Section A LABORATORY QUALITY ASSURANCE/QUALITY CONTROL - Free Download PDF

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Section ALABORATORYQUALITY ASSURANCE/QUALITY CONTROL Her Majesty the Queen inRight of the Province of British Columbia2015All Rights Reserved

TABLE OF CONTENTSSECTION ALaboratory Quality Assurance/Quality Control GuidelinesLABORATORY QA/QC GUIDELINES .32.0GENERAL GUIDELINES.32.1Quality Manual .32.2Laboratory Record Keeping .32.3Sample History Requirements .32.4Sample Collection and Preservation .42.5Test Methods, Existing .92.6Test Methods, New .92.7Equipment .92.8Analyst Qualifications .92.9Reagents and Standard Solutions . 102.10Reagent Water . 102.11Gravimetric Measurement . 102.12Volumetric Measurement . 112.13Glassware Cleaning . 112.14Contamination Control . 112.15Calibration Practices . 112.16Quality Control Approaches . 112.17Control Limits . 122.18Recommended Data Quality Objectives for Laboratory Duplicates . 122.19Expression of Results in the Final Report . 132.20Guidelines for Analytical Parameters Determined by Calculation (Ver.: Jan. 8, 2004) 142.21Performance Audits. 162.22Inter-Lab Comparison Studies . 163.0Recommended Protocol for Establishing Method Detection Limits .163.1Introduction . 163.2Calculation of Standard Deviation. 173.3Calculation of Method Detection Limits. 183.4Recorded Figures. 183.5Limit of Quantitation . 183.6Confidence Interval Convention . 184.0BLANKS .194.1Documentation of Blanks . 194.2Determination of Long Term Blank . 194.3Application . 194.4Evaluation of batch blanks . 194.5Documentation of Blank QC . 214.6Blank Correction Summary . 215.0QC FOR SMALL LABORATORIES .215.1Small Laboratory Quality Control Level . 215.2Small Laboratory Quality Control Criteria . 226.0REFERENCES.226.1QA/QC General . 226.2Method Detection Limits . 226.3Blank Correction. 22A-1

7.0REVISION HISTORY .23GLOSSARY OF STATISTICAL TERMS USED IN QUALITY ASSURANCE .27LIST OF TABLESTable 1. Summary of sample preservation and hold time requirements .5Table 2. Recommended data quality objectives for laboratory duplicates .13Table 3. Values of the one-tailed ‘t’ statistic at p 0.05, applied to the standard deviation, SD,appear in the following table .24Table 4. Example 1: MDL estimation from duplicates .24Table 5. Example 2: MDL estimation from replicates in same batch .25Table 6. Example 3: MDL estimation from pooled standard deviations from replicates insuccessive batches .26A-2

Quality AssuranceRevision Date: October 2015LABORATORY QA/QC GUIDELINES1.0INTRODUCTIONThis chapter specifies essential QA/QC activities to enable laboratories to achieve reproducible results onan ongoing basis. The first part of Section E ‘Microbiological Examination’ discusses QA/QC as theypertain to microbiological methods.Guidelines alone cannot guarantee high quality results. Common sense steps to avoid contamination,ongoing programs of staff training, and proactive method improvement procedures are also essential.All laboratories should regularly participate in cooperative inter-laboratory studies, and standard referencematerials should be analyzed frequently, preferably on a blind or semi-blind basis. Large laboratoriesshould have a full time QA Officer.The procedures for determining method detection limits and for handling blank corrections arecontroversial. Different procedures and calculation algorithms are being used by various laboratories.2.0GENERAL GUIDELINES2.1Quality ManualA Quality Manual shall be set up that documents all resources, policies and procedures making up theQuality System. The Quality Manual is to include detailed descriptions of the topics outlined in thissection and clearly define the responsibilities of management, supervisory staff, and laboratory staff withrespect to the quality systems. It shall be reviewed and updated regularly.2.2Laboratory Record KeepingThe laboratory record system shall be designed to ensure sample, analytical data, and analysttraceability, including dates and analysts’ initials or signatures. Dated and signed material shall includeforms, instrumental records and printouts, as well as notebooks.The sample numbering system of the laboratory must be designed to eliminate the possibility of a samplemix-up.The record storage system should be designed for easy retrieval. A policy on the length of storage anddisposal of records should be established.2.3Sample History RequirementsDocumentation and procedures on sample history shall be maintained, including:- sample collection- field sample preparation- chemical preservation- sample containers- holding times- storage conditions- condition of samples on receipt at laboratoryA-3

Potential deficiencies in sample history requirements shall be monitored and noncompliance must beidentified and any affected analytical data flagged.a.Sample collectionDocumentation accompanying all samples should include a test requisition form, or shouldcomply with chain of custody requirements.b.Sample containersSample containers may be purchased pre-cleaned from commercial suppliers. Alternatively,sample containers may be cleaned and prepared by the laboratory using documentedprocedures. Contaminants or interferences in sample containers and preservatives should bemonitored by the analysis of container blanks on a per-batch basis. Results of this monitoringshould be documented. Container blanks may be prepared by leaching or rinsing containers withreagent water and performing analyses for the parameters of interest. It is recommended that themonitoring of sample containers for cleanliness be focused on ‘low level’ studies; i.e., whereanalytical results are anticipated to be 10 times MDLs (e.g., trace metals, dioxins).2.4Sample Collection and Preservationa.Sample condition on receiptInspect sample containers for damage; record and report temperature on receipt whereappropriate. Where critical, temperature limits should be established and maximum/minimumthermometers should accompany the samples to document compliance with the limits.b.Storage conditionsTemperatures of refrigerated and frozen storage facilities shall be monitored and recorded daily.c.Sample Pre-treatmentDocumentation on sample preparation and pre-treatment procedures shall be maintained,including:-drying or removal of moisturedetermination of moisture contentsub-samplingpreparation of geological samples including splitting, sieving, grinding, pulverizingpreparation of biological tissue sampleshomogenizationfiltrationComplete records shall be maintained to ensure that potential problems, including crosscontamination, are traceable.d.Hold Times and PreservationThe hold times and preservation listed below in Table 1 will take precedent over the hold timesand preservation criteria listed in the individual methods. The intent of this table is to ensure thathold times, sample containers and preservation practices reflect the most current and approvedtreatment.A-4

Table 1. Summary of sample preservation and hold time requirementsBC MOE SAMPLE PRESERVATION & HOLDING TIME REQUIREMENTS(1,2)Parameter NameVersion: tainerStorage(3)TempPreservationPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, Glass 6ºC 6ºC 6ºC 6ºC 6ºC 6ºC 6ºC 6ºCnonenonenonenonenonenonenonenone14 days14 days3 days28 days15 minutes7 days3 days3 daysAPHAAPHAAPHA / BC MOEAPHAAPHAAPHAEPA 40CFR 2012 / BC MOEAPHA / BC MOEPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, Amber Glassno requirementno requirement 6ºCnone 6ºCnonenone50 mg/L EDAnone50 mg/L EDAfield NaOH, store in darknoneWinkler kit, store in neHClnonefilter (field or lab)28 days28 days28 days15 minutes14 days14 days24 hours8 hours28 days28 days3 days28 days3 days3 days3 days28 days3 days28 days3 days28 days3 days3 daysEPA 300.1APHA / EPA 300.1EPA 317.0APHAEPA 317.0APHAAPHAAPHAAPHA / EPA 300.1APHABC MOEAPHABC MOEAPHA / BC MOEAPHA / BC MOEAPHABC MOEAPHABC MOEAPHABC MOEEPA 40CFR 2012 / BC MOEnonefilter, H2SO4noneH2SO4nonenonenoneZnAc / NaOH to pH 93 days28 days3 days28 days3 days28 days28 days7 daysAPHA / BC MOEAPHABC MOEAPHABC MOEAPHAAPHA / SW846 Ch3 2007APHA1 mL 50% NaOH per 125 mLnone30 days24 hours180 daysEPA 1669APHAAPHA / EPA 200.2180 daysAPHAWaterPhysical & Aggregate ids (Total, TSS, TDS, Fixed, Volatile, etc.)TurbidityUV TransmittanceInorganic Non-metallicsBromideChlorideChlorate, BromateChlorine, Total Residual (Free Chlorine)ChloriteCyanide (SAD, WAD)Dissolved Oxygen (Winkler Method)FluorideNitrogen, Nitrate NitritePlastic, Glass 6ºCGlass BOD bottlePlastic 6ºCno requirementPlastic, Glass 6ºCNitrogen, AmmoniaPlastic, Glass 6ºCNitrogen, NitrateNitrogen, NitritePlastic, GlassPlastic, Glass 6ºC, do not freeze 6ºC, do not freezeNitrogen, Total KjeldahlPlastic, Glass 6ºCNitrogen, Total, Persulfate MethodPlastic, Glass 6ºCNitrogen, Total, Combustion MethodPlastic, Glass 6ºCPhosphorus, Dissolved (Orthophosphate)Plastic, Glass 6ºCPhosphorus, Total Reactive (Orthophosphate)Plastic, Glass 6ºCPhosphorus, Total DissolvedPlastic, Glass 6ºCPhosphorus, TotalPlastic, Glass 6ºCSilica, ReactiveSulfateSulfidePlasticPlastic, GlassPlastic, Glass 6ºC, do not freeze 6ºC 6ºCHexavalent ChromiumPlastic, Glass 6ºCMetals, TotalPlastic, Glassno requirementMetals, DissolvedPlastic, Glassno requirementMetalsMercury, TotalGlass, PTFEno requirementMercury, DissolvedGlass, PTFEno requirementAdsorbable Organic Halides (AOX)Amber Glass 6ºCBiochemical Oxygen Demand (BOD)Carbonaceous Biochemical Oxygen Demand (CBOD)Plastic, GlassPlastic, Glass 6ºC, do not freeze 6ºC, do not freezeCarbon, Dissolved OrganicPlastic, Glass 6ºCCarbon, Dissolved InorganicCarbon, Total OrganicCarbon, Total InorganicPlastic, GlassPlastic, GlassPlastic, Glass 6ºC 6ºC 6ºCChemical Oxygen Demand (COD)Plastic, Glass 6ºCFilterDark Plastic, Amber GlassPlastic, GlassPlastic, GlassFilters: freeze 6ºC 6ºC 6ºCHNO3 (7)field filter 0.45 um HNO3,qualify if lab-filtered (7)(8)HCl or BrClfield filter 0.45 um HCl or BrCl,qualify if lab-filtered (8)28 daysAPHA / EPA 1631E28 daysAPHA / EPA 1631EAggregate OrganicsChlorophyll a and PhaeophytinSurfactants (Methylene Blue Active Substances)Total Phenols (4AAP)HNO3, store in dark,sodium sulfite if chlorinated,collect with no headspacenonenonefilter, H2SO4 or HClnonefield filterH2SO4 or HClnoneH2SO4 (field or lab)nonefield filter, store in darkunfiltered, store in darknoneH2SO414 daysAPHA 53203 days3 days28 days3 days14 days28 days14 days28 days3 daysFilters: 28 days2 days3 days28 daysAPHA / BC MOEAPHA / BC MOEAPHABC MOEAPHA (alkalinity)APHAAPHA (alkalinity)APHABC MOEAPHA / BC MOEAPHANaHSO4, HCl, or H2SO4noneHCl or H2SO4none14 / 40 days7 / 40 days28 days28 daysEPA 3511SW846 Ch4 2007EPA 40CFR 2012BC MOEAPHAExtractable HydrocarbonsExtractable Hydrocarbons (LEPH, HEPH, EPH)Amber Glass 6ºCOil and Grease / Mineral Oil and GreaseWaste Oil ContentAmber GlassAmber Glass 6ºC 6ºCA-5

BC MOE SAMPLE PRESERVATION & HOLDING TIME REQUIREMENTS(1,2)Parameter on: l Organic CompoundsGlass 6ºCHalogenated Hydrocarbons (Semi-Volatile)Amber Glass 6ºCHerbicides, Acid ExtractableAmber Glass 6ºCPotassium Dihydrogen Citrate (solid), pH 3.8, 9.2-9.5 g/L, 100 mg/L Na2S2O3 if chlorinatedChlorAC buffer, pH 3,1.8mL / 60 mL sample, 100 mg/L Na2S2O3 if chlorinatednone,100 mg/L Na2S2O3 if chlorinated0.5g Ascorbic Acid / L NaHSO4 or H2SO4nonenone100 mg/L Na2S2O3 if chlorinatedNaHSO4, HCl, or H2SO4none100 mg/L Na2S2O3 if chlorinatedHCl (optional), store in dark,50 mg/L Na2SO3 if chlorinated 6ºC100 mg/L Na2S2O3 if chlorinated7 / 21 daysEPA 549.2 6ºC 6ºCnonenoneNaHSO4, HCl, or H2SO4none(0.5g Ascorbic Acid 0.4g NaOH) / Lnone3 mg Na2S2O3 (see BC Lab Manual methodfor more details)7 / 40 daysunlimited14 / 40 days7 / 40 days14 / 40 days7 / 40 daysSW846 Ch4 2007SW846 Ch4 2007EPA 3511SW846 Ch4 2007Alberta Env AE129SW846 Ch4 2007Carbamate PesticidesChlorinated and Non-chlorinated PhenolicsDioxins / FuransGlyphosate / AMPAGlycolsParaquat / DiquatPesticides (NP, OP, OC)Polychlorinated Biphenyls (PCBs)Polycyclic Aromatic Hydrocarbons (PAHs)Resin Acids, Fatty AcidsVolatile Organic Compounds (Trihalomethanes)Amber GlassAmber GlassAmber GlassAmber Glass or PolypropyleneDark Plastic(protect from light)Amber GlassAmber Glass 6ºC 6ºC 6ºC 6ºCAmber Glass 6ºCAmber Glass 6ºC43mL Glass VOC Vials(2-3) 6ºC28 daysEPA 531.2,APHA 6610B28 daysEPA 531.17 daysEPA 8321A14 / 40 daysAlberta Env AE1307 / 40 daysunlimited14 days14 / 40 days7 / 40 days7 / 40 daysSW846 Ch4 2007SW846 Ch4 2007APHA 6651BEPA 3511SW846 Ch4 2007SW846 Ch4 2007APHA 6640AAPHA 6640A14 / 21 days14 daysBC MOE14 daysBC MOE43mL Glass VOC Vials(2-3) 6ºC200 mg NaHSO4, or 3 mg Na2S2O3 ifchlorinated (see BC Lab Manual method forother options and details)Sterile Glass or PlasticSterile Glass or PlasticSterile Glass or PlasticSterile Glass or Plastic 8ºC, do not freeze 8ºC, do not freeze 8ºC, do not freeze 8ºC, do not freezeNa2S2O3Na2S2O3Na2S2O3Na2S2O330 hours (5)96 hours30 hours (5)24 hoursBC CDC / APHA 9060BEPA 1623 / APHA 9060BAPHA 9060BAPHA 9215Plastic, Glass (non-toxic)Plastic, Glass (non-toxic)Plastic, Glass (non-toxic)Plastic, Glass (non-toxic)Plastic, Glass (non-toxic)4 2ºC4 2ºC4 2ºC4 2ºC4 2ºCcollect with no headspacecollect with no headspacecollect with no headspacecollect with no headspacecollect with no headspace5 days5 days3 days5 days5 daysEC EPS 1/RM/14 & 11EC EPS 1/RM/14 & 11EC EPS 1/RM/24EC EPS 1/RM/13 & 9EC EPS 1/RM/13 & 9Bromide / Chloride / FluorideCyanide (WAD / SAD)Hexavalent ChromiumMetals, TotalMercury, TotalMoisturepHSulfidePlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, GlassPlastic, Glassno requirement 6ºC 6ºCno requirementno requirement 6ºCno requirement 6ºCunlimited14 days30 / 7 days180 days28 days14 days365 days7 daysCarter (Table 4.1)SW846 Ch3 2007SW846 Ch3 2007 / EPA 3060ASW846 Ch3 2007SW846 Ch3 2007Puget Sound ProtocolsCarterPuget Sound ProtocolsTCLP - MercuryPlastic, Glassno requirementTCLP - MetalsPlastic, Glassno requirementnonestore in dark, field moiststore field moistnonenonenonenonestore field moistsample: noneTCLP extract: HNO3, HCl, or BrClsample: noneTCLP extract: HNO3Plastic, GlassPlastic, GlassGlassGlassGlassGlassGlass 6ºCno requirement 6ºC 6ºC 6ºC 6ºC 6ºCnonedried statenonenonenonenonenoneGlass 6ºCnone28 daysGlassGlassGlassGlass 6ºC 6ºC 6ºC 6ºCGlass 6ºCGlassPre-weighed sealed glass vialcharged with methanolpreservative glass soil jar for moistureHermetic sampler glass soil jar for moisture(6) 6ºCnonenonenonenonesample: noneTCLP extract: NaHSO4, HCl, or H2SO4none 6ºC 6ºCVolatile Organic Compounds (VOC, BTEX,VH)Microbiological ParametersColiforms, Total, Fecal, and EcoliCryptosporidium, GiardiaEnterococcusHeterotrophic Plate CountToxicityDaphnia, Chronic 21day / Chronic EC25Daphnia, LC50 / LT50MicrotoxTrout, LC50Trout, LT50Soil and SedimentInorganics28 / 28 daysEPA 1311180 / 180 daysEPA 131128 daysunlimited14 / 40 daysunlimited14 / 40 days14 / 40 days14 / 40 days14 / 40 daysunlimited14 / 40 days14 / 40 daysSW846 Ch3 2007Carter (Table 4.1)SW846 Ch4 2007SW846 Ch4 2007SW846 Ch4 2007SW846 Ch4 2007SW846 Ch4 2007SW846 Ch3 2007,Puget Sound ProtocolsSW846 Ch4 2007SW84

A - 3 Quality Assurance Revision Date: October 2015 . LABORATORY QA/QC GUIDELINES . 1.0 INTRODUCTION . This chapter specifies essential QA/QC activities to enable laboratories to achieve reproducible results on