1、Designation: D6328 12Standard Guide forQuality Assurance Protocols for Chemical Analysis ofAtmospheric Wet Deposition1This standard is issued under the fixed designation D6328; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye
2、ar of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide describes quality assurance (QA) protocolsfor the determination of the anions and cations in Atmosphe
3、ricWet Deposition (AWD) shown in Table 1.1.2 Included in this guide are minimum recommendedrequirements for the preparation of calibration standards andsuggested procedures for validating laboratory measurementresults.1.3 This guide describes minimum requirements for thefrequency of analysis of qual
4、ity assurance samples and recom-mends procedures for the evaluation of quality assurance data.1.4 The guides recommendations are based upon expectedanion and cation concentrations in AWD (1)2and AppendixX1.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement
5、 are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitation
6、s prior to use.2. Referenced Documents2.1 ASTM Standards:3D596 Guide for Reporting Results of Analysis of WaterD1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtmospheresD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD5012 Gui
7、de for Preparation of Materials Used for theCollection and Preservation of Atmospheric Wet Deposi-tionD5015 Test Method for pH of Atmospheric Wet DepositionSamples by Electrometric DeterminationD5085 Test Method for Determination of Chloride, Nitrate,and Sulfate inAtmosphericWet Deposition by Chemic
8、allySuppressed Ion ChromatographyD5086 Test Method for Determination of Calcium,Magnesium, Potassium, and Sodium in Atmospheric WetDeposition by Flame Atomic Absorption Spectrophotom-etryD5111 Guide for Choosing Locations and Sampling Meth-ods to Monitor Atmospheric Deposition at Non-UrbanLocationsE
9、200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical Analysis3. Terminology3.1 DefinitionsFor definitions of terms used in this guiderefer to Terminology D1356 or the ASTM Dictionary ofEngineering Science and Technology.44. Summary of Guide4.1 This
10、 guide describes QA procedures to be used inconjunction with standard test methods.4.2 This guide does not include all components of a com-plete QAprogram forAWD measurement systems but providesminimum protocols to assist in the development of such aprogram. The procedures for the preparation of mat
11、erials usedfor the collection and preservation of AWD are included inGuide D5012. The procedures for choosing locations andsampling atmospheric deposition are included in Guide D5111.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is
12、 intended that1This guide is under the jurisdiction of ASTM Committee D22 on Air Qualityand is the direct responsibility of Subcommittee D22.03 on Ambient Atmospheresand Source Emissions.Current edition approved Oct. 1, 2012. Published November 2012. Originallyapproved in 1998. Last previous edition
13、 approved in 2006 as D6328 - 06. DOI:10.1520/D6328-12.2The boldface numbers in parentheses refer to the list of references at the end ofthis guide.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandard
14、s volume information, refer to the standards Document Summary page onthe ASTM website.4ASTM Dictionary of Engineering Science and Technology, Tenth Edition,2005. Stock# DEF05.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1all reagent
15、s shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical Society(ACS), where such specifications are available.5Other reagentsmay be used provided it can be demonstrated that they are ofsufficiently high purity to permit their use without decreasingthe
16、accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water conformingto Specification D1193, Type I.5.3 Standard SolutionsUnless otherwise indicated, refer-ence to standard solutions shall be understood to mean solu-tions
17、conforming to Practice E200. Standard Solutions areprepared from primary standards orACS reagent grade salts ormay be purchased as secondary standards from commerciallaboratory suppliers.6. Storage of Standard Solutions6.1 TFE-fluorocarbon, polyethylene, and polypropylenecontainers are recommended f
18、or the storage of standard solu-tions. Glass containers are not suitable for storage of moststandard solutions needed to analyzeAWD due to the potentialfor sodium contamination.7. Verification of Standard Solutions7.1 Use two or more of the following procedures to ensurethat the standard solutions a
19、re correctly formulated.7.1.1 Confirmation of standard solution analyte concentra-tion by an independent laboratory determination;7.1.2 Confirmation of standard solution analyte concentra-tion by an independent analytical procedure within the labora-tory.7.1.3 Comparison of the standard solution ana
20、lyte concen-trations of the same standard solution prepared by differentanalysts from the same laboratory or comparison of the analyteconcentration of the new standard solution with the analyteconcentration of a prior standard solution; or7.1.4 Comparison of the analyte concentration from thestandar
21、d solution with the concentration of a certified referencematerial (CRM) (2).7.2 If the confidence intervals of the two measurements (ata 95 % confidence level) intersect, the two solutions arestatistically the same. New standard solution(s) must be pre-pared if the results are not in statistical ag
22、reement.8. Reference Materials8.1 The reference materials (RM) should be a commerciallyavailable CRM.8.2 Immediately following calibration (Test MethodsD5015, D5085, D5086), at least one RM is to be analyzed toensure that the system is functioning properly and that stan-dards were correctly prepared
23、 and that no degradation orcontamination of the standards has occurred. The frequency ofRM analysis is specified in the test method but must be at leastone per analytical run.8.3 Evaluation of RM DataCompare the measured RMconcentration to the certified value immediately after measure-ment. The anal
24、yst must ensure that the concentration valuefalls within the limits previously established from the repeatedanalysis of solutions at that concentration level. The measure-ment of samples must be suspended whenever the RM mea-surement system is out of control.NOTE 1If the confidence interval (at a 95
25、 % confidence level) of themeasurement intersects the confidence or tolerance interval of the RM,there is agreement. If not, then a discrepancy exists that needs to beinvestigated (2).8.3.1 When the concentration of the RM differs from thecertified value by greater than the established acceptancelim
26、its, reanalyze the RM immediately to determine if thecurrent measurement is reproducible. If this second measure-ment also differs from the acceptance limits about the certifiedvalue, cease analyzing samples.8.3.2 Whenever RM values indicate that the system is out ofcontrol, determine the reason and
27、 correct the condition. Reana-lyze all samples measured after the last RM value that was incontrol.9. Blanks9.1 Preparation and Frequency of Analysis:9.1.1 Prepare reagent blanks according to the proceduresrecommended in the appropriate test method. Use waterconforming to Specification D1193, Type I
28、.9.1.2 Measure reagent blanks each day determinations areperformed or whenever new reagents are used to check forcontamination in sample preparation or analysis.9.1.3 Use field blanks for analytes whose expected concen-trations are less than 1 mg/L. Field blanks are Type I watersamples subjected to
29、all aspects of sample collection, fieldprocessing, preservation, transportation, and laboratory han-dling as an environmental sample.9.1.4 Other types of blanks may be necessary to determinethe cleanliness of collection vessels, sample storage bottles,and membrane filters. Refer to Guide D5012 for s
30、pecificprocedures.9.2 Evaluation of Blank Data:9.2.1 Reagent blank contamination can be highly variabledepending on the source of contamination. When variable5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reag
31、ents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Common Techniques of Analysis for Atmospheric WetDe
32、position SamplesAutomated Colorimetry Ion ChromatographyNH4+Cl,NO3,SO42,NH4+,Ca2+,Mg2+,Na+,K+Flame Atomic Absorption Spectrophotometry ElectrometricNa+,K+,Ca2+,Mg2+pH, specific conductanceInductively Coupled Plasma SpectrometryNa+,K+,Ca2+,Mg2+D6328 122concentrations of analytes are found in reagent
33、blanks, thesource(s) of contamination should be determined and mini-mized.9.2.2 Subtract the concentration of the analyte in the reagentblank from the concentration of the analyte in the sample onlywhen the analyte concentration in the blank is low, for example) +10 Yesconductivity % difference5calc
34、ulated conductivity2measured conductivitymeasured conductivity3100D6328 124reanalysis criteria in Table 3 are violated. If no errors arefound, reanalyze the samples.13.4.3.2 If neither a transcription, mathematical, or analyti-cal error is responsible for a large negative conductivitydifference valu
35、e, it is probable that the sample contains ionsthat have not been measured and thus have not been includedin the equation. A large positive conductivity difference valueindicates that at least one of the concentration values in thecalculation is incorrect.14. Keywords14.1 atmospheric deposition; ato
36、mic absorption spectropho-tometry; ion chromatography; quality assurance; quality con-trol; wet depositionAPPENDIXES(Nonmandatory Information)X1. PERCENTILE CONCENTRATION VALUES OF CHEMICAL AND PHYSICAL PARAMETERS MEASURED IN WEEKLYATMOSPHERIC WET DEPOSITION SAMPLESX1.1 Table X1.1 gives the percenti
37、le concentration valuesof chemical and physical parameters measured in weeklyAWDsamples.TABLE X1.1 Percentile Concentration Values of Chemical andPhysical Parameters Measured in Weekly Atmospheric WetDeposition SamplesAPercentile Concentration Value (mg/L)Parameter 5th 25th 50th 75th 95thCa2+0.023 0
38、.061 0.130 0.272 0.849Mg2+0.035 0.011 0.024 0.050 0.157K+0.007 0.021 0.052 0.157 0.888Na+0.004 0.011 0.021 0.040 0.119NH4+0.010 0.093 0.230 0.456 1.05NO30.158 0.493 0.895 1.51 3.17Cl0.021 0.051 0.106 0.272 1.57SO420.131 0.475 0.944 1.66 3.42PO430.003 0.005 0.009 0.016 0.045pH (units) 4.25 4.62 4.98
39、5.46 6.45Cond. (S/cm) 3.2 7 10.8 17.7 35.2ANational Atmospheric Deposition Program (NADP)/National Trends Network(NTN) 20052009 (1) wet side samples.D6328 125X2. AGENCIES THAT PROVIDE REFERENCE SAMPLES FOR ATMOSPHERIC WET DEPOSITION STUDIES OR CON-DUCT ATMOSPHERIC WET DEPOSITION LABORATORY INTERCOMP
40、ARISONSX2.1 The agencies listed in X2.1.1-X2.1.3 provide refer-ence samples for AWD studies or conduct AWD laboratoryintercomparisons.X2.1.1U.S. Geological Survey,Office of Water Quality,Branch of Quality SystemsBox 25046, Mail Stop 401,Building 53, Denver Federal CenterDenver, CO 80225-0046X2.1.2No
41、rwegian Institute for Air Research (NILU)P.O. Box 100Instittveien 18N-2027 KjellerNorwayX2.1.3National Water Research Institute (NWRI)867 Lakeshore RoadP.O. Box 5050Burlington, Ontario L7R 4A6CanadaX3. CONVERSION FACTORSX3.1 Table X3.1 gives the conversion factors for the per-centile concentrations
42、of chemical and physical parametersmeasured in weekly AWD samples (see Table X1.1).TABLE X3.1 Conversion FactorsConcentration UnitGivenOperation Performed for Conversion DesiredConcentration UnitMultiply Bymg L1A equiv L1mol L1Bmg1mol L1C equiv L1Divide Byequiv L1Amg1mg L1B mol L1equiv L1C mol L1Tab
43、le of ConstantsAB CCa2+49.9 0.04008 2Mg2+82.288 0.024305 2Na+43.4975 0.02299 1K+25.574 0.039098 1NH4+55.436 0.018039 1NO316.128 0.062007 1SO4220.821 0.09606 2Cl28.206 0.035453 1PO4331.59 0.01053 3D6328 126REFERENCES(1) Central Analytical Laboratory Quality Assurance Reports, NationalAtmospheric Depo
44、sition Program (NRSP-3). 2012. NADP ProgramOffice, Illinois State Water Survey, 2204 Griffith Dr., Champaign, IL61820.(2) Taylor, John K., Quality Assurance of Chemical Measurements,Lewis Publishers, Inc., Chelsea, MI, 48118, 1987, p. 328.(3) Rules and Regulations, 1984, Federal Register, Vol 49, No
45、. 209, p.198.(4) Semonin, R.G., et al., Study of Air Pollution Scavenging, Pub. No.COO-1199-58, Illinois State Water Survey, 1977, p. 63.(5) Peden, M.E., et al., Standard Methods for the Collection andAnalysisof Wet Deposition, Vol. 1, Illinois State Water Survey, EPA ContractNo. CR 810780-01, 1986
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