1、Designation: D6806 02 (Reapproved 2012)Standard Practice forAnalysis of Halogenated Organic Solvents and TheirAdmixtures by Gas Chromatography1This standard is issued under the fixed designation D6806; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 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 practice covers the determination of impurities,stabilizers and assay of halogenat
3、ed organic solvents and theiradmixtures by gas chromatography.1.2 It is not the intent of this practice to provide a specificmethod of gas chromatography. The intent of this practice is todefine what is required for a user to demonstrate that a methodto be used is valid. The reason for this approach
4、, as opposed tostating a method, is that gas chromatography is such a dynamicfield that methods are often obsolete by the time they arevalidated. The use of this practice allows the user to use mosteffective technology and demonstrate that the method in usecomplies with a standard practice and is va
5、lid for the analysisof halogenated organic solvents and their admixtures.1.3 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-priate safety and health practices and determine
6、the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals33. Terminology3.1 Purity and assay are used interchangeably in this stan-dar
7、d.3.1.1 Purity or assay are defined as 100 sum(impurities +stabilizer) when impurities and stabilizers are expressed in %;3.1.2 Or 100 sum(impurities + stabilizer)/10 000 whenimpurities are expressed in ppm.3.2 Accuracy is defined per A2.2.1 of Practice E180 or theagreement between an experimentally
8、 determined value andthe accepted reference value.3.3 Precision is defined per A2.1.7 of Practice E180 or thedegree of agreement of repeated measurements of the sameproperty. It is generally expressed in standard deviations orpercent relative standard deviation (s/X) 100, also known ascoefficient of
9、 variation.4. Summary of Practice4.1 This practice will define the requirements for a gaschromatographic (GC) method to be valid for the determina-tion of impurities, stabilizers and assay of halogenated organicsolvents and their admixtures.5. Method Requirements5.1 The GC method must give adequate
10、separation of theimpurities and stabilizers common to the product in question sothat the instrument response (area counts, millivolts, etc.) to theindividual impurities or stabilizers can be measured withadequate precision and accuracy as defined in Section 6.Process knowledge from the supplier or m
11、anufacturer of theproduct is a resource of information as to what those impuritiesand stabilizers are. GC-Mass Spectrometry (GC-MS) is an-other resource to initially determine what components arepresent to be measured. See Table 1 for a list of possibleimpurities and stabilizers for each product.5.2
12、 Non polar capillary columns of about 0.32 mm by 30 mgenerally work well. Table 2 provides a list of columns thatmay prove suitable for the analysis of the halogenated organicproducts.5.3 Instrument ConditionsThe following GC conditionsare often appropriate for the analysis of halogenated organicpro
13、ducts and their admixtures though actual conditions shouldbe optimized for the analysis being performed.5.4 The separation is determined to be adequate by prepar-ing standards of known amounts of the impurities and stabi-lizers in concentrations near enough to the expected concen-trations in the sam
14、ple for the instrument response to be linearover the concentration range of interest. Repeated injections1This practice is under the jurisdiction of ASTM Committee D26 on Haloge-nated Organic Solvents and Fire Extinguishing Agents and is the direct responsi-bility of Subcommittee D26.04 on Test Meth
15、ods.Current edition approved March 1, 2012. Published June 2012. Originallyapproved in 2002. Last previous edition approved in 2007 as D6806 - 02 (2007).DOI: 10.1520/D6806-02R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.
16、For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. 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
17、 19428-2959, United States.(minimum of three) of this standard are made and the accuracyand precision of the method for the individual impurities andstabilizers are determined.5.5 Response to components must not be out of range of thedetector and should be sufficiently Gaussian (symmetrical) toallow
18、 adequate measurement as defined by Section 6. Out ofrange response can be corrected by changing the range of theinstrument or changing sample size.5.6 Purity or assay of unblended halogenated organic sol-vents will be determined by determining the amounts of theindividual impurities and stabilizers
19、 and subtracting the total ofthose impurities and stabilizers from 100 %. Purity or assaywill, unless otherwise stated, be determined by subtractingfrom 100, the sum of impurities (as determined by gaschromatography) and stabilizers only. The values for water,acidity, non-volatile matter and other s
20、uch components will notbe subtracted from 100 % to determine the purity or assay ofthe material in question unless the specifications call for theseitems to be included in the total to be subtracted from 100.5.7 Area percent is generally not suitable for halogenatedorganic products as the sensitivit
21、y to a flame ionizationdetector varies greatly between components, particularly sta-bilizers which do not contain chlorine. Calibration of theinstrument should be done using a standard containing thecomponents of interest in concentrations similar to that ex-pected in the sample being analyzed.5.8 P
22、recision for the assay is determined by performingstatistical analysis of the purity or assay of individual injectionswhich is determined by 100 % sum(stabilizers + impurities).The units for assay or purity will be weight percent unlessotherwise specified.6. Precision and Bias46.1 Adequate precision
23、 and bias is defined by the needs ofthe user of the method.6.2 As a general guideline, the following table showsprecision of a good gas chromatographic method. These valueswere determined experimentally in a round robin betweendifferent laboratories in different companies. Automatic injec-tors were
24、in common use in all participating laboratories andwere used in the round robin.6.3 The average and standard deviation of recovery (aver-age of 3 or 4 results) has been determined to be 100.29 68.02 % with 99.7 % falling between 76 and 124 %. Eighty fivepercent were found to fall between 95 and 105
25、% recovery.6.4 The lower detection limit can be assumed to be threetimes the noise level of the chromatogram. The lower quanti-fication limit can be assumed to be ten times the noise level.The noise level is determined by starting a run without aninjection and allowing the run to go to completion th
26、rough thenormal temperature program and time. Take an average of all4A research report is available from ASTM Headquarters. Request RR:D26-1018.TABLE 1 Impurities and StabilizerProductPossible Impuritiesand StabilizersMethylene Chloride Methyl ChlorideVinyl ChlorideEthyl ChlorideVinylidene ChlorideT
27、rans 1,2-DichloroethyleneCis 1,2-DichloroethyleneChloroformCarbon Tetrachloride2-Methyl-2-ButeneCyclohexaneCyclohexenePropylene OxidePerchloroethylene TrichloroethyleneCarbon Tetrachloride1,1,2-Trichloroethane1,1,2,2-tetrachloroethane1,1,1,2-tetrachloroethanePenta ChloroethaneHexachloroethaneN-Methy
28、l MorpholinePara Tertiary Amyl PhenolCyclohexene OxideBHTN-Methyl PyrroleEthoxy PropionitrileTrichloroethylene Cis and trans 1,2-dichloroethylene1,1,2-trichloroethaneCarbon tetrachloride1,1,2,2-tetrachloroethane1,1,1,2-tetrachloroethaneEthylene DichloridePropylene DichlorideDiisopropyl AmineButylene
29、 OxideThymolN-Methyl PyrroleEthyl AcetateDiisobutyleneTABLE 2 Suggested GC ColumnsDB 624DB 5DB 1701TABLE 3 Instrument ConditionsDetectorFlame ionization detector or other detectorof sufficient sensitivity to accuratelymeasure components of interestInjector Temperature 200CDetector Temperature 200COv
30、en Temperature for Isothermal 80CProgrammed Oven Temperature 50 to 200CCarrier Gas Helium or hydrogenCarrier Gas Flow Rate 1 to 3 mL/minSample Size 0.5 to 1.0 Split Ratio 50:1TABLE 4 Expected PrecisionConcentration% RelativeStandard Deviation1to25ppm 1225 to 100 ppm 2100 to 10 000 11to25% 0.825 to 7
31、5 % 0.575 to 100 % Direct MeasurementBy Difference0.50.1D6806 02 (2012)2of the area counts seen in three such blank runs. This averagearea count will be the background noise for the method.7. Keywords7.1 accuracy; gas chromatography; halogenated organic sol-vent; precisionASTM International takes no
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34、o 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 add
35、ress 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D6806 02 (2012)3
