ASTM D2222-2013 Standard Test Method for Methanol Extract of Vinyl Chloride Resins《氯乙烯树脂的甲醇萃取标准试验方法》.pdf

1、Designation: D2222 09D2222 13Standard 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

2、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 methanol extract, or nonvolatile methanol-soluble portion, of vinyl chlorideresins.1.

3、2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish app

4、ropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.NOTE 1There is no known ISO equivalent to this test method.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating to Pl

5、astics3. Terminology3.1 Definitions: Definitions are in accordance with Terminologies D883 and D1600 unless otherwise indicated.4. Summary of Test Method4.1 The methanol-soluble materials are extracted from the resin in a Soxhlet extractor, the methanol evaporated to dryness, andthe residue weighed

6、as the weight percent methanol extract.5. Significance and Use5.1 The methanol extract test is most commonly employed with paste- or dispersion-type vinyl resins intended for organosolor plastisol applications. The test result is a quantitative measure of the methanol-soluble, nonvolatile, essential

7、ly nonpolymericcontent of the virgin, unmodified resin. The major ingredient removed is the soap system employed in the polymerization reaction;methanol extract provides a measure of lot-to-lot uniformity of the resin in this respect.6. Apparatus6.1 Soxhlet Extractor.6.2 Extraction Thimbles, 33 by 9

8、4-mm.6.3 Oven, 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 variable transformerto control the rate of heating.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall be used in all t

9、ests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where1 This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subc

10、ommittee D20.15 on Thermoplastic Materials(Section D20.15.08).Current edition approved Sept. 1, 2009Nov. 1, 2013. Published September 2009November 2013. Originally approved in 1963. Last previous edition approved in 20042009as D2222 94 (2004).D2222 09. DOI: 10.1520/D2222-09.10.1520/D2222-13.2 For re

11、ferencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide

12、 the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the sta

13、ndard as published by ASTM is to be considered the official document.*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 States1such specifications are available. Other grades may

14、be used, It is possible to use other grades, provided it is first ascertained thatthe reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.8. Procedure8.1 Weigh to the nearest 0.001 g approximately 12 g of the resin sample into an empty extract

15、ion thimble.8.2 Cover the resin in the thimble with a small pad of glass wool to prevent spattering of resin during the extraction and placethe thimble in the extractor.8.3 Weigh to the nearest 0.001 g and record the tare weight of a clean, dry, flat-bottom, extractor flask containing a Raschig ring

16、.8.4 Add 200 mL of anhydrous methanol to the flask and connect the flask to the extractor.8.5 Run a blank determination on the methanol simultaneously with each set of extractions.8.6 Start the extraction and regulate the reflux so that the methanol collecting in the thimble drains at least six time

17、s per hour.8.7 Timing the extraction from the complement of the first cycle, extract the resin for 6 h 6 10 min.NOTE 2Continuous or bulk extractions that do not employ an extractor assembly require approximately 12 h to complete.8.8 Drain all the methanol from the extractor into the flask and evapor

18、ate most of the methanol over a steam bath.8.9 Complete the methanol evaporation by heating the flask in an oven at 105 6 3C for 30 min.8.10 AllowCool the flask to cool in a desiccator for 1 h.8.11 Obtain two weights within 30-min intervals that agree to 60.001 g.8.12 Run a blank using the same proc

19、edure but omitting the resin sample.9. Calculation9.1 Calculate the percentage of methanol extract as follows:Methanol extract,%5A 2B 2C!3100/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 blank tes

20、t, andS = weight of sample.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 agreeDuplicate determinations shall average to within 0.

21、1 %.NOTE 3Supporting round-robin data has not been found.12. Keywords12.1 methanol extract; PVC resinD2222 132SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D2222 - 94D2222 - 09(2004) that may impact the use of this standard. (Se

22、ptember(November 1, 2009)2013)(1) Reworded ISO equivalency statement in accordance with Guide D4968.(2) Deleted footnotes 3, 4, and 5.(1) RewordedRemoved Note 3non-mandatory language from 7.1, 8.10, and 11.1.(4) No mercury references were found.ASTM International takes no position respecting the val

23、idity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly 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 sub

24、ject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquar

25、ters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may 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 standar

26、d 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2222 133