ASTM_D_3742_-_98.pdf

Designation:D 3742 98Standard Test Method for1,1,1-Trichloroethane Content1This standard is issued under the fixed designation D 3742;the number immediately following the designation indicates the 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(e)indicates an editorial change since the last revision or reapproval.e1NOTESection 10,Keywords,was added in June 1994.1.Scope1.1 This test method provides a basis for the determinationof the 1,1,1-trichloroethane(weight%)in the presence ofstabilizers and impurities,in virgin or reclaimed 1,1,1-trichloroethane products.2.Referenced Documents2.1 ASTM Standards:E 260 Practice for Packed Column Gas Chromatography23.Summary of Test Method3.1 Gas chromatographic scans of 1,1,1-trichloroethane ofknown purity and the sample under test are prepared.The1,1,1-trichloroethane concentration of the unknown is calcu-lated by comparison of the respective elution peak areas.4.Significance and Use4.1 This test method provides an analysis in weight percentof the 1,1,1-trichloroethane concentration of virgin,or re-claimed 1,1,1-trichloroethane.Compounds that co-elute with1,1,1-trichloroethane may interfere with this test.5.Apparatus5.1 Gas Chromatograph having the following minimumcapabilities:5.1.1 Temperature programmable column over with controlsystems capable of maintaining the chromatographic column atthe prescribed temperature 60.5C.5.1.2 Heated sample injection port.5.1.3 Differential katharometer(hot wire),thermistor-typethermal conductivity detector or hydrogen flame detector.5.1.4 Heated detector section.5.2 Syringe,10 L.5.3 Chromatographic Column,of suitable length and pack-ing similar to:5.3.1 ColumnAnnealed copper or stainless steel tubing,20 ft by18in.(2.4 m by 3.2 mm)in outside diameter.5.3.2 PackingChromosorb W HP,380/100 mesh coatedwith 20 weight%OV1014(or equivalent,polydimethylsiloxane)as the liquid phase.5.3.3 Or other columns or packings capable of providingseparation of 1,1,1-trichloroethane from stabilizers and processimpurities.5.4 Carrier GasDry helium of 99.95 mol%purity.5.5 StandardUninhibited 1,1,1-trichloroethane of knownhigh purity of at least 98.0%.5.6 Flow MeterCapable of measuring in the prescribedgas flow ranges.6.Suggested Analysis Conditions6.1 The following analysis conditions are recommended:Initial Column temperature85CInitial hold time4 minRate8C/minFinal temperature160CFinal hold time16 minDetector temperature250CInjector temperature250CCarrier gas and flow20 He/20 cm3/minSample size2 LNOTE1With a hydrogen flame detector,sample size should bereduced to around 0.2 L to prevent overloading the detector.6.1.1 Employing the conditions recommended,all constitu-ents of 1,1,1-trichloroethane solvents should elute from thecolumn within approximately 30 min.7.Analytical Procedure7.1 Chromatograph 2-L samples of both the standard1,1,1-trichloroethane and unknown material under the condi-tions described in 6.1 or equivalent.Both analyses must beconducted under identical operating conditions.Determinepeak areas of the eluted 1,1,1-trichloroethane in each sample.Calculate weight percentage of 1,1,1-trichloroethane in thesample as shown in 8.1.1This test method is under the jurisdiction of ASTM Committee D-26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved May 10,1998.Published December 1998.Originallypublished as D 3742 79.Last previous edition D 3742 89(Reapproved 1994)e1.2Annual Book of ASTM Standards,Vol 14.01.3Johns-Manville product available from any chromatographic supply company.4Available from any chromatographic supply company.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM8.Calculation8.1 Calculate the percentage of 1,1,1-trichloroethane in thesample as follows:1,1,12TCE%5peak area sample 3%assay standardpeak area standard sample(1)9.Precision and Bias9.1 The precision and bias of this test method have not beendetermined.Good sample volume reproducibility is critical tooverall precision of the method.10.Keywords10.1 assay;chlorinated;gas chromatography;halogenated;1,1,1-trichloroethane;purity;solventThe American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connectionwith any item mentioned in this standard.Users of this standard are expressly advised that determination of the validity of any suchpatent rights,and the risk of 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 withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be a