ASTM_D_3447_-_00a.pdf

Designation:D 3447 00aAn American National StandardStandard Test Method forPurity of Halogenated Organic Solvents1This standard is issued under the fixed designation D 3447;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.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 This test method covers the determination of commonimpurities found in halogenated organic solvents introducedduring the manufacturing of the solvent.Although the absolutesensitivity may vary,sensitivity in the parts per million rangemay be achieved under the chromatographic conditions speci-fied in this test method.1.2 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 Method2.1 This test method is based on a temperature-programmedgas chromatographic separation achieved on a packed columncontaining 30%by weight silicone oil on 80/100 meshdiatomaceous earth.23.Significance and Use3.1 This test method can be used to check the purity ofhalogenated organic solvents by determining the impuritiespresent under the chromatographic conditions specified.3.2 This test can be used for establishing manufacturing andpurchasing specifications.4.Apparatus4.1 Gas Chromatograph,equipped with a 1-mv recorder orelectronic integrator and a thermal conductivity or flameionization detector.4.2 Column,6-m by 3.2-mm outside diameter stainless steeltubing packed with 30%by weight silicone fluid2on 80/100mesh diatomaceous earth or similar capillary.34.3 Syringe,10-L gas chromatographic.4.4 Flow Meter,soap-bubble type or equivalent.4.5 Helium,research grade carrier gas.5.Procedure5.1 Install the column and adjust the helium carrier gas flowto 40 mL/min.5.2 Set up the gas chromatograph according to the param-eters listed as follows:Injection port temperature:200CDetector temperature:220COven initial temperature:50COven final temperature:170CTemperature program rate:10C/min5.3 Inject 1.0 L of sample into the gas chromatograph andstart the temperature program.Simultaneously start the record-ing device to begin recording peak areas.5.4 If an integrator is not used,record the chromatogramusing the minimum detector attenuation setting necessary tokeep each peak on-scale at all times.5.5 Terminate the chromatogram after all peaks have elutedfrom the column.6.Calculation6.1 Obtain from the integrator the areas of all of the peakseluted in the chromatogram and calculate the solvent purity asfollows:purity,%5 100 2A 3 100!/A 1 B!#(1)where:A=summation of the peak areas of the impurities,andB=peak area of trichlorotrifluoroethane.6.2 If an integrator was not used,measure the area of eachpeak from the recorder strip chart as follows:peak area 5 Pn3 Pw1/23 Atten(2)where:Pn=peak height,Pw1/2=peak width measured at12of the peak height,Atten=detector attenuation setting.Proceed to calculate the solvent purity as in 6.1.6.3 The purity in area percent is a reasonable approximationof purity in weight percent when the concentration of impuri-ties is low and when the molecular weights and thermalconductivities of the impurities are similar to the halogenatedorganic solvent being tested.1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved June 10,2000.Published July 2000.Originallypublished as D 3447 91.Last previous edition D 3447 00.2Thirty percent DC-200 on 80/100 mesh Chromosorb W has been found to bea satisfactory packing.Columns containing this packing may be obtained from mostchromatography supply houses.3Chromosorb W has been found satisfactory and can be obtained from mostchromatography supply houses.1Copyright ASTM,100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.7.Precision and Bias7.1 The 95%confidence limits for analyses at the 220 and1000-ppm impurity level are 69 and 628 ppm,respectively.This is based on the analyses of two impurities in two samplesby four analysts on two different days.NOTE1The precision and bias were determined using trichlorotrif-luoroethane.8.Keywords8.1 gas chromatography;halogenated solvent;puritytrichlorotrifluoroethaneThe 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 entir