ASTM_D_5320_-_96.pdf

Designation:D 5320 96Standard Test Methods forDetermination of 1,1,1-Trichloroethane and MethyleneChloride Content in Stabilized Trichloroethylene andTetrachloroethylene1This standard is issued under the fixed designation D 5320;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.1.Scope1.1 These test methods provide a means for determining lowlevels of 1,1,1-trichloroethane and methylene chloride in virginor reclaimed trichloroethylene and tetrachloroethylene.1.2 Two test methods are covered,as follows:1.2.1 Test Method ACapillary column gas chromato-graphic determination of 1,1,1-trichloroethane and methylenechloride in trichloroethylene and tetrachloroethylene.1.2.2 Test Method BPacked column gas chromatographicdetermination of 1,1,1-trichloroethane and methylene chloridein trichloroethylene and tetrachloroethylene.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 the applica-bility of regulatory limitations prior to use.2.Summary of Test Methods2.1 Samples of trichloroethylene or tetrachloroethylene areintroduced into a gas chromatography(GC)equipped witheither a thermal conductivity detector(TCD)or a flameionization detector(FID).Calibration mixtures containingknownconcentrationsofmethylenechloride,1,1,1-trichloroethane,or other impurities of interest are introducedinto the chromatograph in the same manner.The amount ofthese impurities in the samples is then calculated by comparingthe peak areas of these compounds from sample chromato-grams with the corresponding peak areas from calibrationstandard chromatograms.Instrumental parameters are providedto allow the use of either capillary or packed gas chromatog-raphy columns.3.Significance and Use3.1 These test methods can be used to determine theimpurity levels of 1,1,1-trichloroethane and methylene chloridein both trichloroethylene and tetrachloroethylene.3.2 These test methods can be used to determine theimpurity levels of other components,such as stabilizers,foundin trichloroethylene and tetrachloroethylene.The other compo-nents shall be able to be resolved by recommended GCcolumns and the gas chromatograph shall be calibrated withknown concentration of these compounds.4.Interferences4.1 Compounds that co-elute with 1,1,1-trichloroethane,methylene chloride,or other components of interest caninterfere with the accuracy of these test methods.5.Apparatus5.1 Gas Chromatograph,temperature programmable andhaving the following minimum capabilities:5.1.1 Chart Recorder or Electronic IntegratorAn elec-tronic integrator is preferable.5.1.2 Flame Ionization Detector and Capillary Split/Splitless Injection Port(for Test Method A).5.1.3 Thermal Conductivity Detector and Packed ColumnInjection Port(for Test Method B).NOTE1This procedure was tested using the combinations of capillarycolumn with flame ionization detector and packed GC column withthermal conductivity detector.It should be possible,however,to performthis analysis with either column and detector combination.5.2 Gas Chromatography Columns:5.2.1 Column for Test Method A30-m by 0.53-mm innerdiameter fused silica capillary,internally coated to a 3-mthickness with a cross-linked polymethyl silicone.25.2.2 Column for Test Method B10-ft by18-in.outerdiameter stainless steel packed with 3%SP1500 on 80/100mesh Carbopack B,or equivalent.5.3 Syringe,10 L.5.4 Microsyringes,assorted sizes for preparing calibrationstandards.5.5 Volumetric Flasks,100 mL.5.6 Flow Meter,soap bubble or electronic type.5.7 Analytical Balance,capable of weighing to four decimalplaces.1These test methods are under the jurisdiction of ASTM Committee D-26 onHalogenated Organic Solvents and Fire Extinguishing Agents and are the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 10,1996.Published August 1996.Originallypublished as D 5320 92.Last previous edition D 5320 92.2J&W Scientific DB-1 fused silica capillary column(Cat#125-1035)availablefrom J&W Scientific,91 Blue Ravine Rd.,Folsom,CA 95630-4917,or Supelco(SPB-1 Cat#2-5341M)available from Supelco,Inc.,Supelco Park,Bellefonte,PA16823-0048,have been found satisfactory for this purpose.Any equivalent may beused.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM6.Reagents and Materials6.1 Carrier GasChromatographic-grade helium(mini-mum purity:99.99%).6.2 HydrogenHigh purity,for use with flame ionizationdetectors.6.3 AirChromatographic or zero grade,for use with flameionization detectors.6.4 Trichloroethylene,high-purity,for use as a base solvent