ASTM D4671-21

Standard Test Method for Polyurethane Raw Materials: Determination of Unsaturation of Polyols

SIGNIFICANCE AND USE
5.1 This test method is suitable for quality control, as specification tests, and for research.  
5.2 Side reactions that form unsaturated compounds in polypropylene oxides produce small amounts of polymers with only one hydroxyl group per chain. These unsaturated polymers lower functionality and molecular weight, while broadening the overall molecular-weight distribution.
SCOPE
1.1 This test method measures unsaturation in polyether polyols. (See Note 1.) It uses 2 mL of ca. 0.05 M mercuric acetate reagent in methanol and about 1 g of sample or less. This test method uses a potentiometric determination of an end point.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Safety Data Sheet (SDS) for additional information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be prohibited by law.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: This standard is equivalent to ISO 17710.  
1.5 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.

General Information

• Status: Published
• Publication Date: 30-Jun-2021
• ICS: 83.040.30 - Auxiliary materials and additives for plastics
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.22 - Cellular Materials - Plastics and Elastomers

Standards Content (Sample)

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.
Designation: D4671 − 21
Standard Test Method for
Polyurethane Raw Materials: Determination of Unsaturation
1
of Polyols
This standard is issued under the fixed designation D4671; 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* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method measures unsaturation in polyether
D883 Terminology Relating to Plastics
polyols. (See Note 1.) It uses 2 mL of ca. 0.05 M mercuric
E180 Practice for Determining the Precision of ASTM
acetate reagent in methanol and about1gof sample or less.
Methods for Analysis and Testing of Industrial and Spe-
This test method uses a potentiometric determination of an end
3
cialty Chemicals (Withdrawn 2009)
point.
E456 Terminology Relating to Quality and Statistics
1.2 The values stated in SI units are to be regarded as
E2935 Practice for Evaluating Equivalence of Two Testing
standard. No other units of measurement are included in this
Processes
standard.
2.2 ISO Standards:
1.3 Mercury has been designated by many regulatory agen- ISO 17710 Plastics—Polyols for Use in the Production of
Polyurethane—Determination of Degree of Unsaturation
cies as a hazardous substance that can cause serious medical
4
issues. Mercury, or its vapor, has been demonstrated to be by Microtitration
hazardous to health and corrosive to materials. Caution should
3. Terminology
be taken when handling mercury and mercury containing
products. See the applicable product Safety Data Sheet (SDS) 3.1 Definitions—Terms used in this standard are defined in
for additional information. Users should be aware that selling accordance with Terminology D883, unless otherwise speci-
mercury and/or mercury containing products into your state or fied. For terms relating to precision and bias and associated
country may be prohibited by law. issues,thetermsusedinthisstandardaredefinedinaccordance
with Terminology E456.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Carbon-to-carbon unsaturated compounds in the sample
priate safety, health, and environmental practices and deter-
arereactedwithmercuricacetateandmethanolinamethanolic
mine the applicability of regulatory limitations prior to use.
solution to produce acetoxymercuricmethoxy compounds and
5
NOTE 1—This standard is equivalent to ISO 17710.
acetic acid. The amount of acetic acid released in this
equimolar reaction, which is determined by titration with
1.5 This international standard was developed in accor-
standard alcoholic potassium hydroxide, is a measure of the
dance with internationally recognized principles on standard-
unsaturation originally present. Because the acid cannot be
ization established in the Decision on Principles for the
titrated in the presence of excess mercuric acetate, due to the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM 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.
1 3
These test methods are under the jurisdiction of ASTM Committee D20 on The last approved version of this historical standard is referenced on
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular www.astm.org.
4
Materials - Plastics and Elastomers. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
Current edition approved July 1, 2021. Published July 2021. Originally approved 4th Floor, New York, NY 10036, http://www.ansi.org.
5
in 1987. Last previous edition approved in 2016 as D4671 - 16. DOI: 10.1520/ Sigia, S. and Hanna, J.G., “Quantitative Organic Analysis via Functional
D4671-21. Groups,” John Wiley and Sons, New York, 1979.
*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 ----------------------
D4671 − 21
formation of insoluble mercuric oxide, sodium bromide is KOH for a 2-mL aliquot. Usually several drops of acid are
added to convert the mercuric acetate to the bromide, wh
...

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: D4671 − 16 D4671 − 21
Standard Test Method for
Polyurethane Raw Materials: Determination of Unsaturation
1
of Polyols
This standard is issued under the fixed designation D4671; 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 This test method measures unsaturation in polyether polyols. (See Note 1.) It uses 2 mL of ca. 0.05 M mercuric acetate reagent
in methanol and about 1 g of sample or less. This test method uses a potentiometric determination of an end point.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues.
Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Caution should be taken when
handling mercury and mercury containing products. See the applicable product Safety Data Sheet (SDS) for additional
information. Users should be aware that selling mercury and/or mercury containing products into your state or country may be
prohibited by law.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
NOTE 1—This standard is equivalent to ISO 17710.
1.5 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E456 Terminology Relating to Quality and Statistics
E2935 Practice for Evaluating Equivalence of Two Testing Processes
1
These test methods are under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular Materials -
Plastics and Elastomers.
Current edition approved April 1, 2016July 1, 2021. Published April 2016July 2021. Originally approved in 1987. Last previous edition approved in 20102016 as
ɛ1
D4671 - 05 (2010)D4671 - 16. . DOI: 10.1520/D4671-16.10.1520/D4671-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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.
3
The last approved version of this historical standard is referenced on www.astm.org.
*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 ----------------------
D4671 − 21
2.2 ISO Standards:
ISO 17710 Plastics—Polyols for Use in the Production of Polyurethane—Determination of Degree of Unsaturation by
4
Microtitration
3. Terminology
3.1 Definitions—For definitions of terms used in these test methods, see Terms used in this standard are defined in accordance with
Terminology D883, unless otherwise specified. For terms relating to precision and bias and associated issues, the terms used in
this standard are defined in accordance with Terminology E456.
4. Summary of Test Method
4.1 Carbon-to-carbon unsaturated compounds in the sample are reacted with mercuric acetate and methanol in a methanolic
5
solution to produce acetoxymercuricmethoxy compounds and acetic acid. The amount of acetic acid released in this equimolar
reaction, which is determined by titration with standard alcoholic potassium hydroxide, is a measure of the unsaturation originally
present. Because the acid cannot be titrated in the presence of excess mercuric acetate, due to the formation of insoluble mercuric
oxide, sodium bromide is added to convert the mercuric acetate to the bromide, which does not interfere. Inasmuch as
...