ASTM D4671-16

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 and health practices and determine the applicability of regulatory limitations prior to use.
Note 1: This standard is equivalent to ISO 17710.

General Information

• Status: Historical
• Publication Date: 31-Mar-2016
• 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)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4671 − 16
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.
3
1. Scope* cialty Chemicals (Withdrawn 2009)
2.2 ISO Standards:
1.1 This test method measures unsaturation in polyether
ISO 17710 Plastics—Polyols for Use in the Production of
polyols. (See Note 1.) It uses 2 mL of ca. 0.05 M mercuric
Polyurethane—Determination of Degree of Unsaturation
acetate reagent in methanol and about1gof sample or less.
4
by Microtitration
This test method uses a potentiometric determination of an end
point.
3. Terminology
1.2 The values stated in SI units are to be regarded as
3.1 Definitions—For definitions of terms used in these test
standard. No other units of measurement are included in this
methods, see Terminology D883.
standard.
1.3 Mercury has been designated by many regulatory agen- 4. Summary of Test Method
cies as a hazardous substance that can cause serious medical
4.1 Carbon-to-carbon unsaturated compounds in the sample
issues. Mercury, or its vapor, has been demonstrated to be
arereactedwithmercuricacetateandmethanolinamethanolic
hazardous to health and corrosive to materials. Caution should
solution to produce acetoxymercuricmethoxy compounds and
5
be taken when handling mercury and mercury containing
acetic acid. The amount of acetic acid released in this
products. See the applicable product Safety Data Sheet (SDS)
equimolar reaction, which is determined by titration with
for additional information. Users should be aware that selling
standard alcoholic potassium hydroxide, is a measure of the
mercury and/or mercury containing products into your state or
unsaturation originally present. Because the acid cannot be
country may be prohibited by law.
titrated in the presence of excess mercuric acetate, due to the
formation of insoluble mercuric oxide, sodium bromide is
1.4 This standard does not purport to address all of the
added to convert the mercuric acetate to the bromide, which
safety concerns, if any, associated with its use. It is the
doesnotinterfere.Inasmuchasthesetestmethodsarebasedon
responsibility of the user of this standard to establish appro-
an acidimetric titration, a suitable correction must be applied if
priate safety and health practices and determine the applica-
the sample is not neutral to phenolphthalein indicator. Take
bility of regulatory limitations prior to use.
care to exclude carbon dioxide, which titrates as an acid and
NOTE 1—This standard is equivalent to ISO 17710.
gives erroneous results.
2. Referenced Documents
5. Significance and Use
2
2.1 ASTM Standards:
5.1 This test method is suitable for quality control, as
D883 Terminology Relating to Plastics
specification tests, and for research.
E180 Practice for Determining the Precision of ASTM
5.2 Side reactions that form unsaturated compounds in
Methods for Analysis and Testing of Industrial and Spe-
polypropylene oxides produce small amounts of polymers with
only one hydroxyl group per chain. These unsaturated poly-
mers lower functionality and molecular weight, while broad-
1
These test methods are under the jurisdiction of ASTM Committee D20 on
ening the overall molecular-weight distribution.
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials - Plastics and Elastomers.
Current edition approved April 1, 2016. Published April 2016. Originally
ɛ1
3
approved in 1987. Last previous edition approved in 2010 as D4671 - 05 (2010) . The last approved version of this historical standard is referenced on
DOI: 10.1520/D4671-16. www.astm.org.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM 4th Floor, New York, NY 10036, http://www.ansi.org.
5
Standards volume information, refer to the standard’s Document Summary page on Sigia, S. and Hanna, J.G., “Quantitative Organic Analysis via Functional
the ASTM website. 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 − 16
6. Interferences mg to a 100-mL titration flask. If the unsaturation value is not
known for a sample, determine an approximate value by using
6.1 This test meth
...

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.
´1
Designation: D4671 − 05(Reapproved 2010) D4671 − 16
Standard Test MethodsMethod 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
ε NOTE—Reapproved with editorial changes in July 2010.
1. Scope Scope*
1.1 TheseThis test methods measuremethod 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.
1.1.1 Test Method A, High-Volume Reagent Method—Uses about 50 mL of 0.1 M mercuric acetate reagent in methanol and 15
g or more of sample. These test methods use an indicator for colorimetric determination of an end point. It is recommended for
polyols with low values (below 0.01 millequivalents per gram (meq/g)) of unsaturation where large sample sizes are required.
1.1.2 Test Method B, Low-Volume Reagent Method—Uses 2 mL of ca. 0.05 M mercuric acetate reagent in methanol and about
1 g of sample or less. These test methods use 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 and health practices and determine the applicability of regulatory
limitations prior to use.
NOTE 1—There is no known ISO equivalent to this standard.This standard is equivalent to ISO 17710.
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)
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 Terminology D883.
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. Test Method A was recommended to ASTM by the Society of the Plastics Industry Polyurethane Raw Materials Analysis Committee.
Current edition approved July 1, 2010April 1, 2016. Published October 2010April 2016. Originally approved in 1987. Last previous edition approved in 20052010 as
ɛ1
D4671 - 05.D4671 - 05 (2010) . DOI: 10.1520/D4671-05R10E01.10.1520/D4671-16.
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.
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.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 − 16
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 potassi
...