ASTM D4273-05

Standard Test Methods 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 %.
Note 1—There is no equivalent ISO standard.
1.2 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.

General Information

• Status: Historical
• Publication Date: 30-Jun-2005
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.22 - Cellular Materials - Plastics and Elastomers

Relations

• Replaces: ASTM D4273-99 - Standard Test Methods for Polyurethane Raw Materials Determination of Primary Hydroxyl Content of Polyether Polyols
• Effective Date: 01-Jul-2005
• Replaced By: ASTM D4273-11 - Standard Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols
• Effective Date: 01-Apr-2011
• Referred By: ASTM E1899-23 - Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide
• Effective Date: 01-Jul-2005

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D4273–05
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* 4. Summary of Test Method
1.1 Carbon-13 Nuclear Magnetic Resonance 4.1 The resonance peaks of the primary and secondary
Spectroscopy (carbon-13 NMR), measures the primary hy- hydroxyl carbons of the polyethers used in flexible urethane
droxyl content of ethylene oxide-propylene oxide polyethers foams are well-resolved in high-resolution carbon-13 NMR
used in preparing flexible foams. It is best suited for polyethers spectra. The peak areas are measured by the spectrometer’s
with primary hydroxyl contents of 10 to 90 %. integrationsystem,andtherelativeprimaryhydroxylcontentis
determined from the ratio of the primary hydroxyl area to the
NOTE 1—There is no equivalent ISO standard.
total area of the primary and secondary hydroxyl resonance
1.2 This standard does not purport to address all of the
peaks.
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5.1 Measurements of primary hydroxyl content are useful
bility of regulatory limitations prior to use.
for providing information regarding the relative reactivities of
polyols.
2. Referenced Documents
2
6. Equipment
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
6.1 Pulse Fourier-Transform NMR (FT-NMR) Spectrom-
E180 Practice for Determining the Precision of ASTM
eter, with carbon-13 capability and a carbon-13 resonance
Methods for Analysis and Testing of Industrial and Spe-
frequency of 15 MHz or higher. The spectrometer is to have a
3
cialty Chemicals
minimum signal-to-noise ratio of 70:1, based on the largest
E386 Practice for Data Presentation Relating to High-
aromatic peak of 90 % ethylbenzene sample that has been
Resolution Nuclear Magnetic Resonance (NMR) Spectros-
pulsed one time using a 90° pulse.
copy
6.2 NMR Sample Tubes, with outer diameters of 5 mm or
E691 Practice for Conducting an Interlaboratory Study to
more.
Determine the Precision of a Test Method
7. Reagents
3. Terminology
7.1 All reagents are to be NMR-grade, deuterated solvents.
3.1 Definitions: The terminology in this test method follows
7.2 Deuterated Chloroform or Deuterated Acetone,contain-
the standard terminology defined in Practice E386 and in
ing tetramethylsilane (TMS) as an internal standard.
Terminology D883.
8. Standards
8.1 This test method does not require standards.To evaluate
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
the test method, standards can be prepared by mixing in
and is the direct responsibility of Subcommittee D20.22 on Cellular Materials -
Plastics and Elastomers.
solution commercially available poly(propylene oxide) and
Current edition approved July 1, 2005. Published August 2005. Originally
poly(ethylene oxide) diols. The molecular weight of the
approved in 1983. Last previous edition approved in 1999 as D4273 - 99. DOI:
standard would ideally be 300 or more since lower-molecular-
10.1520/D4273-05.
2
weight polyols can contain structural configurations that are
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
not typical of polyethers used in flexible urethane foams.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Withdrawn. 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.
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D4273–05
FIG. 1 Primary Hydroxyl Carbon Peaks of 3500 MW Triol (52% Primary)
9. Preparation of Sample repetitive scans for the analysis. The number required depends
on the spectrometer, the molecular weight of the polyol, and
9.1 Add 3 mL of the polyol and 1.5 to 2 mL of deuterated
the functionality of the polyol. Some samples will require
chloroform or deuterated acetone to the NMR tube. Cap the
repetitive scanning for 30 min or less, while some will require
tube and mix the contents thoroughly.
an hour or more. After scanning, transform the free induction
10. Instrument Preparation decay (FID) to the frequency-doma
...