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ASTM D3643-98

(Test Method)

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

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

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 problems, 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
09-Sep-1998
ICS
83.080.10 - Thermosetting materials
Technical Committee
D21 - Polishes
Drafting Committee
D21.02 - Raw Materials
Current Stage
Ref Project

Relations

Replaced By
ASTM D3643-98(2004) - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
Effective Date
01-Sep-2004

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ASTM D3643-98 - Standard Test Method for Acid Number of Certain Alkali-Soluble ResinsASTM D3643-98 - Standard Test Method for Acid Number of Certain Alkali-Soluble Resins
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ASTM D3643-98 - 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 3643 – 98
Standard Test Method for
Acid Number of Certain Alkali-Soluble Resins
This standard is issued under the fixed designation D 3643; 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.
1. Scope 5. Reagents and Materials
1.1 This test method covers the measurement of the free 5.1 Purity of Reagents—Reagent grade chemicals shall be
acidity present in certain alkali-soluble resins. used in all tests. Unless otherwise indicated, it is intended that
1.2 This test method is not suitable for styrene-maleic all reagents shall conform to the specifications of the Commit-
anhydride resins. tee on Analytical Reagents of the American Chemical Society,
1.3 The resin manufacturer should specify whether or not where such specifications are available. Other grades may be
this test method may be used for his product(s). used, provided it is first ascertained that the reagent is of
1.4 This standard does not purport to address all of the sufficiently high purity to permit its use without lessening the
safety concerns, if any, associated with its use. It is the accuracy of the determination.
responsibility of the user of this standard to establish appro- 5.2 Purity of Water—Unless otherwise indicated, references
priate safety and health practices and determine the applica- to water shall be understood to mean reagent water conforming
bility of regulatory limitations prior to use. to Specification D 1193.
5.3 Neutral Solvent Mixture—Mix equal parts of denatured
2. Referenced Documents
alcohol and industrial toluene conforming respectively to the
2.1 ASTM Standards:
requirements described for SDA. 3A (200 proof) and Specifi-
D 362 Specification for Industrial Grade Toluene cation D 362. Neutralize the mixture using 0.1 N KOH solution
D 1152 Specification for Methanol (Methyl Alcohol)
and phenolphthalein indicator solution, until the faint pink
D 1193 Specification for Reagent Water color persists for 1 min.
5.4 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
3. Terminology
1.0 g of phenolphthalein in 100 mL of denatured alcohol (SDA
3.1 Definition:
3A, 200 proof).
3.1.1 acid number—the number of milligrams of potassium
5.5 Potassium Hydroxide, Methyl Alcohol Solution (1
hydroxide (KOH) required to neutralize the alkali-reactive
mL 5 5.6 mg KOH)—Dissolve 6.6 g of potassium hydroxide
groups in1gof material under the conditions of test.
(KOH) in 1 L of methyl alcohol conforming to the require-
3.1.1.1 Discussion—If carboxylic anhydrides are present,
ments described in Specification D 1152. Standardize against
only one half of these groups will be titrated and indicated by
National Institute of Standards and Technology standard
this test method.
sample of acid potassium phthalate No. 84, using phenolphtha-
lein as the indicator. Do not adjust the concentration of the
4. Significance and Use
solution, but calculate the milligrams of KOH per L of
4.1 This test method is used to determine the property of
solution.
maleic anhydride resins functionality. Maleic acid anhydride
6. Procedure
resins functio
...

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ASTM D3643-15(2022)(Test Method)
Standard Test Method for Acid Number of Certain Alkali-Soluble Resins

SIGNIFICANCE AND USE
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.  
4.2 This test method is used to measure a property of acid functionalized resins. Acid number determines the utility of resins as well as being a significant quality control measure.
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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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Standard Test Method for Acid Number of Styrene-Maleic Anhydride Resins

SIGNIFICANCE AND USE
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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4.1 In general, with materials of this type, softening does not take place at a definite temperature. As the temperature rises, these materials gradually and imperceptibly change from brittle solids to soft, viscous liquids. For this reason, the determination of the softening point must be made by a fixed, arbitrary, and closely defined methods if the results are to be comparable.
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1.1 This test method covers the determination of the softening point of certain alkali-soluble resins having uniform plastic flow characteristics as the melting point is approached.  
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4.1 This practice is suitable for all types of akalali-soluble resins. The resin manufacturer shall specify the percent ammonium hydroxide to be used (based on the equivalent weight of resin) and the maximum temperature to be used to achieve solution.
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1.1 This practice is a procedure for preparing solutions of alkali-soluble resins in aqueous ammonia and determining the characteristics of such solutions.  
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1.1 This specification2 covers polytetrafluoroethylene (PTFE) prepared by coagulation of a dispersion. These PTFE resins are homopolymers of tetrafluoroethylene or modified homopolymers containing not more than 1 % by weight of other fluoromonomers. The materials covered herein do not include mixtures of PTFE with additives such as colors, fillers, or plasticizers; nor do they include reprocessed or reground resin or any fabricated articles because the properties of such materials have been irreversibly changed when they were fibrillated or sintered.  
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ASTM D7750-23(Test Method)
Standard Test Method for Cure Behavior of Thermosetting Resins by Dynamic Mechanical Procedures using an Encapsulated Specimen Rheometer

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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.  
5.2 Dynamic mechanical testing provides a sensitive method for determining cure characteristics by measuring the elastic and loss moduli as a function of temperature or time, or both. Plots of cure behavior and tan delta of a material provide graphical representation indicative of cure behavior under a specified time-temperature profile. The presence of fibers within the resin may change the dynamic properties measured within a material. However, it is still possible to compare different resins with the same fiber structure and obtain the relative difference due to the resin cure properties.  
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5.3.2 Processing behavior, as well as changes as a function of temperature or time, or both,  
5.3.3 The effects of processing treatments,  
5.3.4 Relative resin behavioral properties, including cure behavior, damping and impact resistance,  
5.3.5 The effects of reinforcement on cure; the reinforcement can be a fiber or a filler,  
5.3.6 The effects of materials used to bond the resin and reinforcement,  
5.3.7 The effect of formulation additives that might affect processability or performance.  
5.4 This provides a method to assess the cure properties of a thermosetting resin containing woven fiber or other reinforcing materials.  
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.  
1.2 This method is intended to provide means for determining the cure behavior of thermosetting resins on fibers over a range of temperatures from room temperature to 250 °C by forced-constant amplitude techniques (in accordance with Practice D4065). Plots of complex modulus, complex viscosity, and damping ratio or tan delta as a function of time or temperature, or both, quantify the thermal advancement or cure characteristics of a resin or a resin on filler or fiber.  
1.3 Test data obtained by this method is relevant and appropriate for optimizing cure cycles.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4.1 Exception—The Fahrenheit temperature measurement in 10.1 is provided for information only and is not considered standard.  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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