1、Designation: D 6328 06Standard Guide forQuality Assurance Protocols for Chemical Analysis ofAtmospheric Wet Deposition1This standard is issued under the fixed designation D 6328; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 Atmos
3、phericWet 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 q
4、uality 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 AppendixX2.1.5 This standard does not purport to address all of thesafety concerns, if any, associated
5、 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 limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 596 Guide for Reporting Results of Analysis of WaterD 1193 Sp
6、ecification for Reagent WaterD 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 5012 Guide for Preparation of Materials Used for theCollection and Preservation of Atmospheric Wet Dep
7、osi-tionD 5015 Test Method for pH ofAtmospheric Wet DepositionSamples by Electrometric DeterminationD 5085 Test Method for Determination of Chloride, Nitrate,and Sulfate in Atmospheric Wet Deposition by ChemicallySuppressed Ion ChromatographyD 5086 Test Method for Determination of Calcium, Mag-nesiu
8、m, Potassium, and Sodium in Atmospheric WetDeposition by Flame Atomic Absorption Spectrophotom-etryD 5111 Guide for Choosing Locations and Sampling Meth-ods to Monitor Atmospheric Deposition at Non-UrbanLocationsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent So
9、lutions for ChemicalAnalysis3. Terminology3.1 DefinitionsFor definitions of terms used in this guiderefer to Terminology D 1356 or the ASTM Dictionary ofEngineering Science and Technology.44. Summary of Guide4.1 This guide describes QA procedures to be used inconjunction with standard test methods.4
10、.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 materials usedfor the collection and preservation of AWD are included inGuide D 5012. T
11、he procedures for choosing locations andsampling atmospheric deposition are included in GuideD 5111.1This 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 Ap
12、ril 1, 2006. Published May 2006. Originallyapproved in 1998. Last previous edition approved in 1998 as D 6328 - 98.2The 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 Custome
13、r Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4ASTM Dictionary of Engineering Science and Technology, Tenth Edition,2005. Stock# DEF05.TABLE 1 Common Techniques of Analysis for Atmospheric WetDeposit
14、ion 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+1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C
15、700, West Conshohocken, PA 19428-2959, United States.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the commit-tee on Analytical Reagents of the American Chemical S
16、ociety(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 accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referenceto water shall be u
17、nderstood to mean reagent water conformingto Specification D 1193, Type I.5.3 Standard SolutionsUnless otherwise indicated, refer-ence to standard solutions shall be understood to mean solu-tions conforming to Practice E 200. Standard Solutions areprepared from primary standards or ACS reagent grade
18、 salts ormay be purchased as secondary standards from commerciallaboratory suppliers.6. Storage of Standard Solutions6.1 TFE-fluorocarbon, polyethylene, and polypropylenecontainers are recommended for the storage of standard solu-tions. Glass containers are not suitable for storage of moststandard s
19、olutions needed to analyze AWD 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 are correctly formulated.7.1.1 Confirmation of standard solution analyte concentra-tion by an independ
20、ent 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 analyte concen-trations of the same standard solution prepared by differentanalysts from the same labora
21、tory 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 thestandard solution with the concentration of a certified referencematerial (CRM) (2).7.2 If the confidence in
22、tervals 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 agreement.8. Reference Materials8.1 The reference materials (RM) should be a commerciallyavailable CRM.
23、8.2 Immediately following calibration (Test MethodsD 5015, D 5085, D 5086), at least one RM is to be analyzed toensure that the system is functioning properly and that stan-dards were correctly prepared and that no degradation orcontamination of the standards has occurred. The frequency ofRM analysi
24、s 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 analyst must ensure that the concentration valuefalls within the limits previously established from th
25、e 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 % confidence level) of themeasurement intersects the confidence or tolerance interval of the RM,t
26、here 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 acceptancelimits, reanalyze the RM immediately to determine if thecurrent measurement is reproducible. If this
27、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 correct the condition. Reana-lyze all samples measured after the last RM value that was incontrol
28、.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 D 1193, Type I.9.1.2 Measure reagent blanks each day determinations areperformed or whenever new reagents are u
29、sed 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 all aspects of sample collection, fieldprocessing, preservation, transportation, and laboratory h
30、an-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 D 5012 for specificprocedures.9.2 Evaluation of Blank Data:9.2.1 Reagent blank contamination can be highly v
31、ariabledepending on the source of contamination. When variableconcentrations of analytes are found in reagent 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 sam
32、ple onlywhen the analyte concentration in the blank is low, for example) +10 Yesconductivity % difference 5calculated conductivity measured conductivitymeasured conductivity3 100D6328064APPENDIXES(Nonmandatory Information)X1. AGENCIES THAT PROVIDE REFERENCE SAMPLES FOR ATMOSPHERIC WET DEPOSITION STU
33、DIES ORCONDUCT ATMOSPHERIC WET DEPOSITION LABORATORY INTERCOMPARISONSX1.1 The agencies listed in X1.1.1-X1.1.4 provide refer-ence samples for AWD studies or conduct AWD laboratoryintercomparisons.X1.1.1U.S. Geological Survey,Water Resources Discipline,Branch of Quality AssuranceBox 25046, Mail Stop
34、401,Building 53, Denver Federal CenterDenver, CO 80225-0046X1.1.2Norwegian Institute for Air Research (NILU)P.O. Box 100Instittveien 18N-2027 KjellerNorwayX1.1.3National Water Research Institute (NWRI)867 Lakeshore RoadP.O. Box 5050Burlington, Ontario L7R 4A6CanadaX1.1.4Timothy Coleman (WMO/GAW)CEST
35、MAtmospheric Sciences Research Center251 Fuller RoadAlbany, NY 12203X2. PERCENTILE CONCENTRATION VALUES OF CHEMICAL AND PHYSICAL PARAMETERS MEASURED IN WEEKLYATMOSPHERIC WET DEPOSITION SAMPLESX2.1 Table X2.1 gives the percentile concentration valuesof chemical and physical parameters measured in wee
36、klyAWDsamples.D6328065X3. CONVERSION FACTORSX3.1 Table X3.1 gives the conversion factors for thepercentile concentrations of chemical and physical parametersmeasured in weekly AWD samples (see Table X2.1).TABLE X2.1 Percentile Concentration Values of Chemical andPhysical Parameters Measured in Weekl
37、y Atmospheric WetDeposition SamplesAPercentile Concentration Value (mg/L)Parameter 5th 25th 50th 75th 95thCa2+0.014 0.049 0.111 0.261 0.889Mg2+0.003 0.010 0.023 0.047 0.145K+0.003 0.007 0.017 0.037 0.119Na+0.005 0.019 0.053 0.151 0.825NH4+0.02 0.11 0.24 0.49 1.21NO30.182 0.580 1.075 1.827 3.711Cl0.0
38、21 0.051 0.108 0.259 1.45SO420.133 0.515 0.998 1.706 3.611PO430.009 0.009 0.009 0.009 0.009pH (units) 4.23 4.60 4.96 5.46 6.47Cond. (S/cm) 3.5 7.5 12.3 19.6 39.0ANational Atmospheric Deposition Program (NADP)/National Trends Network(NTN) 2002 (1) wet side samples.TABLE X3.1 Conversion FactorsConcent
39、ration UnitGivenOperation Performed for Conversion DesiredConcentration UnitMultiply Bymg L1A equiv L1mol L1Bmg1mol L1C equiv L1Divide Byequiv L1AmgL1mg L-1 B mol L1equiv L1C mol L1Table of ConstantsABCCa2+49.9 0.04008 2Mg2+82.288 0.024305 2Na+43.4975 0.02299 1K+25.574 0.039098 1NH4+55.436 0.018039
40、1NO316.128 0.062007 1SO4220.821 0.09606 2Cl28.206 0.035453 1D6328066REFERENCES(1) Rothert, Jane, Quality Assurance Report, National Atmospheric Depo-sition Program, 2002, Illinois State Water Survey, Champaign, IL,61820-7495, 2004, pp 8-10.(2) Taylor, John K., Quality Assurance of Chemical Measureme
41、nts, LewisPublishers, Inc., Chelsea, MI, 48118, 1987, p. 328.(3) Rules and Regulations, 1984, Federal Register, Vol 49, No. 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
42、 for the Collection and Analysisof Wet Deposition, Vol. 1, Illinois State Water Survey, EPA ContractNo. CR 810780-01, 1986, p. 14.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard a
43、re expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not
44、 revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which y
45、ou may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D6328067
