1、Designation: D 2222 94 (Reapproved 2004)Standard Test Method forMethanol Extract of Vinyl Chloride Resins1This standard is issued under the fixed designation D 2222; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、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 This test method covers the determination of the metha-nol extract, or nonvolatile methanol-soluble portion, of vinylchlor
3、ide resins.1.2 The values stated in SI units are to be regarded asstandard.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 determin
4、e the applica-bility of regulatory limitations prior to use.NOTE 1There are no ISO standard covering the primary subjectmatter of this ASTM standard.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1600 Terminology of Abbreviated Terms Relating toPlastics3. Terminol
5、ogy3.1 Definitions: Definitions are in accordance with Termi-nologies D 883 and D 1600 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 p
6、ercentmethanol extract.5. Significance and Use5.1 The methanol extract test is most commonly employedwith paste- or dispersion-type vinyl resins intended for orga-nosol or plastisol applications. The test result is a quantitativemeasure of the methanol-soluble, nonvolatile, essentially non-polymeric
7、 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.36.2 Extraction Thimbles, 33 by 94-mm.46.3 Oven,
8、 Constant-Temperature, maintained at 105 6 3C.6.4 Electric Heating Mantle for a 250-mL extractor flask,or electric strip heaters, equipped with a suitable variabletransformer to control the rate of heating.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless oth
9、erwise 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.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high p
10、urity to permit its use without lessening theaccuracy 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 ex
11、traction 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.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommitt
12、ee D20.15 on Thermoplastic Materials(Section D20.15.08).Current edition approved May 1, 2004. Published June 2004. Originallyapproved in 1963. Last previous edition approved in 1999 as D 2222 94 (1999).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Serv
13、ice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Corning Glass Co. No. 3840, Fisher Scientific Co. No. 9-556 (Size B), orequivalent have been found satisfactory for this purpose.4Fisher Scientific Co. No. 9-
14、655, or equivalent, has been found satisfactory forthis purpose.5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals,
15、 BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.4 Add 200 mL of anhydrous methanol t
16、o the flask andconnect the flask to the extractor.8.5 Run a blank determination on the methanol simulta-neously 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.8.7 Timing the extraction from
17、 the complement of the firstcycle, extract the resin for 6 h 6 10 min.NOTE 2Continuous or bulk extractions that do not employ an extrac-tor 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
18、.8.9 Complete the methanol evaporation by heating the flaskin an oven at 105 6 3C for 30 min.8.10 Allow the flask to cool in a desiccator for 1 h.8.11 Obtain two weights within 30-min intervals that agreeto 60.001 g.8.12 Run a blank using the same procedure but omitting theresin sample.9. Calculatio
19、n9.1 Calculate the percentage of methanol extract as follows:Methanol extract, % 5 A 2 B 2 C! 3 100/S!where:A = weight of flask, Raschig ring, and extract,B = tare weight of flask and Raschig ring,C = gain in weight of flask and Raschig ring during blanktest, andS = weight of sample.10. Report10.1 T
20、he report shall include the following:10.1.1 Complete sampling identification, and10.1.2 Percentage methanol extract, average and range.11. Precision11.1 The average of duplicate determinations should agreeto within 0.1 %.NOTE 3Supporting round-robin data have not been found as yet. Atask group has
21、been formed to generate new data in the event that noprevious data can be found.12. Keywords12.1 methanol extract; PVC resinASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are exp
22、ressly advised that determination of the validity of any such patent rights, and the riskof 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 revis
23、ed, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may
24、 attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 2222 94 (2004)2
