ASTM D5317-1998(2011) Standard Test Method for Determination of Chlorinated Organic Acid Compounds in Water by Gas Chromatography with an Electron Capture Detector《通过伴有电子俘获检测器的气相色谱.pdf
《ASTM D5317-1998(2011) Standard Test Method for Determination of Chlorinated Organic Acid Compounds in Water by Gas Chromatography with an Electron Capture Detector《通过伴有电子俘获检测器的气相色谱.pdf》由会员分享,可在线阅读,更多相关《ASTM D5317-1998(2011) Standard Test Method for Determination of Chlorinated Organic Acid Compounds in Water by Gas Chromatography with an Electron Capture Detector《通过伴有电子俘获检测器的气相色谱.pdf(15页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D5317 98 (Reapproved 2011)Standard Test Method forDetermination of Chlorinated Organic Acid Compounds inWater by Gas Chromatography with an Electron CaptureDetector1This standard is issued under the fixed designation D5317; 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 a gas chromatographic proce-
3、dure for the quantitative determination of selected chlorinatedacids and other acidic herbicides in water. Similar chemicalsmay also be determined by this test method, but it is the usersresponsibility to verify the applicability of this test method toany compounds not listed in this scope. The acid
4、 form of thefollowing compounds were interlaboratory tested using thistest method, and the results were found acceptable:2Analyte Chemical Abstract ServicesRegistry NumberBentazon 25057-89-02,4-D 94-75-72,4-DB 94-82-6DCPA acid metabolites2Dicamba 1918-00-93,5-Dichlorobenzoic acid 51-36-5Dichlorprop
5、120-36-55-Hydroxydicamba 7600-50-2Pentachlorophenol (PCP) 87-86-5Picloram 1918-02-12,4,5-T 93-76-52,4,5-TP (Silvex) 93-72-11.2 This test method may be applicable to the determinationof salts and esters of analyte compounds. The form of each acidis not distinguished by this test method. Results are c
6、alculatedand reported for each listed analyte as the total free acid.1.3 This test method has been validated in an interlaboratorytest for reagent water and finished tap water. The analyst shouldrecognize that precision and bias reported in Section 18 maynot be applicable to other waters.1.4 This te
7、st method is restricted to use by or under thesupervision of analysts experienced in the use of gas chroma-tography (GC) and in the interpretation of gas chromatograms.Each analyst must demonstrate the ability to generate accept-able results with this test method using the procedure describedin 19.3
8、. It is the users responsibility to ensure the validity ofthis test method for waters of untested matrices.1.5 Analytes that are not separated chromatographically,that is, which have very similar retention times, cannot beindividually identified and measured in the same calibrationmixture or water s
9、ample unless an alternate technique foridentification and quantitation exists (16.6, 16.7, and 16.8).1.6 When this test method is used to analyze unfamiliarsamples for any or all of the analytes given in 1.1, analyteidentifications must be confirmed by at least one additionalqualitative technique.1.
10、7 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.8 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
11、-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Sections 6, 8, 9, and 10.2. Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice
12、for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD4210 Practice for Intralaboratory Quality Control Pro
13、ce-dures and a Discussion on Reporting Low-Level Data4D5789 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Organic Constituents42.2 EPA Standard:1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommitte
14、e D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 1992. Last previous edition approved in 2003 as D5317 93 (2003)1.DOI: 10.1520/D5317-98R11.2DCPA monoacid and diacid metabolites are included in the scope of
15、 this testmethod; DCPA diacid metabolite is used for validation studies.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe AS
16、TM website.4Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Method 515.1, Revision 4.0, Methods for the Determinationof Organic Compounds i
17、n Drinking Water52.3 OSHA Standard:29 CFR 1910 OSHA Safety and Health Standards, GeneralIndustry63. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 internal standarda pure analyte(s) added
18、 to a solu-tion in known amount(s) and used to measure the relativeresponses of other method analytes and surrogates that arecomponents of the same solution.3.2.1.1 DiscussionThe internal standard must be an ana-lyte that is not a sample component.3.2.2 surrogate analytea pure analyte(s), which is e
19、x-tremely unlikely to be found in any sample, and which is addedto a sample aliquot in known amount(s) before extraction andis measured with the same procedures used to measure othersample components.3.2.2.1 DiscussionThe purpose of a surrogate analyte is tomonitor method performance with each sampl
20、e.4. Summary of Test Method4.1 The compounds listed in 1.1, in water samples, areconverted into sodium salts by adjusting the pH to 12 withsodium hydroxide solution (240 g/L) and shaking for 1 h.Extraneous neutral material is removed by extraction withmethylene chloride. The sample is acidified, the
21、 acids areextracted with ethyl ether and converted to methyl esters usingdiazomethane. After the excess reagent is removed, the methylesters are determined by capillary column GC using an electroncapture (EC) detector. Other detection systems, such as micro-coulometric and electrolytic conductivity,
22、 are not as sensitiveas EC for measurement of chlorinated acid esters but are morespecific and less subject to interferences. A mass spectrometermay also be used as a detector.4.2 This test method provides a magnesium silicate7cleanup procedure to aid in the elimination of interferences thatmay be p
23、resent.5. Significance and Use5.1 Chlorinated phenoxyacid herbicides, and other organicacids are used extensively for weed control. Esters and salts of2,4-D and silvex have been used as aquatic herbicides in lakes,streams, and irrigation canals. Phenoxy acid herbicides can betoxic even at low concen
24、trations. For example, the 96 h, TLmfor silvex is 2.4 mg/L for bluegills (1)8. These reasons makeapparent the need for a standard test method for such com-pounds in water.6. Interferences6.1 Method interferences may be caused by contaminants insolvents, reagents, glassware and other sample processin
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