ASTM D5790-2018 Standard Test Method for Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography Mass Spectrometry.pdf

1、Designation: D5790 95 (Reapproved 2012)D5790 18Standard Test Method forMeasurement of Purgeable Organic Compounds in Water byCapillary Column Gas Chromatography/Mass Spectrometry1This standard is issued under the fixed designation D5790; the number immediately following the designation indicates the

2、 year oforiginal adoption or, in the case of revision, 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 test method covers the identification and simu

3、ltaneous measurement of purgeable volatile organic compounds. It hasbeen validated for treated drinking water, wastewater, and ground water. This test method is not limited to these particular aqueousmatrices; however, the applicability of this test method to other aqueous matrices must be demonstra

4、ted.1.2 This test method is applicable to a wide range of organic compounds that have sufficiently high volatility and low watersolubility to be efficiently removed from water samples using purge and trap procedures. Table 1 lists the compounds that havebeen validated for this test method. This test

5、 method is not limited to the compounds listed in Table 1; however, the applicabilityof the test method to other compounds must be demonstrated.1.3 Analyte concentrations up to approximately 200 g/L may be determined without dilution of the sample. Analytes that areinefficiently purged from water wi

6、ll not be detected when present at low concentrations, but they can be measured with acceptableaccuracy and precision when present in sufficient amounts.1.4 Analytes that are not separated chromatographically, but that have different mass spectra and noninterferingnon-interferingquantitation ions, c

7、an be identified and measured in the same calibration mixture or water sample.Analytes that have very similarmass spectra cannot be individually identified and measured in the same calibration mixture or water sample unless they havedifferent retention times. Coeluting compounds with very similar ma

8、ss spectra, such as structural isomers, must be reported as anisomeric group or pair. Two of the three isomeric xylenes are examples of structural isomers that may not be resolved on thecapillary column, and if not, must be reported as an isomeric pair.1.5 It is the responsibility of the user to ens

9、ure the validity of this test method for untested matrices.1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.standard. No other units of measurement are included in this standard.1.7 This standard does not purport to addres

10、s all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.8 This international standard was developed

11、 in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.

12、1 ASTM Standards:2D1129 Terminology Relating to WaterD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3871 Test Method for Purgeable Organic Compounds in Water Using Headspace SamplingD3973 Test Method for Low-Molecular Weight Halogenated Hy

13、drocarbons in WaterD4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data (Withdrawn2002)31 This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis fo

14、rOrganic Substances in Water.Current edition approved June 15, 2012Dec. 15, 2018. Published June 2012January 2019. Originally approved in 1995. Last previous edition approved in 20062012 asD5790 95 (2012). (2006). DOI: 10.1520/D5790-95R12.10.1520/D5790-18.2 For referencedASTM standards, visit theAST

15、M 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 website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an ind

16、ication 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 prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be

17、considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E355 Practice for Gas Chromatography Terms and Relationships2.2 Other Document:Documents:Code of Federal Regulations 40 CFR Part 26133. Terminology3.1 De

18、finitionsDefinitions: For definitions of terms used in this test method, refer to Definitions D1129 and Practice E355.3.1.1 For definitions of terms used in this standard, refer to Terminology D1129 and Practice E355.3 Available from the Superintendent of Documents, U.S. Government Printing Office,

19、Washington, DC 20402.Superintendent of Documents, 732 N. Capitol St., NW,Washington, DC 20401-0001, http:/www.access.gpo.gov.D5790 1823.2 Definitions of Terms Specific to This Standard:3.2.1 calibration standardstandard, na solution prepared from the primary dilution standard solution and stock stan

20、dardsolutions of the internal standards and surrogate analytes. The calibration standards are used to calibrate the instrument responsewith respect to analyte concentration.3.2.1.1 DiscussionThe calibration standards are used to calibrate the instrument response with respect to analyte concentration

21、.3.2.2 field duplicates, ntwo separate samples collected at the same time and place under identical circumstances and treatedexactly the same throughout field and laboratory procedures. Analysis of field duplicates gives an indication of the precisionassociated with sample collection, preservation,

22、and storage, as well as with laboratory procedures.3.2.2.1 DiscussionAnalysis of field duplicates gives an indication of the precision associated with sample collection, preservation, and storage, as wellas with laboratory procedures.3.2.3 field reagent blankblank, nreagent water placed in a sample

23、container, taken to the field along with the samples, andtreated as a sample in all respects, including exposure to sampling site conditions, storage, preservation, and all analyticalprocedures. The purpose of the field reagent blank is to determine if test method analytes or other interferences are

24、 present in thefield environment.3.2.3.1 DiscussionThe purpose of the field reagent blank is to determine if test method analytes or other interferences are present in the fieldenvironment.3.2.4 internal standardstandard, na pure analyte analyte, that is not a sample component, added to a solution i

25、n a knownamount, that is used to measure the relative responses of other test method analytes and surrogates that are components of the samesolution. The internal standard must be an analyte that is not a sample component.3.2.5 laboratory duplicatesduplicates, ntwo sample aliquots taken in the analy

26、tical laboratory and analyzed separately withidentical procedures. Analysis of laboratory duplicates gives an indication of the precision associated with laboratory procedures,but not with sample collection, preservation, or storage procedures.3.2.5.1 DiscussionAnalysis of laboratory duplicates give

27、s an indication of the precision associated with laboratory procedures, but not with samplecollection, preservation, or storage procedures.3.2.6 laboratory-fortified blankblank, nan aliquot of reagent water to which known quantities of the test method analytesare added in the laboratory.The laborato

28、ry-fortified blank is analyzed exactly like a sample, and its purpose is to determine whetherthe methodology is in control and whether the laboratory is capable of making accurate and precise measurements at the requireddetection limit.3.2.6.1 DiscussionThe laboratory-fortified blank is analyzed exa

29、ctly like a sample, and its purpose is to determine whether the methodology is incontrol and whether the laboratory is capable of making accurate and precise measurements at the required detection limit.3.2.7 laboratory-fortified sample matrixmatrix, nan aliquot of an environmental sample to which k

30、nown quantities of thetest method analytes are added in the laboratory. The laboratoryfortified sample matrix is analyzed exactly like a sample, and itspurpose is to determine whether or not the sample matrix or the addition of preservatives or dechlorinating agents to the samplecontributes bias to

31、the analytical results. The background concentrations of the analytes in the sample matrix must be determinedin a separate aliquot, and the measured values in the laboratory-fortified sample matrix must be corrected for backgroundconcentrations.3.2.7.1 DiscussionThe laboratory-fortified sample matri

32、x is analyzed exactly like a sample, and its purpose is to determine whether or not the sampleD5790 183matrix or the addition of preservatives or dechlorinating agents to the sample contributes bias to the analytical results. Thebackground concentrations of the analytes in the sample matrix must be

33、determined in a separate aliquot, and the measured valuesin the laboratory-fortified sample matrix must be corrected for background concentrations.3.2.8 laboratory performance check solutionsolution, na solution of one or more compounds (analytes, surrogates, internalstandard, or other test compound

34、s) used to evaluate the performance of the instrument system with respect to a defined set of testmethod criteria.3.2.9 laboratory reagent blankblank, nan aliquot of reagent water that is treated exactly as a sample including exposure toall glassware, equipment, solvents, reagents, internal standard

35、s, and surrogates that are used with other samples. The laboratoryreagent blank is used to determine if test method analytes or other interferences are present in the laboratory environment, thereagents, or the apparatus.3.2.9.1 DiscussionThe laboratory reagent blank is used to determine if test met

36、hod analytes or other interferences are present in the laboratoryenvironment, the reagents, or the apparatus.3.2.10 primary dilution standard solutionsolution, na solution of several analytes prepared in the laboratory from stockstandard solutions and diluted as needed to prepare calibration solutio

37、ns and other needed analyte solutions.3.2.11 purgeable organicorganic, nany organic material that is removed from aqueous solution under the purgingconditions described in this test method.3.2.12 quality control samplesample, na sample matrix containing test method analytes or a solution of method a

38、nalytes ina water-miscible solvent that is used to fortify reagent water or environmental samples.The quality control sample is obtained froma source external to the laboratory and is used to check laboratory performance with externally prepared test materials.3.2.12.1 DiscussionThe quality control

39、sample is obtained from a source external to the laboratory and is used to check laboratory performance withexternally prepared test materials.3.2.13 stock standard solutionsolution, na concentrated solution containing a single certified standard that is a test methodanalyte prepared in the laborato

40、ry with an assayed reference compound. Stock standard solutions are used to prepare primarydilution standards. Commercially available stock standard solutions may be used.3.2.13.1 DiscussionStock standard solutions are used to prepare primary dilution standards. Commercially available stock standard

41、 solutions may beused.3.2.14 surrogate analyteanalyte, na pure analyte that is extremely unlikely to be found in any sample, that is added to asample aliquot in a known amount, and is measured with the same procedures used to measure other components. The purposeof a surrogate analyte is to monitor

42、test method performance with each sample.3.2.14.1 DiscussionThe purpose of a surrogate analyte is to monitor test method performance with each sample.4. Summary of Test Method4.1 Volatile organic compounds with low water-solubility are purged from the sample matrix by bubbling an inert gas throughth

43、e aqueous sample. Purged sample components are trapped in a tube containing suitable sorbent materials. When purging iscomplete, the sorbent tube is heated and backflushed with inert gas to desorb the trapped sample components into a capillary gaschromatography (GC) column interfaced to a mass spect

44、rometer (MS). The GC column is temperature programmed to separatethe test method analytes which are then detected with the MS. Compounds eluting from the GC column are identified by comparingtheir measured mass spectra and retention times to reference spectra and retention times in a database. Refer

45、ence spectra andretention times for analytes are obtained by the measurement of calibration standards under the same conditions used for thesamples. The concentration of each identified component is measured by relating the MS response of the quantitation ion producedby that compound to the MS respo

46、nse of the quantitation ion produced by a compound that is used as an internal standard.Surrogate analytes, whose concentrations are known in every sample, are measured with the same internal standard calibrationprocedure.D5790 1845. Significance and Use5.1 Purgeable organic compounds have been iden

47、tified as contaminants in treated drinking water, wastewater, ground water, andToxicity Characteristic Leaching Procedure (TCLP) leachate. These contaminants may be harmful to the environment and topeople. Purge and trap sampling is a generally applicable procedure for concentrating these components

48、 prior to gaschromatographic analysis.6. Interferences6.1 During analysis, major contaminant sources are volatile materials in the laboratory and impurities in the inert purging gasand in the sorbent trap. Avoid the use of plastic tubing or thread sealants other than PTFE, and avoid the use of flow

49、controllerswith rubber components in the purging device. These materials out-gas organic compounds that will be concentrated in the trapduring the purge operation. Analyses of laboratory reagent blanks provide information about the presence of contaminants. Whenpotential interfering peaks are noted in laboratory reagent blanks, the analyst should change the purge gas source and regeneratethe molecular sieve purge gas filter. Reagents should also be checked for the presence of contaminants. Subtracting blank valuesfrom sample results is