ASTM D4660-12
(Test Method)Standard Test Methods for Polyurethane Raw Materials: Determination of the Isomer Content of Toluenediisocyanate
Standard Test Methods for Polyurethane Raw Materials: Determination of the Isomer Content of Toluenediisocyanate
SIGNIFICANCE AND USE
These test methods can be used for research or for quality control to determine the isomer content of toluene diisocyanates.
The isomer content of a toluene diisocyanate relates to its reactivity.
SCOPE
1.1 These test methods measure the amount of toluene-2,6-diisocyanate (2,6-TDI) isomer or toluene–2,4–diisocyanate (2,4-TDI) isomer in mixtures of the 2,4- and 2,6-isomers of toluenediisocyanate (TDI). Two different test methods are provided to give accurate results over the broad range of isomer concentrations possible.
1.1.1 Test Method A—Applicable to TDI samples containing 5 to 95 % of 2,6-TDI isomer (5 to 95 % 2,4-TDI isomer).
1.1.2 Test Method B—Applicable to TDI samples containing 0 to 5 % of 2,6-TDI isomer (95 to 100 % 2,4-TDI isomer).
Note 1—These test methods are equivalent to ISO 15064.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D4660 − 12
Standard Test Methods for
Polyurethane Raw Materials: Determination of the Isomer
1
Content of Toluenediisocyanate
This standard is issued under the fixed designation D4660; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* mer Ratio in Toluenediisocyanate
1.1 These test methods measure the amount of toluene-2,6-
3. Terminology
diisocyanate (2,6-TDI) isomer or toluene–2,4–diisocyanate
3.1 Terminologyinthesetestmethodsisinaccordancewith
(2,4-TDI) isomer in mixtures of the 2,4- and 2,6-isomers of
Terminology D883.
toluenediisocyanate (TDI). Two different test methods are
provided to give accurate results over the broad range of
3.2 Definitions of Terms Specific to This Standard:
isomer concentrations possible. 3.2.1 isomer—a compound having the same molecular for-
1.1.1 Test Method A—ApplicabletoTDIsamplescontaining
mula (percentage composition and molecular weight) as an-
5 to 95% of 2,6-TDI isomer (5 to 95% 2,4-TDI isomer). other compound but differs in chemical or physical properties.
1.1.2 Test Method B—ApplicabletoTDIsamplescontaining
3.2.2 isomer content—theamountofanisomerexpressedas
0 to 5% of 2,6-TDI isomer (95 to 100% 2,4-TDI isomer). a percentage of total 2,4 and 2,6-TDI isomer amount.
NOTE 1—These test methods are equivalent to ISO15064.
4. Summary of Test Methods
1.2 The values stated in SI units are to be regarded as
4.1 Both test methods are based on the quantitative mea-
standard.
surement of absorption bands arising from out-of-plane C-H
1.3 This standard does not purport to address all of the
deformation vibrations of the aromatic ring.
safety concerns, if any, associated with its use. It is the
4.2 In Test Method A, the infrared spectrum of a cyclo-
responsibility of the user of this standard to establish appro-
hexane solution of the sample is recorded in the 770 to
priate safety and health practices and determine the applica-
−1 −1
840-cm region. The absorbance ratio of the 805 cm to the
bility of regulatory limitations prior to use.
–1
782 cm band is measured and converted to percent 2,6-TDI,
or percent 2,4-TDI, or both, from a previously established
2. Referenced Documents
calibration curve.
2
2.1 ASTM Standards:
−1
4.3 InTest Method B, the absorbance of the 782-cm band
D883Terminology Relating to Plastics
is measured from an infrared spectrum of an undiluted sample
E180Practice for Determining the Precision of ASTM
and then converted to percent 2,6-TDI from a previously
Methods for Analysis and Testing of Industrial and Spe-
3
established calibration curve.
cialty Chemicals (Withdrawn 2009)
4
2.2 ISO Standard:
5. Significance and Use
ISO15064Plastics—Aromatic Isocyanates for Use in the
5.1 These test methods can be used for research or for
Production of Polyurethanes—Determination of the Iso-
quality control to determine the isomer content of toluene
diisocyanates.
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 5.2 The isomer content of a toluene diisocyanate relates to
Materials - Plastics and Elastomers.
its reactivity.
Current edition approved May 1, 2012. Published June 2012. Originally
approved in 1959. Last previous edition approved in 2006 as D4660-06. DOI:
6. Apparatus
10.1520/D4660-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 Spectrophotometer—Any single- or double-beam re-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
cordinginfraredspectrophotometeraccurateto0.2%transmis-
Standards volume information, refer to the standard’s Document Summary page on
sion and capable of resolving the two peaks of the 2,4-TDI
the ASTM website.
−1
3
The last approved version of this historical standard is referenced on isomer doublet at 805-815 cm (see Fig. 1).
www.astm.org.
4
6.2 Cells, sealed sodium chloride (NaCl) liquid absorption
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org. cells with 0.2-mm (Test MethodA) and 0.1-mm (Test Method
*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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D4660 − 12
–1 –1
FIG. 1 IR Scan of TDI Showing 2,4-TDI Isomer Doublet at 810 cm and 2,6 TDI Isomer at 782 cm
B) path lengths. The actual thicknesses of the cells are to be skinandeyeprotection,aretobeusedwhenthereisapotential
known to 60.002 mm
...
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:D4660–06 Designation:D4660–12
Standard Test Methods for
Polyurethane Raw Materials: Determination of the Isomer
1
Content of Toluenediisocyanate
This standard is issued under the fixed designation D4660; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 These test methods measure the amount of toluene-2,6-diisocyanate (2,6-TDI) isomer or toluene–2,4–diisocyanate
(2,4-TDI) isomer in mixtures of the 2,4- and 2,6-isomers of toluenediisocyanate (TDI). Two different test methods are
requiredprovided to give accurate results over athe broad range of isomer concentrations possible.
1.1.1 Test Method A—ApplicabletoTDIsamplescontaining5to95%2,6–isomer(95to5%2,4–isomer).—ApplicabletoTDI
samples containing 5 to 95% of 2,6-TDI isomer (5 to 95% 2,4-TDI isomer).
1.1.2 Test Method B—ApplicabletoTDIsamplescontaining0to5%2,6–isomer(95to100%2,4–isomer).—ApplicabletoTDI
samples containing 0 to 5% of 2,6-TDI isomer (95 to 100% 2,4-TDI isomer).
NOTE 1—These test methods are equivalent to ISO15064.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific warning and precautionary statements see Note 3.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
E180 PracticeforDeterminingthePrecisionofASTMMethodsforAnalysisandTestingofIndustrialandSpecialtyChemicals
3
2.2 ISO Standard:
ISO15064 Plastics—Aromatic Isocyanates for Use in the Production of Polyurethanes—Determination of the Isomer Ratio in
Toluenediisocyanate
3. Terminology
3.1 Terminology in these test methods is in accordance with Terminology D883.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 isomer —a compound having the same molecular formula (percentage composition and molecular weight) as another
compound but differs in chemical or physical properties.
3.2.2 isomer content—the amount of an isomer expressed as a percentage of total 2,4 and 2,6-TDI isomer amount.
4. Summary of Test Methods
4.1Bothtestmethodsarebasedonthequantitativemeasurementofabsorptionbandsarisingfromout-of-planeC-Hdeformation
vibrations of the aromatic ring at 810 and 782 cm
4.1 Both test methods are based on the quantitative measurement of absorption bands arising from out-of-plane C-H
deformation vibrations of the aromatic ring.
−1
4.2 In Test MethodA, the infrared spectrum of a cyclohexane solution of the sample is recorded in the 770 to 840-cm (12.3
and 13.8 µm).
region. The
4.2In Test MethodA, the infrared spectrum of a cyclohexane solution of the sample is recorded in the 770 to 840-cm
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 Sept.May 1, 2006.2012. Published September 2006.June 2012. Originally approved in 1959. Last previous edition approved in 2006 as
´1
D4660-00(2006) .D4660-06. DOI: 10.1520/D4660-06.10.1520/D4660-12.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
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
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D4660–12
−1 −1
absorbance ratio of the 805 cm (12 to 13-µm) region. The absorbance ratio of the 810 and 782-cm bands is measured and converted to percent toluene-2,6-diisocyanate
–1
fromapreviouslyestablishedcalibrationcurve.tothe782cm bandismeasuredandconvertedtopercent2,6-TDI,orpercent2,4-TDI,orboth,fromapreviouslyestablished
calibration curve.
−1
4.3 InTestMethodB,theabsorbanceofthe782-cm bandismeasuredfromaninfraredspectrumofanundilutedsampleand
then converted to pe
...
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