1、Designation: D5175 91 (Reapproved 2017)1Standard Test Method forOrganohalide Pesticides and Polychlorinated Biphenyls inWater by Microextraction and Gas Chromatography1This standard is issued under the fixed designation D5175; the number immediately following the designation indicates the year ofori
2、ginal 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.1NOTEWarning notes were editorially updated throughout in December 2017.1.
3、 Scope1.1 This test method (1-3)2is applicable to the determina-tion of the following analytes in finished drinking water,drinking water during intermediate stages of treatment, and theraw source water:AnalyteChemical Abstract ServiceRegistry NumberAAlachlor 5972-60-8Aldrin 309-00-2Chlordane 57-74-9
4、Dieldrin 60-57-1Endrin 72-20-8Heptachlor 76-44-8Heptachlor Epoxide 1024-57-3Hexachlorobenzene 118-74-1Lindane 58-89-9Methoxychlor 72-43-5Toxaphene 8001-35-2AroclorB1016 12674-11-2AroclorB1221 11104-28-2AroclorB1232 11141-16-5AroclorB1242 53469-21-9AroclorB1248 12672-29-6AroclorB1254 11097-69-1Aroclo
5、rB1260 11096-82-5ANumbering system of CAS Registry Services, P.O. Box 3343, Columbus, OH43210-0334.BAroclor is a registered trademark of Monsanto Co.1.2 Detection limits for most test method analytes are lessthan 1 g/L. Actual detection limits are highly dependent onthe characteristics of the sample
6、 matrix and the gas chroma-tography system. Table 1 contains the applicable concentrationrange for the precision and bias statements. Only Aroclor 1016and 1254 were included in the interlaboratory test used toderive the precision and bias statements. Data for other PCBproducts are likely to be simil
7、ar.1.3 Chlordane, toxaphene, and Aroclor products (polychlo-rinated biphenyls) are multicomponent materials. Precision andbias statements reflect recovery of these materials dosed intowater samples. The precision and bias statements may notapply to environmentally altered materials or to samplescont
8、aining complex mixtures of polychlorinated biphenyls(PCBs) and organochlorine pesticides.1.4 For compounds other than those listed in 1.1 or for othersample sources, the analyst must demonstrate the applicabilityof this test method by collecting precision and bias data onspiked samples (groundwater,
9、 tap water) (4) and providequalitative confirmation of results by gas chromatography/mass spectrometry (GC/MS) (5) or by GC analysis usingdissimilar columns.1.5 This test method is restricted to use by or under thesupervision of analysts experienced in the use of GC and in theinterpretation of gas c
10、hromatograms. Each analyst must dem-onstrate the ability to generate acceptable results using theprocedure described in Section 13.1.6 Analytes that are not separated chromatographically,(analytes that have very similar retention times) cannot beindividually identified and measured in the same calib
11、rationmixture or water sample unless an alternative technique foridentification and quantitation exists (see 13.4).1.7 When this test method is used to analyze unfamiliarsamples for any or all of the analytes listed in 1.1, analyteidentifications and concentrations should be confirmed by atleast one
12、 additional technique.1.8 The values stated in SI units are to be regarded asstandard. The values given in parentheses are mathematicalconversions to inch-pound units that are provided for informa-tion only and are not considered standard.1.9 This standard does not purport to address all of thesafet
13、y concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific hazard statements, see Section 9.1This test met
14、hod is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnalysis forOrganic Substances in Water.Current edition approved Dec. 15, 2017. Published January 2018. Originallyapproved in 1991. Last previous edition approved in 2011
15、 as D5175 91 (2011).DOI: 10.1520/D5175-91R17E01.2The boldface numbers in parentheses refer to a list of references at the end ofthis standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in
16、accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.11.10 This international sta
17、ndard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2.
18、Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterTABLE 1 Test Method Precision and BiasAas Functions of ConcentrationCompound Applicable Concentration Range, g/LWater TypeBCDEReagent water Ground waterAlachlor 0.50 to 37.50 So= 0.077X +
19、0.09 So= 0.075X + 0.05St= 0.107X + 0.15 St= 0.086X + 0.29X = 1.004C 0.08 X = 1.059C + 0.03Aldrin 0.04 to 1.42 So= 0.030X + 0.02 So=0.115X + 0.00St= 0.251X + 0.00 St= 0.189X + 0.01X = 1.066C + 0.00 X = 0.945C 0.00Chlordane 0.51 to 50.90 So= 0.083X + 0.06St= 0.125X + 0.19X = 1.037C + 0.06So= 0.062X +
20、0.09St= 0.147X + 0.24X = 0.941C + 0.09Dieldrin 0.10 to 7.53 So= 0.091X + 0.01St= 0.199X + 0.02X = 1.027C + 0.00So= 0.089X + 0.04St= 0.221X + 0.04X = 0.961C + 0.01Endrin 0.10 to 7.50 So=0.116X + 0.01St= 0.134X + 0.02X = 0.958C + 0.01So= 0.045X + 0.15St= 0.196X + 0.07X = 0.958C + 0.05Heptachlor 0.04 t
21、o 1.41 So= 0.104X + 0.01St= 0.206X + 0.02X = 1.002C + 0.02So= 0.058X + 0.02St= 0.153X + 0.02X = 0.964C + 0.02Heptachlor Epoxide 0.04 to 1.42 So= 0.031X + 0.02St= 0.127X + 0.02X = 0.952C + 0.00So= 0.032X + 0.00St= 0.103X + 0.02X = 0.932C + 0.01Hexachlorobenzene 0.01 to 0.37 So= 0.104X + 0.00St= 0.231
22、X + 0.00X = 1.028C 0.00So= 0.148X + 0.00St= 0.301X + 0.00X = 0.901C 0.00Lindane 0.04 to 1.39 So= 0.056X + 0.01St= 0.141X + 0.00X = 1.009C 0.00So= 0.095X + 0.00St= 0.134X 0.00X = 0.909C + 0.00Methoxychlor 0.20 to 15.00 So=0.115X + 0.12St= 0.122X + 0.21X = 0.950C + 0.15So= 0.179X + 0.02St= 0.210X + 0.
23、08X = 1.014C + 0.07Toxaphene 5.63 to 70.40 So= 0.132X 0.32St= 0.273X 0.72X = 1.087C + 0.24So= 0.067X + 0.28St= 0.181X + 1.52X = 0.903C + 0.50PCB-1016 0.50 to 49.80 So= 0.106X + 0.31St= 0.144X + 0.46X = 0.856C + 0.31So= 0.141X + 0.13St= 0.218X + 0.06X = 0.958C + 0.07PCB-1254 0.50 to 50.40 So= 0.122X
24、+ 0.12St= 0.282X + 0.05X = 0.872C 0.01So= 0.126X + 0.17St= 0.396X + 0.02X = 0.938C 0.02ABias = CX.BX = Mean recovery.CC = True concentration value.DSt= Overall standard deviation.ESo= Single analyst standard deviation.D5175 91 (2017)12D3534 Test Method for Polychlorinated Biphenyls (PCBs)in Water (W
25、ithdrawn 2003)4D3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4128 Guide for Identification and Quantitation of OrganicCompounds in Water by Combined Gas Chromatographyand Electron Impact Mass SpectrometryD4210 Practice for Intralaboratory Quality Control Proce-dures
26、and a Discussion on Reporting Low-Level Data(Withdrawn 2002)4E355 Practice for Gas Chromatography Terms and Relation-ships2.2 EPA Standards:5Method 505 Analysis of Organohalide Pesticides and Aro-clors in Water by Microextraction and Gas Chromatogra-phyMethod 680 Determination of Pesticides and PCBs
27、 in Waterand Soil/Sediment by Gas Chromatography/Mass Spec-trometry3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer toTerminology D1129 and Practice E355.3.2 Definitions of Terms Specific to This Standard:3.2.1 field duplicates (FD 1 and FD 2), ntwo separates
28、amples collected at the same time and placed under identicalcircumstances and treated exactly the same throughout fieldand laboratory procedures. Analyses of FD 1 and FD 2 give ameasure of the precision associated with sample collection,preservation and storage, as well as with laboratory procedures
29、.3.2.2 field reagent blank (FRB), nreagent water placed ina sample container in the laboratory and treated as a sample inall respects, including exposure to sampling site conditions,storage, preservation, and all analytical procedures. The re-agent water must be transferred to an empty, clean sample
30、container in the field. The purpose of the FRB is to determineif analytes or other interferences are present in the fieldenvironment.3.2.3 instrument performance check solution (IPC), nasolution of analytes used to evaluate the performance of theinstrument system with respect to test method criteria
31、.3.2.4 laboratory duplicates (LD 1 and LD 2), ntwosample aliquots taken in the analytical laboratory and analyzedseparately with identical procedures. Analyses of LD 1 and LD2 give a measure of the precision associated with laboratoryprocedures but not with sample collection, preservation, orstorage
32、 procedures.3.2.5 laboratory fortified blank (LFB), nan aliquot ofreagent water to which known quantities of the analytes areadded in the laboratory. The LFB is analyzed exactly like asample, and its purpose is to determine whether the method-ology is in control, and whether the laboratory is capabl
33、e ofmaking accurate and precise measurements.3.2.6 laboratory fortified sample matrix (LFM), nan ali-quot of an environmental sample to which known quantities ofthe analytes are added in the laboratory. The LFM is analyzedas a sample, and its purpose is to determine whether the samplematrix contribu
34、tes bias to the analytical results. The back-ground concentrations of the analytes in the sample matrixmust be determined in a separate aliquot and the measuredvalues in the LFM corrected for background concentrations.3.2.7 laboratory reagent blank (LRB), nan aliquot ofreagent water that is treated
35、as a sample including exposure toall glassware, equipment, solvents, and reagents used withother samples. The LRB is used to determine if methodanalytes or other interferences are present in the laboratoryenvironment, the reagents, or the apparatus.3.2.8 standard solution, secondary dilution, na sol
36、ution ofseveral analytes prepared in the laboratory from stock standardsolutions and diluted as needed to prepare calibration solutionsand other needed analyte solutions.3.2.9 standard solution, stock, na concentrated solutioncontaining a single certified standard that is an analyte or aconcentrated
37、 solution of a single analyte prepared in thelaboratory with an assayed reference compound. Stock stan-dard solutions are used to prepare secondary dilution standards.3.2.10 quality control sample (QCS), na sample contain-ing analytes or a solution of analytes in a water-misciblesolvent used to fort
38、ify reagent water or environmental samples.The QCS must be independent of solutions used to preparestandards and should be obtained from a source external to thelaboratory. The QCS is used to check laboratory performancewith externally prepared test materials.4. Summary of Test Method4.1 This is a m
39、icroextraction method in which 35 mL ofsample are extracted with 2 mL of hexane. Two L of theextract are injected into a gas chromatograph equipped with alinearized electron capture detector for separation and analysis.Aqueous calibration standards are extracted and analyzed in anidentical manner to
40、 compensate for possible extraction losses.4.2 The extraction and analysis time is 30 to 50 min persample depending upon the analytes and the analytical condi-tions chosen.4.3 This test method is based largely on EPA Method 505.5. Significance and Use5.1 The extensive and widespread use of organochl
41、orinepesticides and PCBs has resulted in their presence in all partsof the environment. These compounds are persistent and mayhave adverse effects on the environment. Thus, there is a needto identify and quantitate these compounds in water samples.3For referenced ASTM standards, visit the ASTM websi
42、te, 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 ASTM website.4The last approved version of this historical standard is referenced onwww.astm.org.5Available from United States
43、 Environmental ProtectionAgency (EPA), WilliamJefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.D5175 91 (2017)136. Interferences6.1 Interferences may be caused by contaminants insolvents, reagents, glassware, and other sample processingapparatus that lead t
44、o discrete artifacts or elevated baselines ingas chromatograms. All reagents and apparatus must be rou-tinely demonstrated to be free from interferences under theconditions of the analysis by running laboratory reagent blanksas described in 12.2.6.1.1 Glassware must be scrupulously cleaned (2). Clea
45、n allglassware as soon as possible after use by thoroughly rinsingwith the last solvent used in it. Follow by washing with hot tapwater and detergent and thoroughly rinsing with tap andreagent water. Drain dry and heat in an oven or muffle furnaceat 400C for 1 h. Do not heat volumetric ware. Thermal
46、lystable materials might not be eliminated by this treatment.Thorough rinsing with acetone may be substituted for theheating. After drying and cooling, seal and store glassware ina clean environment to prevent any accumulation of dust orother contaminants. Store inverted or capped with aluminumfoil.
47、6.1.2 The use of high purity reagents and solvents helps tominimize interference problems. Purification of solvents bydistillation in all-glass systems may be required.6.2 Phthalate esters, frequently found in plastics, paints, andother common laboratory items, produce a positive response onan elect
48、ron capture detector. Therefore, samples and solventsshould come in contact only with those materials specified inthis test method.6.3 Interfering contamination may occur when a samplecontaining low concentrations of analytes is analyzed imme-diately following a sample containing relatively high con
49、cen-trations of analytes. Between-sample rinsing of the samplesyringe and associated equipment with hexane can minimizesample cross contamination. After analysis of a sample con-taining high concentrations of analytes, one or more injectionsof hexane should be made to ensure that accurate values areobtained for the next sample.6.4 Matrix interferences may be caused by contaminantsthat are coextracted from the sample. Also, note that all theanalytes listed in the scope are not resolved from each other onany one column; one analyte of interes
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