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ASTM D3643-98(2004)

(Test Method)

Standard Test Method for Acid Number of Certain Alkali-Soluble Resins

Standard Test Method for Acid Number of Certain Alkali-Soluble Resins

SIGNIFICANCE AND USE
This test method is used to determine the property of maleic anhydride resins functionality. Maleic acid anhydride resins functionality determines the utility of resin as well as being a significant quality control test.
SCOPE
1.1 This test method covers the measurement of the free acidity present in certain alkali-soluble resins.
1.2 This test method is not suitable for styrene-maleic anhydride resins.
1.3 The resin manufacturer should specify whether or not this test method may be used for his product(s).
1.4 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.

General Information

Status
Historical
Publication Date
31-Aug-2004
ICS
83.080.10 - Thermosetting materials
Technical Committee
D21 - Polishes
Drafting Committee
D21.02 - Raw Materials
Current Stage
Ref Project

Relations

Replaces
ASTM D3643-98 - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
Effective Date
01-Sep-2004
Replaced By
ASTM D3643-10 - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
Effective Date
01-May-2010

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ASTM D3643-98(2004) - Standard Test Method for Acid Number of Certain Alkali-Soluble ResinsASTM D3643-98(2004) - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
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ASTM D3643-98(2004) - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3643 – 98 (Reapproved 2004)
Standard Test Method for
Acid Number of Certain Alkali-Soluble Resins
This standard is issued under the fixed designation D3643; 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 resins functionality determines the utility of resin as well as
being a significant quality control test.
1.1 This test method covers the measurement of the free
acidity present in certain alkali-soluble resins.
5. Reagents and Materials
1.2 This test method is not suitable for styrene-maleic
5.1 Purity of Reagents—Reagent grade chemicals shall be
anhydride resins.
used in all tests. Unless otherwise indicated, it is intended that
1.3 The resin manufacturer should specify whether or not
all reagents shall conform to the specifications of the Commit-
this test method may be used for his product(s).
tee onAnalytical Reagents of theAmerican Chemical Society,
1.4 This standard does not purport to address all of the
where such specifications are available. Other grades may be
safety concerns, if any, associated with its use. It is the
used, provided it is first ascertained that the reagent is of
responsibility of the user of this standard to establish appro-
sufficiently high purity to permit its use without lessening the
priate safety and health practices and determine the applica-
accuracy of the determination.
bility of regulatory limitations prior to use.
5.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents to water shall be understood to mean reagent water conforming
to Specification D1193.
2.1 ASTM Standards:
5.3 Neutral Solvent Mixture—Mix equal parts of denatured
D362 Specification for Industrial Grade Toluene
alcohol and industrial toluene conforming respectively to the
D1152 Specification for Methanol (Methyl Alcohol)
requirements described for SDA. 3A (200 proof) and Specifi-
D1193 Specification for Reagent Water
cation D362. Neutralize the mixture using 0.1 N KOH solution
3. Terminology
and phenolphthalein indicator solution, until the faint pink
color persists for 1 min.
3.1 Definition:
5.4 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
3.1.1 acid number—the number of milligrams of potassium
1.0 g of phenolphthalein in 100 mLof denatured alcohol (SDA
hydroxide (KOH) required to neutralize the alkali-reactive
3A, 200 proof).
groups in1gof material under the conditions of test.
5.5 Potassium Hydroxide, Methyl Alcohol Solution (1
3.1.1.1 Discussion—If carboxylic anhydrides are present,
mL = 5.6 mg KOH)—Dissolve 6.6 g of potassium hydroxide
only one half of these groups will be titrated and indicated by
(KOH) in 1 L of methyl alcohol conforming to the require-
this test method.
ments described in Specification D1152. Standardize against
4. Significance and Use
National Institute of Standards and Technology standard
sample of acid potassium phthalate No. 84, using phenolphtha-
4.1 This test method is used to determine the property of
lein as the indicator. Do not adjust the concentration of the
maleic anhydride resins functionality. Maleic acid anhydride
solution, but calculate the mill
...

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4.1 This test method is not appropriate for alkali-soluble resins whose acid functionality is due to incorporated anhydrides. Variations in manufacture, storage, and possible contamination of anhydride functional resins may cause partial hydrolysis, or esterification, which will invalidate data from this test method. Anhydride functional resins should be characterized by Test Method D3644.  
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1.1 This test method covers the measurement of the free acidity present in certain alkali-soluble resins.  
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4.1 This test method is used to determine the property of styrene-maleic anhydride resins functionality. Acid functionality determines the utility of resin as well as being a significant quality control test.  
4.2 Because some of the anhydride functionality has been hydrolyzed in the manufacturing process, direct titration with base will produce erroneous data on the total acid content of the fully hydrolyzed resin in use. This test method charges excess alkali to hydrolize the anhydride functionality and neutralize the resulting acid. The remaining unreacted alkali is then back titrated with a standardized acid solution and the acid content is determined by difference.
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5.1 This method provides a simple means of characterizing the cure behavior of a thermosetting resin specimen that is a representation of a composite part. The diameter of the specimen is approximately 38 mm and the thickness ranges from 2.6 mm to 3.2 mm. This corresponds to a sample volume of approximately 3 cm3 to 4 cm3. The data may be used for quality control, research and development, and verifying the cure within processing equipment including autoclaves.  
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5.5 This method is valid for a wide range of oscillation frequencies typically from 0.002 Hz to 50 Hz.
Note 1: It is recommended tha...
SCOPE
1.1 This method covers the use of dynamic mechanical instrumentation for determination and reporting of the thermal advancement of cure behavior of thermosetting resin on an inert filler or fiber in a laboratory. It may also be used for determining the cure properties of resins without fillers or fibers. These encapsulated specimens are deformed in torsional shear using dynamic mechanical methods.  
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