1、Designation: D6328 12D6328 18Standard 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
2、, the year 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) protocols for the determination of the anions and cations in
3、 Atmospheric WetDeposition (AWD) shown in Table 1.1.2 Included in this guide are minimum recommended requirements for the preparation of calibration standards and suggestedprocedures for validating laboratory measurement results.1.3 This guide describes minimum requirements for the frequency of anal
4、ysis of quality assurance samples and recommendsprocedures for the evaluation of quality assurance data.1.4 The guides recommendations are based upon expected anion and cation concentrations in AWD (1)2 and Appendix X1.1.5 The values stated in SI units are to be regarded as standard. No other units
5、of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine
6、 theapplicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issue
7、dby the World Trade Organization Technical Barriers to Trade (TBT) Committee.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 of AtmospheresD3856 Guide for Manageme
8、nt Systems in Laboratories Engaged in Analysis of WaterD5012 Guide for Preparation of Materials Used for the Collection and Preservation of Atmospheric Wet DepositionD5015 Test Method for pH of Atmospheric Wet Deposition Samples by Electrometric DeterminationD5085 Test Method for Determination of Ch
9、loride, Nitrate, and Sulfate in Atmospheric Wet Deposition by ChemicallySuppressed Ion ChromatographyD5086 Test Method for Determination of Calcium, Magnesium, Potassium, and Sodium in Atmospheric Wet Deposition byFlame Atomic Absorption SpectrophotometryD5111 Guide for Choosing Locations and Sampli
10、ng Methods to Monitor Atmospheric Deposition at Non-Urban LocationsE200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis1 This guide is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcom
11、mittee D22.03 on Ambient Atmospheres andSource Emissions.Current edition approved Oct. 1, 2012May 1, 2018. Published November 2012May 2018. Originally approved in 1998. Last previous edition approved in 20062012 asD6328 06.D6328 12. DOI: 10.1520/D6328-12.10.1520/D6328-18.2 The boldface numbers in pa
12、rentheses refer to the list of references at the end of this guide.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM we
13、bsite.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult pri
14、or editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsFor definitio
15、ns of terms used in this guide refer to Terminology D1356 or theASTM Dictionary of EngineeringScience and Technology.44. Summary of Guide4.1 This guide describes QA procedures to be used in conjunction with standard test methods.4.2 This guide does not include all components of a complete QA program
16、 for AWD measurement systems but providesminimum protocols to assist in the development of such a program. The procedures for the preparation of materials used for thecollection and preservation of AWD are included in Guide D5012. The procedures for choosing locations and samplingatmospheric deposit
17、ion are included in Guide D5111.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the committee on Analytical Reagents of the American Chemical Society (ACS),where su
18、ch specifications are available.5 Other reagents may be used provided it can be demonstrated that they are of sufficientlyhigh purity to permit their use without decreasing the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean
19、 reagent water conforming toSpecification D1193, Type I.5.3 Standard SolutionsUnless otherwise indicated, reference to standard solutions shall be understood to mean solutionsconforming to Practice E200. Standard Solutionssolutions are prepared from primary standards orACS reagent grade salts or may
20、be purchased as secondary standards from commercial laboratory suppliers.6. Storage of Standard Solutions6.1 TFE-fluorocarbon, polyethylene, and polypropylene containers are recommended for the storage of standard solutions.Glass containers are not suitable for storage of most standard solutions nee
21、ded to analyze AWD due to the potential for sodiumcontamination.7. Verification of Standard Solutions7.1 Use two or more of the following procedures to ensure that the standard solutions are correctly formulated.7.1.1 Confirmation of standard solution analyte concentration by an independent laborato
22、ry determination;7.1.2 Confirmation of standard solution analyte concentration by an independent analytical procedure within the laboratory.7.1.3 Comparison of the standard solution analyte concentrations of the same standard solution prepared by different analystsfrom the same laboratory or compari
23、son of the analyte concentration of the new standard solution with the analyte concentrationof a prior standard solution; or7.1.4 Comparison of the analyte concentration from the standard solution with the concentration of a certified reference material(CRM) (2).7.2 If the confidence intervals of th
24、e two measurements (at a 95 % confidence level) intersect, the two solutions are statisticallythe same. New standard solution(s) must be prepared if the results are not in statistical agreement.8. Reference Materials8.1 The reference materials (RM) should be a commercially available CRM.4 ASTM Dicti
25、onary of Engineering Science and Technology, Tenth Edition, 2005. Stock# DEF05.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Lab
26、oratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Common Techniques of Analysis for Atmospheric WetDeposition SamplesAutomated Colorimetry Ion ChromatographyNH4+ Cl, NO3, SO42,
27、 NH4+, Ca2+,Mg2+, Na+, K+Flame Atomic Absorption Spectrophotometry ElectrometricNa+, K+, Ca2+ , Mg2+ pH, specific conductanceInductively Coupled Plasma SpectrometryNa+, K+, Ca2+, Mg2+D6328 1828.2 Immediately following calibration (Test Methods D5015, D5085, D5086), at least one RM is to be analyzed
28、to ensure thatthe system is functioning properly and that standards were correctly prepared and that no degradation or contamination of thestandards has occurred. The frequency of RM analysis is specified in the test method but must be at least one per analytical run.8.3 Evaluation of RM DataCompare
29、 the measured RM concentration to the certified value immediately after measurement.The analyst must ensure that the concentration value falls within the limits previously established from the repeated analysis ofsolutions at that concentration level. The measurement of samples must be suspended whe
30、never the RM measurement system isout of control.NOTE 1If the confidence interval (at a 95 % confidence level) of the measurement intersects the confidence or tolerance interval of the RM, thereis agreement. If not, then a discrepancy exists that needs to be investigated (2).8.3.1 When the concentra
31、tion of the RM differs from the certified value by greater than the established acceptance limits,reanalyze the RM immediately to determine if the current measurement is reproducible. If this second measurement also differsfrom the acceptance limits about the certified value, cease analyzing samples
32、.8.3.2 Whenever RM values indicate that the system is out of control, determine the reason and correct the condition.performcorrective action. Reanalyze all samples measured after the last RM value that was in control.9. Blanks9.1 Preparation and Frequency of Analysis:9.1.1 Prepare reagent blanks ac
33、cording to the procedures recommended in the appropriate test method. Use water conformingto Specification D1193, Type I.9.1.2 Measure reagent blanks each day determinations are performed or whenever new reagents are used to check forcontamination in sample preparation or analysis.9.1.3 Use field bl
34、anks for analytes whose expected concentrations are less than 1 mg/L. Field blanks are Type I water samplessubjected to all aspects of sample collection, field processing, preservation, transportation, and laboratory handling as anenvironmental sample.9.1.4 Other types of blanks may be necessary to
35、determine the cleanliness of collection vessels, sample storage bottles, andmembrane filters. Refer to Guide D5012 for or the EPA Quality Assurance Handbook for Air Pollution Measurement Systems,Volume II for procedures (3)specific procedures. for guidance on specific procedures and criteria.9.2 Eva
36、luation of Blank Data:9.2.1 Reagent blank contamination can be highly variable depending on the source of contamination. When variableconcentrations of analytes are found in reagent blanks, the source(s) of contamination should be determined and minimized.9.2.2 Subtract the concentration of the anal
37、yte in the reagent blank from the concentration of the analyte in the sample onlywhen the analyte concentration in the blank is low, for example ) +10 Yesconductivity %difference5calculated conductivity2measured conductivitymeasured conductivity 3100TABLE X1.1 Percentile Concentration Values of Chem
38、ical andPhysical Parameters Measured in Weekly Atmospheric WetDeposition SamplesAPercentile Concentration Value (mg/L)Parameter 5th 25th 50th 75th 95thCa2+ 0.023 0.061 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
39、 0.230 0.456 1.05NO3 0.158 0.493 0.895 1.51 3.17Cl 0.021 0.051 0.106 0.272 1.57SO42 0.131 0.475 0.944 1.66 3.42PO43 0.003 0.005 0.009 0.016 0.045pH (units) 4.25 4.62 4.98 5.46 6.45Cond. (S/cm) 3.2 7 10.8 17.7 35.2A National Atmospheric Deposition Program (NADP)/National Trends Network(NTN) 20052009
40、(1) wet side samples.D6328 186X2.1.2Norwegian 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 facto
41、rs for the percentile concentrations of chemical and physical parameters measured inweekly AWD samples (see Table X1.1).REFERENCES(1) Central Analytical Laboratory Quality Assurance Reports, National Atmospheric Deposition Program (NRSP-3).(NRSP-3), 20122012 NADPProgram Office, Illinois State Water
42、Survey, 2204 Griffith Dr., Champaign, IL 61820.(2) Taylor, JohnJ. K., Quality Assurance of Chemical MeasurementsQualityAssurance of Chemical Measurements, , Lewis Publishers, Inc., Chelsea, MI,48118, 1987, p. 328.(3) Environmental Protection Agency (EPA), Quality Assurance Handbook for Air Pollution
43、 Measurement Systems, Volume II, EPA Publication No.EPA-454/B-13-003, Office of Air Quality Planning and Standards, RTP, NC, May 2013, available at: https:/www3.epa.gov/ttnamti1/files/ambient/pm25/qa/QA-Handbook-Vol-II.pdf (accessed October 19, 2016).(4) Rules and RegulationsRules and Regulations, ,
44、 1984, Federal Register, Vol 49, No. 209, p. 198.(5) Semonin, R.G., R. G., et al., Study of Air Pollution ScavengingStudy of Air Pollution Scavenging, , Pub. No. COO-1199-58, Illinois State WaterSurvey, 1977, p. 63.(6) Peden, M.E., et al., Standard Methods for the Collection and Analysis of Wet Depo
45、sitionStandard Methods, Vol 1for the Collection and Analysis ofWet Deposition, Vol. 1, , Illinois State Water Survey, EPA Contract No. CR 810780-01, 1986, p. 14.TABLE X3.1 Conversion FactorsConcentration UnitGivenOperation Performed for Conversion DesiredConcentration UnitMultiply Bymg L1 A equiv L1
46、mol L1 B mg L1mol L1 C equiv L1Divide Byequiv L1 A mg L1mg L1 B mol L1equiv L1 C mol L1Table of ConstantsA B 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 1NO3 16.128 0.062007 1SO42 20.821 0.09606 2Cl 28.206 0.035453 1PO43 31.59 0.01053 3D632
47、8 187(7) CRC Handbook of Chemistry and PhysicsCRC, 1987Handbook of Chemistry and Physics (1987)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 are expressly advised that determina
48、tion 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 revised, either reapproved or with
49、drawn.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 you 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 Conshohoc
