ASTM D4273-23

Standard Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols

SIGNIFICANCE AND USE
5.1 The primary hydroxyl content provides information about the relative reactivities of polyols in the urethane forming reaction with isocyanates.
SCOPE
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy (13C NMR) measures the primary hydroxyl content of ethylene oxide (EO)-propylene oxide (PO) polyether polyols used in preparing flexible polyurethane foams. This method is best suited for polyether polyols with primary hydroxyl contents of 10 to 90 %.  
1.2 The values stated in SI units are to be regarded as standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: There is no known ISO equivalent to this standard.  
1.4 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: 28-Feb-2023
• ICS: 83.080.20 - Thermoplastic materials
• 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: D4273 − 23
Standard Test Method for
Polyurethane Raw Materials: Determination of Primary
1
Hydroxyl Content of Polyether Polyols
This standard is issued under the fixed designation D4273; 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* Fourier-Transform Nuclear Magnetic Resonance (FT-
NMR) Spectrometers for Liquid Samples
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy
13
( C NMR) measures the primary hydroxyl content of ethylene
3. Terminology
oxide (EO)-propylene oxide (PO) polyether polyols used in
3.1 Definitions—Terms used in this standard are defined in
preparing flexible polyurethane foams. This method is best
accordance with Terminology D883 and Practice E2977, unless
suited for polyether polyols with primary hydroxyl contents of
otherwise specified. For terms relating to precision and bias
10 to 90 %.
and associated issues, the terms used in this standard are
1.2 The values stated in SI units are to be regarded as
defined in accordance with Terminology E456.
standard.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 Peaks of the primary and secondary hydroxyl carbons of
responsibility of the user of this standard to establish appro-
polyether polyols used in flexible polyurethane foams are
priate safety, health, and environmental practices and deter- 13
well-resolved in high-resolution C NMR spectra. The pri-
mine the applicability of regulatory limitations prior to use.
mary hydroxyl content is determined from the ratio of the
primary hydroxyl area to the total hydroxyl (primary and
NOTE 1—There is no known ISO equivalent to this standard.
secondary) area.
1.4 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
5.1 The primary hydroxyl content provides information
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical about the relative reactivities of polyols in the urethane
Barriers to Trade (TBT) Committee. forming reaction with isocyanates.
6. Interferences
2. Referenced Documents
2
6.1 Primary hydroxyl PO methylene carbons (where the
2.1 ASTM Standards:
methylene carbon is next to the hydroxyl group and the
D883 Terminology Relating to Plastics
methine carbon is next to the ether oxygen) are integrated with
E456 Terminology Relating to Quality and Statistics
the secondary hydroxyl carbons and are therefore not included
E691 Practice for Conducting an Interlaboratory Study to
in the primary hydroxyl content as measured by this method.
Determine the Precision of a Test Method
Any additional non-polyether polyol compounds in the sample
E2935 Practice for Evaluating Equivalence of Two Testing
that produce NMR peaks in the 68-60 ppm region may
Processes
interfere with the measurement.
E2977 Practice for Measuring and Reporting Performance of
7. Apparatus
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
7.1 Fourier-Transform NMR (FT-NMR) Spectrometer, with
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
carbon-13 capability and a carbon-13 resonance frequency of
Plastics and Elastomers.
50 MHz (proton resonance frequency of 200 MHz) or higher.
Current edition approved March 1, 2023. Published March 2023. Originally
The spectrometer is to have a minimum carbon-13 signal-to-
approved in 1983. Last previous edition approved in 2018 as D4273 - 18. DOI:
10.1520/D4273-23.
noise ratio of 70:1 based on the benzene carbon signal in a
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
60 % benzene-d6, 40 % p-dioxane (v/v) sample (ASTM NMR
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
standard) that has been pulsed once using a 90° pulse angle
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. under the conditions specified in Practice E2977.
*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

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D4273 − 23
7.2 NMR sample tubes having outside diameters of 5 mm or 12.4 Obtain a stable de
...

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: D4273 − 18 D4273 − 23
Standard Test Method for
Polyurethane Raw Materials: Determination of Primary
1
Hydroxyl Content of Polyether Polyols
This standard is issued under the fixed designation D4273; 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*
13
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy ( C NMR) measures the primary hydroxyl content of ethylene oxide
(EO)-propylene oxide (PO) polyether polyols used in preparing flexible polyurethane foams. This method is best suited for
polyether polyols with primary hydroxyl contents of 10 to 90 %.
1.2 The values stated in SI units are to be regarded as standard.
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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
NOTE 1—There is no known ISO equivalent to this standard.
1.4 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
E456 Terminology Relating to Quality and Statistics
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E2935 Practice for Evaluating Equivalence of Two Testing Processes
E2977 Practice for Measuring and Reporting Performance of Fourier-Transform Nuclear Magnetic Resonance (FT-NMR)
Spectrometers for Liquid Samples
3. Terminology
3.1 Definitions—For definitions of terms that appear in this method, refer to Terms used in this standard are defined in accordance
with Terminology D883 and Practice E2977, 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.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved April 1, 2018March 1, 2023. Published April 2018March 2023. Originally approved in 1983. Last previous edition approved in 20112018 as
D4273 - 11.D4273 - 18. DOI: 10.1520/D4273-18.10.1520/D4273-23.
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.
*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 ----------------------
D4273 − 23
4. Summary of Test Method
4.1 Peaks of the primary and secondary hydroxyl carbons of polyether polyols used in flexible polyurethane foams are
13
well-resolved in high-resolution C NMR spectra. The primary hydroxyl content is determined from the ratio of the primary
hydroxyl area to the total hydroxyl (primary and secondary) area.
5. Significance and Use
5.1 The primary hydroxyl content provides information about the relative reactivities of polyols.polyols in the urethane forming
reaction with isocyanates.
6. Interferences
6.1 Primary hydroxyl PO methylene carbons (where the methylene carbon is next to the hydroxyl group and the methine carbon
is next to the ether oxygen) are integrated with the secondary hydroxyl carbons and are therefore not included in the primary
hydroxyl content as measured by this method. Any additional non-polyether polyol compounds in the sample that produce NMR
peaks in the 68-60 ppm region may interfere with the measurement.
7. Apparatus
7.1 Fourier-Transform NMR (FT-NMR) Spectrometer, with carbon-13 capability and a carbon-13 resonance frequency of 50 MHz
(proton resonance frequency of 200 MHz) or higher. The spectrometer is to have a minimum carbon-13 signal-to-noise ratio of
70:1 based on the benzene carbon signal in a 6
...