ASTM D2222-09

Standard Test Method for Methanol Extract of Vinyl Chloride Resins

SIGNIFICANCE AND USE
The methanol extract test is most commonly employed with paste- or dispersion-type vinyl resins intended for organosol or plastisol applications. The test result is a quantitative measure of the methanol-soluble, nonvolatile, essentially nonpolymeric content 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.
SCOPE
1.1 This test method covers the determination of the methanol extract, or nonvolatile methanol-soluble portion, of vinyl chloride resins.
1.2 The values stated in SI units are to be regarded as standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
Note 1—There is no known ISO equivalent to this test method.

General Information

• Status: Historical
• Publication Date: 31-Aug-2009
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.15 - Thermoplastic Materials

Relations

• Replaces: ASTM D2222-94(2004) - Standard Test Method for Methanol Extract of Vinyl Chloride Resins
• Effective Date: 01-Sep-2009
• Replaced By: ASTM D2222-13 - Standard Test Method for Methanol Extract of Vinyl Chloride Resins
• Effective Date: 01-Nov-2013

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2222 − 09
StandardTest Method for
1
Methanol Extract of Vinyl Chloride Resins
This standard is issued under the fixed designation D2222; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* measure of the methanol-soluble, nonvolatile, essentially non-
polymeric content of the virgin, unmodified resin. The major
1.1 This test method covers the determination of the metha-
ingredient removed is the soap system employed in the
nol extract, or nonvolatile methanol-soluble portion, of vinyl
polymerization reaction; methanol extract provides a measure
chloride resins.
of lot-to-lot uniformity of the resin in this respect.
1.2 The values stated in SI units are to be regarded as
standard.
6. Apparatus
1.3 This standard does not purport to address all of the
6.1 Soxhlet Extractor.
safety concerns, if any, associated with its use. It is the
6.2 Extraction Thimbles, 33 by 94-mm.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6.3 Oven, Constant-Temperature, maintained at 105 6 3°C.
bility of regulatory limitations prior to use.
6.4 Electric Heating Mantle for a 250-mLextractor flask, or
NOTE 1—There is no known ISO equivalent to this test method.
electric strip heaters, equipped with a suitable variable trans-
former to control the rate of heating.
2. Referenced Documents
2
2.1 ASTM Standards:
7. Reagents
D883 Terminology Relating to Plastics
7.1 Purity of Reagents—Reagent grade chemicals shall be
D1600 Terminology forAbbreviatedTerms Relating to Plas-
used in all tests. Unless otherwise indicated, it is intended that
tics
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
3. Terminology
where such specifications are available. Other grades may be
3.1 Definitions: Definitions are in accordance with Termi-
used, provided it is first ascertained that the reagent is of
nologies D883 and D1600 unless otherwise indicated.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
4. Summary of Test Method
4.1 The methanol-soluble materials are extracted from the
8. Procedure
resin in a Soxhlet extractor, the methanol evaporated to
8.1 Weigh to the nearest 0.001 g approximately 12 g of the
dryness, and the residue weighed as the weight percent
resin sample into an empty extraction thimble.
methanol extract.
8.2 Cover the resin in the thimble with a small pad of glass
5. Significance and Use
wool to prevent spattering of resin during the extraction and
5.1 The methanol extract test is most commonly employed
place the thimble in the extractor.
with paste- or dispersion-type vinyl resins intended for organo-
8.3 Weigh to the nearest 0.001 g and record the tare weight
sol or plastisol applications. The test result is a quantitative
ofaclean,dry,flat-bottom,extractorflaskcontainingaRaschig
ring.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
8.4 Add 200 mL of anhydrous methanol to the flask and
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
connect the flask to the extractor.
(Section D20.15.08).
Current edition approved Sept. 1, 2009. Published September 2009. Originally
8.5 Run a blank determination on the methanol simultane-
approved in 1963. Last previous edition approved in 2004 as D2222 – 94 (2004).
ously with each set of extractions.
DOI: 10.1520/D2222-09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
8.6 Start the extraction and regulate the reflux so that the
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
methanol collecting in the thimble drains at least six times per
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. hour.
*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
1

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D2222 − 09
8.7 Timing the extraction from the complement of the first where:
cycle, extract the resin for 6 h 6 10 min.
A = weight of flask, Raschig ring, and extract,
B = tare weight of flask and Raschig ring,
NOTE 2—Continuous or bulk extractions that do not employ an
C = gain in weight of flask and Raschig ring during blank
extractor assembly require approximately 12 h to complete.
test, and
8.8 Drain all the methanol from the extractor into the flask
S = weight of sample.
and evaporate most of the m
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation:D2222–94 (Reapproved 2004) Designation: D 2222 – 09
Standard Test Method for
1
Methanol Extract of Vinyl Chloride Resins
This standard is issued under the fixed designation D 2222; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 Thistestmethodcoversthedeterminationofthemethanolextract,ornonvolatilemethanol-solubleportion,ofvinylchloride
resins.
1.2 The values stated in SI units are to be regarded as standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
NOTE1—There are no ISO standard covering the primary subject matter of this ASTM standard. 1—There is no known ISO equivalent to this test
method.
2. Referenced Documents
2
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics
D 1600 Terminology offor Abbreviated Terms Relating to Plastics
3. Terminology
3.1 Definitions: Definitions are in accordance with Terminologies D 883 and D1600 and D 1600 unless otherwise indicated.
4. Summary of Test Method
4.1 The methanol-soluble materials are extracted from the resin in a Soxhlet extractor, the methanol evaporated to dryness, and
the residue weighed as the weight percent methanol extract.
5. Significance and Use
5.1 The methanol extract test is most commonly employed with paste- or dispersion-type vinyl resins intended for organosol
or plastisol applications. The test result is a quantitative measure of the methanol-soluble, nonvolatile, essentially nonpolymeric
content 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. Apparatus
6.1 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 fora250-mLextractorflask,orelectricstripheaters,equippedwithasuitablevariabletransformer
to control the rate of heating.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
(Section D20.15.08).
Current edition approved May 1, 2004. Published June 2004. Originally approved in 1963. Last previous edition approved in 1999 as D2222–94(1999).
Current edition approved Sept. 1, 2009. Published September 2009. Originally approved in 1963. Last previous edition approved in 2004 as D 2222 – 94 (2004).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
1

---------------------- Page: 1 ----------------------
D2222–09
8. Procedure
8.1 Weigh to the nearest 0.001 g approximately 12 g of the resin sample into an empty extraction 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 place
the thimble in the extractor.
8.3 Weightothenearest0.001gandrecordthetareweightofaclean,dry,flat-bottom,extractorflaskcontainingaRaschigring.
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 times per hour.
8.7
...