1、Designation: D 2222 09Standard 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 revision. A number
2、 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
3、 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 determine the applica-bili
4、ty of regulatory limitations prior to use.NOTE 1There is no known ISO equivalent to this test method.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlastics3. Terminology3.1 Definitions: Definitions are in accordan
5、ce 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 percentmethanol extract.5. Significance and Use5
6、.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 content of the virgin, unmodified resin. The m
7、ajoringredient 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 3C.6.4
8、 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 otherwise indicated, it is intended thatall reagents
9、 shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available. Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccu
10、racy 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.
11、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 simulta-neously with each set of extra
12、ctions.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 the complement of the firstcycle, extract the resin for 6 h 6 10 min.NOTE 2Continuous or bulk extractions that do not employ an extra
13、c-tor assembly require approximately 12 h to complete.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 Sept. 1, 2009. Published September 2009. O
14、riginallyapproved in 1963. Last previous edition approved in 2004 as D 2222 94 (2004).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
15、 page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.8 Drain all the methanol from the extractor into the flaskand evaporate most of the methanol
16、 over a steam bath.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 sa
17、mple.9. Calculation9.1 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 sampl
18、e.10. Report10.1 The 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 has not been found.12. Key
19、words12.1 methanol extract; PVC resinSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D 2222 - 94(2004) that may impact the use of this standard. (September 1, 2009)(1) Reworded ISO equivalency statement in accordance withGuide D 4
20、968.(2) Deleted footnotes 3, 4, and 5.(3) Reworded Note 3.(4) No mercury references were found.ASTM 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 expressly advised that determina
21、tion 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 revised, either reapproved or with
22、drawn. 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 attend. If you feel that you
23、r 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).D2222092
