ASTM_D_2222_-_14.pdf

Designation:D222214Standard Test Method forMethanol Extract of Vinyl Chloride Resins1This standard is issued under the fixed designation D2222;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.Scope*1.1 This test method covers the determination of the metha-nol extract,or nonvolatile methanol-soluble portion,of vinylchloride resins.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.NOTE1There is no known ISO equivalent to this standard.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-tics3.Terminology3.1 DefinitionsDefinitions are in accordance with Termi-nologies D883 and D1600 unless otherwise indicated.4.Summary of Test Method4.1 The methanol-soluble materials are extracted from theresin in a Soxhlet extractor,the methanol evaporated todryness,and the residue weighed as the weight percentmethanol extract.5.Significance and Use5.1 The methanol extract test is most commonly employedwith paste-or dispersion-type vinyl resins intended for organo-sol or plastisol applications.The test result is a quantitativemeasure of the methanol-soluble,nonvolatile,essentially non-polymeric content of the virgin,unmodified resin.The majoringredient removed is the soap system employed in thepolymerization reaction;methanol extract provides a measureof lot-to-lot uniformity of the resin in this respect.6.Apparatus6.1 Soxhlet Extractor.6.2 Extraction Thimbles,33 by 94-mm.6.3 Oven,Constant-Temperature,maintained at 105 6 3 C.6.4 Electric Heating Mantle for a 250-mL extractor flask,orelectric strip heaters,equipped with a suitable variable trans-former to control the rate of heating.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.It is possible to useother grades,provided it is first ascertained that the reagent isof sufficiently high purity to permit its use without lesseningthe accuracy of the determination.8.Procedure8.1 Weigh to the nearest 0.001 g approximately 12 g of theresin sample into an empty extraction thimble.8.2 Cover the resin in the thimble with a small pad of glasswool to prevent spattering of resin during the extraction andplace the thimble in the extractor.8.3 Weigh to the nearest 0.001 g and record the tare weightof a clean,dry,flat-bottom,extractor flask containing a Raschigring.8.4 Add 200 mL of anhydrous methanol to the flask andconnect the flask to the extractor.8.5 Run a blank determination on the methanol simultane-ously with each set of extractions.8.6 Start the extraction and regulate the reflux so that themethanol collecting in the thimble drains at least six times perhour.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials(Section D20.15.08).Current edition approved Aug.1,2014.Published September 2014.Originallyapproved in 1963.Last previous edition approved in 2013 as D2222 13.DOI:10.1520/D2222-14.2For 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 8.7 Timing the extraction from the complement of the firstcycle,extract the resin for 6 h 6 10 minutes.NOTE2Continuous or bulk extractions that do not employ anextractor assembly require approximately 12 h to complete.8.8 Drain all the methanol from the extractor into the flaskand evaporate most of the methanol over a steam bath.8.9 Complete the methanol evaporation by heating the flaskin an oven at 105 6 3 C for 30 minutes.8.10 Cool the flask in a desiccator for 1 hour.8.11 Obtain two weights within 30-min intervals that agreeto 60.001 gram.8.12 Run a blank using the same procedure but omitting theresin sample.9.Calculation9.1 Calculate the percentage of methanol extract as follows:Methanol extract,%5A 2 B 2 C!3100/S!where:A=weight of flask,Raschig ring,and extract,B=tare weight of flas