ASTM_D_4457_-_02_2014.pdf

Designation:D445702(Reapproved 2014)Standard Test Method forDetermination of Dichloromethane and 1,1,1-Trichloroethanein Paints and Coatings by Direct Injection into a GasChromatograph1This standard is issued under the fixed designation D4457;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()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of totalamount of dichloromethane or 1,1,1-trichloroethane,or both,inpaints and coatings.It has been evaluated for cellulose nitrate,alkyd,vinyl,and styrene-butadiene systems.It has not yet beenevaluated for other formulations,but is believed to be appli-cable.The established working range of this test method isfrom 31 to 65%for 1,1,1-trichloroethane and 32 to 78%fordichloromethane.There is no reason to believe it will not workoutside of these ranges.The presence of 1-propanol in paintsand coatings requires the use of a different internal standard.(See also Practice E260.)1.2 The values stated in inch-pound units are to be regardedas standard.The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.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.Specific hazardstatements are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E260 Practice for Packed Column Gas Chromatography3.Summary of Test Method3.1 Anhydrous 1-propanol(see 10.5)is added as an internalstandard to suitable aliquot of the whole paint.The aliquot isthen diluted with dimethylformamide and injected onto a gaschromatographic column containing a porous polymer packingthat separates dichloromethane and 1,1,1-trichloroethane fromother volatile compounds.4.Significance and Use4.1 Use of 1,1,1-trichloroethane and dichloromethane,which do not measurably contribute to the atmospheric oxidantlevel,is a way for industry to meet government or otherregulations on volatile organic compounds.This test method isdesigned to determine the content of these halohydrocarbonsolvents in paints and coatings.That content can subsequentlybe used in calculating the volatile organic compound content ofa coating.5.Apparatus5.1 Chromatograph,any gas-liquid chromatographic instru-ment equipped with a thermal conductivity detector andcapable of being temperature programmed(see Table 1).Optionally,a flame ionization detector may be used if thesample is diluted so that no more than 1000 ppm each ofdichloromethane and 1,1,1-trichloroethane is present in theinjected specimen.5.2 Recorder,a recording potentiometer with a full-scaledeflection of 10 mV,a full-scale response time of 2 s or less,and a maximum noise of 60.03%of full scale.5.3 Pre-Column,40 in.(100 mm)long by18in.(3.2 mm)outside diameter stainless steel,packed with glass wool,fittedon the entrance end of the column to retain any nonvolatilematerials and minimize sludge buildup in the column.5.4 Column,4 ft(1.22 m)long by18in.(3.2 mm)outsidediameter stainless steel,packed with 80/100 mesh(150 to180 m)porous polymer packing material,4or other suitablematerial.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved July 1,2014.Published July 2014.Originally approvedin 1985.Last previous edition approved in 2008 as D4457 02(2008).DOI:10.1520/D4457-02R14.2For referenced ASTM standards,visit the ASTM website,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.3The last approved version of this historical standard is referenced onwww.astm.org.4Porapak R,a registered trademark of WatersAssociates,Inc.,Milford,MA,hasbeen found satisfactory for this purpose.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.5 Liquid Charging Devices,such as microsyringes of 5-Lor 10-L capacity,cleaned with acetone or other suitablesolvent.Visually inspect for plugs or cracks before and aftereach injection.5.6 Vials,25-mL to minimize head space,capable of beingseptum sealed.56.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests,unless otherwise specified(as in 6.7).Unlessotherwise indicate