ASTM D2998-89(1996)e1

Standard Test Method for Polyhydric Alcohols in Alkyd Resins (Withdrawn 2004)

SCOPE
1.1 This test method covers the qualitative and quantitative determination of the polyols in alkyl resins, including resin- and polymer-modified alkyds. Quantities as low as 0.5% may be detected and measured.
1.2 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.  
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. For a specific hazard statement, see Section 7.
WITHDRAWN RATIONALE
This test method covers the qualitative and quantitative determination of the polyols in alkyl resins, including resin- and polymer-modified alkyds. Quantities as low as 0.5 % may be detected and measured.
Formerly under the jurisdiction of Committee D01 on Paint and Related Coatings, Materials, and Applications, this test method was withdrawn in December 2004 in accordance with section 10.6.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1995
• Withdrawal Date: 14-Dec-2004
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.33 - Polymers and Resins

Relations

• Referred By: ASTM D4626-95(2019) - Standard Practice for Calculation of Gas Chromatographic Response Factors
• Effective Date: 01-Jan-1996

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
e1
Designation:D2998–89(Reapproved 1996)
Standard Test Method for
Polyhydric Alcohols in Alkyd Resins
This standard is issued under the fixed designation D 2998; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Editorial changes were made throughout in November 1996.
1. Scope impact on such important physical parameters of alkyd paints
as weatherability, flexibility, moisture resistance, and adhesion.
1.1 This test method covers the qualitative and quantitative
Use of this test method will provide a means whereby the
determination of the polyols in alkyl resins, including resin-
relative applicability of the alkyd resin to the particular end use
and polymer-modified alkyds. Quantities as low as 0.5 % may
may be estimated by the buyer and the seller.
be detected and measured.
1.2 The values stated in inch-pound units are to be regarded
5. Apparatus
as the standard. The values given in parentheses are for
5.1 Linear Programmed Temperature Gas
information only.
Chromatograph—Any instrument with a thermal conductivity
1.3 This standard does not purport to address all of the
detector and with programming features should be suitable if
safety concerns, if any, associated with its use. It is the
adaptable to the following recommended operating conditions:
responsibility of the user of this standard to establish appro-
Detector cell temperature, °C 300
priate safety and health practices and determine the applica-
Detector cell current, mA 160
bility of regulatory limitations prior to use. For a specific
Injection port temperature, °C 300
hazard statement, see Section 7. Helium flow at exit, cm /min 80
Programmed temperature details:
Approximate column heating rate, °C/min 6
2. Referenced Documents
Starting column temperature, °C 100
2.1 ASTM Standards:
Finishing column temperature, °C 300
D 1193 Specification for Reagent Water
NOTE 1—Flame ionization detectors are not recommended for this test
E 260 Practice for Packed Column Gas Chromatography
as the reaction medium can contaminate the flame jet.
5.2 Column—A 16-ft (4.9-m) length of ⁄4-in. (6.4-mm)
3. Summary of Test Method
outside diameter copper tubing packed with 20 weight percent
3.1 The resin sample is dried, subjected to aminolysis to
of silicone grease on 60 to 80-mesh white flux-calcined
release the polyols, treated directly to form the trimethylsilyl
diatomaceous earth, and conditioned at 315°C until “bleed-
(TMS) ether derivatives of the polyhydric alcohols which are
ing” reaches a minimum.
separated by gas-liquid chromatography. An internal standard
5.3 Column and Instrument Performance—Note the sepa-
is used for quantitative purposes. The description of apparatus
ration of closely adjacent polyol peaks and express as peak
and the recommended operating conditions are presented as a
resolution R as follows:
guide to a satisfactory analysis as all suitable variations in
R 5 2Y/ A 1 B! (1)
~
temperatures, column lengths, substrates, liquid phases, pro-
gramming rates, etc., have not been determined.
where:
Y 5 distance between maxima of closely adjacent peaks,
4. Significance and Use
A 5 base width of first peak A, and
4.1 This test method is designed to identify polyhydric
B 5 base width of peak B.
alcohols and to quantify amounts of polyols contained in alkyl
NOTE 2—If the peak resolution is equal to or greater than 1.0, the
resins. Polyols are significant ingredients in alkyl resins and
column and instrument are in satisfactory condition.
5.4 Syringe, having a fixed needle, 50-µL capacity.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.33 on Polymers and Resins. The sole source of supply of the flux-calcined diatomaceous earth, Chromosorb
Current edition approved April 28, 1989. Published June 1989. Originally W known to the committee at this time is Celite Corp., P. O. Box 5108, Denver, CO
published as D2998 – 71. Last previous edition D2998 – 71 (1981)e . 80217-5108. If you are aware of alternative suppliers, please provide this informa-
Annual Book of ASTM Standards, Vol 11.01. tion toASTM Headquarters. Your comments will receive careful consideration at a
3 1
Annual Book of ASTM Standards, Vol 14.02. meeting of the responsible technical committee, which you may attend.
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D2998
5.5 Erlenmeyer Flask, 125-mL, with standard joint and the silicone grease column of the chromatograph and follow
water-cooled condenser to fit. the operating conditions recommended in 5.1. Hold the tem-
5.6 Micro Test Tube or screw cap vial. perature at 300°C at the completion of the program until all the
volatile components have emerged as shown by the chromato-
6. Reagents
gram.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that TABLE 1 Relative Retention Time of Trimethylsilyl Ethers
all reagents shall conform to the specifications of the Commit-
Retention Time Relative to
Polyol
1,4-Butanediol
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be Ethylene glycol 0.58
Propylene glycol 0.63
used, provided it is first ascertained that the reagent is of
2,3-Butanediol 0.73
sufficiently high purity to permit
...