meters),oratthemanufacturer-specifiedintervalforinstrumentsrequiringfactoryservicingor
otherwiseincapableoffieldrecalibration.
Completenessoffieldmeasurementisevaluatedasapercentageofusablemeasurementsout
ofthetotalnumberofmeasurementsdesired.Morethan90%offieldmeasurementsshouldbe
usable.Ifalowerpercentageisachievedforanysamplingeventortimeperiod,causesshallbe
investigatedandfixedwherepossible,throughinstrumentmaintenance(e.g.defouling),
recalibration,repair,orreplacement(withthesameordifferentinstrumenttype)asneeded.If
completenesstargetsarenotachieved,instrumentchoice,settings,deploymentmethod,
maintenance,and/orotheractivitiesshallbeadjustedtoimprovemeasurementreliability
beforethenextsamplingeventormeasurementperiod.
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4.1.2. FieldQCMeasurements
Calibrationofanyfieldmeters(pH,conductivity,DO,orothermeasurements)shouldbe
checkedinthefieldatleastoncedailyandrecalibratedusingcertifiedstandardsorprocedures
wherepossible.Instrumentswillberecalibratedwhensignificantdriftoracalibrationerroris
found.
Beyondinitialcalibrationofhandheldfieldinstrumentsandperiodiccalibrationchecksinthe
field,QCmeasurestakenforfieldinstrumentmeasurementsshouldincludereportingof
replicates.FieldmeasurementacceptancecriteriaaresummarizedinTable4.2.
Table4.2.Acceptancecriteriaforfieldmeasurements.
Method Parameters Sampletype Matrix Frequency Acceptablelimits
YSI6920Water
QualityMeter
DO,pH,EC,
temperature,
turbidity
Calibration Water
Within24hrs
beforesampling
aswellasamid-
dayandend-of-
the-daychecks
againstthe
standards
Allowabledrift+
10%forDOand
Specific
Conductivity,+
0.2forpH,+5
turbidityunitsor
+5%ofthe
measuredvalue
(whicheveris
greater)for
turbidity
YSI6920Water
QualityMeterSC
Instrument
BlankWater 1per20sitevisits <MDLforSC
4.1.3. FieldQCSamples
FieldQCsamplesthatarefrequentlycollectedforlaterlabanalysisinsamplingprotocolsare
listedbelow.FieldQCsamplesareanalyzedforalltargetanalytesofasamplingevent.Field
blanksandfieldduplicates/replicateswillbecollectedatafrequencyofoneper20samples(5%
ofsamples)orperbatch/event,whicheverismorefrequent:
1. FieldBlanks:Theseaccountforallofthesourcesofcontaminationthatmightbeintroduced
toasampleaswellasthoseduetotheimmediatefieldenvironment,suchasallthe
possiblecontaminationsourcesincontainerandequipmentpreparation,transport,
handling,andsamplingmethodology.Fieldblanksaregeneratedunderactualfield
conditionsandaresubjectedtothesameaspectsofsamplecollection,fieldprocessing,
preservation,transport,andlaboratoryhandlingastheenvironmentalsamples.
2. FieldDuplicates/Replicates:Theseaccountforvariabilityinthefieldcollectionand
laboratoryanalysiscombined.
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Travel/bottleblanksmaybecollectedatthediscretionoftheQAO,whenanestablished
procedureischangedorwhenproblemsareidentified:
1. Travel/bottleBlanks:Theseaccountforcontaminantsintroducedduringthetransport
processbetweenthelaboratoryandfieldsite,inadditiontoanycontaminationfromthe
sourcesolutionandcontainer.
2. EquipmentBlanks:Theseaccountforcontaminationintroducedbythefieldsampling
equipmentinadditiontotheabovesources.
Fieldblankswillroutinelybecollectedandanalyzed,astheywillencompassallthepossible
contaminationsourcesincontainerandequipmentpreparation,transport,handling,and
samplingmethodology.Unlessotherwisespecified,goalsforfieldblanksarethesameasforlab
blanks,i.e.,notdetected.Ifproblemsarefoundwithfieldblanks,otherblanksampletypesmay
becollectedinfollow-upsamplingtotryanddeterminethesourceofcontamination.
Fieldblanksforwaterwillbegeneratedunderactualfieldconditionsataminimumfrequency
ofonepersamplingevent(e.g.asetofsamplescollectedbythesamemethodsoverthe
durationofasamplingcruise)orapproximatelyper20samples.Theywillbetreatedinboththe
fieldandlaboratoryproceduresinassimilaramanneraspossibleastheenvironmentalfield
samples.Wholewaterfieldblankswillbetakenbyexposingsamplingcontainersthrougha
simulatedprocessofcollectingsamples.Filedblankcollectionlocationswillbevariedoverthe
courseofastudy.
InstudiesperformedforotherSFEI-ASCprojects,travel/bottleblanksanalyzedusuallyshowed
thattheyarenotasignificantsourceofcontaminationbeyondthatalreadyincludedin
laboratoryblanks,sotravelblanksareseldomcollected.However,ifcontinuedcontamination
isidentifiedinfieldblanks,travelblanksmaybecollectedandanalyzedtoidentifyapotential
source,atthediscretionoftheDeltaRMPQAO.
Fieldduplicates/replicatesofwatersampleswillberoutinelycollectedataminimumfrequency
ofofoneperbatch/samplingeventorper20samplestoevaluatevariabilityincluding
performanceofthesamplingsystemandmethodology.Unlessotherwisespecified,precision
targetsandacceptancecriteriaforfieldduplicates/replicateswillbethesameasthoseforlab
replicates.
4.2. LaboratoryPerformanceMeasurementsforChemicalAnalyses
LaboratoryperformancemeasurementsareincludedintheQAdatareviewtocheckif
measurementqualityobjectivesaremet.ResultsofanalysesofQCsamplesaretobereported
withresultsoffieldsamples.Minimumfrequenciesandtargetperformancerequirementsfor
QCmeasuresofreportedanalytesarespecifiedinTable4.3.
QCmeasurestypicallyusedforevaluationoflaboratoryandfieldsamplingperformanceinclude
thefollowing:
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1. Method(orextraction/preparation)Blanks:samplesofacleanornull(e.g.,empty
container)matrixtakenthroughtheentireanalyticalprocedure,includingpreservatives,
reagents,andequipmentusedinpreparationandquantitationofanalytesinsamples.
2. Field(orequipment/collection)Blanks:samplesofacleanornullmatrixtakenthrough
thesamplingprocedure,thenanalyzedmuchlikeanordinaryfieldsample.
3. SurrogateStandards:analytesintroducedtosamplespriortosampleextractionto
monitorsampleextractionmethodrecoveries.
4. InternalStandards:analytesintroduceafterthelastsample-processingsteppriorto
analysis,tomeasureandcorrectforlossesanderrorsintroducedduringanalysis,with
recoveriesandcorrectionstoreportedvaluesgenerallyreportedforeachsample
individually.
5. MatrixSpikeSamples/Duplicates:fieldsamplestowhichknownamountsoftarget
analytesareadded,indicatingpotentialanalyticalinterferencespresentinfieldsamples
anderrorsorlossesinanalysesnotaccountedforbysurrogatecorrection.
6. CertifiedReferenceMaterials(CRM):CRMsarecreatedorcollectedsamplescontaining
analytesofinterestthathavebeenanalyzedandreportedbymultiplelabsusinga
varietyofmethodstoarriveataconsensus“certified”or“reference”value.Certified
analyteshaveahigherdegreeofcertaintyinreportedvaluesduetoexternalvalidation.
7. LabReferenceMaterials/LaboratoryControlSamples:materialscollectedorcreatedby
alaboratoryasinternalreferencesamples,totrackperformanceacrossbatches.Unlike
CRMs,LRMsandLCSsseldomhaveexternalvalidation(i.e.,measurementbyanother
methodoranotherlab)andarethuslesscertainasmeasuresofaccuracy,butaregood
forday-to-dayindicationofprocesscontrol.
8. InstrumentReplicates:replicateanalysesofextractedmaterialorstandardsthat
measuretheinstrumentalprecision.
9. LaboratoryReplicates:replicatesub-samplesoffieldsamples,standardreference
materials,labreferencematerials,matrixspikesamples,orlaboratorycontrolsamples,
takenthroughthefullanalyticalprocedureincludingalllabprocessescombined.
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Table4.3.Chemical-analyticalQC.
Method Sampletype Matrix Frequency Acceptablelimits
Conventional–Chlorophylla
EPA446.0 LaboratoryBlank Water 1per20orbatch <RL
EPA446.0 CRM Water 1per20orbatch Expectedvalue+/-20%
EPA446.0 LabDuplicate Water 1perbatch
RPD<25%;n/aif
concentrationofeithersample
<RL
EPA446.0 FieldDuplicates Water 5%ofallsamples
RPD<25%;n/aif
concentrationofeithersample
<RL
Conventional–DOC
METH011.00or
TM-O-1122-92LaboratoryBlank Water 1per20orbatch <RL
METH011.00or
TM-O-1122-92CRM Water 1per20orbatch Expectedvalue+/-20%
METH011.00or
TM-O-1122-92
Matrix
Spikes/DuplicatesWater 1per20orbatch
Expectedvalue+/-20%;
RPD<25%
METH011.00or
TM-O-1122-92LabDuplicate Water 1per20orbatch
RPD<25%;n/aif
concentrationofeithersample
<RL
METH011.00or
TM-O-1122-92FieldDuplicates Water 5%ofallsamples
RPD<25%;n/aif
concentrationofeithersample
<RL
Conventional–POC
EPA440 LaboratoryBlank Water 1per20orbatch <MDL
EPA440 CRM Water 1per20orset Expectedvalue+/-10%
EPA440Matrix
Spikes/DuplicatesWater 1per20orbatch Expectedvalue+/-10%
EPA440 LabDuplicate Water 1per20orbatch RPD<10%
EPA440 InstrumentBlank Water 12hours <MDL
EPA440 FieldDuplicates Water 5%ofallsamples RPD<25%
EPA440 FilterBlank Water
1perlotof
filtersorhigher
frequency
<MDL
Conventional–TSS,VSS
SM2540DorTWRI-5-
A1LaboratoryBlank Water 1per20orbatch <RL
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Method Sampletype Matrix Frequency Acceptablelimits
SM2540DorTWRI-5-
A1FieldDuplicates Water 5%ofallsamples
RPD<25%;n/aif
concentrationofeithersample
<RL
Pesticides
USGSTM-5-C2 Calibration Water
Ateach
instrumentset
up,major
disruption,and
whenroutine
calibrationcheck
exceedsspecific
controllimits.
Linearregression,r2>0.995
usinga7pointcalibration
curverangingfrom0.01to1
ng/uL
USGSTM-5-C2 CalibrationCheck Water Every6samples. Recovery=75-125%
USGSTM-5-C2 LaboratoryBlanks Water1per20or
batch.<MDL
USGSTM-5-C2Matrix
Spikes/DuplicatesWater 1per20 Recovery70-130%,RPD<25%
USGSTM-5-C2 SurrogateSpikes Water Everysample Recovery=70-130%
USGSTM-5-C2Internal
StandardsWater Everysample Recovery=70-130%
USGSTM-5-C2 FieldBlanks Water 1per20 <MDL
USGSTM-5-C2FieldDuplicate/
ReplicateWater 1per20 RPD<25%
USGS–SIR2012-5026 Calibration Water
Ateach
instrumentset
up,major
disruption,and
whenroutine
calibrationcheck
exceedsspecific
controllimits.
Linearregression,r2>0.995
usingan7pointcalibration
curverangingfrom0.01to1
ng/uL
USGS–SIR2012-5026 CalibrationCheck Water Every6samples. Recovery=75-125%
USGS–SIR2012-5026 LaboratoryBlanks Water1per20or
batch.<MDL
USGS–SIR2012-5026Matrix
Spikes/DuplicatesWater 1per20 Recovery70-130%,RPD<25%
USGS–SIR2012-5026 SurrogateSpikes Water Everysample Recovery=70-130%
USGS–SIR2012-5026Internal
StandardsWater Everysample Recovery=70-130%
USGS–SIR2012-5026 FieldBlanks Water 1per20 <MDL
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Method Sampletype Matrix Frequency Acceptablelimits
USGS–SIR2012-5026FieldDuplicate/
ReplicateWater 1per20 RPD<25%
TraceMetals–Copper(dissolved)
USGSTM-5-B1 LaboratoryBlank Water 1per20orbatch <MDL
USGSTM-5-B1 CRM Water 1per20 Expectedvalue+/-25%
USGSTM-5-B1Matrix
Spikes/DuplicatesWater
1per20orone
batchExpectedvalue+/-25%
USGSTM-5-B1 LabDuplicate Water 1per20 RPD<25%
USGSTM-5-B1 InstrumentBlank Water Every6samples <MDL
USGSTM-5-B1 FieldDuplicates Water 5%ofallsamples RPD<25%
TraceMetals–Mercury
EPA7473 LaboratoryBlank Tissue 1per20orbatch <RL
EPA7473 CRM Tissue 1per20orbatch Expectedvalue+/-25%
EPA7473Matrix
Spikes/DuplicatesTissue 1per20orbatch Expectedvalue+/-25%
EPA7473 LabDuplicate Tissue 1per20
RPD<25%;n/aif
concentrationofeithersample
<RL
EPA1631,RevisionE LaboratoryBlank Water1per20or
batch.<RL
EPA1631,RevisionE CRM Water 1per20orbatch Expectedvalue+/-25%
EPA1631,RevisionEMatrix
Spikes/DuplicatesWater 1per20orbatch Expectedvalue+/-25%
EPA1631,RevisionE LabDuplicate Water 1per20
RPD<25%;n/aif
concentrationofeithersample
<RL
EPA1631,RevisionE FieldDuplicates Water 5%ofallsamples
RPD<25%:n/aif
concentrationofeithersample
<RL
EPA1631,RevisionE FieldBlank Water 1per20orbatch <RL
TraceMetals–Mercury,Methyl
EPA1630 LaboratoryBlank Water 1per20orbatch <RL
EPA1630 LCS Water 1per20orbatch Expectedvalue+/-30%
EPA1630Matrix
Spikes/DuplicatesWater 1per20orbatch Expectedvalue+/-30%
EPA1630 LabDuplicate Water 1per20 RPD<25%;n/aif
concentrationofeithersample
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Method Sampletype Matrix Frequency Acceptablelimits
<RL
EPA1630 FieldDuplicates Water 5%ofallsamples
RPD<25%:n/aif
concentrationofeithersample
<RL
EPA1630 FieldBlank Water 1per20orbatch <RL
4.3. LaboratoryQualityControlProceduresforChemicalAnalyses
Priortotheinitialanalysesofsamplesfortheproject,eachlaboratorywilldemonstrate
capabilityandproficiencyformeetingMQOsfortheDeltaRMP.Performance-basedmeasures
forchemicalanalysesconsistoftwobasicelements:initialdemonstrationoflaboratory
capabilityandon-goingdemonstrationofcapabilityduringanalysisofprojectsamples.Initial
demonstrationincludesdocumentationthatsampleanalysescanbeperformedwithinthedata
qualityobjectivesandmethodqualityobjectiveslistedintheQAPP(Tables4.3,4.4,and4.5).
On-goingdemonstrationofcapabilityduringanalysisofprojectsamplesincludeslaboratory
participationinroutineanalyses(e.g.inter-comparisonstudies)toevaluatelaboratory
capabilitiesonacontinualbasistomeetMQOslistedintheQAPP.
4.3.1. LaboratoryQCMeasurements
4.3.1.1 Sensitivity
Inthiscontext,sensitivityreferstothecapabilityofamethodorinstrumenttodetectagiven
analyteatagivenconcentrationandreliablyquantitatetheanalyteatthatconcentration.
Achievingthedesiredsensitivityrequirestheselectionofappropriateanalyticalmethods.The
keymeasurementqualityobjectives(MQOs)forachievingsensitivityarethedesiredReporting
Limit(RL)andMethodDetectionLimit(MDL)foranalytes(Table4.4)andtherangesand
resolutionoflaboratorymeters(Table4.5).AdditionalQCinformationrequiredtoevaluatethe
sensitivityofdataincludelaboratoryormethodblanksand,ifappropriate,instrumentblanks
(Table4.3).
4.3.1.2 Precision
Precisionisthereproducibilityofananalyticalmethodandcanbeevaluatedforanysample
thatisanalyzedinreplicate.Ingeneral,laboratoryreplicatesoffieldsamplesarepreferredas
measuresofprecision,butincaseswhereaveragevaluesforfieldsamplesareexpected(based
onhistoricalorliteratureresults)tofallinanon-quantitativerange,othersamplessuchas
CRMs,LRMs,matrixspikes,orblankspikescanbeanalyzedinreplicatetodetermineprecision.
Ifsamplesotherthanfieldsamplesareusedtoevaluateprecision,targetconcentrationsshould
beatleasthighenoughtobequantitativebutlessthan100timesthoseinfieldsamples,as
precisioninhighconcentrationsamplesisnotlikelyrepresentativeformuchlowerambient
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samples.WhenusingMS/MSD,samplesofasimilarmatrixaremostrelevantandthus
preferredforevaluatingprecision.
Aminimumofonefieldsample(oralternativesampletype,e.g.MS,wheresamplematerialis
insufficientorconcentrationsarelargelynotdetectedinfieldsamples)perbatchofsamples
submittedtothelaboratory(minimumoneper20,or5%,inlargebatches)willbeprocessed
andanalyzedinreplicateforprecision.Previouslyanalyzedmaterial(e.g.fromthesameproject
inprioryears,orfromotherprojects)mayalsobeanalyzedasreplicatestohelpensureresults
inaquantitativerange.Therelativepercentdifference(RPD)amongreplicatesampleswillbe
lessthantheMQOlistedinTable4.3foreachanalyteofinterest.RPDiscalculatedas:
PrecisionmaybeexpressedrelativetoanMQOasap-score:
p=|RPDorRSD|/MQO%
IfresultsforanyanalytedonotmeettheMQOforprecision(p-score>1),calculationsand
instrumentswillbechecked.Repeatanalysesmayberequiredtoconfirmtheresultsand
reduceuncertaintyinthemeasurement.Resultsthatrepeatedlyfailtomeetthecriteria
indicatesampleheterogeneity,unusuallyhighcontaminationofanalytes,orothercausesof
poorlaboratoryprecision.Ifthevariabilityisnotreduced,thelaboratoryisobligatedtohaltthe
analysisofsamples,identifythesourceoftheimprecision,andnotifytheSFEI-ASCProject
ManagerandQAObeforeproceedingwithfurtheranalysis.Insomecaseswhenthecausesof
imprecisioncannotbecorrected(particularlyforlessabundantorlessimportantanalytesina
largegroupreportedbyasingleanalyticalmethod),andwiththeapprovaloftheProject
ManagerandQAO,theresultscanbereportedas-isandflaggedforpoorprecision(p-score>1)
orcensoredifextremelypoor(p-score>2).
4.3.1.3 Accuracy
Theaccuracyoflabmeasurementswillbeevaluatedbasedondataqualitycriteria(Table4.3)
forMS/MSD,CRM,internalstandards,surrogaterecoveries,initialcalibration,andcalibration
checks.
ThepercentrecoveryforMS/MSDiscalculatedusingtheequation
Ifinsufficientsampleisavailable,theanalystcanrunaLCS(LaboratoryControlSample)anda
LCSduplicate.Thecalculationusedisthesame.
%100samples) (replicate Average
samples) replicate(between Difference RPD ×=
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4.3.1.4 Completeness
Completenessisdefinedas“ameasureoftheamountofdatacollectedfromameasurement
processcomparedtotheamountthatwasexpectedtobeobtainedundertheconditionsof
measurement”(StanleyandVerner1985).ThegoaloftheDeltaRMPistoachieve>90%
completenessforallanalyses.
Completenesswillbequantifiedasthetotalnumberofusableresultsdividedbythetotal
numberofsitevisits,aggregatedbyallanalytesofinterest.However,additionalfactorsmaybe
consideredonacase-by-casebasis.Forexample,ananalysismayresultin0%usabledatafora
minorgroupofanalytesandpotentiallynotmeetthecompletenessgoalof90%overallasa
result,butmaystillprovidevaluabledataandmeetthecompletenesscriteriaforallthe
remaininganalyteresultscombined.Incontrast,if>90%completenesscouldnotbeobtained
foragroupofpesticideanalytesthatarethemostabundantinthemajorityofstudiesinthe
literature,itwouldlikelyneedtobeseenasafailurethatneededimmediatecorrection.
4.3.1.5 Contamination
Laboratorymethodblanks(alsocalledextractionblanks,proceduralblanks,orpreparation
blanks)areusedtoassesslaboratorycontaminationduringallstagesofsamplepreparationand
analysis.Forlaboratoryanalyses,atleastonelaboratorymethodblankwillberuninevery
samplebatch.Themethodblankwillbeprocessedthroughtheentireanalyticalprocedureina
manneridenticaltothesamples(i.e.,usingthesamereagentsandequipment).Methodblanks
shouldcontainanalyteconcentrationlessthantheMDL.Amethodblankconcentration>RLfor
anyanalytesofinterestwillrequirecorrectiveaction(e.g.,checkingofreagents,re-cleaning
andre-checkingofequipment)toidentifyandeliminatethesource(s)ofcontaminationbefore
proceedingwithsampleanalysis.Ifeliminatingtheblankcontaminationandreanalysisisnot
possible,resultsforallimpactedanalytesintheanalyticalbatchshallbeflagged.Inaddition,a
detaileddescriptionofthecontaminationsourcesandthestepstakentoidentifyand
eliminate/minimizethemshallbeincludedinthetransmittalletter.Subtractingmethodblank
resultsfromsampleresultsisnotpermitted.
4.3.1.6 Comparability
TheDeltaRMPadherestoEPAguidance,specifiedSOPs,andSWAMP-comparableQA
measures.Therefore,resultscanbecomparedwithotherprojectsandlaboratoriesthatadhere
tothesameorcompatibleprotocolsandQAmeasures.
4.3.1.7 Dataanalysis
Datawillbeanalyzedusingappropriategraphicaltools,spatialanalyses,andstatisticaltestsas
describedintheDeltaRMPCommunicationsPlan.
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Table4.4.SummaryofReportingLimits(RL)andMethodDetectionLimits(MDL)ofDeltaRMP
constituents.
Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Oxygen,Dissolved Water FieldParameters 0.5 0.5 mg/L
MPSL(mercury
monitoring),
USGS(pesticide
monitoring)
NationalField
Manualfor
the
Collectionfor
Water-
QualityData,
ChapterA6,
Field
Measure-
ments
pH Water FieldParameters NA NA NA
MPSL(mercury
monitoring),
USGS(pesticide
monitoring)
SpecificConductivity Water FieldParameters 10 10 uS/cm
MPSL(mercury
monitoring),
USGS(pesticide
monitoring)
Temperature Water FieldParameters NA NA NA
MPSL(mercury
monitoring),
USGS(pesticide
monitoring)
Turbidity Water FieldParameters 1 1 FNU USGS
AlkalinityasCaCO3 Water Conventional 12 4 mg/L AHPL SM2320B
AmmoniaasN Water Conventional 0.15 0.05 mg/L AHPLSM4500-
NH3F
Chlorophylla Water Conventional 30 24 µg/L WPCL EPA446.0
HardnessasCaCO3 Water Conventional 6 2 mg/L AHPL SM2340C
DissolvedOrganic
CarbonWater Conventional 0.23 0.23 mg/L
WPCL(mercury
monitoring),
USGS(pesticide
monitoring)
TMO-1122-
92,
METH011.00
ParticulateOrganic
CarbonWater Conventional 0.05 0.05 mg/L USGS EPA440
Copper,dissolved Water TraceMetals 0.8 0.8 ug/L USGS TM-5-B1
Mercury,total Tissue TraceMetals 0.012 0.004µg/gww
MPSL EPA7473
Mercury,total
(unfiltered)Water TraceMetals 0.200 0.200 ng/L MPSL EPA1631E
Mercury,dissolved
(filtered)Water TraceMetals 0.200 0.200 ng/L MPSL EPA1631E
Mercury,Methyl,
total(unfiltered)Water TraceMetals 0.031 0.02 ng/L MPSL EPA1630
Mercury,Methyl,
dissolved(filtered)Water TraceMetals 0.031 0.02 ng/L MPSL EPA1630
ChlorpyrifosOxon Water Degradates 5.0 5.0 ng/L USGS TM-5-C2
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Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Dichlorophenyl-3-
methylUrea,3,4-Water Herbicides 3.5 3.5 ng/L USGS
USGS–SIR
2012-5026
DDD(p,p') Water Degradates 6.1 6.1 ng/L USGS TM-5-C2
DDE(p,p') Water Degradates 6.9 6.9 ng/L USGS TM-5-C2
Diazoxon Water Degradates 5.0 5.0 ng/L USGS TM-5-C2
Dichloroaniline,3,4- Water Degradates 3.2 3.2 ng/L USGSUSGS–SIR
2012-5026
Dichloroaniline,3,5- Water Degradates 7.6 7.6 ng/L USGS TM-5-C2
Dichlorophenylurea,
3.,4-Water Degradates 3.4 3.4 ng/L USGS
USGS–SIR
2012-5026
FipronilDesulfinyl Water Degradates 1.6 1.6 ng/L USGS TM-5-C2
FipronilDesulfinyl
AmideWater Degradates 3.2 3.2 ng/L USGS TM-5-C2
FipronilSulfide Water Degradates 1.8 1.8 ng/L USGS TM-5-C2
FipronilSulfone Water Degradates 3.5 3.5 ng/L USGS TM-5-C2
Malaoxon Water Degradates 5.0 5.0 ng/L USGS TM-5-C2
TebupirimphosOxon Water Degradates 2.8 2.8 ng/L USGS TM-5-C2
Acibenzolar-S-methyl Water Fungicides 3.0 3.0 ng/L USGS
Azoxystrobin Water Fungicides 3.1 3.1 ng/L USGS TM-5-C2
Boscalid Water Fungicides 2.8 2.8 ng/L USGS TM-5-C2
Captan Water Fungicides 10.2 10.2 ng/L USGS
Carbendazim Water Fungicides 4.2 4.2 ng/L USGSUSGS–SIR
2012-5026
Chlorothalonil Water Fungicides 4.1 4.1 ng/L USGS TM-5-C2
Cyazofamid Water Fungicides 4.1 4.1 ng/L USGSUSGS–SIR
2012-5026
Cymoxanil Water Fungicides 3.9 3.9 ng/L USGSUSGS–SIR
2012-5026
Cyproconazole Water Fungicides 4.7 4.7 ng/L USGS TM-5-C2
Cyprodinil Water Fungicides 7.4 7.4 ng/L USGS TM-5-C2
Desthio-
ProthioconazoleWater Fungicides 3.0 3.0 ng/L USGS
USGS–SIR
2012-5026
Difenoconazole Water Fungicides 10.5 10.5 ng/L USGS TM-5-C2
Dimethomorph Water Fungicides 6.0 6.0 ng/L USGS TM-5-C2
Ethaboxam Water Fungicides 3.8 3.8 ng/L USGSUSGS–SIR
2012-5026
Famoxadone Water Fungicides 2.5 2.5 ng/L USGS TM-5-C2
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Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Fenamidone Water Fungicides 5.1 5.1 ng/L USGS TM-5-C2
Fenarimol Water Fungicides 6.5 6.5 ng/L USGS TM-5-C2
Fenbuconazole Water Fungicides 5.2 5.2 ng/L USGS TM-5-C2
Fenhexamid Water Fungicides 7.6 7.6 ng/L USGS TM-5-C2
Fluazinam Water Fungicides 4.4 4.4 ng/L USGS TM-5-C2
Fludioxonil Water Fungicides 7.3 7.3 ng/L USGS TM-5-C2
Fluopicolide Water Fungicides 3.9 3.9 ng/L USGS TM-5-C2
Fluoxastrobin Water Fungicides 9.5 9.5 ng/L USGS TM-5-C2
Flusilazole Water Fungicides 4.5 4.5 ng/L USGS TM-5-C2
Flutolanil Water Fungicides 4.4 4.4 ng/L USGS TM-5-C2
Flutriafol Water Fungicides 4.2 4.2 ng/L USGS TM-5-C2
Fluxapyroxad Water Fungicides 4.8 4.8 ng/L USGS TM-5-C2
Imazalil Water Fungicides 10.5 10.5 ng/L USGS TM-5-C2
Ipconazole Water Fungicides -- -- ng/L USGS TM-5-C2
Iprodione Water Fungicides 4.4 4.4 ng/L USGS TM-5-C2
Kresoxim-methyl Water Fungicides 4.0 4.0 ng/L USGS TM-5-C2
Mandipropamid Water Fungicides 3.3 3.3 ng/L USGSUSGS–SIR
2012-5026
Metalaxyl Water Fungicides 5.1 5.1 ng/L USGS TM-5-C2
Metconazole Water Fungicides 5.2 5.2 ng/L USGS TM-5-C2
Myclobutanil Water Fungicides 6.0 6.0 ng/L USGS TM-5-C2
Paclobutrazol Water Fungicides 6.2 6.2 ng/L USGS TM-5-C2
PCNB Water Organochlorines 3.1 3.1 ng/L USGS TM-5-C2
Picoxystrobin Water Fungicides 4.2 4.2 ng/L USGS TM-5-C2
Propiconazole Water Fungicides 5.0 5.0 ng/L USGS TM-5-C2
Pyraclostrobin Water Fungicides 2.9 2.9 ng/L USGS TM-5-C2
Pyrimethanil Water Fungicides 4.1 4.1 ng/L USGS TM-5-C2
Quinoxyfen Water Fungicides 3.3 3.3 ng/L USGS TM-5-C2
Sedaxane Water Fungicides -- -- ng/L USGS TM-5-C2
Tebuconazole Water Fungicides 3.7 3.7 ng/L USGS TM-5-C2
Tetraconazole Water Fungicides 5.6 5.6 ng/L USGS TM-5-C2
Thiabendazole Water Fungicides 3.6 3.6 ng/L USGSUSGS–SIR
2012-5026
Triadimefon Water Fungicides 8.9 8.9 ng/L USGS TM-5-C2
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Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Triadimenol Water Fungicides 8.0 8.0 ng/L USGS TM-5-C2
Trifloxystrobin Water Fungicides 4.7 4.7 ng/L USGS TM-5-C2
Triflumizole Water Fungicides 6.1 6.1 ng/L USGS TM-5-C2
Triticonazole Water Fungicides 6.9 6.9 ng/L USGS TM-5-C2
Zoxamide Water Fungicides 3.5 3.5 ng/L USGS TM-5-C2
Alachlor Water Herbicides 1.7 1.7 ng/L USGS TM-5-C2
Atrazine Water Herbicides 2.3 2.3 ng/L USGS TM-5-C2
Benefin Water Herbicides 2.0 2.0 ng/L USGS TM-5-C2
Butralin Water Herbicides 2.6 2.6 ng/L USGS TM-5-C2
Butylate Water Herbicides 1.8 1.8 ng/L USGS TM-5-C2
Clomazone Water Herbicides 2.5 2.5 ng/L USGS TM-5-C2
Cycloate Water Herbicides 1.1 1.1 ng/L USGS TM-5-C2
Cyhalofop-butyl Water Herbicides 1.9 1.9 ng/L USGS TM-5-C2
Dacthal Water Herbicides 2.0 2.0 ng/L USGS TM-5-C2
Diuron Water Herbicides 3.2 3.2 ng/L USGSUSGS–SIR
2012-5026
Dithiopyr Water Herbicides 1.6 1.6 ng/L USGS TM-5-C2
EPTC Water Herbicides 1.5 1.5 ng/L USGS TM-5-C2
Ethalfluralin Water Herbicides 3.0 3.0 ng/L USGS TM-5-C2
Flufenacet Water Herbicides 4.7 4.7 ng/L USGS TM-5-C2
Fluridone Water Herbicides 3.7 3.7 ng/L USGSUSGS–SIR
2012-5026
Hexazinone Water Herbicides 8.4 8.4 ng/L USGS TM-5-C2
Metolachlor Water Herbicides 1.5 1.5 ng/L USGS TM-5-C2
Molinate Water Herbicides 3.2 3.2 ng/L USGS TM-5-C2
Napropamide Water Herbicides 8.2 8.2 ng/L USGS TM-5-C2
Novaluron Water Herbicides 2.9 2.9 ng/L USGS TM-5-C2
Oryzalin Water Herbicides 5.0 5.0 ng/L USGSUSGS–SIR
2012-5026
Oxadiazon Water Herbicides 2.1 2.1 ng/L USGS TM-5-C2
Oxyfluorfen Water Herbicides 3.1 3.1 ng/L USGS TM-5-C2
Pebulate Water Herbicides 2.3 2.3 ng/L USGS TM-5-C2
Pendimethalin Water Herbicides 2.3 2.3 ng/L USGS TM-5-C2
Penoxsulam Water Herbicides 3.5 3.5 ng/L USGSUSGS–SIR
2012-5026
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Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Prodiamine Water Herbicides 5.2 5.2 ng/L USGS TM-5-C2
Prometon Water Herbicides 2.5 2.5 ng/L USGS TM-5-C2
Prometryn Water Herbicides 1.8 1.8 ng/L USGS TM-5-C2
Propanil Water Herbicides 10.1 10.1 ng/L USGS TM-5-C2
Pronamide Water Herbicides 5.0 5.0 ng/L USGS TM-5-C2
Simazine Water Herbicides 5.0 5.0 ng/L USGS TM-5-C2
Thiazopyr Water Herbicides 4.1 4.1 ng/L USGS TM-5-C2
Thiobencarb Water Herbicides 1.9 1.9 ng/L USGS TM-5-C2
Triallate Water Herbicides 2.4 2.4 ng/L USGS TM-5-C2
Tributyl
Phosphorotrithioate,
S,S,S-
Water Herbicides 3.1 3.1 ng/L USGS TM-5-C2
Trifluralin Water Herbicides 2.1 2.1 ng/L USGS TM-5-C2
Acetamiprid Water Insecticides 3.3 3.3 ng/L USGSUSGS–SIR
2012-5026
Allethrin Water Insecticides 4.1 4.1 ng/L USGS TM-5-C2
Bifenthrin Water Insecticides 4.7 4.7 ng/L USGS TM-5-C2
Carbaryl Water Insecticides 6.5 6.5 ng/L USGS TM-5-C2
Carbofuran Water Insecticides 3.1 3.1 ng/L USGS TM-5-C2
Chlorantraniliprole Water Insecticides 4.0 4.0 ng/L USGSUSGS–SIR
2012-5026
Chlorpyrifos Water Insecticides 2.1 2.1 ng/L USGS TM-5-C2
Clothianidin Water Insecticides 3.9 3.9 ng/L USGSUSGS–SIR
2012-5026
Coumaphos Water Insecticides 3.1 3.1 ng/L USGS TM-5-C2
Cyantraniliprole Water Insecticides 4.2 4.2 ng/L USGSUSGS–SIR
2012-5026
Cyfluthrin,total Water Insecticides 5.2 5.2 ng/L USGS TM-5-C2
Cyhalothrin,total Water Insecticides 4.5 4.5 ng/L USGS TM-5-C2
Cypermethrin,total Water Insecticides 5.6 5.6 ng/L USGS TM-5-C2
DDT(p,p') Water Insecticides 3.5 3.5 ng/L USGS TM-5-C2
Deltamethrin Water Insecticides 3.5 3.5 ng/L USGS TM-5-C2
Diazinon Water Insecticides 0.9 0.9 ng/L USGS TM-5-C2
Dinotefuran Water Insecticides 4.5 4.5 ng/L USGSUSGS–SIR
2012-5026
Esfenvalerate Water Insecticides 3.9 3.9 ng/L USGS TM-5-C2
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Constituent Matrix Reportinggroup RL MDL Unit
Analyzing
laboratory/
laboratories
Methodused
Ethofenprox Water Insecticides 2.2 2.2 ng/L USGS TM-5-C2
Fenpropathrin Water Insecticides 4.1 4.1 ng/L USGS TM-5-C2
Fenpyroximate Water Insecticides 5.2 5.2 ng/L USGS TM-5-C2
Fenthion Water Insecticides 5.5 5.5 ng/L USGS TM-5-C2
Fipronil Water Insecticides 2.9 2.9 ng/L USGS TM-5-C2
Flonicamid Water Insecticides 3.4 3.4 ng/L USGSUSGS–SIR
2012-5026
Imidacloprid Water Insecticides 3.8 3.8 ng/L USGSUSGS–SIR
2012-5026
Indoxacarb Water Insecticides 4.9 4.9 ng/L USGS TM-5-C2
Malathion Water Insecticides 3.7 3.7 ng/L USGS TM-5-C2
Methoprene Water Insecticides 6.4 6.4 ng/L USGS TM-5-C2
Methoxyfenozide Water Insecticides 2.7 2.7 ng/L USGSUSGS–SIR
2012-5026
Methidathion Water Insecticides 7.2 7.2 ng/L USGS TM-5-C2
Parathion,Methyl Water Insecticides 3.4 3.4 ng/L USGS TM-5-C2
Pentachloroanisole Water Insecticides 6.5 6.5 ng/L USGS TM-5-C2
Permethrin,total Water Insecticides 3.4 3.4 ng/L USGS TM-5-C2
Phenothrin Water Insecticides 5.1 5.1 ng/L USGS TM-5-C2
Phosmet Water Insecticides 4.4 4.4 ng/L USGS TM-5-C2
Propargite Water Insecticides 6.1 6.1 ng/L USGS TM-5-C2
Pyridaben Water Insecticides 5.4 5.4 ng/L USGS TM-5-C2
Resmethrin Water Insecticides 5.7 5.7 ng/L USGS TM-5-C2
Tebupirimfos Water Insecticides 1.9 1.9 ng/L USGS TM-5-C2
Tefluthrin Water Insecticides 4.2 4.2 ng/L USGS TM-5-C2
Tetradifon Water Insecticides 3.8 3.8 ng/L USGS TM-5-C2
Tetramethrin Water Insecticides 2.9 2.9 ng/L USGS TM-5-C2
Thiacloprid Water Insecticides 3.2 3.2 ng/L USGSUSGS–SIR
2012-5026
Thiamethoxam Water Insecticides 3.4 3.4 ng/L USGSUSGS–SIR
2012-5026
Tolfenpyrad Water Insecticides 2.9 2.9 ng/L USGSUSGS–SIR
2012-5026
Piperonylbutoxide Water Synergists 2.3 2.3 ng/L USGS TM-5-C2
Flumetralin WaterPlantGrowth
Regulator5.8 5.8 ng/L USGS TM-5-C2
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--=MDL/RLnotyetdetermined.
Table4.5.Summaryofinstrumentrangesandresolutionforlaboratorymeters.
Constituent MatrixReporting
group
Instrument
RangeResolution Unit
Analyzing
laboratory
Instrument
used
Oxygen,
DissolvedWater Conventional 0to20 0.1 mg/L AHPL YSI58
pH Water Conventional 1to16 0.01 NA AHPL Beckman255
Specific
ConductivityWater Conventional
0to499.9
0to4999
0.1
1uS/cm AHPL YSI30
Temperature Water Conventional -200to100 0.1 °C AHPLOnset
HOBOware
4.3.2. LaboratoryQCSamples
DatafromthelaboratoryshouldincludeattheleastthefollowingQCdata:
1. SurrogateRecovery(forallfieldandQCsamples,ifapplicable)
2. MethodBlank
3. MatrixSpikeRecovery(ifapplicable)
4. Replicateprecision(field,CRM,matrixspike,blankmatrixspikesamples)
5. Certified/LabReferenceMaterial(CRM/LRM)Recovery(ifapplicable)
Surrogatespikesshouldbeincludedinallsampleswhereappropriatefortheanalysis.Although
surrogatespikerecoveriescanbeusedtoestimateandcorrectforlossesofthetargetanalytes
intheanalyticalprocess,unusuallyloworhighrecoveriesreflectanalyticalissuesthatarenot
overcomesimplybysurrogatecorrection,becauseatlowrecoveries,surrogatecorrection
factorsbecomeinverselylarger.Itisgenerallylefttotheprofessionaljudgmentofthelab’s
QAOtosetappropriatecontrol/acceptancelimitsandcorrectiveactionsforsurrogate
recoveries.
Methodblanksshouldberunataminimumfrequencyofoneperanalyticalbatch(foranalytical
batchesconsistingofupto20fieldsamples)orper20(field)samplesforlargeranalytical
batches.Resultsforlaboratorymethodblanks,combinedwiththoseforfieldblanks,canhelp
identifywhetherprobablecausesofsamplecontaminationoriginatedinthefieldorin
laboratoryanalyses.Ifbothfieldandlabmethodblankshavesimilarlevelsofcontamination,it
islikelycausedprimarilyinlabprocedures.Iffieldblankshavehighercontamination,sample
collectionmethodsarelikelythecause.Rawresultsformethodblanksshouldbereported.
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Matrixspikes(MS)shouldberunataminimumfrequencyofoneperbatchorper20samples.
Matrixspikeresultsaretobereported,alongwiththeexpectedresult(unspikedsample
concentration+spikeconcentration),andarecoveryestimate.Thespikingconcentrations
shouldbehighenoughtoproduceanexpectedresultsufficientlyovertheanalyticalvariability
inquantifyingtheunspikedsampletoquantifyrecovery(atleast~3timestheunspikedresult),
butalsolowenoughtobearelevantaccuracyindicatorintheconcentrationrangeoffield
samples(below100xandpreferablynearer10xtheunspikedresult).Incaseswhereanalytes
aremostlynotdetectedinunspikedsamples,aconcentrationrangeofthatmagnitude(10-
100x)overtheMDLmaybeappropriatetouseinstead.
Precisioncanbedeterminedwithallsampletypesanalyzedandreportedinreplicate.Lab
replicates(splitandanalyzedinthelaboratory)offieldsamplesaregenerallythepreferred
indicatorofprecisionfortypicalfieldsamples,asthetargetanalyteconcentrationrange,
matrix,andinterferencesaremostsimilartopreviousanalyzedsamplesorsamplesfrom
nearbysites.However,sometimesfieldsampleconcentrationsarebelowdetectionlimitsfor
manyanalytes,soreplicateresultsonCRMs,LRMs,MS/MSDs,orblankspikes(LCSs)maybe
neededtosupplementandobtainquantitativeprecisionestimates.Thesealternativesample
types,inparticularblankspikes(LCSs),shouldnotserveastheprimaryorexclusiveindicatorof
measurementprecisionwithoutpriorapprovalbytheProjectManagerandQAO.LCSsareoften
createdfromacleanlaboratorymatrix,sotheyarelikelynotrepresentativeofthe
measurementprecisionroutinelyachievableinmorecomplexmatricesofrealfield-originated
samples.RPDsshouldbecalculatedasdescribedpreviouslyandreportedforallsamples
analyzedinreplicate.
Certifiedreferencematerial(CRM)orotherexternallyestablishedperformancetestingsamples
shouldberunataminimumfrequencyofoneperanalyticalbatch(foranalyticalbatches
consistingofupto20fieldsamples)orper20(field)samplesforlargeranalyticalbatches.
Resultsshouldbereportedalongwiththeexpectedvaluesandrecoveries(as%oftheexpected
value),whereavailablefortargetanalytesinappropriatematrices.Insomecases,nowidely
availablereferencematerialshavebeenestablishedandlaboratoriesmaintaininternallab
referencematerials(LRM)totracktherelativeinternalaccuracyofananalyticalmethod.CRMs
arelikelythemostrobustindicatorsofmeasurementaccuracy,givenrequirementsfor
consensusamonglabsaswellasvalidationthroughdifferentmethodsofmeasurement.
ReferencevaluesforCRMsorinternalLRMs,althoughlessrigorous(fewerlabsinconsensus,or
onlyoneanalyticalmethodprovided),provideatleastsomeindicatorofmeasurement
accuracy.Althoughpoorrecoveriesontheseuncertifiedvaluesmaybeusedtoflagpotentially
unreliabledataforuseindataanalysesanddecision-making,theyshouldnotbeusedtociteor
sanctionalabfor“failing”tomeetMQOrequirements.
Table4.6listsrecoverysurrogatestandardsusedforpesticideanalysesandassociated
measurementqualityobjectives.
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Table4.6. Recoverysurrogatestandardsusedforpesticideanalysesandassociatedmeasurementqualityobjectives.
Recoverysurrogate
standardMatrix Method
Acceptablelimits
(%recovery)13C3-atrazine Water TM-5-C2 70-130%
Di-N-propyl-d14trifluralin Water TM-5-C2 70-130%
Monuron Water USGS–SIR2012-5026 70-130%
Imidacloprid-d4 Water USGS–SIR2012-5026 70-130%
4.4. DataQualityIndicatorsandTestAcceptabilityCriteriaforToxicityTestingandAssociatedWaterQualityMeasurements
InthecontextoftheRMP,toxicitymonitoringshouldbeviewedprimarilyasasetoftoolsto
helpidentifypesticidesthatarecausingsignificantaquatictoxicityintheDelta.Becausetoxicity
testingisanintegrativetool,itcandetermineeffectsofmultipleconstituentsconcurrently,and
canbemorecost-effectivethanchemicalanalysisofindividualconstituents.
ToxicityIdentificationEvaluations(TIEs)areplannedforDeltaRMPsampleswherethereis>50
percenteffectwithin96hoursofthetestperiod.TIEsshouldbeinitiatedwithin48hoursofthe
observationoftheTIEtriggerbeingmetintheinitialsamplescreening(seealsoSection8.3).
TheprimarygoalofDeltaRMPTIEtestingistoidentifywhetherpesticidesarecausingor
contributingtoobservedtoxicity,andifso,whichpesticides(ordegradates,oranyoftheinert
ingredientsintheformulatedproduct)arethedrivers.Asecondarygoalistoidentifyother
factors(i.e.,waterqualityconditionsorothertoxicants)contributingtoreducedsurvival,
growth,orreproduction.
Dataqualityindicatorsfortoxicitytestingandassociatedwaterqualitymeasurementsare
outlinedinTable4.7,andtestacceptabilitycriteriaaresummarizedinTable4.8.Testresults
willberejectedwhenmeasurementqualityobjectivesandtestacceptabilitycriteriaarenot
met.However,thesamplemayberetestedandqualifiedwithanextendedholdingtimeifSFEI-
ASCandtheDeltaRMPSCpermit.Toxicitydatawillbequalifiedininstanceswheredatadoes
notmeetaccuracyandprecisioncriteriabelow.
Thewaterqualitymeasurementsspecificallycoupledtotoxicitytestsareintendedtohelp
interprettoxicitytestdata.QualitycontrolpracticesandMQOsparallelthoseusedforfield
meterinstrumentation.Metersarecalibratedatthebeginningofeachdayandcalibration
checksareperformedwhenmeasurementsforthedayexceed20readingsforeachmeter.
MetersarerecalibratedwhendriftexceedstheMQOforaccuracyinTable4.7below.Field
duplicatesareexpectedtofallwithintheprecisionMQOsbelowanddataarequalifiedin
instanceswhentheseareexceeded.
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Table4.7.Measurementqualityobjectivesfortoxicitytestingandassociatedwaterquality
measurements.
ToxicityTestingLaboratoryAnalysis
Parameter Accuracy Precision Completeness
pH ±0.2 ±0.5pHunits 90%
Specific
Conductance ±0.5% ±10% 90%
Temperature ±0.1 ±10% 90%
DissolvedOxygen ±0.2 ±10% 90%
Ammonia ±0.5% ±10% 90%
Hardness
Standard
ReferenceMaterial
(SRM)within80to
120%recovery
RPD<20% 90%
Alkalinity SRMwithin80to
120%recovery RPD<20% 90%
ToxicityTesting N/A
Referencetoxicant
performance,based
oncumulativecontrol
charts:LC50and/or
EC25within2standard
deviationsofthe
runningmeanfromat
least20datapoints
90%
Table4.8.Summaryoftestacceptabilitycriteria.
Species Duration Endpoint(s) Method Testacceptabilitycriteria
S.capricornutum 4-days Growth UCDAHPLSOP1-1 Meancelldensityofat
least2X105cells/mLinthe
controls;andvariability
(CV%)amongcontrol
replicates≤20%
C.dubia
6-8days Survival,
Reproduction
UCDAHPLSOP1-2 >80%survivalofallcontrol
organismsandanaverage
of15ormoreyoungper
survivingfemaleinthe
controlsolutions.60%of
survivingcontrolfemales
mustproducethreebroods
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Species Duration Endpoint(s) Method Testacceptabilitycriteria
(required)
H.azteca10
4days Survival UCDAHPLSOP1-6 >90%survival
P.promelas 7-days Survival,
Biomass
UCDAHPLSOP1-3 >80%survivalincontrols;
averagedryweightper
survivingorganismin
controlchambersequalsor
exceeds0.25mg/surviving
fish
4.4.1. QualityAssuranceActivities
Alltoxicitytestprotocolsarebasedonmethodsoutlinedin“SummaryofTestConditionsand
TestAcceptabilityCriteria”tablesinEPA(2002aandb).Deviationsfromprotocolsmustbe
reportedtotheQAO,theprojectmanager,andininterimandfinalreports,dependingonthe
degreeofdepartureandtheobjectiveofthetest.Deviationsmayormaynotinvalidateatest
result.Beforerejectingoracceptingatestresultasvalid,thedegreeofthedeviationandthe
potentialorobservedimpactofthedeviationonthetestresultwillbeevaluated.
Predetermineddeviationsinprotocolssuchasalternatetestproceduresoruseofsurrogate
speciesmustbediscussedandapprovedpriortotestinitiation.Dataqualityindicatorsforthis
projectwillconsistofthefollowing:
Variabilityandbias
TheDeltaRMPhasseveralmechanismstoensurethatvariabilityandbiasareminimized
throughouttheproject.Techniciansaretrainedaccordingtostandardlaboratoryprotocolsto
ensurethatsamplesarecollectedandanalyzedinaconsistentmanner.Referencetoxicant
testswillbeconductedthroughouttheprojecttoensurethatorganismsensitivityremains
constantovertime.Therelativepercentdifferencebetweenfieldduplicatewaterquality
measurementswillbemeasuredtoensuretechniciansareanalyzingsamplesinaconsistent
manner.AmbientsamplesaretrackedandlabelledwithsitecodesandSampleIDnumbers
ratherthanassociatedwithwaterbodynamestoreducetechnicianbiasofsamples,and
laboratorytestreplicatesareinitiatedwithtestorganismsrandomlytoreducebiasoforganism
health.
10InclusionofHyalellawatertoxicitytestingispendingafinaldecisionbytheSC.
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Testsensitivity
TheDeltaRMPutilizestherequiredminimumnumberofreplicatesspecifiedbyEPAtoensure
adequatetestsensitivity.Testsensitivityisalsoevaluatedthroughreferencetoxicanttesting,
whichmeasuresboththelaboratoryperformanceandtherelativesensitivityofthetestspecies
overtime.
Positivecontroltests.Referencetoxicanttestswillbeperformedconcurrentlyforeachevent
forH.aztecaandP.promelas.ReferencetoxicanttestsforC.dubiaandS.capricornutumwillbe
performedmonthlyaccordingtoEPAtestmethodforin-housecultures.
Zincchloride(ZnCl2)willbeusedasthereferencetoxicantforS.capricornutum;sodium
chloride(NaCl)willbethereferencetoxicantusedfortheC.dubia,H.azteca,andP.promelasspecies.TheLC50(theconcentrationatwhich50%oftestorganismsexhibitmortality)for
survivalorEC25sublethalendpoint(theconcentrationatwhich25%oftestorganismsexhibita
response)foreachreferencetoxicanttestiscomparedtothelaboratory’srunningmeanto
ascertainwhetheritfallswithintheacceptablerange.EPAtestmethodmanualsincludethe
addedcautionthatreferencetoxicanttestresultsshouldnotbeusedasadefactocriterionforrejectionofindividualreceivingwatertests.Referencetoxicanttestsdoprovideinformationon
trendsinorganismsensitivityandlaboratoryperformancethatcanbeusefulinevaluatingand
interpretingtoxicitytestresults.Forthisreason,EPAhasrecommendedevaluatingthe
followingelementsofreferencetoxicanttestresultsinthereviewofthereceivingwatertest
data:thedegreetowhichthereferencetoxicanttestsresultisoutsideofcontrolchartlimits:
thewidthofthelimits;thedirectionofadeviation(towardincreasedtestorganismsensitivity
ortowarddecreasedtestorganismsensitivity);thetestconditionsofboththeambientorsite
waterandthereferencetoxicanttests;andtheobjectiveofthetest.TheEPAacceptablerange
iswithintwostandarddeviationsoftherunningmean.IftheLC50and/orEC25falloutsideofthe
upperandlowertwostandarddeviationlimits,testorganismsensitivitymaybeatypicaland
resultsofambientsampletoxicitytestsconductednearesttothetimewhenthereference
toxicanttestwasperformedwillbequalifiedaseithermoresensitiveorlesssensitivethan
usual.SeeEPA2002aformoreinformation.
Precision
Precisionisthedegreetowhichindependentanalysesofagivensampleagreewithone
another.Itisthereproducibility,consistencyandrepeatabilityofresults.UCDAHPLassesses
precisionthroughfieldduplicates.Afieldduplicateisasecondsamplecollectedinaseparate
container,immediatelyaftertheinitial/primarytestsample.Fieldduplicatesaretested
concurrentlywithitsprimarysampleandtheresultsareevaluatedtodetermineprecisionof
fieldandlaboratorystaff.Fieldduplicatesamplesareinagreementwhentheyarebotheither
statisticallysimilar,orstatisticallydifferentfromthecontrol.Fieldduplicateswillbeconducted
atarateof5%oftotalprojectsamplecount.
Therelativepercentdifference(RPD)betweenduplicatesiscalculatedonwaterchemistry
measurementsusingthefollowingformula:
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Accuracy
Accuracyoftoxicitytestscannotbedirectlymeasuredbecauseofthelackofdatatosupporta
standardorganismresponseagainstcomparabletestresults.However,inferencescanbemade
regardingaccuracyfromreferencetoxicanttestsinordertoassessthesensitivityofthe
organismsinaknownconcentrationoftoxicant,andtodeterminethattheorganisms’response
iswithinacceptablelimits.Accuracyofinstrumentswillbeevaluatedusingtheformulafor
accuracylistedinAppendixAoftheSWAMPQAPrPandwillfollowtheMQOslistedinTable4-
7.
Completeness
TheDeltaRMPstrivesforaminimumof90%completionofdata.Fortoxicitytests,
completenessisdefinedbythetotalnumberofsamplesthatmetTestAcceptabilityCriteriafor
eachspeciesdividedbythetotalnumberofuseablesamplessubmittedtothelaboratoryfor
eachspecies.Anindividualsamplemaynotbeusableifitsconductivityiswellaboveorbelow
conductivitiestypicallyfoundinfreshwater.Theseconductivitythresholdsaredifferentfor
eachspecies.Toxicitycompletenessisassessedbythenumberofuseableresultsdividedbythe
totalnumberofsamplescollected.
Forwaterqualitydataassociatedwithtoxicitytesting,datawillbeconsideredcompletewhen
eachsampleismeasuredwithinasamplebatchthatmeetstheaccuracyrequirementsforthe
referencematerial(hardness,alkalinityandtotalammonia),ormeterdrift(DO,ECandpH)is
withinacceptablelimits.
Representativeness
Intermsoflaboratorytoxicitytestingofambientsamples,representativenessreferstothe
degreetowhichdataaccuratelyreflectthepresenceorabsenceoftoxiccontaminantsinthe
environmentatthesiteswheresamplesarecollected.Locationofsamplingsites,sample
preservationandappropriatespeciesselectionareimportantconsiderationsfor
representativeness.
Comparability
TheDeltaRMPdocumentsadheretoEPAtestmethods,SOPsandQAmeasuresspecifiedinthe
QAPP,andacceptablereferencetoxicanttestresults.Therefore,resultscanbecomparedwith
otherprojectsandlaboratoriesthatadheretothesameEPAprotocolsandQAmeasures.
[ ][ ]
100*2121*2⎟⎟⎠
⎞⎜⎜⎝
⎛
+
−=
DupDupDupDup
RPD
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Dataanalysis
Toxicitytestswillbeconductedusingasingle-concentrationtestdesign.Datafromlaboratory
toxicitytestswillbeanalyzedaccordingtotheEPAstandardsingleconcentrationstatistical
protocols(EPA,2002,AppendixH).TheEPAmethodofdataanalysisinvolvesthecomparisonof
eachsampletoonecontrol(laboratorycontroloraconductivitycontrol),andcalculatesthe
testresultaccordingtothestandardizedstatisticalapproachusedinaquatictoxicology.
ComprehensiveEnvironmentalToxicityInformationSystem™ (CETIS;TidepoolScientific,McKinleyville,CA,USA)toxicitydataanalysisanddatabase)softwareapplicationwillbeusedto
calculateEffectConcentrationandLethalConcentrationvalues(EC25forsublethalendpoints
andLC50forsurvivalendpoints)forreferencetoxicanttests.
4.4.2. QualityControl
Table4.9providesasummaryofQCmeasuresandalsoliststhetoxicityendpointsthattriggera
TIE.Table4.10providesMQOsrelatedtotoxicitytesting.Section8.3CorrectiveActions
providesinformationonqualitycontrolactionswhenacceptancelimits(i.e.“actionlimits”)are
exceeded.
Table4.9. QualityControlMeasuresfortoxicitytesting.
Method Analyte/Test Matrix
HoldingTime/
Preservation AcceptabilityLimit
SM2320B;
UCDAHPSOP6-5Alkalinity(asCaCO3) Water
14days;
Coolto0to6°CNA
SM4500-NH3F;
UCDAHPSOP6-3Ammonia Water
48hours,28daysif
acidified
Coolto0to6°C;
samplesmaybe
preservedwith2
mLofH2SO4/L
<5mg/L
SM2510B;
UCDAHPSOP8-7Conductivity Water
28days;
Coolto0to6°C;if
analysisisnot
completedwithin
24hoursofsample
collection,sample
shouldbefiltered
througha0.45
micronfilterand
storedat≤6°C
Additionofconductivity
controlsintestbatches:
>1500µS/cmforS.capricornutum,<100or>
1900µS/cmforC.dubia,<100or>1900µS/cmforP.promelas;and<100mS/cm
or>10,000µS/cmforH.azteca.
SM4500OG;
UCDAHPSOP8-9DissolvedOxygen Water
48hours;
Coolto0to6°C;
add1gFAS
crystalsperliterif
residualchlorineis
<8.6mg/L(saturation)(H.azteca<8.9[saturation]mg/L)
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Method Analyte/Test Matrix
HoldingTime/
Preservation AcceptabilityLimit
present
SM2340C;
UCDAHPSOP6-1Hardness Water
14days;
Coolto0to6°CNA
SM4500H+B;
UCDAHPSOP8-8pH Water NA 6-9
SM2550B Temperature Water NA
25+1°C
(H.azteca23+1°C)Testtemperaturesmustnot
deviate(i.e.,maximum
minusminimum
temperature)bymorethan
3°Cduringthetest
EPA1003.0 S.capricornutum Water48hours;
Coolto0to6°C
LaboratoryControlmust
meettestacceptability
criterialistedinTable4.8
TIEtrigger:>50%reduction
incellgrowth
EPA1002.0 C.dubia Water36hours;
Coolto0to6°C
LaboratoryControlmust
meettestacceptability
criterialistedinTable4.8
TIEtrigger:>50%mortalityin
96hours
EPA1000.0 P.promelas Water36hours;
Coolto0to6°C
LaboratoryControlmust
meettestacceptability
criterialistedinTable4.8
TIEtrigger:>50%mortalityin
96hours
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Table4.10. MeasurementQualityObjectivesfortoxicitytesting.
Method Analyte/Test QualityControl Frequencyof
Analysis
ControlLimit/
MQO
SM2320B;
UCDAHPSOP6-5
Alkalinity(as
CaCO3)
Reference
Material
Peranalytical
batch±10%
Laboratory
Blank
Peranalytical
batch<12mg/L
SM4500-NH3F;
UCDAHPSOP6-3Ammonia
Reference
Material
Peranalytical
batch±10%
Laboratory
Blank
Peranalytical
batch<0.15mg/L
SM2510B;
UCDAHPSOP8-7Conductivity
Calibration
Standard:
InternalCell
Constant
Peranalytical
batch
(atleastoncedaily)
Permanufacturer’s
specifications
SM4500OG;
UCDAHPSOP8-9
Dissolved
Oxygen
Oxygen
Saturated
Waterat25°C
Peranalytical
batch
(atleastoncedaily)
Peranalyticalmethod
ormanufacturer’s
specifications
SM2340C;
UCDAHPSOP6-1Hardness
Reference
Material
Peranalytical
batch±10%
Laboratory
Blank
Peranalytical
batch<6mg/L
SM4500H+B;
UCDAHPSOP8-8pH
Calibration
Standard
Peranalytical
batch
(atleastoncedaily)
Permanufacturer’s
specifications
SM2550B TemperatureCertified
ThermometerOnceannually ±0.5°C
ChronicToxicity
TestingAllspecies
Laboratory
ControlWater
Peranalytical
batch
Mustmeetalltest
acceptabilitycriteriafor
thespeciesofinterest
(seeTable4.8)
Conductivity
ControlWater
Peranalytical
batchwhen
conductivity
parametersare
aboveorbelowthe
species’tolerance
(seeTable4.9a)
FollowEPAguidanceon
interpretingdata
Additional
ControlWater
Peranalytical
batchwhen
manipulationsare
performedonone
Nostatisticaldifference
betweenthelaboratory
controlwaterandeach
adidionalcontrolwater
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Method Analyte/Test QualityControl Frequencyof
Analysis
ControlLimit/
MQO
ormoreambient
samplewithineach
analyiticalbatch
withinananalytical
batch
Reference
ToxicantTests
Monthlyforin-
housecultured
organismsorper
analyticalbatch
whenorganisms
arecommercially
supplied.
Lastplotteddatapoint
(LC50orEC50/25)must
bewithin2SDofthe
cumulativemean
(n=20)
Sample
Duplicate
5%totalproject
samplecount
(3peryear)
Recommended
acceptableRPD<20%
FieldBlank Oneperyear
Nostatisticaldifference
betweenthelaboratory
controlwaterandthe
fieldblankwithinan
analyticalbatch
BottleBlank Twoperyear
Nostatisticaldifference
betweenthelaboratory
controlaterandthe
bottleblankwithinan
analyticalbatch
4.4.3. Project-specificcorrectiveactionlimits
IndividualresultsproducedbytheDeltaRMParenotintendedtotriggerenforcementactions,
eventhoughcollectivelythedatamayguidemanagementactionsbyotherpartiesthrough
planning.Consequently,therearenoproject-specificcorrectiveactionsrequiredforthedata.
However,anycorrectiveactionsthatarewarrantedshallbemadeatthediscretionoftheQAO
followingtheSWAMPGuidance:
LaboratoryControlWater:Iftestedwithin-housecultures,affectedsamplesandassociated
qualitycontrolmustberetestedwithin24hoursoftestfailure.Ifcommercialculturesare
used,theymustbeorderedwithin16hoftestfailurefortheearliestpossiblereceipt.Retests
mustbeinitiatedwithin30hofreceipt,dependingontheneedfororganismacclimation.The
laboratoryshouldtrytodeterminethesourceofthecontrolfailure,documenttheinvestigation
anddocumentthestepstakentopreventarecurrence.
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ConductivityControlWater:Affectedambientsamplesandassociatedqualitycontrolmustbe
flaggedtoreflectthatconductivitymaybeoutsideofthephysiologicaltoleranceforthespecies
tested.
AdditionalControlWater:Basedontheobjectivesofthestudy,awatersamplethathassimilar
qualitiestothetestsamplemaybeusedasanadditionalcontrol(e.g.pHadjustments,
continuousaeration).Resultsthatshowstatisticaldifferencesfromthelaboratorycontrol
shouldbeflagged.Thelaboratoryshouldtrytodeterminethesourceofvariation,document
theinvestigationanddocumentthestepstakentopreventarecurrence.Thisisnotapplicable
forTIEmethodblanks.
ReferenceToxicantTests:IftheLC50exceeds+/-twostandarddeviationsoftherunningmean
ofthelast20referencetoxicantteststheassociatedambienttestshouldbeflaggedaseither
moreorlesssensitivethannormal.
FieldDuplicate:VisuallyinspectthesamplestodetermineifahighRPDbetweenresultscould
beattributedtosampleheterogeneity.Forduplicateresultsvaryingduetomatrix
heterogeneity,orwhereambientconcentrationsarebelowthereportinglimit,qualifythe
resultsanddocumenttheheterogeneity.ResultsthatdonotmeetSWAMPRPDcriteriashould
beflagged,regardlessofwhetherthesampleisheterogeneousornot.Theprojectcoordinator
shouldbenotifiedsothatthesamplingteamcanidentifythesourceofvariationandperform
correctiveactionpriortothenextsamplingevent.
FieldBlanks:Ifcontaminationofthefieldblanksandassociatedsamplesisknownorsuspected,
thelaboratoryshouldflagtheaffecteddata.Theprojectcoordinatorshouldbenotifiedsothat
thesamplingteamcanidentifythecontaminationsource(s)andperformcorrectiveactionprior
tothenextsamplingevent.
BottleBlanks:Ifcontaminationoftheequipmentblanksandassociatesampleisknownor
suspected,thelaboratoryshouldflagtheaffecteddata.Thelaboratorymanagershouldbe
notifiedsothatthelaboratorytechnicianscanidentifythecontaminationsource(s)and
performcorrectiveactionspriortothenextsamplingevent.
CalibrationStandard:Recalibratetheinstrument.Affectedsamplesandassociatedquality
controlmustbereanalyzedfollowingsuccessfulinstrumentrecalibration.
LaboratoryBlank:Reanalyzetheblanktoconfirmtheresult.Investigatethesourceof
contamination.Ifthesourceofthecontaminationisisolatedtothesamplepreparation,the
entirebatchofsamples,alongwiththenewlaboratoryblanksandassociatedQCsamples,
shouldbepreparedand/orre-extractedoranalyzed.Ifthesourceofcontaminationisisolated
totheanalysisprocedures,reanalyzetheentirebatchofsamples.Ifreanalysisisnotpossible,
theassociatedsampleresultsmustbeflaggedtoindicatethepotentialpresenceof
contamination.
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4.5. Performance-basedmethodconceptforthedeterminationofLT2pathogens(CryptosporidiumandGiardia)
TheDeltaRMPpathogen(CryptosporidiumandGiardia)monitoringisdesignedastheambient
monitoringcomponentoftheRegionalBoard’sBasinPlanAmendmenttoestablishaDrinking
WaterPolicytoprotectsourcewater,andisbeingconductedconcurrentlywiththedrinking
wateragencies’requiredLongTerm2(LT2)EnhancedSurfaceWaterTreatmentRule
monitoring(asdescribedintheDeltaRMPPathogenStudyDesignSummary).ThePathogen
Studyisintendedtosatisfydataneedsandmonitoringforanyfollow-uprequiredifBasinPlan
triggervaluesareexceededduringLT2monitoring.ThedirectionfromtheCentralValley
DrinkingWaterPolicyWorkgroupisthatdatacollectedfortheRMPpathogenmonitoring
shouldbeconsistentwithdatacollectedduringLT2monitoring.
EPAMethod1623wasdevelopedtosupportthesupportpromulgationofEPA’sLT2.Its
purposeistosupporttheassessmentofprotozoan(CryptosporidiumandGiardia)pathogenoccurrenceinrawsurfacewatersusedassourcewatersfordrinkingwatertreatmentplants.
EPAMethod1623providesqualitycontrol(QC)acceptancecriteriaforCryptosporidiumandGiardia,butnotesthatsomesamplematricesmaypreventtheacceptancecriteriafrombeing
met.EPAnotesthatfieldsampleswithmatrixspikerecoveriesbelowtheQCacceptancecriteria
identifiedinMethod1623(13%-111%forCryptosporidiumand15%-118%forGiardia)arevalid,andwillbeacceptedfordeterminingLT2binconcentrations.TobeconsistentwiththeLT2
data,theRMPwillconsiderdataoutsidetheacceptancecriteriatobevalid,butwillflagsuch
results.
ThePathogenStudymayuseEPAMethod1623.1,whichisreportedtohavehigher
Cryptosporidiumrecoveries.TheQCacceptancecriteriaidentifiedinMethod1623.1formatrix
spikerecoveriesare32%-100%forCryptosporidiumand8%-100%forGiardia.
TobeapprovedforLT2protozoantestingusingMethod1623and1623.1,laboratoriesare
requiredtodemonstrateacceptableperformanceforCryptosporidiumandGiardia.EPAMethod1623and1623.1areperformance-basedmethodsapplicabletothedeterminationof
CryptosporidiumandGiardiainaqueousmatrices.Demonstrationofacceptableperformance
includesinitialandongoingprecisionandrecoverytests,whichareconductedusingspiked
reagentwaterandmatrixsamples.Eachlaboratorythatusesthismethodisrequiredtooperate
aformalqualityassurance(QA)programthataddressesanddocumentsdataquality,
instrumentandequipmentmaintenanceandperformance,reagentqualityandperformance,
analysttrainingandcertification,andrecordsstorageandretrieval.Theminimumanalytical
requirementsofthisprogramconsistofaninitialdemonstrationoflaboratorycapability(IDC)
throughperformanceofaninitialprecisionandrecovery(IPR)test,andongoingdemonstration
oflaboratorycapabilityandmethodperformancethroughthematrixspike(MS)test,the
methodblanktest,anongoingprecisionandrecovery(OPR)test,stainingcontrols,andanalyst
verificationtests.Laboratoryperformanceiscomparedtoestablishedperformancecriteriato
determineiftheresultsofanalysesmeettheperformancecharacteristicsofthemethod.A
principalanalystverifiesthequalityandaccuracyofallsampleresults.Laboratoryperformance
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iscomparedtoestablishedperformancecriteriatodetermineiftheresultsofanalysesmeet
theperformancecharacteristicsofthemethod.Table4.11summarizestheminimumQC
requirementsforMethod1623,andTable4.12summarizestheminimumQCrequirementsfor
Method1623.1.DetailsaredescribedinEPAMethod1623 and1623.1.
Table4.11. QCrequirementsandacceptancecriteriafordeterminationofCryptosporidiumand
Giardiainaqueousmatrices(EPAMethod1623)
QCsampleor
procedure Frequency Acceptablelimits
Cryptosporidium
IPR Eachequipment/supplychange MeanRecovery=24-100%/RSD<55%
MethodBlank 1per20orweek Nofalsepositives
OPR 1per20orweek Recovery=22-100%
MatrixSpikes 1per20 Recovery=13-111%/RPD<61%
Matrix
Spikes/Duplicates
Initialuseandeachprocedural
changeRecovery=13-111%/RPD<61%
Positivestaining
controlEverybatch Nofalsenegatives
Negativestaining
controlEverybatch Nofalsepositives
Verificationofanalyst
performanceMonthly <10%differenceincounts
Giardia
IPR Eachequipment/supplychange MeanRecovery=24-100%/RSD<49%
MethodBlank 1per20orweek Nofalsepositives
OPR 1per20orweek Recovery=14-100%
MatrixSpikes 1per20 Recovery=15-118%/RPD<30%
Matrix
Spikes/Duplicates
Initialuseandeachprocedural
changeRecovery=15-118%/RPD<30%
Positivestaining
controlEverybatch Nofalsenegatives
Negativestaining
controlEverybatch Nofalsepositives
Verificationofanalyst
performanceMonthly <10%differenceincounts
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Table4.12. QCrequirementsandacceptancecriteriafordeterminationofCryptosporidiumand
Giardiainaqueousmatrices(EPAMethod1623.1)
QCsampleor
procedure Frequency Acceptablelimits
Cryptosporidium
IPR Eachequipment/supplychange MeanRecovery=38-100%/RSD<37%
MethodBlank EachIPRandOPRset Nofalsepositives
OPR 1per20orweek Recovery=33-100%
MatrixSpikes 1per20 Recovery=32-100%/RSD<46%
Matrix
Spikes/Duplicates
Initialuseandeachprocedural
change,andmulti-labvalidationof
modification
Recovery=32-100%/RSD<46%
Positivestaining
controlEverybatch Nofalsenegatives
Negativestaining
controlEverybatch Nofalsepositives
Verificationofanalyst
performanceMonthly <10%differenceincounts
Giardia
IPR Eachequipment/supplychange MeanRecovery=27-100%/RSD<39%
MethodBlank EachIPRandOPRset Nofalsepositives
OPR 1per20orweek Recovery=22-100%
MatrixSpikes 1per20 Recovery=8-100%/RSD<97%
Matrix
Spikes/Duplicates
Initialuseandeachprocedural
change,andmulti-labvalidationof
modification
Recovery=8-100%/RSD<97%
Positivestaining
controlEverybatch Nofalsenegatives
Negativestaining
controlEverybatch Nofalsepositives
Verificationofanalyst
performanceMonthly <10%differenceincounts
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5. Special Training Needs and Certification
5.1. SpecializedTrainingorCertifications
BecausetheDeltaRMPusesperformance-basedmethodsforlaboratoryevaluation,laboratory
certifications(e.g.byNELAP/ELAP11)fortheanalysesplannedarepreferredbutnotrequired.
ThelaboratoryprovidinganalyticalsupporttotheDeltaRMPmusthaveadesignatedon-site
QAOfficerfortheparticularanalyticalcomponent(s)performedatthatlaboratory.This
individualwillserveasthepointofcontactfortheSFEI-ASCQAstaffinidentifyingandresolving
issuesrelatedtodataquality.
Toensurethatthesamplesareanalyzedinaconsistentmannerthroughoutthedurationofthe
program,keylaboratorypersonnelwillparticipateinanorientationsessionconductedduring
aninitialsitevisitorviacommunicationswithSFEI-ASCstaff.Thepurposeoftheorientation
sessionistofamiliarizekeylaboratorypersonnelwiththisQAPPandtheDeltaRMPQA/QC
program.Participatinglaboratoriesmayberequiredtodemonstrateacceptableperformance
beforeanalysisofsamplescanproceed,describedinsubsequentsections.Laboratory
operationswillbeevaluatedonacontinualbasisthroughtechnicalsystemsaudits,andby
participationinlaboratoryinter-comparisonprograms.
Personnelinanylaboratoryperforminganalyseswillbewellversedingoodlaboratory
practices(GLPs),includingstandardsafetyprocedures.Itistheresponsibilityoftheanalytical
laboratorymanager,and/orsafetystafftoensurethatalllaboratorypersonnelareproperly
trained.Eachlaboratoryisresponsibleformaintainingacurrentsafetymanualincompliance
withtheOccupationalSafetyandHealthAdministration(OSHA)orequivalentstateorlocal
regulations.Thesafetymanualwillbereadilyavailabletolaboratorypersonnel.Proper
proceduresforsafestorage,handling,anddisposalofchemicalswillbefollowedatalltimes;
eachchemicalwillbetreatedasapotentialhealthhazardandGLPswillbeimplemented
accordingly.
Personnelcollectingsamplesmusthavebeentrainedonthefieldsamplingmethodsdescribed
intheQAPP.Forpesticidesmonitoring,theUSGSfieldsamplingcoordinatorwillberesponsible
fortrainingtheUSGSfieldstaff.Forpathogenmonitoring,MWQIwillberesponsiblefortraining
thefieldstaff.Thesign-insheetofthetrainingcanbethedocumentationofthetraining.
11EnvironmentalLaboratoryAccreditationProgram(ELAP).ELAPprovidesevaluationandaccreditationofenvironmentaltestinglaboratoriesto
ensurethequalityofanalyticaldatausedforregulatorypurposestomeettherequirementsoftheState'sdrinkingwater,wastewater,shellfish,
food,andhazardouswasteprograms
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5.2. TrainingCertificationandDocumentation
Contractorsperformingsamplingareresponsibleforprovidingtrainingtotheirstaffand
maintainingrecordsofalltrainings.Thoserecordscanbeobtainedifneededfromcontractors
throughtheirrespectiveQAorSafetyOfficers.
5.3. TrainingPersonnel
Eachcontractlaboratory’sQAOfficerandSafetyOfficershallprovideand/ordesignatestaffto
providetrainingtotheirrespectivepersonnel.Allpersonnelresponsibleforsamplingwillbe
trainedinfieldsamplecollectionandsafetypriortothefirstdaytheyarescheduletosample
fortheDeltaRMP.
6. Documents and Records
AllDeltaRMPdocumentswillbeprovidedtotheSteeringCommittee,whichincludesthe
RegionalBoard.
SFEI-ASCwillcollectrecordsforsamplecollection,fieldanalyses,laboratorychemicalanalyses,
toxicitytesting,andpathogenanalyses.Samplessenttoanalyticallaboratorieswillincludea
Chain-of-Custody(COC)form.Theanalyticallaboratorieswillmaintainrecordsofsample
receiptandstorage,analyses,andreportedresults.
SFEI-ASCwillmaintainhardcopyorscannedfilesoffieldnotesandmeasurements,aswellas
laboratorysubmitteddocumentationandresultsattheSFEI-ASCmainoffice.TheSFEI-ASCData
Managerwillberesponsibleforthestorageandorganizationofinformation.
Contractlaboratorieswillalsoberesponsibleformaintainingcopiesofprojectdocumentation
originatingfromtheirrespectivelaboratories,withbackuparchivalstorageoffsitewhere
possible.AllSOPsusedfortheDeltaRMPwillbestoredindefinitelyincasefuturereviewis
necessary.
QualityAssuranceDocumentation
AlllaboratorieswillhavethelatestrevisionoftheDeltaRMPQAPP.Inaddition,thefollowing
documentsandinformationwillbecurrentandavailabletoalllaboratorypersonnel
participatingintheprocessingofProjectsamples,aswellastoSFEI-ASCprogramofficials:
1. LaboratoryQAPlan:Clearlydefinedpoliciesandprotocolsspecifictoaparticular
laboratory,includingpersonnelresponsibilities,laboratoryacceptancecriteriaand
correctiveactionstobeappliedtotheaffectedanalyticalbatches,qualificationofdata,and
proceduresfordeterminingtheacceptabilityofresults.
2. LaboratoryStandardOperatingProcedures(SOPs):Containinginstructionsforperforming
routinelaboratoryprocedures,suchaslogging,labelling,andstorageofsamples,cleaning
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ofequipment,checkingofreagents,etc.,thatarenotnecessarilypartofanyanalytical
methodologyforspecificanalytesoranalytetypes.
3. LaboratoryAnalyticalMethods:Step-by-stepinstructionsdescribingexactlyhowamethod
isimplementedinthelaboratoryforaparticularanalyticalprocedure.Containsallanalytical
methodsutilizedintheparticularlaboratoryfortheDeltaRMP.
4. InstrumentPerformanceInformation:Informationoninstrumentbaselinenoise,calibration
standardresponse,analyticalprecisionandbiasdata,detectionlimits,etc.Thisinformation
shouldbereportedfortheperiodsduringwhichDeltaRMPsamplesareanalyzed.
5. ControlCharts:Controlchartsareusefulinevaluatinginternallaboratoryproceduresand
arehelpfulinidentifyingandcorrectingsystematicerrorsources.Contractlaboratoriesare
encouragedtodevelopandmaintaincontrolchartswhenevertheymayservein
determiningsourcesofanalyticalproblems.
Copiesoflaboratorymethods,SOPs,andQAplansareavailablebyrequestfromtheSFEI-ASC
QAOfficer.SomelaboratorymethodsandSOPsmaybeeditedtoexcludeproprietarydetails
abouttheanalyses.Qualityassurancedocumentsarereviewedtoassureconformanceto
programneedsbytheDeltaRMPProjectManagerandQAOortheirdesignees.
CopiesofallrecordswillbemaintainedatSFEI-ASCandatthelaboratoryforaminimumfive
yearsafterprojectcompletion,afterwhichtheymaybediscarded,exceptforthedatabaseat
SFEI-ASC,whichwillbemaintainedwithoutdiscarding.Alldatawillbebackedupandsecured
ataremotelocation(i.e.,separatefromtheSFEI-ASCoffice).Asneeded,datarecoverycanbe
initiatedbycontactingtheback-upfacilityforrestorationandthiswillbecoveredthroughSFEI-
ASCoverhead.
AllparticipantslistedinTable0.1willreceivethemostcurrentversionoftheDeltaRMPQAPP.
6.1. ReportPackageInformation
Analyticalresults,includingassociatedqualitycontrolsamples,willbeprovidedtoSFEI-ASCby
theanalyticallaboratories.Thelaboratoriesanalyzesamplesaccordingtotheholdtimeslisted
intheDeltaRMPQAPP,butthefinalreportmaybefinalizedforreviewupto90daysafter
samplesarereceivedfromthelaboratory.Exceedancesofthestandardturnaroundtimeshould
bediscussedwithandapprovedbytheDeltaRMPProjectManagerandQAO.
Laboratorypersonnelwillverify,screen,validate,andpreparealldata,includingQA/QCresults,
inaccordancewiththeDeltaRMP’sQAPPandwillprovide(uponrequest)detailedQA/QC
documentationthatcanbereferredtoforanexplanationofanyfactorsaffectingdataquality
orinterpretation.AnydetailedQA/QCdatanotsubmittedaspartofthereportingpackage(see
below)shouldbemaintainedinthelaboratory’sdatabaseforfuturereference.
Laboratorieswillprovideelectroniccopiesofthetabulatedanalyticaldata(includingassociated
QA/QCinformationoutlinedbelow)inaformatagreeduponwiththeDeltaRMPProject/Data
Managerordesignee.
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EachElectronicDataDeliverable(EDD)reportwillconsistofthefollowing:AnalyticalandQA
dataresultsinanappropriateCEDENformatandCRMcertificates(whenapplicable).
ResultsshouldbeflaggedbythelaboratoryforexceedancesofDeltaRMPMQOsfor
completeness,sensitivity,precision,andaccuracy,usingdataqualitycodesasdefinedby
CEDEN’slistofcodes,whichhavebeenadoptedbytheDeltaRMPforreportingdata.Thedata
qualitycodesshouldbeprovidedintheLabResulttableintheResQualCodeandQACodefields.
AlistofcommonlyusedresultqualifiercodesandQAcodesareprovidedinTables6.1and6.2,
respectively.AcompletedlistofcodesisavailableonCEDEN’sControlledVocabularywebpage.
Detailsonthemeasurementsandproceduresthatareexpectedtobeusedtodemonstratethe
qualityofreporteddatacanbefoundinSection4,QualityObjectives,Criteria,andControl
ProceduresforMeasurementData.
6.1.1. AnalyticalandQAdataresults
ToxicitydatathatisgeneratedusingfundsprovidedbySWAMPwillbesubmittedtotheOffice
ofInformationManagementandAnalysis(OIMA)bythedataproviderusingSWAMPdata
templates,SWAMPformatting,completenessandbusinessrulesandthroughtheSWAMP’s
DataChecker.Thisonlinetoolalertsuserstodatathatdonotconformtothebusinessrules
outlinedintheapplicableSWAMPDataManagementPlanorthevaluesestablishedin
SWAMP’sLookUpLists.Datamustbereviewedandverifiedforformat,completeness,and
qualitycontrolrequirements,includingresultqualificationsandappropriatesampleandbatch
comments,priortosubmissiontoOIMA.Thelaboratorymustbereachabletoanswerquestions
regardingthedatasubmittalifnecessary.Ifthedataisdeterminedtobeincompleteor
requiringsignificantcorrections,thedatamaybereturnedtothelaboratoryforcorrectionand
re-submission.OncethesedatahavebeenapprovedbySWAMP,theappropriateSWAMPData
ManagerwillprovidethedatawithintheCaliforniaEnvironmentalDataExchangeNetwork’s
(CEDEN)electronicdatadeliverable(EDD)templatestoSFEI/ASCforfurtherprocessing.SFEI-
ASCstaffisencouragedtocontacttheOIMAHelpDeskwithanydataquestionstheymayhave.
Resultsforfieldmeasurements,pesticides,copper,DOC/POCandpathogenswillbesubmitted
intheEDDtemplatesuppliedbySFEI-ASC.Tabulateddatawillincludethefollowinginformation
foreachsample(whenapplicable):
1. Sampleidentification:UniquesampleID,sitecode,sitename,collectiondate,collection
time,analysisdate,sampletype(fieldorQCtypes),andmatrix(water).
2. Analyticalmethods:Preparation,extraction,andquantitationmethods(codesshould
referenceSOPssubmittedwiththedatasubmissionpackage).Alsoincludepreparation,
extraction,andanalysisdates.
3. Analyticalresults:Analytename,fraction,result,unit,methoddetectionlimit(MDL),and
reportinglimit(RL)foralltargetparameters.Theappropriatedataqualifiersshouldbe
submittedwiththeresults.
Requiredadditionaldatainclude:
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• Controlresults(fortoxicitytests)
• Summaryandindividualreplicateresults,includingwaterqualityparameters(for
toxicitytests)
• Labreplicateresults(andfieldreplicates,whensentforanalysis)
• Qualityassuranceinformationforeachanalyticalchemistrybatch:
• CRMorLRMresults:absoluteconcentrationsmeasured,certifiedvalue,and%recovery
relativetocertifiedorexpectedvalue.
• Matrix(orblank)spikeresults:includeexpectedvalue(native+spike)foreachanalyte,
actualrecoveredconcentrations,andcalculated%recovery.
• Methodblanksampleresultsinunitsequivalenttofieldsampleresults(e.g.,ifthefield
samplesarereportedasng/g,methodblanksaregiveninthesameunits).
• Fieldandlabreplicateresultsandcalculated%RPDor%RSD.
6.1.2. ElectronicDataDeliverableTemplate
SFEI-ASCisaRegionalDataCenter(RDC)fortheStateofCaliforniaandusestemplates,
standardizedvocabularyandbusinessrulesdevelopedandmaintainedbyCEDENtomanage
dataforfieldcollection,chemistry,taxonomy,tissue,toxicity,andbioassessmentsampling.
SFEI-ASCwillprovidetrainingandguidancetocollectionagenciesandlaboratoriesonhowto
usetheCEDENtemplates.
Priortofieldcollection,SFEI-ASCwillprovidethefieldcollectionagencyacopyoftheCEDEN
LocationsandChemResults tablestobepopulatedwithinformationaboutthesample
collection.
Priortoanalyses,SFEI-ASCwillprovidethelaboratorywithacopyoftheappropriateCEDEN
template(populatedbythefieldcollectionagencywithinformationaboutthesample
collection)anddocumentationforpopulatingtheCEDENtemplate.Thedocumentationdetails
attributesofeachfieldincludingfieldname,datatype,whetherthefieldisrequiredornot,the
appropriatelookuplistforapprovedvocabularyandadescriptionofeachfield.TheCEDEN
templatesanddocumentationareavailableon-linefromCEDENat
http://www.ceden.org/ceden_datatemplates.shtml.Lookuplistvaluesareavailableonthe
CEDENControlledVocabularywebsite.
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Table6.1.CEDENcontrolledvocabularyforresultqualifiers.
ResultQualifierName ResultQualifierCode
Absent A
Colonial COL
ConfluentGrowth CG
Cw/C-ConfluentGrowthwithColiforms w/C
Cw/oC-ConfluentGrowthwithoutColiforms /oC
DetectedNotQuantifiable DNQ
EqualTo =
FieldEstimated JF
GreaterThan >
Greaterthanorequalto >=
LessThan <
Lessthanorequalto <=
NoReportableSum NRS
NoReportableTotal NRT
NoSurvivingIndividuals NSI
NotAnalyzed NA
NotDetected ND
NotRecorded NR
PercentRecovery PR
Present P
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Table6.2.CommonCEDENQAcodes.
QACode QADescr
BRK Noconcentrationsamplecontainerbroken
BRKA Samplecontainerbrokenbutanalyzed
BS InsufficientsampleavailabletofollowstandardQCprocedures
DO Coelution
DS BatchQualityAssurancedatafromanotherproject
H Aholdingtimeviolationhasoccurred
IL RPDexceedslaboratorycontrollimit
IP Analytedetectedinfieldorlabgeneratedblank
IU PercentRecoveryexceedslaboratorycontrollimit
J Estimatedvalue-EPAFlag
M Amatrixeffectispresent
NBC Valuenotblankcorrected
None None-NoQAQualifier
R Datarejected-EPAFlag
SC SurrogateCorrectedValue
OtherQACodes
BB Sample>4xspikeconcentration
BE Lowsurrogaterecovery;analyzedtwice
BLM CompoundunidentifiedorbelowtheRLduetooverdilution
BT Insufficientsampletoperformtheanalysis
BY Samplereceivedatimpropertemperature
BZ Samplepreservedimproperly
CS QCcriterianotmetduetoanalyteconcentrationnearRL
CT QCcriterianotmetduetohighlevelofanalyteconcentration
D EPAFlag-Analytesanalyzedatasecondarydilution
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QACode QADescr
DRM Spikeamountlessthan5XtheMDL
EU LCSisoutsideofacceptancelimits.MS/MSDareaccept.,nocorr.
EUM LCSisoutsideofcontrollimits
FO Estimatedmaximumpossibleconcentration(EMPC)
GN Surrogaterecoveryisoutsideofcontrollimits
GR Internalstandardrecoveryisoutsidemethodrecoverylimit
H24 Holdingtimewas>24hoursforBacteriatestsonly
H6 Holdingtimewas>6hrsbut<24hoursforBacteriatestsonly
HH Resultexceedslinearrange;concentrationmaybeunderstated
HR Post-digestionspike
HT Analyticalvaluecalculatedusingresultsfromassociatedtests
IF Sampleresultisgreaterthanreportedvalue
JA Analytepositivelyidentifiedbutquantitationisanestimate
LC LaboratoryContamination
N TentativelyIdentifiedCompound
NC AnalyteconcentrationnotcertifiableinCertifiedReferenceMaterial
NMDL NoMethodDetectionLimitreportedfromlaboratory
NRL NoReportingLimitreportedbythelaboratory
PG Calibrationverificationoutsidecontrollimits
PJ Resultfromre-extract/re-analtoconfirmoriginalMS/MSDresult
PJM Resultfromre-extract/re-analtoconfirmoriginalresult
QAX WhenthenativesamplefortheMS/MSDorDUPisnotincludedinthebatchreported
RE Elevatedreportinglimitsdue to limited sample volume
SCR Screeninglevelanalysis
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6.1.3. StandardOperatingProcedures(SOPs)
ThelaboratorysubmittedSOPsforpreparation,extraction,andanalyticalmethodsupon
approvingtheQAPP.TheSOPsarelistedinAppendixDinthisQAPP.TheQAOfficer/Project
Managerwillneedtoapproveanychangesinmethods.
6.2. DataReportingRequirements
Eachlaboratoryshallestablishasystemfordetectingandreducingtranscriptionandcalculation
errorspriortoreportingdata.
DatawillbereportedinCEDENtemplatesorprovidedinacomparableformatapprovedby
SFEI’sDataManager.Chemical-analyticaldataandpathogendatawillbereportedinCEDEN’s
WaterQuality(WQ)template.ToxicitydatawillbereportedtoSWAMPusingtheSWAMP
toxicitytemplate.TheminimumfieldsrequiredfordatareportedintheCEDENWQtemplate
fortheLabResultstabare:StationCode,SampleDate,ProjectCode,CollectionTime,
CollectionMethodCode,SampleTypeCode,Replicate,CollectionDepth,UnitCollectionDepth,
LabBatch,AnalysisDate,MatrixName,MethodName,AnalyteName,FractionName,UnitName,
LabReplicate,Result,ResQualCode,MDL,RL,QACode.Thesefieldsshouldincludetruevalues
(notnulls).Otherfieldssuchaspreparationcodeandextractionmethodshouldbefilledoutto
theextentpossible.TheminimumfieldsrequiredfordatareportedintheCEDENWQtemplate
fortheLabBatchtabare:LabBatchandLabAgencyCode.BatchesmustbereviewedforQC
completenessandanydeviationinQCresultsshouldbedocumentedintheaccompanyingcase
narrative.Therequiredfieldswillbeidentifiedinthetemplateingreenfont.TheEDDtemplate
providedtothelaboratorybySFEIwillhavethefieldsconcerningfieldcollectionofthesamples
alreadypopulated.
Documentationcontainingdefinitions,fieldlength,fieldrequirement,andassociatedlookup
lists(ifapplicable)foreachfieldisavailableontheCEDENwebsite
(http://www.ceden.org/ceden_datatemplates.shtml)..Fieldsrequiringcontrolledvocabulary
canbeidentifiedbyhoveringoverthefieldnameinthetemplateandreferringtothelookup
listthatisreferenced.LookuplistsareavailableontheCEDENwebsiteat
http://www.ceden.org/CEDEN_Checker/Checker/LookUpLists.php.
OnlydatathathavemetMQOsorthathavedeviationsexplainedappropriatelywillbeaccepted
fromthelaboratory.WhenQArequirementshavenotbeenmet,thesampleswillbe
reanalyzedwhenpossible.Onlytheresultsofthereanalysisshouldbesubmitted,providedthey
areacceptable.
Reportingturnaroundtimesforsubmissionofresultsfromsampleanalysesarespecifiedin
contractswiththeanalyticallaboratories.However,samplesshouldbeextractedandanalyzed
withintheholdingtimesspecifiedfortheanalyticalmethodsused(Table9-2).Turnaroundtime
requirementsspecifiedinsubcontractsaregenerally90daysorless.
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6.3. DataStorage/Database
DataaremanagedbySFEI-ASCDataServicesasestablishedinSection13.Uponcompletionof
QA/QCreviewanddatavalidation,dataarecompiledintotheSFEI-ASCRDCdatabaseand
distributedtotheprojectmanagers.
DatathatareapprovedforpublicreleasearemadeavailablethroughSFEI-ASC’sContaminant
DataDisplayandDownload(CD3)tool,usuallywithinoneyearofsamplecollection.Datawill
alsobemadeavailablethroughCEDEN’sAdvancedQuerytool.
7. Sampling Process Design
7.1. StudyAreaandPeriod
Samplecollectionpointsandajustificationforsiteselectionforthedifferentelementsare
describedinthespecificdesignsforeachoftheDeltaRMPmonitoringelements(AppendixB).
TheDeltaRMPmonitoringsitesarelocatedinandupstreamoftheDelta(Figures3-1,3-2,and
3-3).Themonitoringsitesforpesticidesurfacewatersamplingrepresentkeyinflowstothe
Delta(Figure3-1).Themonitoringsitesformercurysamplingrepresentdifferentsubareasof
theDelta(Figure3-2).Ambientpathogenmonitoringsites(Figure3-3)areco-locatedwith
existingsitesoftheMunicipalWaterQualityInvestigationsprogram.
Samplingtimingandfrequencyvariesforthedifferentelementsofthemonitoringprogram:
• Pesticidesitesarevisitedmonthly.Themonthlyvisitscapturetwowetevents(firstflush
rain,2ndsignificantstorminwinter)andthreedryevents(1
stirrigation,2
ndirrigation,
andsnowmelt/springrunoff).
• Mercurymonitoringincludesannualsportfishsamplingatsixsitesandquarterlywater
samplingat5ofthesesites.Bothsportfishandwatersamplingwillbeginin2016.
• Pathogenambientwatermonitoringoccursmonthlyat12sites.
Collecteddataareusedtoevaluatefuturedataneedsandadjustthesamplingandanalysisplan
asneededtooptimizedatacollectioninanadaptivemanner.Theprogramwillbecontinually
adjustedtooptimizedatacollection.ThemonitoringdesignisdescribedintheMonitoring
DesignSummarydocument.
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7.2. SamplingSites
Table7.1. Samplingsitesandschedule.
SiteName SiteCode
Target
Latitude
Target
Longitude
Sampling
frequency
Sampling
Day
Pesticides
MokelumneR@NewHope
Road 544SAC00238.23611 -121.41889 Monthly 3
rdTuesday
SacramentoR@Hood 510SACC3A 38.36691 -121.52037 Monthly 3rdTuesday
SanJoaquinR@BuckleyCove 544LSAC13 37.97667 -121.37889 Monthly 3rdTuesday
SanJoaquinR@
Vernalis/AirportWay 541SJC50137.67556 -121.26417 Monthly 3
rdTuesday
UlatisC@BrownRd 511ULCABR 38.30667 -121.79472 Monthly 3rdTuesday
Mercury
LibertyIsland 38.24210 -121.68490Fish:Annually
Water:QuarterlyNotspecified
LittlePotatoSlough 38.09627 -121.49602Fish:Annually
Water:QuarterlyNotspecified
MiddleR@BordenHwy(Hwy4) 37.89083 -121.48833Fish:Annually
Water:QuarterlyNotspecified
MokelumneRdsCosumnesR 38.25528 -121.44000 Fish:Annually Notspecified
SacramentoR@Freeport 38.45570 -121.50120Fish:Annually
Water:QuarterlyNotspecified
SanJoaquinR@
Vernalis/AirportWay541SJC501 37.67556 -121.26417
Fish:Annually
Water:QuarterlyNotspecified
Pathogens
BanksPumpingPlant KA000331 37.81480 -121.61573 Monthly 1stWednesday
CacheSloughnrRyderIsland B9D81281401 38.22500 -121.67481 Monthly 1stTuesday
CalaverasR@UoPFootbridge B9D75891188 37.98003 -121.33648 Monthly 1stTuesday
ColusaBasinAgDrain A0294500 38.80197 -121.72552 Monthly 1stMonday
JonesPumpingPlant B9C74781351 37.79690 -121.58550 Monthly 1stWednesday
MokelumneR@BensonFerry B9D81531264 38.25461 -121.43658 Monthly 1stTuesday
NatomasEastMainDrainage
Canal A0V8367128038.61110 -121.467300 Monthly 1
stMonday
OldR@BaconIsland B9D75811344 37.96910 -121.57290 Monthly 1stMonday
RockSlough@CCWDFish
Facility B9C7586138537.99550 -121.70180 Monthly 1
stMonday
SacramentoR@Hood B9D82211312 38.36691 -121.52037 Monthly 1stTuesday
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SiteName SiteCode
Target
Latitude
Target
Longitude
Sampling
frequency
Sampling
Day
SacramentoR@WestinBoat
Dock B9D8322131038.53003 -121.53091 Monthly 1
stTuesday
SanJoaquinR@
Vernalis/AirportWay B070200037.67556 -121.26417 Monthly 1
stTuesday
8. Sampling Methods
Thequalityofsamplescollectedinthefieldisaddressedthroughanumberofprocedures.
Properselectionofequipment,suppliesandtrainingforuseofthoseitemsensuresthat
collectionproceduresandmaterialsdonotorminimallyaffectsamples.Collectionandanalyses
ofappropriatequalitycontrolsamplesallowsmeasurementandassessmentofartifactsor
influencesofsamplingonsamplecharacteristics,todifferentiateuncertaintiesandvariability
introducedbythesamplingprocessfromthoseinherentinthemonitoredsystem.Thissection
willdescribequalityassuranceandqualitycontrolproceduresimplementedfortheDeltaRMP.
8.1. FieldEquipmentandSupplies
Samplingequipmentandsupplieswillvarydependingontheprojectelement.Sample
containersappropriatetothematricesbeingsampledandtheanalysestowhichtheywillbe
subjectedwillbechosen.Allcontainersshouldmeetorexceedtherequiredtracelimits
establishedbytheUSEPAinthedocumentEPA/540/R-93/051,SpecificationsandGuidancefor
Contaminant-FreeSampleContainers.Chemical-resistantpowder-freenitrileandpolyethylene
gloveswillbewornandclean-handsdirty-handsprotocolswillbefollowedtominimize
contaminationofexposedsamples.Fieldcleaningproceduresofsamplingequipmentwillbe
employedtominimizecross-contaminationbetweensamplesfortheparametersofinterest.
FieldpersonnelwillrefertothedetailedworkplanfortheappropriateDeltaRMPsampling
elementtoensurethatallequipmentandsuppliesarebroughtinthefield.However,ata
minimumthefollowingsuppliesarerequiredfortherespectiveprojectelements:
Fish
Boats(electro-fishingand/orforsettingnets)
Waterprooflabels
Bonesaw,gillnets(varioussizes),filetknives,fishpicks,shackles,pliers,
sharpeningstone
Rodandreels,bait,tacklebox,landingnet,livebaitcontainer
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Plasticicechests,inflatablebuoy,floats,anchorchains,anchors,patchkit
Heavy-dutyaluminumfoil(prepared),zipper-closurepolyethylenebags
Ottertrawls
Blocks
Measuringboards,tapemeasure,idkeys,Tefloncuttingboards
Rodandreels,landingnet
Water
Samplingcontainersandlabels
Collectiondevicesappropriateforsite
Powder-freenitrilegloves
Fieldmeters
Deionizedwatersquirtbottle
Fieldsheet(seeAppendixE)
Coolersandice
Chain-of-custodyform(seeAppendixF)
8.2. FieldSampleCollectionandQualityAssuranceProcedures
8.2.1. SurfaceWaterSampleCollection
Samplesforpesticidemonitoringarecollectedmonthlyasgrabsamples0.5metersbelow
surface.SpecifictargetedeventssamplingdescribedinTable8.1willreplaceroutinemonthly
samplecollectionasappropriate.Thetriggersandcriteriaforeventssamplingaresummarized
inTable8.1.
Watersamplesformercurymonitoringarecollectedquarterly.
TheDeltaRMPPathogenStudyDesignSummaryspecifiesmonthlyambientmonitoringsample
collectionfortwoyearsbeginninginApril2015tomatchtheLongTerm2EnhancedSurface
WaterTreatmentRule(LT2)-requiredwatersupplyintakesamplecollection.MWQIwillcollect
grabsamplesateachofthelocationsshowninFigure7.2duringthefirstweekofeachmonth
onthesite-specificday.Thespecifiedsamplecollectiondepthforthepathogensamplingis1
meter/3feet.MWQImaypostponeorcancelsamplecollectionduetosafetyorlogistical
concerns.
ReferencesandlinksforaccessingSOPsforsurfacewatersamplecollectionareprovidedin
AppendixD.
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Table8.1. Samplingeventtriggersforpesticideeventssampling.
Event SamplingTriggers Criteria Notes
Wet
1stseasonalflush
(WaterYear)
• Guidanceplotsprojectsignificantincrease(~25%)in
flowatfoursites:lower
SacramentoRiver,lower
AmericanRiver,SanJoaquin
RiveratVernalis,and
MokelumneRiver.
• Precededby>30daysdryweather(SacSW
criteria).
• Sampleeventstohitallsitesin1to2days.
• WhenfavorablestormconditionsandrunoffareforecastcoordinatedirectlywithAHPlab.
• AlertAHPL7daysinadvanceofupcomingstormfororganismpreparationand2daysinadvanceaboutlikelihoodofadequateprecipitation
Significant
winterstorm
• Guidanceplotsprojectsignificantincrease(~25%)at
foursites:lowerSacramento
River,lowerAmericanRiver,
SanJoaquinRiveratVernalis,
andMokelumneRiver.
• Minimum2weeks
since1stflushsample
event.
• Ifcollectmorethan1eventsampleinthesamemonth,donotsampleinfollowingmonth.
• WhenfavorablestormconditionsandrunoffareforecastcoordinatedirectlywithAHPlab.
• AlertAHPL7daysinadvanceofupcomingstormfororganismpreparationand2daysinadvanceaboutlikelihoodofadequateprecipitation
Dry
EarlySpring • Notriggers,cansampleina
particularmonth(March-
April).
• None • Meanttocapturesnowmeltbutrecognizesignificantimpactofupstreamdams.
• CoordinatesamplingschedulewithAHPlab7ormoredaysinadvance.
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Event SamplingTriggers Criteria Notes
1stirrigation
seasonsampling
(latespring/
earlysummer)
• Notriggers,cansampleina
particularmonth(May-June).
• None • Meanttocapturelatewinterandspringpesticideapplications(poststorms).
• Accountforplanting/pesticideapplicationtiming.
• CoordinatesamplingschedulewithAHPlab7ormoredaysinadvance.
2ndirrigation
seasonsampling
(latesummer)
• Notriggers,cansamplea
particularmonth(August).
• None • Meanttocapturesummerpesticideapplications(rice,etc.).
• Accountforplanting/pesticideapplicationtiming.
• CoordinatesamplingschedulewithAHPlab7ormoredaysinadvance.
Collectionofwatersamplesforanalysisofpesticidesandtoxicitytesting:
USGSpersonnelwillcollectwatersamplesforanalysisofpesticides,dissolvedcopper,and
toxicitytesting.Atsiteswherestreamflowisaffectedbytides,sampleswillbecollectedonthe
ebbtide.Duetothelargevolumesofwaterrequiredpersite,perevent(40litersfortoxicity
testingand2-4litersforpesticideanalyses),allsampleswillbecollectedasgrabsamples.
Waterwillbecollectedbysubmergingpre-cleaned4liter(toxicity),1liter(pesticides)
combustedamberglassbottles,andacidrinsed3literTeflonbottles(copper,DOCandPOC)0.5
metersbelowthewatersurface(Table8.2).Samplebottlesfordissolvedcopperwillberinsed
threetimeswithsitewaterpriortofilling,andcontainerswillbefilledcompletely,leavingno
headspace,tominimizevolatilization.
Theamountofwatertobefilteredinordertoobtainasufficientquantityofmaterialforthe
POCanalysisdependsonthesuspended-sedimentconcentrationand/ortheconcentrationof
humicandothersubstancesthatcausecoloredwater,suchasorganicandinorganiccolloids.
Approximatesuspended-materialsconcentrationvolumeofsampletobefiltered(mL):
Suspendedmaterials
concentration(mg/L)
Volumeofsample
tobefiltered(mL)
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1–30 250
>30–300 100
>300–1,000 30
>1,000 10
Number,typeandtimingoffieldcollectedQA/QCsampleswillbedeterminedbytheUSGS
OCRLandwillmeetorexceedSWAMPguidelines
(http://www.waterboards.ca.gov/water_issues/programs/swamp/docs/mqo/6_syn_water.pdf.
Measurementsofbasicfieldparameters(temperature,pH,specificconductance,dissolved
oxygenconcentration,dissolvedoxygensaturation,andturbidity)willbemadeatthetimeof
samplecollectionusingaYSI6920V2multiparametermetercalibratedwithappropriate
standards.
Collectionofwatersamplesforanalysisofmercuryandmethylmercury:
MPSLpersonnelwillcollectwatersamplesforanalysisofunfilteredandfilteredtotalmercury,
unfilteredandfilteredmethylmercury,andancillaryparameters.Duringannualeventswhen
fishsamplingoccurs,watersampleswillbecollectedafterfisharecollected.Sampleswillbe
collectedaccordingtoMPSLFieldSOPv1.1;ultratrace-leveltechniquesforequipmentcleaning
andsamplecollection(USGSNationalFieldManual,ChapterA5.6.4.B.LowLevelMercury);and
theclean-handsdirty-handscollectionmethodswhereappropriate.Itisimportanttofollowthe
clean-handsdirty-handscollectionmethodwhencollectingtotalandmethylmercurysamplesto
avoidsamplecontamination.Adepth-integratedsamplewillbecollectedfromaboatatthe
pointinthechannelwheredischargeisthegreatest(Table8.2).Samplecollectionwilloccurin
anareawheretheboatdoesnotinterferewiththesample,withthecollectorwearingclean
polyethylenegloves.
Number,type,andtimingoffieldcollectedQA/QCsampleswillbedeterminedbyMPSLandwill
meetorexceedSWAMPguidelines(Table4.3)
Samplecontainerswillconsistof4-Lclearglassbottles(Table8.2).Sampleswillbeprocessed
andfilteredinthelab(MPSL).
Collectingandprocessingwatersamplesforanalysisofmercuryatalow(subnanogramper
liter)levelrequiresuseofultratrace-leveltechniquesforequipmentcleaning,sample
collection,andsampleprocessing.
Section9.1.describesfieldsamplehandlingandshippingproceduresandTable9.1.provides
informationonstorageandholdtimerequiremtns
CollectionofwatersamplesforanalysisofLT2pathogens:
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SampleswillbecollectedfortheDeltaRMPPathogenStudyfollowingthegeneralfield
proceduresdescribedintheMunicipalWaterQualityInvestigations(MWQI)ProgramField
Manual.SpecificprotocolsforCryptosporidiumandGiardiasamplingfollowEPAMethod1623.
MWQIwillcollectonefieldduplicatesamplepereventonasequentiallyrotatingsiteschedule.
MWQIwillfillone10-Lcubitainerforeachsampleandshippedtothelaboratoryonicefor
analysisbyEPAMethod1623(Holdtime:96hours).
MWQIwilluseastainlesssteelbucketandastainlesssteelfunnelforgrabsampling.MWQIwill
rinsesamplingdevicestwicewithambientwaterpriortosampling.Samplingdeviceswillbe
decontaminatedbetweensitesbyrinsingwithde-ionizedwater.MWQISampleCollection
Teamswillfilloutfielddatasheetsimmediatelyaftersamplecollection.Allsamplecontainers
willbelabeledwiththedate,locationsampledoruniquesiteID,parametertobemeasured,
andsamplepreparation(unfiltered).
Table8.2. Samplecontainertypeandvolumeusedforeachparametergroupforcollectionof
watersamples.(Section9.1providesmoreinformationonfieldsamplehandlingandshipping
procedures.Table9.1providesinformationaboutstorageandholdtimerequirementsforeach
parametergroup.)
Program
Element ParameterGroup Bottletype*
Numberofbottles/event
Sample
Volume/Site
Mercury
Tracemetals
Conventional12 Clearglass 5 4L
Pathogens Pathogens
LDPE
cubitainer 15 950mL
Pesticides Watertoxicity Amberglass 40
4L/bottlex8
bottles
Pesticides Pesticides Amberglass 5 1L
Pesticides DOC/POC Amberglass 5 125mL
Pesticides Copper Teflon 5 3L
8.2.2. FishSampleCollection
Sportfishsamplesformercurymonitoringarecollectedannually.Theappropriatesample
collectionmethodmayvarybysiteandwillbedeterminedbytheMPSLfieldsamplecollection
team.
ReferencesandlinksforaccessingSOPsforfishsamplecollectionareprovidedinAppendixD.
12Conventionalparameters(DOC,TSS,VSS)willbeanalysedinsamplealiquots.
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Collectionoffishtissuesamplesforanalysisoftotalmercury:
FishwillbecollectedinaccordancewithMPSL-102a,Section7.4.Becausehabitatsmayvary
greatly,thereisnoonemethodofcollectionthatisappropriate.Fieldcrewswillevaluateeach
fishingsitetodeterminethecorrectmethodtobeemployed.Potentialsamplingmethods
include,butarenotlimitedto:electroshocking,seining,gillnetting,andhookandline.Field
crewwilldeterminetheappropriatecollectionmethodbasedonphysicalsiteparameterssuch
asdepth,width,flow,andaccessibility.Fieldcrewwillindicatethecollectionmethodondata
sheets(AppendixE).
Thetargetedfishspeciesislargemouthbass.Thegoalistocollect11individualsspanninga
rangeoftotallengthfrom200-500mmateachsite(Table8.3).Specimensofsimilarpredator
speciesmaybecollectedifthedesirednumberofindividualsoftheprimarytargetfishspecies
inthedesiredsizerangecannotbecollectedatasite.
FurtherdetailsonsamplecollectioncanbefoundinMPSL-102a,Section7.4(seeAppendixD
forreferenceandlink).
Table8.3. Targetspecies,numberofindividuals,andsizerangesforcollectionoffishtissue
samples.
Program
Element
Parameter
Group PrimaryTarget1
Numberof
Individuals
Individuals/
Site(Size)
Mercury Mercury LargemouthBass 66
11total:2X(200-249
mm),2X(250-304mm),
5X(305-407mm),
2X(>407mm)
1Collectsimilarpredatorspecies(e.g.,smallmouthbass,Sacramentopikeminnow)ifprimarytargetisnotavailable.
8.3. CorrectiveAction
FieldSampling
Ifgoalsstatedforthecollectionofsamplesorthemeasurementofwaterqualityparameters
arenotachieved,sampleswillberecollectedormeasurementsrepeated,wherepossible,after
necessaryre-calibrationsofequipmentorre-evaluationofthesamplingscenario.Allnecessary
stepsforcorrectiveactionwillbedocumentedonthefieldformandonenteredintothe
electronicversionoftheFieldSamplingReportthatismaintainedbySFEI-ASC.Theindividuals
responsibleforassuringthatthefieldstaffareproperlytrainedandimplementtheField
SamplingSOPsaretheFieldCollectionCoordinators(i.e.,MPSLProjectCoordinator,MWQI
SampleCollectionTeamLead,andUSGSSamplingCoordinator),SFEI-ASCProjectManager,and
theQAOfficer.
Fieldsamplingqualitygoalsincludethemeetingofdataqualityobjectivesfor:
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• Completenessofsamplecollection
• Representativeness
• Accuracyandprecision(asindicatedbyfieldduplicates)
• Avoidanceofcontamination(asindicatedbyfieldblanks,equipmentblanks,andtravel
blanks)
Ifanydataindicatethatqualityobjectivesarenotbeingmet,FieldCollectionCoordinatorswill
consultwiththeirPrincipalInvestigator(ifapplicable),LaboratoryManager,andtheSFEI-ASC
QAOtodetermineifthefailureismostlikelyduetofieldorlaboratoryprocedures/methods.If
itisdeterminedthatfieldmethodsarethelikelycause,thePIwillworkwiththefieldsampling
teamtoensurethatprotocolsarebeingfollowedcorrectlyandifanyadditionalprotocols
(specifictothisproject)needtobeimplemented.
LaboratoryChemicalAnalyses
Ifchemicalanalyticallaboratoryresults13failtomeettheQArequirementsoutlinedintheDelta
RMPQAPPanditisdeterminedthatlaboratoryproceduresarethelikelycause,thenthePI(if
applicable)andLaboratoryManagerwillensurethatproperproceduresasoutlinedintheQAPP
arebeingimplementedandtodevelopanyadditionalprocedurestobringQAsampleresultsin
linewithmeasurementqualityobjectives.Correctiveactionswillbedocumented,resolved,and
followed-uponfollowingtheprocessforcorrectiveactionsthatisoutlinedbytheSWAMP.The
processisbasedontheSWAMPCorrectiveActionForm,andisappliedtosampleresultsthat
failtomeetthetechnicalandnon-technicalrequirementsofSWAMPanditsassociated
projects.
ToxicityTesting
DataQualityIndicatorsandtestacceptabilitycriteriafortoxicitytestingarelistedinTables4.7
and4.8,respectively.MQOsandTIEtriggersaresummarizedinTable4.9and4.10.TheAHPL
QAOwillbealertedwhenthesethresholdsareexceeded.TheAHPLQAOmaytakethe
followingactions,ifapplicable:
Ammonia:Whenasample’sammonia-nitrogenmeasurementexceeds5mg/L,theambient
samplemayberetestedatdifferentpHlevelstodeterminewhateffectammonia-nitrogen
levelshaveontestorganisms.Commensuratecontrolswillbeincludedanddataanalysiswill
followtheguidelinesprovidedandlistedinSWAMPChronicFreshwaterToxicityTestingQuality
ControlTable.
Conductivity:Whenasample’sconductivitymeetsorexceedstheacceptabilitythresholdfor
eachspecies,ahighorlowconductivitycontrolwillbeincludedinthetesttodetermine
13Includingchlorophylla.
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whetherhighorlowconductivitymayhavearoleinreducedmortality,growthorreproduction.
Alternatecontrolswillbenotedinthetoxicitytransformerworkbookandstatistical
comparisonswillfollowEPAandSWAMPguidelines.
DissolvedOxygen:Whenasample’sdissolvedoxygenexceeds8.6mg/L(forS.capricornutum,
C.dubiaandP.promelas;8.9mg/LforH.azteca)followingthesamplewarmingperiod,the
samplewillbegentlyaeratedpriortosamplerenewal,inordertodegasharmfuldissolved
gases.Ifasample’sdissolvedoxygenlevelislessthan4.0mg/L,theambientsamplewillbe
constantlyaeratedtoensureadequateoxygenlevelsforthedurationofthetest,aswellas
includingaconcurrentaerationcontrol.Dataanalysiswillfollowtheguidelinesprovidedinthe
SWAMPChronicFreshwaterToxicityTestingQualityControlTable.
pH:Whenasample’spHisbelow6orexceeds9,thesamplewillbetestedatitsoriginalpHand
alsoadjustedto7.5.ApHmethodblankwillalsobetestedthatincludesanadjustmenttothe
ambientsample’soriginalpHandthenreturnedto7.0.Dataanalysiswillfollowtheguidelines
providedintheSWAMPChronicFreshwaterToxicityTestingQualityControlTable.
Temperature:Sampletemperaturesmustnotdeviatebymorethan3°Cofthetargettest
temperatureforthedurationofthetest.Ifsampletemperaturesexceedthisrange,stepswill
betakentominimizesampletemperaturedeviations,suchasadjustingenvironmentalchamber
temperaturestoatighterrangeormovingatestintoamoretemperature-regulatedtesting
area,anddatawillbeflaggedaccordingly.
Toxicity:Ifasampletestspeciesexhibits>50%mortalitywithin96-hours,theAHPLQAOor
LaboratoryManagerwillcontacttheSFEI-ASCProjectManagerwithin24hourstodiscuss
potentialafollow-upwithatoxicityidentificationevaluationinordertodeterminewhatclass
ofchemical(s)iscausingtoxicity.TheDeltaRMPTAC’sTIEsubcommitteewilldecidepotential
TIEs.
Ifasampletestspeciesexhibits100%mortalityin48hours,theAHPLQAOorLaboratory
ManagerwillcontacttheSFEI-ASCProjectManagerwithin24hours,andadilutionseriestest
willbesetupassoonasorganismsareavailable(potentialcourierlimitations).
TestsareconductedaccordingtoproceduresandconditionsasdescribedintheSOPsprovidein
AppendixD.Beyondthoseidentified,deviationsfromtheserecommendedconditionsare
reportedtotheUCDAHPLQAO.ThePIandSFEI-ASCQAOandProjectManagerwillbenotified
ofthesedeviations.
IntheeventofanSOP/QAPPdeviationorcorrectiveaction,adeviation/correctiveactionform
willbeprepared,completed,signedandtheSFEI-ASCQAOandProjectManagernotified.Best
professionaljudgmentwillbeusedininterpretationofresultsobtainedwhenprotocol
deviationshaveoccurred.Alldeviationsandassociatedinterpretationswillbereportedin
interimandfinallaboratoryreports.ProtocolamendmentswillbesubmittedtotheSFEI-ASC
QAOandProjectManager.Uponapproval,protocolamendmentswillbeemployed.
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FailuretomeetIPRorOPRqualitycontrolacceptancecriteriaindicatessystemicproblemsthe
laboratorymustaddresspriortoprocessinganysamples.
9. Sample Handling and Custody
9.1. FieldSampleHandlingandShippingProcedures
Pesticides
Samplecontainerswillbelabeledwiththelocation,date,andtimecollectedandpackedinice
chestswithsufficientweticetomaintainsampletransportcriteria.Fieldsheetsandchain-of-
custodyforms(COC)willbefilledoutatthetimeofcollectionandwillincludesiteID,site
description,collectiondate/time,containertype,samplepreservation,fieldwaterchemistry
measurements,sampler(s)nameandrequestedanalyses.Allformswillbeincludedwiththe
appropriatesamplesduringshipping.Samplesforpesticideanalysiswillbedeliveredtothe
USGSOCRLlaboratoryinSacramentoCalifornia.IfuponarrivalattheOCRLsamplesarefound
tobewarm(icemelted)orifsamplecontainersarebrokentheProjectManagerandPrincipal
Investigatorwillbeimmediatelynotified.Icechestsareexaminedupondeliverytoensurethat
sampleshavebeenproperlychilled(acceptabletemperaturerange=0-6°C).
Watersamplesforpesticideanalyseswillgenerallybeprocessedtoextractionuponarrivalat
theOCRL.Ifthisisnotpossible,thesampleswillberefrigeratedat0-6°Cinthedarkfora
periodnottoexceedtheOCRLholdingtimerequirementof48hoursbetweensample
collectionandextraction.Uponarrivalofsamples,appropriatelaboratoryprocessingforms
notinguniquelaboratoryID,sitename,collectiontimeanddate,receivingtechnician’sname,
requestedanalysis,anddateandtimeofreceiptwillbefilledout.SignedcopiesofCOCswillbe
maintainedwiththeappropriateOCRLfieldandlaboratoryforms.
SamplesfordissolvedcopperanalysisandDOC/POCanalysiswillbeprocessedattheUSGS
OCRL,within24hoursofcollection.Samplesfordissolvedcopperanalysiswillbefilteredusing
0.45-micrometer(μm)filtersandacidifiedtopHlessthan2with2mlof7.5Nnitricacid.
SamplesforDOCanalysiswillbefilteredusing0.7-umporesize,pre-combustedglass-fiber
filters,collectedin125-mLbakedamberglassbottles,andacidifiedusing4.5Nsulfuricacid.The
0.7-umporesizefilterholdingtheretainedsuspendedmaterialwillbeusedforthePOC
analysisandwillbewrappedinanaluminumfoilsquareofappropriatesize.
Samplesfordissolvedcopper,DOC,andPOCwillbeplacedinacooleronweticeandshipped
overnighttotheUSGSNWQLinLakewood,CO.
Receipttemperatureandsamplecondition(broken/compromisedcontainers,incorrect
preservatives,holdingtimeexceedance,etc.)willberecordedbyreceivinglaboratories.
ToxicityTesting
ToxicitytestsampleswillbedeliveredtotheUCDavisAHPLaboratoryinDavis,California,
within24hoursofsamplecollection.UponarrivalatAHPL,toxicitytestingsampleswillbe
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immediatelyremovedfromtheice-chestsandthelaboratorystaffreceivingthecoolerswill
completetheaccompanyingCOC.TheAHPLwillinitiatetestswithin36hoursofsample
collection,althoughunderrarecircumstances,thisholdingtimemaybeextendedto120hours
forprecipitation-basedevents,whencourierdeliveryschedulesonweekendsandholidayslimit
theavailabilityoftestorganisms.IntheseinstancestheAHPLwillcontacttheSFEI-ASCQAO
andProjectManager,andassociateddatawillbeflaggedininterimandfinalreports.
Table9.1providesinformationaboutstorageandholdtimerequirementsforeachparameter
group.
Table9.1. Storageandholdtimerequirementsforeachparametergroup.
Parametergroup Storage
Holdtime
(CollectiontoExtraction,
whereapplicable)
Holdtime
(Extractiontoanalysis,
whereapplicable)
Storage
(Extractiontoanalysis,
whereapplicable)
Chlorophylla 0-6°Cindark
Filtrationwithin24hours
ofcollection 28days -20°Cindark
Copper,dissolved 0-6°Cindark
Filterinthefieldassoonas
possibleaftercollection 180days 0-6°Cindark
DOC/POC 0-6°Cindark
Filtrationwithin24hours
ofcollection
DOC:30days/POC:
100days 0-6°Cindark
Mercury,total
(Water) 0-6°Cindark
Preservewith0.5%v:v
pretested5%BrClor12N
HClwithin48hoursof
collection 90days Roomtemperature
Mercury,total
(Tissue) 0-6°Cindark
Coolto<6°Cwithin24hrs
ofcollection 1year -20°C
Mercury,dissolved
(Water) 0-6°Cindark
Filterandpreservewith
0.5%v:vpretested12NHCl
within48hoursof
collection 90days Roomtemperature
Methylmercury,
total
(Water) 0-6°Cindark
Preservewith0.5%v:v
pretested12NHClwithin
48hoursv 6months 0-6°Cindark
Methylmercury,
dissolved
(Water) 0-6°Cindark
Filterassoonaspossible
aftercollection;preserve
with0.5%v:vpretested
12NHClwithin48hoursof
collection 6months 0-6°Cindark
Pesticides 0-6°Cindark
Extractwithin48hoursof
collection Nottoexceed30days -20°Cindark
Toxicity 0-6°Cindark
InitiateTest36hafter
samplecollection NA NA
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Pathogens 1˚-20˚C
Elutewithin96hofsample
collection
7daysfrom
completionofslide
preparation 1˚-20˚C
Mercury
Samplecontainerswillbelabeledwiththelocation,date,andtimecollectedandpackedinice
chestswithsufficientweticetomaintainsampletransportcriteria.Fieldsheetsandchain-of-
custodyforms(COC)willbefilledoutatthetimeofcollectionandwillincludesiteID,site
description,collectiondate/time,containertype,samplepreservation,fieldmeasurements,
sampler(s)name,andrequestedanalyses.Allformswillbeincludedwiththeappropriate
samplesduringshipping.SampleswillbedeliveredtoMPSLinMossLanding,CA,orWPCLin
RanchoCordova,CA,asappropriate.Ifuponarrivalateitherlaboratory,samplesarefoundto
bewarm(icemelted)orifsamplecontainersarebrokentheProjectManagerandPrincipal
Investigatorwillbeimmediatelynotified.Icechestsareexamineduponreceipttoensurethat
sampleshavebeenproperlychilled(acceptabletemperaturerange=0-6°C).
WatersampleswillbedeliveredtoeitherMPSLorWPCLwithinrequisiteholdingtimes,where
laboratorypersonnelwillfilterpreservewatersamplesfollowingTable9.1.
Uponarrivalofsamples,appropriatelaboratoryprocessingformsnotinguniquelaboratoryID,
sitename,collectiontimeanddate,receivingtechnician’sname,requestedanalysis,anddate
andtimeofreceiptwillbefilledout.Samplesfordissolvedmercuryanddissolved
methylmercuryanalysiswillbefilteredusing0.45-micrometer(μm)filtersandacidifiedto0.5%
withpre-testedBrClasappropriatewithin48hoursofcollection.
Samplesforchlorophyllaanalysiswillbecollectedandfilteredusingasyringesamplemethod
within24hoursofcollection.Sampleswillbefilteredbyforcingwaterwitha60-mLsyringe
throughafilterholdercontaininga25-mmglassmicrofiberfilter.The60-mLsyringeandanin-
linefilterholderarerinsedthreetimeswiththeambientwaterbeforefiltration.Thesyringeis
thenfilledwith60mLofambientwater.Thefilterholderisthenremovedanda25-mmglass
microfiberfilterisplacedinside.Thefilterholderisthenscrewedontothesyringeandthe
ambientwateristhenflushedthroughthefilter.Thefilterholderisremovedeverytimemore
waterneedstobedrawnintothesyringe.Theprocessisthenrepeateduntilthedesired
amountofchlorophyllaispresent(usually60to360mLdependingonthewaterclarity).When
filteringiscomplete,thefilterholderisopenedandthefilterisremovedwithtweezerswithout
touchingthechlorophylla.Thefilteristhenfoldedinhalf,thenagain,inhalfwiththechlorophyllainsidethefolds.Thefoldedfilteristhenwrappedinaluminumfoilandplacedin
anenvelopelabeledwiththesiteinformationandthevolumefiltered.Theenvelopeisthen
immediatelyplacedondryiceuntiltransferredtoWPCL
Receipttemperatureandsamplecondition(broken/compromisedcontainers,incorrect
preservatives,holdingtimeexceedance,etc.)willberecordedbyreceivinglaboratories.
FishwillbeprocessedaccordingtoMPSL102a,exceptwherenotedhere.Collectedfishwillbe
partiallydissectedinthefield.Atthedock,thefishisplacedonameasuringboardcovered
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withcleanaluminumfoilorplastic;forkandtotallengtharerecorded.Weightisrecordedifthe
fishislargeenoughforthescale.Thefishwillthenbeplacedonthecoveredcuttingboard,
wherethehead,tail,andgutsareremovedusingacleancleaver(scrubbedwithMicro™,rinsed
withtapanddeionizedwater).ThefishcrosssectionistaggedwithauniquenumberedID,
wrappedinaluminumfoil,andplacedinacleanlabeledbag.Whenpossible,parasitesandbody
anomaliesarenoted.Thecleaverandcuttingboardarere-cleanedwithMicro™,rinsedwithtap
anddeionizedwaterbetweenfishspecies,persiteifmultiplestationsaresampled.
FurtherdetailsonsamplecollectionandprocessingcanbefoundintheSAP(SeeAppendixD
forreferenceandlink).
Fishsampleswillbewrappedinaluminumfoilandfrozenondryicefortransportationtothe
laboratory,wheretheywillbestoredat-20°Cuntildissectionandhomogenization.Lab
homogenateswillbefrozenuntilanalysisisperformed.Frozentissuesampleshavea12-month
holdtimefromthedateofcollection.Ifahold-timeviolationhasoccurred,datawillbeflagged
appropriatelyinthefinalresults.HoldingtimesforeachanalytecanbefoundinTable9.1.
Pathogens
AcourierwilldeliversamplestoBiovir(primarylab).Eurofinswillpickuponefieldduplicate
sampleperevent(secondarylab).Samplesmustbekeptonice.Thelaboratoriesmustelutethe
sampleswithin96hours(4days)ofsamplecollection.
10. Analytical Methods
10.1. FieldAnalytical/MeasurementMethods
Thefieldcollectionteamswillrecordmeasurementsperformedinthefieldonfieldsheets
(electronicorpaper)thenenterthemintoaCEDENtemplateforsubsequententryintheDelta
RMPdatabasebySFEI-ASC.Samplescollectedinthefieldaretobeplacedincontainersand
storedunderconditionsappropriatefortheanalysestobeperformed.Anyunusualsample
characteristicsorcircumstancespreventingnormalsamplehandlingwillalsobenotedinthe
fieldsheet.Onreturnfromthefield,thesamplingcrewwillpreparesamplesforimmediate
shippingtoanalyticallaboratoriesorstorethemunderappropriateconditionsforsubsequent
shipping
Tominimizediscrepancyinfieldresultsandprovideuseful,accuratescientificdata,all
personnelparticipatinginfieldsamplingarerequiredtofollowtheguidelinessetoutinthe
USGSNationalFieldManualfortheCollectionofWater-QualityData(forpesticideelement),
theMPSLFieldSOPv1.1(formercuryelement),andtheMWQIProgramFieldManual(for
pathogenstudy).
Operationofanyfieldinstrumentsshouldbecheckedatleastonedaybeforesampling.If
failureofaninstrumentshouldoccur,abackupinstrumentshouldbecheckedandcalibrated.
Allsamplingandmeasurementmodificationsorfailuresthatoccurinthefielddueto
instrumentmalfunctionwillberecordedontheFieldFormandtheFieldReferenceSheet.The
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FieldCollectionCoordinators,SFEI-ASCProjectManager,andtheQAOwillberesponsiblefor
ensuringthatstaffdocumentsalldeviationsfromplannedoperationsandschedulerepairs
and/oradditionaltrainingasneeded.
10.2. LaboratoryMethods
Forthemethodsselectedforaparticularapplication,theLaboratoryProjectManagermustbe
abletodemonstrateanddocumentthatthemethodsperformancemeetsthedataquality
requirementsoftheproject.Twoseparatefactorsareinvolvedindemonstratingmethod
applicability:First,demonstratingthatthelaboratorycanperformthemethodproperlyina
cleanmatrixwiththeanalyticalsystemundercontrol,andsecond,demonstratingthatthe
methodselectedgenerates“effectivedata”inthematrixofconcern.Theformeraddresseslab
oroperatortrainingandproficiency,whilethelatterdemonstratesthattheselectedmethod
performswiththeappropriateselectivity,sensitivity,biasandprecision,intheactualanalytical
matrix,toachieveprojectgoals.
Table10.1providesasummaryofanalyticalmethodsandinstrumentsusedbytheDeltaRMP.
Table10.1. Summaryofanalyticalmethodsandinstruments.
Parametergroup Methods Instrument Proprietary?
Chlorophylla InVitrodeterminationbyvisible
spectrophotometry(EPA446.0)Genesis10S No
Copper,dissolved
Collision/reactioncellinductively
coupledplasma–massspectrometry
(USGSTM-5-B1)
cICP-MS
(Agilent7500ce)No
DOC
UVcatalyzedpersulfateoxidationand
infrared(IR)spectrometry(USGSTest
MethodO-1122-92)
CarbonAnalyzer,
DohrmannDC-80,
DC-180,or
equivalent,witha
directconcentration
read-out.
No
DOCOrganicCarbon,Total(Combustionor
Oxidation)(EPA415.1)
TeledyneTekmar
TOCTorchNo
Mercury(Tissue)
Thermaldecompositionamalgamation
andatomicabsorption
spectrophotometry(EPA7473)
MilestoneDMA80 No
Mercury(Water)
Oxidation,purgeandtrap,andcold
vaporatomicfluorescence
spectrometry(EPA1631,RevisionE)
Tekran2600 No
Methylmercury
(Water)
Distillation,aqueousethylation,purge
andtrap,andcoldvaporatomic
fluorescencespectrometry(EPA1630)
Tekran2700 No
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Parametergroup Methods Instrument Proprietary?
POC Elementalanalysis(EPA440.0)
CarbonAnalyzer,
DohrmannDC-80,
DC-180,or
equivalent,witha
directconcentration
read-out.
No
Pesticides14
GasChromatography/Mass
Spectrometry
(USGSTM-5-B1)
Agilent7890GCwith
a5975cmass
spectrometerwitha
DB-5mscolumn(30
m×0.25mm×
0.25µm,Agilent)
No
PesticidesLiquidchromatographywithtandem
massspectrometry(LC/MS/MS).
Agilent1260HPLC
coupledtoa6430
tandemMSsystem
withaZorbaxEclipse
XDB-C18column(2.1
mm×150mm×3.5
mm;Agilent).
No
10.2.1. LaboratorySOPs
AllanalyticalmethodSOPscanbedownloadedfromtheSFEI-ASCGoogleDrive,unlesstheSOPs
areproprietary.CopiesoflaboratorySOPsarealsostoredatSFEI-ASCbutcannotbereleasedto
anyexternalpartieswithoutpriorconsentofthelaboratorywhentheyaremarkedas
proprietary.
10.2.2. CorrectiveActionsProcedures
CorrectiveactionsproceduresforanalyticallaboratoriesaresummarizedinTable10.2.
AdditionaldetailsaredescribedinSection4.3.
Table10.2. Correctiveactionsproceduresforanalyticallaboratories.
14 SeeTable3.2foradetailedlistoftargetanalytesforeachmethod
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LaboratoryQCSampleType Correctiveaction
MatrixSpikes
Thespikinglevelshouldbenearthemidrangeofthe
calibrationcurveoratalevelthatdoesnotrequiresample
dilution.Reanalyzethematrixspiketoconfirmtheresult.
Reviewtherecoveryobtainedforthematrixspike
duplicate.ReviewtheresultsoftheotherQCsamples(such
asreferencematerials)todetermineifotheranalytical
problemsareapotentialsourceofthepoorspikerecovery.
FieldBlanks
Iftargetanalytesarefoundinfieldblanks,samplingand
handlingprocedureswillbereevaluatedandcorrective
actionstaken.Thesemayconsistof,butarenotlimitedto,
a)obtainingsamplingcontainersfromnewsources,b)
trainingofpersonnel,c)discussionswiththelaboratory,d)
invalidationofresults,e)greaterattentiontodetailduring
thenextsamplingevent,orf)otherproceduresdeemed
appropriate.
FieldReplicate
Ifcriteriaareexceeded,fieldsamplingandhandling
procedureswillbeevaluatedandproblemscorrected
throughgreaterattentiontodetail,additionaltraining,
revisedsamplingtechniques,orotherproceduresdeemed
appropriatetocorrecttheproblems.
10.3. SampleArchiveandDisposal
ProjectsampleswillnotbedisposedofuntilallanalysesarecompleteandanalyticalandQC
resultshavebeenreviewedandapprovedbytheProjectManagerandtheQAO.
11. Instrument/Equipment/Supplies
ContractlaboratoriesmaintainequipmentinaccordancewiththeirrespectiveSOPs,which
includethosespecifiedbythemanufacturerandthosespecifiedbythemethod.Underthe
performance-basedapproach,theadequacyofcontractlaboratorytesting,inspection,and
maintenanceproceduresaredeterminedthroughregularreviewofresultsforanalysisoffield
andQCsamplesforallsubmitteddata.
Priortouseinthefield(typicallywithin24hourspriortosampling),handheldwaterquality
instrumentsarecalibratedagainstappropriatestandardsand,ifpossible,checkedagainsta
standardfromadifferentsource.Forsomemeasurementssuchasdissolvedoxygen,probesare
oftencalibratedtoambientconditions(water-saturatedair)ratherthantoknownstandards.In
suchcases,thefieldstaffshouldverifyappropriatequalitativeinstrumentresponse(e.g.in
waterdeoxygenatedbysparging,sodiumsulfiteaddition,orothermeans).Allcalibrationsare
documentedonacalibrationchecklistontheindividualinstrumentoritscasewithdate,time,
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andoperatorname.Ifaninstrumentcannotbecalibratedorisnotreadingcorrectly,abackup
instrumentwillbeusedtomeasurewaterqualityparameters.
Forsingleormultiparameterwaterqualitymeters,thefollowingstandardsaretypicallyusedto
calibrate:
1. pH–commerciallyavailablestandardspH4,7,10.Performa2-pointcalibrationcovering
therangeofexpectedmeasurements.Usethe3rdpHstandard(orstandardsuppliedby
anothermanufacturer)asacheckstandardtoverifycalibrationaccuracy.
2. SpecificConductance–performasingle-pointcalibrationandusetwocheckstandards
bracketingtheexpectedmeasurementrange.
3. Dissolvedoxygen–usecalibrationprocedurerecommendedbymanufacturer,typicallyin
water-saturatedair.
4. Temperature–checkagainstthermometerofknownaccuracyatleastyearly(preferably
quarterly).Anicewaterbathofapproximately0°Ccanbeusedtosemi-quantitativelyverify
temperatureproberesponsebutmayvaryduetouncontrolledfactorssuchascontainer
sizeandgeometry,ice/waterdisequilibrium,orthepresenceofmeltingpoint-lowering
contaminants.
LaboratoriesmaintaincalibrationpracticesaspartoftheirmethodSOPs.Calibration
proceduresaredescribedgenerallybelow.
Uponinitiationofananalyticalrun,aftereachmajorequipmentdisruption,andwheneveron-
goingcalibrationchecksdonotmeetrecommendedMQOs,thesystemwillbecalibratedwitha
fullrangeofanalyticalstandards.Immediatelyafterthisprocedure,theinitialcalibrationmust
beverifiedthroughtheanalysisofastandardobtainedfromadifferentsourcethanthe
standardsusedtocalibratetheinstrumentation,preparedinanindependentmanner,and
ideallyhavingcertifiedconcentrationsoftargetanalytes(e.g.,acertifiedsolution).The
calibrationcurveisacceptableifithasanr2of0.995orgreaterforallanalytespresentinthe
calibrationmixtures.Ifnot,thecalibrationstandards,aswellasallthesamplesinthebatch,
mustbere-analyzed.Allcalibrationstandardswillbetraceabletoanorganizationthatis
recognizedforthepreparationandcertificationofQA/QCmaterials(e.g.,NIST,NRCC,USEPA,
etc.).
Calibrationcurveswillbeestablishedforeachanalyteandbatchanalysisfromacalibration
blankandamulti-pointcalibration(asdescribedorrequiredinthemethod),coveringtherange
ofexpectedsampleconcentrations.Iftheinstrumentresponseisdemonstratedtobelinear
overtheentireconcentrationrangetobemeasuredinthesamplesanduseofasingle-point
calibrationisdescribedorallowedinthemethod,theuseofacalibrationblankandonesingle
standardthatishigherinconcentrationthanthesamplesmaybeappropriate.Otherwise,only
datawithintheworkingcalibrationrange(abovetheMDL)shouldbereported(i.e.
extrapolationisnotacceptable).Samplesoutsidethecalibrationrangewillbedilutedas
appropriate,andreanalyzed.
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LaboratoriesmaintaininternalSOPsforinspectionandqualitycheckingofsupplies.Undera
PBMSapproach,theseproceduresarepresumedtobeeffectiveunlessfieldandQCdatafrom
analysesindicateotherwise.SFEI-ASCwillthenworkwiththelaboratorytoidentifythecauses
andaddressdeficienciesintheSOPsthatresultedinthoseproblems.Iftheproblemisserious
andcannotbecorrectedbythelaboratory,theSFEI-ASCProjectManagerandQAOwilldiscuss
andidentifyalternatives,includingchangingthesamplingmaterialsandmethods,the
extractionandanalyticalmethods,thelaboratory,oranycombinationofthese.
12. Non-direct Measurements (Existing Data)
Non-DeltaRMPdata(e.g.,IrrigatedLandRegulatoryProgram)maybeusedindetermining
rangesofexpectedconcentrationsinfieldsamples,characterizingaverageconditions(e.g.,
temperature,barometricpressure)forcalculations,andotherpurposes.Thesedatawillbe
reviewedagainstthedataqualityobjectivesstatedinSection4andusedonlyiftheymeetallof
thespecifiedcriteria.DatanotmeetingMQOsshouldbeusedonlyinaqualitativemannerfor
developingconceptualmodelsandprioritizingfuturedataneeds.
Hydrologicdata(stage,flow,etc.)willbeobtainedfromexistinggaugesandrecorderslocated
atorneardesignatedmonitoringlocations
TheDeltaRMPwillnotconductanyadditionalmonitoringofpesticidechemistryandtoxicityin
sediments.Instead,sedimenttoxicityandchemistrydatacollectedbytheSurfaceWater
AmbientMonitoringProgram(SWAMP)StreamPollutionTrends(SpoT)monitoringwillbe
includedintheinitialassessment.TheSpoTQAPPisavailableontheSPoTwebsite.
13. Data Management
ThecollectionagenciesandlaboratoriesprovidedatatoSFEI-ASCinappropriateCEDEN
templates(asprovidedbySFEI-ASC)withinthetimeframestipulatedinthecontract,usually90
daysorless.Thelaboratoriesshouldusethecurrenton-linedatacheckertoreviewdatafor
vocabularyandbusinessruleviolationspriortosubmittingtoSFEI-ASC(contactDS@sfei.orgfor
thecurrentURL).SFEI-ASCwillworkwiththelabstoaddressvocabularyandbusinessrule
issuesidentifiedfromusingthedatachecker.SFEI-ASCwillworkwithCEDENtopopulatethe
lookuplistswithnewvaluesasidentifiedbythelabsfromusingtheon-linedatachecker.
ToxicitydatathatisfundedbySWAMPshouldbesubmittedtoSWAMPbythedataprovider
usingSWAMPtemplatesandtheSWAMPdatachecker.Oncethesedatahavebeenapproved
bySWAMP,theSWAMPDataManagershouldprovidethedatainCEDENEDDtemplatesto
SFEI/ASCforfurtherprocessing.
ThelaboratoriesshouldreportdataasoutlinedinSection6.2,DataReportingRequirements.
DataaremaintainedatSFEIasestablishedinSection6.SFEI-ASCtrackseachdataset,from
submittaltofinaluploadtotheRDCdatabase.Onceallexpecteddatahavebeenreceived,
expertstaffonSFEI-ASC’sDataServicesteamprocessthedatausingaseriesofqueries
designedtoidentifyanyissuesremainingwiththeformatofthedata.TheQAOfficeror
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designeethenreviewsdataforqualityassuranceandqualitycontrolandappropriateCEDEN
QAcodesareappliedtothedataset.TheQAofficerordesigneewritesareportforeachdataset
outliningthequalityofthedata.Thisreporthighlightsanyissuesthatneedtobeaddressedby
thelaboratory,projectmanager,ordatamanagementstaff.
TheQASummaryReportincludesthefollowingdetails:
Lab
Matrix
Analyte
ReportingIssuesforLabtoReview
FormattingIssuesforDataManagertoReview
QAReview
Datasetcompleteness
Overallacceptability
MDLssensitivity
QBaverages(procedural,fieldblank)
Averageprecisionfromreplicatefieldsample
Accuracy(usingavarietyofSRMsorMatrixspikeQRECs)
Comparisonofdissolvedandtotalphases
Comparisontopreviousyears
RatioCheckingSummary
SumsSummary
Inaddition,specializedseniorscientistsfurtherrevieworganicsdatasetssuchasPCBs,PBDEs,
andpesticides.DataarethencompiledintotheRDCdatabaseanddistributedtotheproject
managers.DatathatareapprovedforpublicreleasearemadeavailablethroughSFEI-ASC’s
ContaminantDataDisplayandDownloadtool(CD3),usuallywithinoneyearofsample
collection.DatawillalsobemadeavailablethroughCEDEN’sAdvancedQuerytool.Thecontact
individualresponsibleforstepsandtasksofdatamanagementisAmyFranz.
SFEI-ASCmaintainsregularbackupsoftheirenterprisedatabasesbothtodiskandtape,nightly
andweekly,respectively.TheRDCdatabase,specifically,isalsobackeduphourly.Asafurther
protectivemeasure,copiesofthetapesetsarestoredbothonsiteandoffsite.Thelifetimeof
thebackupfilesontapeisabout2-3weeks.Additionally,abackupoftheRDCdatabasefrom
thefirstofeverymonthisstoredondiskindefinitely,allowingforquickrestoreandreviewof
archiveddataastheneedwarrants.
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14. Assessment and Response Actions
Initially,adesktoporon-siteperformanceauditwillbeperformedbytheQAOanddesignated
stafftodetermineifeachlaboratorycanmeettherequirementsoftheQAPPandtoassistthe
laboratorywhereneeded.ReviewofcurrentNELAPand/orstateELAPcertificationofa
laboratoryfortheanalysesperformedfortheDeltaRMPmaybeacceptedinsomecasesinlieu
ofanon-siteaudit.Reviewsmaybeconductedatanytimeduringthescopeofthestudy.
Resultswillbereviewedwithparticipatinglaboratorystaffandcorrectiveactionrecommended
andimplemented,wherenecessary.Furthermore,laboratoryperformancewillbeassessedon
acontinualbasisthroughlaboratoryintercomparisonstudies(roundrobins)whereavailable,
suchasthoseconductedbytheNationalInstituteofStandardsandTechnology(NIST).
Ifdataqualityissuesareidentified,apreliminarymeetingwillbeheldbetweenSFEI-ASC’sQAO
andtheProjectManagertodiscusspossiblesolutions.Ifnecessary,acorrectiveactionplanwill
bedevelopedinconsultationwiththeappropriatelab(s),thecorrectiveactionstaken,andthe
issueanditsresolutionsummarizedinabriefreportormemorandum.Asummaryofthese
issueswillbemaintainedintheProjectfiles,andwillbenotedinanyreportingthatincludes
affecteddata.
15. Reports to Management
ThereportinggoaloftheDeltaRMPistogeneratecommunicationproductsthatinformand
educatetargetaudiencesaboutDeltawaterqualityconditionsandtrends.Theinformationin
suchproductsistargetedatthehighestpriorityquestionsfacedbymanagers.Theprogram
achievesitsfullvalueonlytotheextentthatthedataitproducesaresynthesized,interpreted,
andreportedinamanneraccessibletoitsvariousaudiences.TheDeltaRMPwillproduce
anAnnualMonitoringReport,whichdocumentstheactivitiesoftheprogrameachyear;an
interpretivemainreport(ThePulseofTheDelta)thatsummarizesmonitoringresultsand
synthesizestheinformationtheyprovide;andtechnicalreportsthatdocumentspecificstudies
andsynthesizeinformationfromdiversesourcesinrelationtospecifictopicsandprioritized
assessmentquestions.
TheAnnualMonitoringReportwillpresenttheresultsofthepreviousJuly-Junefiscalyearof
sampling.Interpretationoftheresultswillbeverybasic.Themainpurposeofthisreportisto
sharethefinaldatawithprojectpartnersandcollaboratorsinatimelyway.TheAnnual
MonitoringReportalsoincludesaQAmemothatsummarizesanyQAproblemsanddocuments
anynon-conformanceswiththeQAPP.
TheQAOisresponsibleforsummarizingpotentialQAissueswithreporteddataand
communicatingthoseissuestotheProjectManager.TheQAOalsoreviewsanySFEI-ASC
analysesandreportsgeneratedfromthedata,toensurethatQAissuesareappropriately
acknowledgedandaddressed.
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16. Data Review, Verification, and Validation
AfterdataaresubmittedandincludedintheDeltaRMPdatabase,SFEI-ASCstaffexaminesthe
datasetforcompleteness(e.g.,correctnumbersofsamplesandanalyses,appropriateQC
sampledataincluded)andaccuracy(e.g.,insampleIDs),andspot-checkforconsistencywith
hardcopyresultsreportedbythelaboratory.TheSFEI-ASCQAOordesigneewillexamine
submittedQAdataforconformancewithMQOs,specifiedpreviously(Section4).Datathatare
incomplete,inaccurate,orfailingMQOswithoutappropriateexplanationwillbereferredback
tothelaboratoryforcorrectionorclarification.TheProjectManagerandQAOwilldiscussdata
failingMQOswithlaboratorystafftodeterminewhethermodificationstoanalyticalmethods
canbemadetoimproveresultsonreanalysis.Ifproblemscannotbereadilycorrected
(insufficientsample,irremovableinterferences,orblankcontaminationbasedonpastattempts
withthelab),resultsoutsidetheMQOswillbeflaggedusingCEDENcodesappropriateforthe
specificdeviationstoalertdatauserstouncertaintiesinquantitation.Resultsgreatlyoutside
thetargetMQOrange(z-scoresorp-scores>2,e.g.,foracceptancecriteriaof±25%,>±50%)15
maybecensoredandnotreported.
Inadditiontocontaminationandotherartifactsintroducedbysamplingandanalytical
methods,errorsmayariseatmanypointsintheprocessingandtransmittalofdatagenerated
fortheDeltaRMP.Characteristicsofreporteddataareexaminedtoidentifypossibleproblems
inthegenerationandtransmissionofdata.DatasubmittedtotheDeltaRMParecomparedto
valuesintheliteratureforcomparableenvironmentsandfrompreviousmonitoringtoevaluate
iftheyarewithintheexpectedrangeofvaluesforagivenstudy.Simplestatistics(e.g.,
minimum,maximum,mean,median)maybegeneratedtoquicklyidentifydatasetsor
individualdatapointsgreatlyoutsideoftheirexpectedrange.Anomalousindividualpointswill
beexaminedfortranscriptionerrors.Unitconversionsandsamplequantitationcalculations
maybereviewedtoidentifylargerandsystematicerrors.
17. Verification and Validation Methods
DataaresubmittedtoSFEI-ASCinelectronicform.TheQAOordesignatedprojectstaffverify
thatresultsforappropriatefieldandQCsamplesarereportedbycomparingthesampletypes
andnumbersprovidedagainstthosespecifiedinthedetailedprojectplan,chainofcustody
forms,and/orcontracts.Revieweddataarerecordedascheckedbyinitialsanddatestoensure
thatelectronicandhardcopyreportsagree.Thecontractlaboratory’sQAOfficer(QAO)
performschecksofallofitsrecordsandthelaboratory’sDirectororProjectManagerwill
recheck10%.AllchecksbythelaboratorymaybereviewedbySFEI-ASC.Issuesarenotedina
narrativelistandcommunicatedtothefieldorlaboratoryteamsasneededtocorrectany
problemsfound(e.g.unanalyzedsamplesleftinstorage,transcriptionerrors).
15z-score=|result–expectedvalue|/acceptabledeviation.SeeSection4.3.1.LaboratoryQCMeasurementsforadefinitionofthep-score.
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Aspartofthevalidationprocess,dataareevaluatedasmeetingorfailingMQOs.
ExceedancesofMQOsnotalreadynotedbythelaboratoryareflaggedinanyelectronic
databasesandcommunicatedtotheanalyzinglaboratoryforpossiblerecalculationand/or
reanalysis.Reconciliationandcorrectionoferrorsinreporteddatawillbeaddressedby
consultationamongSFEI-ASC’sProjectManager,SFEI-ASC’sQAO,andSFEI-ASCAnalyst(s)with
theLaboratory’sQAO,Laboratoryand/orProjectManager,andappropriatelabpersonnel.The
involvedpartieswillagreeuponanycorrections.
AnalysessometimesproduceresultsthatfailMQOsandmaynotbepossibletoovercomefora
smallnumberofanalyteswithinalargegroupofrelatedcompounds.Forexample,theremay
becontaminationthatisimpossibletoeliminateforallanalytes,whenanalysesareconducted
atultra-tracelevels.WithagreementoftheSFEI-ASCProjectManagerandQAOinconsultation
withtheLaboratory,resultsforsamplegroupswithdataoutsideofMQOsmaybeflagged
ratherthanreanalyzed,toindicatethegreateruncertaintyinthequantitationofthosedata.
ResultsonindividualanalytesthataregreatlyoutsidethetargetMQOrange(e.g.z-scores>2)
willbecensoredasneededratherthansubjectedtorepeatedanalysis.Reports,graphs,tables,
orsummarystatisticsgeneratedfromdatasetswithcensoreddatashouldnotetheirexclusion
orotherhandling.
Repeatedanalysismaynotfixanyissuesbutratherjustmaskvariability,creatingafalse
impressionofthequantitativecertaintyofresults.Contaminationofmethodblankscan
sometimesrepresentatemporarysourceofcontamination,andflaggingresultsofbatchesin
whichcontaminationisfoundinblanksisappropriate.Sampleresultsinbatcheswithdetected
blankcontaminationwillbeflagged(forfieldsampleswithanalyteconcentration>3xthose
foundinmethodblanks,“IP”whenappliedbythereportinglab,or“VIP”ifaddedlaterbySFEI-
ASC)orcensored(forresults<3xthoseinblanks)bySFEI-ASC,butdatausersshouldbeaware
ofthepossibleinfluenceofsporadiccontaminationinotherbatchesanalyzedaroundthesame
time,particularlyforsampleswithlowconcentrationssimilartothoseinblanks.
SimilaranalogiescanbemadewithfailuresofprecisionoraccuracyQCmeasurements.
Individualfailuresmayfallwithintherangeofthetruevarianceinthemeasurement,e.g.NIST
acceptancerangesaresometimesinexcessof±50%ofthemeanvalues,andwhilereporting
onlysuccessfulreanalysisbatchesmayappeartoproducemoreconsistentandcertainresults,
withoutfundamentalchangestotheanalyticalprocess,theunderlyinguncertaintymayonly
havebeenmasked/censoredratherthantrulyreducedforthereportedfieldsamples.Thisis
nottosaythatreanalysesareneverwarrantedordesirable,butrathertounderscorethat
improvedresultsonQCmeasurements,whichcansometimesbeachievedsimplybyrepeat
analysisanddiscardingpreviousfailedresults,shouldnotbeconfusedwithimproved
measurements,whichareonlyachievedbymakingrealsubstantivechangestothesampling
and/oranalyticalmethods.Ifreanalysisistobeattempted,itisthereforeimperativethatthe
ProjectManagerandQAOworkinconsultationwithlaboratorystafftoidentifyandchangethe
factorsthatmayhaveledtoMQOdeviances,ratherthansimplyrepeattheanalysisuntilthe
QCpasses.ForMQOdeviations(z-scoreorp-score>1)forwhichcausesarenotidentifiedand
thatarenotfixedbycorrectiveactions,fieldsampleresultsmaybequalified,orcensoredif
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grosslydeviating(z-scoreorp-score>2).TheQCdatausedfordeterminationofflaggingis
subjecttotheavailabilityofdataonvariousQCsampletypesandtheprofessionaljudgmentof
theQAO.DecisionswillbedocumentedinanarrativesummaryoftheQAreview.Where
possible,dataforflaggingrecoveryshouldbe1)inasimilarmatrixassamples,2)with
externallyvalidatedexpectedvalues,3)inaquantitativerange,and4)inasimilar
concentrationrangeasfieldsamples.Thusforevaluatingrecovery,theorderofpreferenceis
generallyCRM>LRM>MS>LCS,withexceptionsandchangesinpreferencemadeforfactorssuch
asnon-certifiedvalues,certifiedvalueswithwideuncertaintybands,andconcentrations
greatlydifferentfromthoseinfieldsamples.Similarly,forevaluationandflaggingoflab
precision,QCsamplesshouldbe1)inthesamematrixasfieldsamples,2)isolatelabvariation
fromothercauses,3)inaquantitativerange,and4)inasimilarconcentrationrangeasfield
samples,whereavailable.Forevaluatingprecisionthen,thepreferredsampletypesfor
replicatesare:lab>field>MS~CRM>LCS,againwithexceptionsmadedependingonthe
availablesampletypes,theirinherentvariability,concentrationranges,andotherfactors.Flags
appliedtodataaretobeselectedfromamongthoseapprovedbyCEDENappropriateforthe
specificMQOfailure(e.g.,“GBC-CRManalyterecoverynotwithincontrollimits”toaCRM
resultoutsideofacceptancetargets,“IU-PercentRecoveryexceedslaboratorycontrollimit”
forfieldsamplesreportedatthetimeifthedeviationappearsrandom,or“LHB-Result
positivelybiased,flaggedbylab”,ifresultsappearsystematicallyhighbiased).Thebasesfor
anyflaggingoffieldsampleswillbedocumentedinanarrativesummaryoftheQAreview.
TheQA/QCrequirementspresentedintheprecedingsectionsareintendedtoprovidea
commonfoundationforeachlaboratory’sprotocols;theresultantQCdatawillenable
assessmentofthecomparabilityanduncertaintyofresultsgeneratedbydifferentlaboratories
andanalyticalprocedures.ItshouldbenotedthattheQCrequirementsspecifiedinthisplan
representtheminimumrequirementsforanygivenanalyticalmethod;labsarefreetoperform
additionalQCinaccordancewiththeirstandardpractices.
InadditiontoperformanceonrequiredQCmeasuresandsamples(i.e.MDLs,blanks,matrix
spikes,CRM,replicates),dataarealsoexaminedforinternalandexternalconsistencytoensure
thatreportedvaluesarerealisticandrepresentativeforthelocationsandmatricesofcollected
samples.Thisreviewmayincludebutisnotlimitedto:
1. Comparisonofreportedvaluestothosefrompreviousyearsforthesamelocationsand
matrices,whereavailable–largedifferencesfrompreviouslyreportedvaluesmaynot
necessarilyindicateanalyticalissuesandmaysimplyreflectnaturalspatialandtemporal
variabilityoftheecosystem.
2. Comparisonofreportedvaluestothoseinthepublishedliterature,whereavailable–
differencesfromotherregionsand/orspeciesmaymerelyindicatedifferencesinresident
speciesandecosystemstructure,butverylarge(e.g.2-3ordersofmagnitude)differences
maysometimeshelpidentifyerrorsinanalysisorreporting(e.g.unitconversions).
3. Internalchecksofrelativeanalyteabundance–variationsinconcentrationsofone
compoundorisomerinaclassofchemicalcontaminantsareoftentightlylinkedtothoseof
relatedcompounds,suchasacompoundanditsdegradationproductsormanufacturing
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byproducts,orvariouscongenersinacommercialmixture.Deviationsintheserelative
abundancescansometimesindicatematrixinterferencesorotheranalyticalproblems,
althoughcareshouldbetakentonotdisregardresultsthatmightrevealatypicalsources
and/orecosystemprocesses.
AtthecompletionoftheQAreviewbytheQAO,resultsareassignedacompliancecodeonan
individualrecordlevel.SeeTable17.1forcompliancecodes.Dataarefurtherassignedabatch
verificationcodeonabatchlevel.SeeTable.17.2batchverificationcodes.Resultsfromthe
datareviewwillbesummarizedintheannualQAReport.
Table17.1. ComplianceCodes.
DataCompliance Name DataCompliance Code Compliant Com Do Not Use DNU Estimated Est Historical Hist Not Applicable NA Not Recorded NR Pending QA review Pend Qualified Qual Qualified Historic QualH Rejected Rej Screening Scr
Table17.2. BatchVerificationCodes.
BatchVerification Name BatchVerification Code Alternate Level Validation VAP Alternate Level Validation, Incomplete QC VAP,VI
Alternate Level Validation, Incomplete QC, Flagged by QAO
VAP,VQI
Cursory Verification, Data Rejected - EPA Flag, Flagged by QAO
VAC,VR
Cursory Verification, Minor Deviations, Flagged by QAO
VAC,VMD
Cursory Verification, Minor Deviations, Incomplete QC, Flagged by QAO
VAC,VMD,VQI
Cursory Verificaton VAC Cursory Verificaton, Incomplete QC, Flagged by QAO
VAC,VQI
Cursory Verificaton/Validation VLC Cursory Verificaton/Validation, Incomplete QC, Flagged by QAO
VLC,VQI
Cursory Verificaton/Validation, Minor Deviations, Flagged by QAO
VLC,VMD
Cursory Verificaton/Validation, Minor Deviations, Incomplete QC, Flagged by QAO
VLC,VMD,VQI
Data Rejected - EPA Flag, Flagged by QAO VR
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Full Verification VAF Full Verification, Incomplete QC, Flagged by QAO VAF,VQI
Full Verification, Minor Deviations, Flagged by QAO
VAF,VMD
Full Verification/Validation VLF Incomplete QC, Flagged by QAO VQI Incomplete QC, Temporary Verificaton, Flagged by QAO
VQI,VTC
Minor Deviations, Flagged by QAO VMD No QC, Flagged by QAO VQN Not Applicable NA Not Recorded NR Temporary Verification VTC
18. Reconciliation with User Requirements
AlldataarereviewedbytheQAOtodetermineiftheresultshavemettheDeltaRMPMQOsof
completeness,sensitivity,precision,andaccuracy.Limitationsofthedata,includinguncertainty
ofvalidateddata,arereportedtothedatausersbyaQAcodeorqualifier.TheDeltaRMPhas
adoptedtheCaliforniaDataExchangeNetwork’s(CEDEN)standardlistofcodestoflagdataat
theresultandanalyticalbatchlevel;theDeltaRMPusesasubsetoftheavailablecodestoflag
variousQCissuesasneeded.TheQAReportdescribesnon-conformanceswithQAPP
specifications.ThesefindingsshouldalsobeincludedinthedataitselfinQAcodes,result
qualifiercodes,compliancecodes,batchverificationcodes,andcommentfields,sothatalldata
userswillbeinformedofthequalityofthedata.
ThedatawillbestoredandmaintainedintheRegionalDataCenterdatabasestructureandwill
followCEDEN’sbusinessrules.
Measurementqualityobjectiveslistedpreviously(Section4)establishtargetstoberoutinely
achievedbytheanalyticallaboratory.However,itisuncertainwhetherobtaineddata,even
whenmeetingallstatedMQOs,willbesufficienttoanswertheDeltaRMPmanagement
questionswithsufficientcertainty,astherelativecontributionsofenvironmentalvariabilityand
analyticaluncertaintytooveralluncertainty(e.g.foruseinmodeling,comparisonsto
guidelines,orotherfunctions)cannotbeknownaprioribeforesufficientdatahavebeencollected.However,asDeltaRMPstudiesproceed,theabilityofcollecteddatatoanswerthese
managementquestionsshouldbeperiodicallyre-evaluatedforstudydesignandbudget
planninginsubsequentyears.
19. References
CaliforniaStateWaterResourcesControlBoard(SWRCB).2008.QualityAssuranceProgram
PlanfortheStateofCalifornia'sSurfaceWaterAmbientMonitoringProgram(SWAMP).
PreparedbytheSurfaceWaterAmbientMonitoringProgramQualityAssuranceTeam
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QualityAssuranceResearchGroup.Updated.
http://www.swrcb.ca.gov/water_issues/programs/swamp/docs/mqo/15_acute_toxicity.pdf
CaliforniaStateWaterResourcesControlBoard(SWRCB).QualityControlandSampleHandling
Tables.UpdatedQualityControlandSampleHandlingTables.
http://www.waterboards.ca.gov/water_issues/programs/swamp/mqo.shtml
CentralValleyWaterBoard.1998.TheWaterQualityControlPlan(BasinPlan)fortheCalifornia
RegionalWaterQualityControlBoard,CentralValleyRegion.TheSacramentoRiverBasin
andtheSanJoaquinRiverBasin.FourthEdition.CaliforniaRegionalWaterQualityControl
Board,CentralValleyRegion.
CentralValleyWaterBoard.2007.AmendmenttotheWaterQualityControlPlanforthe
SacramentoRiverandtheSanJoaquinRiverBasinsfortheControlofChlorpyrifosand
DiazinonRunoffIntotheSacramento-SanJoaquinDelta.CaliforniaRegionalWaterQuality
ControlBoard,CentralValleyRegion,ResolutionNo.R5-2006-0061.
CentralValleyWaterBoard.2011.AmendmentstotheWaterQualityControlPlanforthe
SacramentoRiverandSanJoaquinRiverBasinsfortheControlofMethylmercuryandTotal
MercuryintheSacramento-SanJoaquinRiverDeltaEstuary(Attachment1toResolution
No.R5-2010-0043).
CEDEN.2014.CEDEN-CaliforniaEnvironmentalDataExchangeNetwork.DataTemplates
Templates,andDocumentation.Retrievedfrom
http://www.ceden.org/ceden_datatemplates.shtml
EPA.2000.WaterQualityCriteriaforPriorityToxicPollutantsforCaliforniaInlandSurface
Waters,EnclosedBaysandEstuaries.40CFRPart131,U.S.EnvironmentalProtection
Agency.
EPA.2002a.Short-termMethodsforEstimatingtheChronicToxicityofEffluentsandReceiving
WaterstoFreshwaterOrganisms.FourthEdition.EPA-821-R-02-013
EPA.2002b.MethodsforMeasuringtheAcuteToxicityofEffluentsandReceivingWatersto
FreshwaterandMarineOrganisms.FifthEdition.EPA-821-R-02-012
EPA.2013.BinClassificationforFilteredSystems.40CFRPart141.710,U.S.Environmental
ProtectionAgency.
EPA.2015a.AquaticLifeBenchmarksforPesticideRegistration.URL:
http://www2.epa.gov/pesticide-science-and-assessing-pesticide-risks/aquatic-life-
benchmarks-pesticide-registration#benchmarks.AccessedonJuly8,2016.
EPA.2015b.NationalRecommendedWaterQualityCriteria-AquaticLifeCriteriaTable.URL:
http://www2.epa.gov/wqc/national-recommended-water-quality-criteria-aquatic-life-
criteria-table.AccessedonNovember23,2015.
Keith,L.H.1991.EnvironmentalSamplingandAnalysis:APracticalGuide.LewisPublishers.
Chelsea,MI.
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Keith,L.H.,Crummett,W.,Deegan,J.,Libby,R.A.,Taylor,J.K.andWentler,G.1983.Principles
ofEnvironmentalAnalysis.AnalyticalChemistry55(14):2210-2218.
Luo,Y.,Deng,X.,Budd,R.,Starner,K.andEnsminger,M.2013.MethodologyforPrioritizing
PesticidesforSurfaceWaterMonitoringinAgriculturalandUrbanAreas
(http://www.cdpr.ca.gov/docs/emon/surfwtr/monitoring_methods.htm).California
DepartmentofPesticideRegulation,Sacramento,CA.
Taylor,J.1987.QualityAssuranceofChemicalMeasurements.LewisPublishers.Chelsea,MI.
Stanley,T.W,andVerner,S.S.1985.TheU.S.EnvironmentalProtectionAgency’sQuality
AssuranceProgram.In:Taylor,J.K.,andStanley,T.W.(eds.)QualityAssuranceof
EnvironmentalMeasurements.ASTMSTP867.AmericanSocietyforTestingandMaterials.
pp.12-19.
AppendixA
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20. Appendices
20.1. AppendixA.ManagementQuestions
Type
ManagementQuestions
StatusandTrends
Isthereaproblemoraretheresignsofaproblem?
a. Iswaterqualitycurrently,ortrendingtowards,adversely
affectingbeneficialusesoftheDelta?
b. Whichconstituentsmaybeimpairingbeneficialusesin
subregionsoftheDelta?
c. Aretrendssimilarordifferentacrossdifferentsubregionsof
theDelta?
Sources,Pathways,Loadings,
andProcesses
Whichsourcesandprocessesaremostimportanttounderstand
andquantify?
a. Whichsources,pathways,loadings,andprocesses(e.g.,
transformations,bioaccumulation)contributemostto
identifiedproblems?
b. Whatisthemagnitudeofeachsourceand/orpathway(e.g.,
municipalwastewater,atmosphericdeposition)?
c. Whatarethemagnitudesofinternalsourcesand/orpathways
(e.g.benthicflux)andsinksintheDelta?
ForecastingWaterQuality
UnderDifferent
ManagementScenarios
a. Howdoambientwaterqualityconditionsrespondtodifferent
managementscenarios
b. WhatconstituentloadscantheDeltaassimilatewithout
impairmentofbeneficialuses?
c. WhatisthelikelihoodthattheDeltawillbewaterquality-
impairedinthefuture?
EffectivenessTracking
a. Arewaterqualityconditionsimprovingasaresultof
managementactionssuchthatbeneficialuseswillbemet?
b. Areloadingschangingasaresultofmanagementactions?
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20.2. AppendixB.AssessmentQuestions
DeltaRMPassessmentquestionsformercury,pesticides,andpathogens.Questionshighlighted
inyellowarethehighestpriorityforinitialstudies.
Type Core
Management
Questions Mercury Pesticides Pathogens
Status&
Trends
Istherea
problemorare
theresignsofa
problem? a. Iswater
quality
currently,or
trending
towards,
adversely
affecting
beneficial
usesofthe
Delta?
b. Which
constituents
maybe
impairing
beneficial
usesin
subregionsof
theDelta?
c. Aretrendssimilaror
different
across
different
subregionsof
theDelta?
1. Whatarethestatusand
trendsinambient
concentrationsoftotal
mercuryand
methylmercury(MeHg)in
fish,water,andsediment,
particularlyinsubareas
likelytobeaffectedby
majorsourcesornew
sources(e.g.,large-scale
restorationprojects)?
A. Aretrendsovertimein
MeHginsportfish
similarordifferent
amongDeltasubareas?
B. Aretrendsovertimein
MeHginwatersimilar
ordifferentamong
Deltasubareas?
1. Towhatextentdopesticides
contributetoobserved
toxicityintheDelta?
1.1. Whichpesticidesor
degradateshavethehighest
potentialtobecausing
toxicityintheDeltaand
thereforeshouldbethe
priorityformonitoringand
management?
A. Ifsamplesaretoxic,do
detectedpesticidesexplain
thetoxicity?
B. Ifsamplesarenottoxic,do
detectedpesticide
concentrationsexceed
otherthresholdsofconcern
(e.g.,waterquality
objectivesorOfficeof
PesticideProgramsaquatic
toxicitybenchmarks)?
1.2. Whatarethespatialand
temporalextentsoflethal
andsublethalaquaticand
sedimenttoxicityobserved
intheDelta?
A. Doaquaticorsediment
toxicitytestsattargeted
sitesindicateatoxic
response?
B. IfanswertoAisyes,whichothertoxicityindicator(s)
shouldguidemonitoring
andmanagementof
pesticidesinYears2+?
2. Whatarethe
spatial/temporaldistributions
ofconcentrationsofcurrently
usedpesticidesidentifiedas
likelycausesofobserved
toxicity?
2.1. Whichpesticideshavethe
highestriskpotential
1. Arecurrentpathogen
levelssupportiveofthe
municipaldrinkingwater
qualitybeneficialuseas
describedintheBasin
Plan?
A. Arethecurrent
pathogenlevelsfor
eachDeltawater
intakeandthose
immediatelyupstream
(i.e.,SacramentoArea)
differentthanthe
previousLT2
sampling?Areany
drinkingwaterintakes
reclassifiedintoa
higherbinlevel?
B. AreBasinPlantrigger
valuesexceeded?
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Type Core
Management
Questions Mercury Pesticides Pathogens
(basedonDPR’srisk
prioritizationmodel16)and
shouldbeincludedin
chemicalanalyses?
A. Isthelistofpesticides
includedinUSGS
pesticidescansufficient
forDeltaRMP
monitoringdesign?
B. Aremethodsavailableto
monitorpesticideswith
high-riskpotentialnot
includedinUSGS
pesticidescan?
2.2. Howdoconcentrationsofthepesticideswiththe
highestriskpotentialvary
seasonallyandspatially?
Sources,
Pathways,
Loadings&
Processes
Whichsources
andprocesses
aremost
importantto
understandand
quantify? a. Which
sources,
pathways,
loadings,and
processes
(e.g.,
transformatio
ns,
bioaccumulati
on)contribute
mostto
identified
problems?
b. Whatisthe
magnitudeof
eachsource
1. Whichsources,pathways
andprocessescontribute
mosttoobservedlevelsof
methylmercuryinfish?
A. Whataretheloadsfrom
tributariestotheDelta
(measuredatthepoint
wheretributariescross
theboundaryofthe
legalDelta)?
B. Howdointernalsources
andprocessesinfluence
methylmercurylevelsin
fishintheDelta?
C. Howdocurrently
uncontrollablesources
(e.g.,atmospheric
deposition,bothas
directdepositionto
Deltasurfacewaters
andasacontributionto
nonpointrunoff)
influence
methylmercurylevelsin
1. Whataretheprincipal
sourcesandpathways
responsibleforaquaticand
sedimenttoxicityobservedin
theDelta?
2. Whatarethefatesof
prioritizedpesticidesand
degradatesinthe
environment?
2.1. Dophysical/chemical
propertiesofpriority
pesticides,applicationrates
andprocesses,andambient
conditionsinfluencethe
degreeoftoxicityobserved?
3. Whatarethe
spatial/temporalusepatterns
ofprioritypesticides?
1. Cananychangesinbinlevel
17beattributedtoan
identifiableevent,
condition,orchangesina
source?
A. Whatistheinfluenceof
sourcesonpathogen
levelsatdrinkingwater
intakes?
B. Whatistheviabilityand
infectiousnessof
pathogensatdrinking
waterintakes?
C. Aretherenew
dischargesorchangesin
sourcesorconditions
thatcouldexplainthe
changeinbinlevel
comparedtoprevious
LT2monitoring?
2. Whatarethefactors
affectingdecayandgrowth
ratesandcantheybe
quantifiedand
16 http://www.cdpr.ca.gov/docs/emon/pubs/ehapreps/analysis_memos/prioritization_report_2.pdf 17EPAhasdevelopedtheLongTerm2EnhancedSurfaceWaterTreatmentRule(LT2rule),whichclassifiesfilteredwater
systemsintooneoffourtreatmentcategories(bins)basedontheirmonitoringresultsforCryptosporidium.Mostsystemsare
expectedtobeclassifiedinthelowestbinandwillfacenoadditionalrequirements.Systemsclassifiedinhigherbinsmust
provideadditionalwatertreatmenttofurtherreduceCryptosporidiumlevelsby90to99.7percent(1.0to2.5-log),depending
onthebin.From:RuleFactSheet-LongTerm2EnhancedSurfaceWaterTreatmentRule(EPA2005).
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Type Core
Management
Questions Mercury Pesticides Pathogens
and/or
pathway(e.g.,
municipal
wastewater,
atmospheric
deposition)?
c. Whatarethe
magnitudesof
internal
sources
and/or
pathways
(e.g.benthic
flux)andsinks
intheDelta?
fishintheDelta? characterizedforthe
purposeofmodeling?
Forecasting
Scenarios
a. Howdoambient
waterquality
conditions
respondto
different
management
scenarios
b. What
constituent
loadscanthe
Delta
assimilate
without
impairmentof
beneficial
uses?
c. Whatisthe
likelihoodthat
theDeltawill
bewater
quality-
impairedin
thefuture?
1. Whatwillbetheeffectsof
in-progressandplanned
sourcecontrols,restoration
projects,andwater
managementchangeson
ambientmethylmercury
concentrationsinfishinthe
Delta?
1. Howdopesticideconcentrationsrespondto
differentmanagement
scenarios?
2. Whatpesticideloadscanthe
Deltaassimilatewithout
exceedingwaterquality
criteriaestablishedtoprotect
beneficialuses?
3. Howwillclimatechange
affectconcentrationsand/or
loadingsofpesticidesand
impactstoaquaticspecies?
1. Whatistheeffectof
sourcecontrolson
pathogenlevelsat
drinkingwaterintakes?
2. Howwillproposedrestorationprojects,
wateroperations,and
futureurbangrowth
affectmunicipaldrinking
waterintakebinlevels?
Effectiveness
Tracking
a. Arewaterquality
conditions
improvingas
aresultof
management
actionssuch
thatbeneficial
useswillbe
met?
[none] 1. Arepesticide-related
toxicityimpacts
decreasingovertime?
[none]
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Type Core
Management
Questions Mercury Pesticides Pathogens
b. Areloadingschangingasa
resultof
management
actions?
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20.3. AppendixC.DeltaRMPMonitoringElements
Pesticides
Monthlysamplingatfivesites,whichalsocapturetargetedevents.Targetedevents(n=
5/year):WetWeather:(1)1stseasonalflush(WaterYear),(2)Significantwinterstorm;Dry
weather:(1)EarlySpring,(2)Latespring/earlysummerirrigationseason,(3)Latesummer
irrigationseason.Chemicalanalysesandtoxicitytestingonallsamples.Testspecies
(endpoints):(1)Selenastrumcapricornutum(growth)(2)Ceriodaphniadubia(survivalandreproduction),and(3)Pimephalespromelas(larvalsurvivalandgrowth).Chemistry:pesticide
scan(USGS),totalsuspendedsolids,dissolvedorganiccarbon(DOC)andparticulateorganic
carbon(POC),hardness,anddissolvedcopperanalysis.Pesticide-focusedToxicityIdentification
Evaluations(TIEs)forasubsetofsampleswith>50%ofthemeasuredendpoint;tobedecided
real-timebyaTIEsubcommittee.
Mercury
SportFish
Annualsamplingatsixfixedsitesbeginningin2016.Indicatorofprimaryinterestis
methylmercuryinmusclefilletof350-mmlargemouthbass(orsimilarpredatorspecies).Sites
arelocatedtorepresentdifferentsubareasoftheDeltaandtolinkwithwatermonitoring.
Water
Quarterlysamplingatfivesitesthatalignwithsportfishmonitoringsites.Indicatorofprimary
interestistotalmethylmercuryinwater.
ImportantancillaryparametersincludetotalanddissolvedtotalHg,chlorophylla,DOC,suspendedsedimentconcentrations,andvolatilesuspendedsolids.
Pathogens
Monthlysamplingforatwo-yearspecialstudycharacterizingpathogenlevels(Cryptosporidium
andGiardialamblia)toaddresstheobjectivesofthePathogenSpecialStudyrequiredbytheCentralValleyDrinkingWaterPolicyBasinPlanAmendment.Thestudyincludesmonitoringat
ambientlocationsthroughouttheDelta.Thesamplingisaddedtotheroutinemonthlysampling
effortoftheDepartmentofWaterResources(DWR)MunicipalWaterQualityInvestigations
(MWQI).TheDeltaRMPcontributesrequiredadditionallaboratoryanalyses,data
management,andreporting.
AppendixD
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20.4. AppendixD.ListofSOPs
ThefollowingSOPs,manuals,andmethodreferencedocumentswillbemadeavailable
onCDbyrequestorcanbedownloadedfromtheSFEI-ASCGoogleDrive.
Field
USGS
− NationalFieldManualfortheCollectionofWater-QualityData − CollectionofPyrethroidsinWaterandSedimentMatrices:DevelopmentandValidationofa
StandardOperatingProcedure
MPSL
− MPSLFieldSOPv1.1
− MPSL-102aSamplingMarineandFreshwaterBivalves,FishandCrabsforTraceMetaland
SyntheticOrganicAnalysis − Lowlevelmercury(USGSNFMA5.6.4.B)
MWQI
− MWQIProgramFieldManual
− MWQIProgramFieldManual,AppendixA–DeltaRMPPathogenStudyCryptosporidiumand
GiardiaSampling
ChemicalAnalysis
USGS
− DeterminationofElementsinNatural-Water,Biota,Sediment,andSoilSamplesUsing
Collision/ReactionCellInductivelyCoupledPlasma–MassSpectrometry(USGSTM-5-B1) − MethodsofAnalysis—DeterminationofPyrethroidInsecticidesinWaterandSedimentUsingGas
Chromatography/MassSpectrometry(USGSTM-5-C2) − Analysisoftheherbicidediuron,threediurondegradates,andsixneonicotinoidinsecticidesin
water—MethoddetailsandapplicationtotwoGeorgiastreams(USGSSIR2012-5026) − AMulti-residueMethodfortheAnalysisofPesticidesandPesticideDegradatesinWaterUsing
HLBSolid-phaseExtractionandGasChromatography–IonTrapMassSpectrometry − WATEREXTRACTIONforGCMSanalysisusingHLBcartridges − SuspendedsedimentonFilterPaperEXTRACTIONforGCMSanalysis − WATEREXTRACTIONforLCMSMSanalysisusingHLBcartridges − ProceduresforProcessingSamplesforAnalysisofDissolvedOrganicCarbonandOrganic
ParticulateCarbon − DeterminationofCarbonandNitrogeninSedimentsandParticulatesofEstuarine/Coastal
WatersUsingElementalAnalysis(EPA440.0) − MethodsofAnalysisbytheU.S.GeologicalSurveyNationalWaterQualityLaboratory-
DeterminationofDissolvedOrganicCarbonbyuv-promotedPersulfateOxidationandInfrared
Spectrometry(USGSTestMethodO-1122-92)
MPSL
− MercuryinSolidsandSolutionsbyThermalDecomposition,Amalgamation,andAtomic
AbsorptionSpectrophotometry(EPA7473)
− MercuryinWaterbyOxidation,PurgeandTrap,andColdVaporAtomicFluorescence
Spectrometry(EPA1631,RevisionE)
− MethylMercuryinWaterbyDistillation,AqueousEthylation,PurgeandTrap,andColdVapor
AtomicFluorescenceSpectrometry(EPA1630)
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− MPSL-101 Sample Container Preparation for Organics and Trace Metals, Including Mercury and Methylmercury
− MPSL-104SampleReceiptandCheck-In
− SM2540DSolids
CDFW-WPCL
− InVitroDeterminationofChlorophyllsa,b,c1+c2andPheopigmentsinMarineAndFreshwater
AlgaebyVisibleSpectrophotometry(EPA446.0)
− TOTALORGANICCARBONinWater(EPA415.1)
− WPCL-AB-001SampleCustody,Receipt,andStorage
− WPCL-QA-050ProtocolforCorrectiveActionProcedures
ToxicityTesting
UCD-AHPL
− InitiationofSelenastrumcapricornutum96-HourChronicToxicityTest(4thEdition)(SOP1-1)
− InitiationofCeriodaphniadubiaChronicToxicityTest(4thEdition)(SOP1-2)− InitiationofPimephalespromelas(FatheadMinnow)ChronicToxicityTest(4thEdition)(SOP1-3)
− InitiationofHyalellaaztecaAcute96-hourWaterColumnToxicityTest(SOP1-6)
− ProtocolforSampleReceivingandStorage–DeltaRMPTesting(SOP12-7)
ToxicityIdentificationEvaluations(TIEs)
UCD-AHPL
− ProtocolforMakinga5ppmSolutionofPBOandSpikingitintoSampleWaters(SOP7-1)
− C8SolidPhaseExtraction(SOP7-2)
− C8ColumnElutionforPhaseITIEs(SOP7-3)
− C8ColumnElutionforPhaseIITIEs(SOP7-4)
− AmendmentofWaterSampleswithEDTAandNa2S2O3(SOP7-9)
− pHAdjustmentstopH3andpH11(SOP7-10)
− Aeration(Volatile/SurfactantStripping)(SOP7-11)
ToxicityTesting-WaterQualityMeasurements
UCD-AHPL
− AnalysisforTotalWaterHardness(SOP6-1)
− AnalysisforAmmoniaNitrogen(mg/L)(SOP6-3)
− AnalysisforAlkalinity(SOP6-5)
− UseofYSIModel33ElectricalConductivityMeter(SOP8-7)
− OperationofBeckman12pH/ISEMeter(SOP8-8)
− ProtocolfortheYSIModel58DissolvedOxygenMeter(SOP8-9)
SWAMPDocumentation
− SWAMPToxicityTemplateDocumentation
− SWAMPToxicityTemplate
− SWAMPSampleHandling,MeasurementQualityObjectives,andCorrectiveActionTables
PathogenAnalysis
BioVir
− EPAMethod1622,1623,1623.1CryptosporidiumandGiardiainWaterbyFiltration/IMS/FA:
SampleFiltration(SOPX.C.2.a)
− EPAMethod1622,1623and1623.1CryptosporidiumandGiardiainWaterbyFiltration/IMS/FA:
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ElutionandConcentration(SOPX.C.2.b)
− EPAMethod1622,1623and1623.1CryptosporidiumandGiardiainWaterbyFiltration/IMS/FA:
ImmunomagneticSeparation(IMS)(SOPX.C.2.c)
− EPAMethod1622,1623and1623.1CryptosporidiumandGiardiainWaterbyFiltration/IMS/FA:
SlideStainingProcedure(SOPX.C.2.d)
− EPAMethod1622,1623and1623.1CryptosporidiumandGiardiainWaterbyFiltration/IMS/FA:
SlideExamination(SOPX.C.2.e)
Eurofins
− EPAMethod1622/1623(Micro-SOP3404)
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20.5. AppendixE.ExampleFieldSheets
November 2013 1 SW Form version 9.0
COMPILED BY: ___________________________ CHECKED BY: ________________________________ LOGGED INTO NWIS BY: _____________________________
SAMPLING INFORMATION
Parameter Pcode Value Information
Sampler Type 84164 see last page for proper codes— consider type of sampler and material
Sampler ID:
Sampling Method 82398 10 EWI; 20 EDI; 30 single vertical; 40 multiple vertical; other ______________________
BAG SAMPLER EFFICIENCY TEST
Sampler bottle/bag material 84182 Plastic Bag (11) Teflon® Bag(12) Glass Bottle(20) Plastic Bottle (21) Teflon® Bottle (22) other (30)
Test Duration Sampler Collected Water
(seconds)
Sample Volume Collected (milliliters)
Sampler Nozzle material 72219 plastic (2) Teflon® (3) Brass (1) 1
Sampler Nozzle Diameter 72220 3/16” (3) 1/4” (4) 5/16” (5) 2
Sampler Transit Rate 50015 feet/second 3
Velocity to Calculate Isokinetic transit rate
72196 feet/second Mean (72217) (72218)
Depth to Calculate Isokinetic transit rate 72195 feet . Bag Sampler Efficiency % (See last page)
Splitter Type 84171 See last page for codes ____________ Splitter ID: Hydrologic Condition N/A A Not Determined; 4 Stable, low stage; 5 Falling stage; 6 Stable, high stage; 7 Peak stage; 8 Rising stage; 9 Stable, normal
stage Observations [Codes: 0=none; 1=mild; 2=moderate; 3=serious; 4=extreme]
Oil-grease (01300) ___ Detergent suds (01305) ___ Floating garbage (01320) ___ Floating algae mats (01325) ___ Floating debris (01345) ___ Turbidity (01350) ___ Atm. Odor (01330) ___ Fish kill (01340) ___ Gas Bubbles (01310) ___ Sewage Solids (01335) ___ Floating Vegetation (84178) ___ Ice Cover(01355) ___
Station No. ____________________ U. S. GEOLOGICAL SURVEY SURFACE-WATER QUALITY FIELD NOTES NWIS Record No. ____________________
Station No. ________________________ Station Name ________________________________________________ Field ID _________________ Sample Date _____________ Mean Sample Time _______ Time Datum ______ (eg. EST, EDT, UTC) End Date _________ End Time _______ *Sample Medium: WS WSQ OAQ *Sample Type: 9 (regular) 7 (replicate) 2 (blank) 1 (spike) __________ *Sample Purpose (71999): 10 (routine) 15 (NAWQA) 20 (NASQAN) 25 (NMN) 30 (Benchmark) _____________________ *Purpose of Site Visit (50280): 1001 (fixed-frequency SW) 1003 (extreme high flow SW) 1004 (extreme low flow SW) 1098 (NAWQA QC) ______ QC Samples Collected? Y N Blank Replicate Spike Other_______________________ Project No. __________________________________________ Project Name_______________________________________________________ Sampling Team ______________________________________ Team Lead Signature ________________________________ Date ___________ START TIME __________ GAGE HT _______ TIME __________ GHT ______ TIME __________ GHT ______ TIME __________ GHT ______ END TIME __________ GHT _______
* see last page for additional codes
FIELD MEASUREMENTS
Property Parm Code
Method Code http://water.usgs.gov/usgs/owq/Forms/
Fieldmeasure-ment_parametersmethods.doc Result Units
Remark Code
Value Quali-
fier
Null Value Quali-
fier NWIS Result-Level Comments Gage Height 00065 ft Discharge, instantaneous
00061 cfs
Temperature, Air 00020 THM04 (Thermistor) THM05 (Thermometer)
˚C
Temperature, Water 00010 THM01 (Thermistor) ˚C Specific Conductance 00095 SC001 (Contacting Sensor) PS/cm Dissolved Oxygen 00300 LUMIN (Luminescent)
MEMBR (Amperometric) SPC10 (Spectrophotometric)
mg/L
Barometric Pressure 00025 BAROM (Barometer) mm Hg pH 00400 PROBE (Electrode) units Alkalinity, filtrd, incr. Alkalinity, filtrd, Gran
39086 29802
TT061 (Digital Titrator) TT062 (Buret) TT056 (Digital Titrator) TT057 (Buret)
mg/L
Carbonate, filtrd, incr. Carbonate, filtrd, Gran
00452 63788
ASM01(Digital Titrator) ASM02(Buret) ASM03(Digital Titrator) ASM04(Buret)
mg/L
Bicarbonate, filtrd, incr. Bicarbonate, filtrd, Gran
00453 63786
ASM01(Digital Titrator) ASM02(Buret) ASM03(Digital Titrator) ASM04(Buret)
mg/L
Hydroxide, filtrd, incr. Hydroxide, filtrd, Gran
71834 29800
ASM01(Digital Titrator) ASM02(Buret) ASM03(Digital Titrator) ASM04(Buret)
mg/L
Turbidity [see attachment for codes and units]
Attach ASR and WatList
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AppendixE
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AppendixE
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AppendixF
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20.1. AppendixF.ExampleforChainofCustodyForm