ASTM D4273-11
(Test Method)Standard Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols
Standard Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols
SIGNIFICANCE AND USE
Measurements of primary hydroxyl content are useful for providing information regarding the relative reactivities of polyols.
SCOPE
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy (carbon-13 NMR), measures the primary hydroxyl content of ethylene oxide-propylene oxide polyethers used in preparing flexible foams. It is best suited for polyethers with primary hydroxyl contents of 10 to 90 %.
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 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.
X1.1.1 Fluorine-19 Nuclear Magnetic Resonance Spectroscopy (fluorine-19 NMR), measures the primary hydroxyl content in ethylene oxide-propylene oxide polyethers used in flexible urethane foams. It is suitable for polyethers with hydroxyl numbers of 24 to 300 and primary hydroxyl percentages of 2 to 98.
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Designation: D4273 − 11
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* 3. Terminology
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy 3.1 Theterminologyinthistestmethodfollowsthestandard
(carbon-13 NMR), measures the primary hydroxyl content of terminology defined in Practice E386 and in Terminology
ethylene oxide-propylene oxide polyethers used in preparing D883.
flexible foams. It is best suited for polyethers with primary
4. Summary of Test Method
hydroxyl contents of 10 to 90 %.
4.1 The resonance peaks of the primary and secondary
1.2 The values stated in SI units are to be regarded as
hydroxyl carbons of the polyethers used in flexible urethane
standard. No other units of measurement are included in this
foams are well-resolved in high-resolution carbon-13 NMR
standard.
spectra. The peak areas are measured by the spectrometer’s
1.3 This standard does not purport to address all of the
integrationsystem,andtherelativeprimaryhydroxylcontentis
safety concerns, if any, associated with its use. It is the
determined from the ratio of the primary hydroxyl area to the
responsibility of the user of this standard to establish appro-
total area of the primary and secondary hydroxyl resonance
priate safety and health practices and determine the applica-
peaks.
bility of regulatory limitations prior to use.
5. Significance and Use
NOTE 1—There is no known ISO equivalent to this standard.
5.1 Measurements of primary hydroxyl content are useful
2. Referenced Documents
for providing information regarding the relative reactivities of
2
2.1 ASTM Standards:
polyols.
D883 Terminology Relating to Plastics
E180 Practice for Determining the Precision of ASTM
6. Interferences
Methods for Analysis and Testing of Industrial and Spe-
6.1 Any primary hydroxyl propoxylate carbons present
3
cialty Chemicals (Withdrawn 2009)
(where the methylene carbon is next to the hydroxyl group and
E386 Practice for Data Presentation Relating to High-
the methine carbon is next to the ether oxygen) are integrated
Resolution Nuclear Magnetic Resonance (NMR) Spec-
with the secondary hydroxyl carbons and are therefore not
troscopy
included in the primary hydroxyl content as measured by this
E691 Practice for Conducting an Interlaboratory Study to
method.
Determine the Precision of a Test Method
7. Equipment
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
7.1 Pulse Fourier-Transform NMR (FT-NMR) Spectrometer,
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
with carbon-13 capability and a carbon-13 resonance fre-
Plastics and Elastomers.
quency of 15 MHz (proton resonance frequency of 60 MHz) or
Current edition approved April 1, 2011. Published April 2011. Originally
approved in 1983. Last previous edition approved in 2005 as D4273 - 05. DOI:
higher. The spectrometer is to have a minimum signal-to-noise
10.1520/D4273-11.
ratio of 70:1, based on the largest aromatic peak of 90 %
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ethylbenzene sample that has been pulsed one time using a 90°
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on pulse.
the ASTM website.
3 7.2 NMR Sample Tubes, with outer diameters of 5 mm or
The last approved version of this historical standard is referenced on
more.
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
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D4273 − 11
FIG. 1 Primary Hydroxyl Carbon Peaks of 3500 MW Triol (52 % Primary)
8. Reagents
Nucleus observed Carbon-13
Spectral width 100 ppm
8.1 All reagents are to be NMR-grade, deuterated solvents.
Pulse angle 90°
Data points 32K
8.2 Deuterated Chloroform or Deuterated Acetone, contain-
Acquisition time ~2 s
ing tetramethylsilane (TMS) as an internal standard.
Pulse delay 5 s
1
H decoupler on, or gated decoupling
9. Standards
12. NMR Analysis
9.1 This test method does not require standards.To evaluate
12.1 Place the NMR tube containing the sample solution
the test method, standards can be prepared by mixing in
into the spectrometer probe. After a stable lock is obtained,
solution commercially available poly(propylene oxide) and
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4273–05 Designation:D4273–11
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*
1.1 Carbon-13 Nuclear Magnetic Resonance Spectroscopy (carbon-13 NMR), measures the primary hydroxyl content of
ethylene oxide-propylene oxide polyethers used in preparing flexible foams. It is best suited for polyethers with primary hydroxyl
contents of 10 to 90 %.
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 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.
NOTE1—There is no equivalent ISO standard.
1.2This 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. 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E180 Practice for Determining the Precision ofASTM Methods forAnalysis and Testing of Industrial and Specialty Chemicals
E386 Practice for Data Presentation Relating to High-Resolution Nuclear Magnetic Resonance (NMR) Spectroscopy
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1Definitions: The3.1 The terminology in this test method follows the standard terminology defined in Practice E386 and in
Terminology D883.
4. Summary of Test Method
4.1 The resonance peaks of the primary and secondary hydroxyl carbons of the polyethers used in flexible urethane foams are
well-resolved in high-resolution carbon-13 NMR spectra. The peak areas are measured by the spectrometer’s integration system,
and the relative primary hydroxyl content is determined from the ratio of the primary hydroxyl area to the total area of the primary
and secondary hydroxyl resonance peaks.
5. Significance and Use
5.1 Measurements of primary hydroxyl content are useful for providing information regarding the relative reactivities of
polyols.
6. Interferences
6.1 Any primary hydroxyl propoxylate carbons present (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.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.22 on Cellular Materials - Plastics
and Elastomers.
Current edition approved JulyApril 1, 2005.2011. Published August 2005.April 2011. Originally approved in 1983. Last previous edition approved in 19992005 as
D4273-99.D4273 - 05. DOI: 10.1520/D4273-05.10.1520/D4273-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. 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 ----------------------
D4273–11
7. Equipment
6.1
7.1 Pulse Fourier-Transform NMR (FT-NMR) Spectrometer, with carbon-13 capability and a carbon-13 resonance frequency of
15 MHz (proton resonance frequency of 60 MHz) or higher. The spectrometer is to have a minimum signal-to-noise ratio of 70:1,
based on the largest aromatic peak of 90 % ethylbenzene sample that has been pulsed one time using a 90° pulse.
6.27.2 NMR Sample Tubes, with outer diameters of 5 mm or more.
7.
8. Reagents
7.1All8.1 All reagents are to be NMR-grade, deuterated solvents.
7.28.2 Deuterated Chloroform or Deuterated Acetone, containing
...
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