ASTM D4660-06
(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 ratios of toluene diisocyanates.
The isomer ratio of a toluene diisocyanate relates to its reactivity.
SCOPE
1.1 These test methods measure the amount of toluene-2,6-diisocyanate (TDI) or toluene-2,4-diisocyanate in mixtures of the 2,4- and 2,6-isomers. Two test methods are required to give accurate results over a broad range of isomer concentrations.
1.1.1 Test Method AApplicable to TDI samples containing 5 to 95 % 2,6-isomer (95 to 5 % 2,4-isomer).
1.1.2 Test Method BApplicable to TDI samples containing 0 to 5 % 2,6-isomer (95 to 100 % 2,4-isomer). These test methods are equivalent to ISO 15064.
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.
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Standards Content (Sample)
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Designation:D4660–06
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* 3. Terminology
1.1 These test methods measure the amount of toluene-2,6- 3.1 Terminologyinthesetestmethodsisinaccordancewith
diisocyanate (TDI) or toluene–2,4–diisocyanate in mixtures of Terminology D883.
the2,4-and2,6-isomers.Twotestmethodsarerequiredtogive 3.2 Definitions of Terms Specific to This Standard:
accurate results over a broad range of isomer concentrations. 3.2.1 isomer—a compound having the same percentage
1.1.1 Test Method A—Applicable to TDI samples contain- composition and molecular weight as another compound but
ing 5 to 95% 2,6–isomer (95 to 5% 2,4–isomer). differs in chemical or physical properties.
1.1.2 Test Method B—Applicable to TDI samples contain- 3.2.2 isomer content—theamountofanisomerexpressedas
ing 0 to 5% 2,6–isomer (95 to 100% 2,4–isomer). a percentage of total isomer amount.
NOTE 1—These test methods are equivalent to ISO15064.
4. Summary of Test Methods
1.2 This standard does not purport to address all of the
4.1 Both test methods are based on the quantitative mea-
safety concerns, if any, associated with its use. It is the
surement of absorption bands arising from out-of-plane C-H
responsibility of the user of this standard to establish appro-
deformation vibrations of the aromatic ring at 810 and 782
−1
priate safety and health practices and determine the applica-
cm (12.3 and 13.8 µm).
bility of regulatory limitations prior to use. For specific
4.2 In Test Method A, the infrared spectrum of a cyclo-
warning and precautionary statements see Note 3.
hexane solution of the sample is recorded in the 770 to
−1
840-cm (12to13-µm)region.Theabsorbanceratioofthe810
2. Referenced Documents
−1
and 782-cm bands is measured and converted to percent
2
2.1 ASTM Standards:
toluene-2,6-diisocyanatefromapreviouslyestablishedcalibra-
D883 Terminology Relating to Plastics
tion curve.
−1
E180 Practice for Determining the Precision of ASTM
4.3 InTestMethodB,theabsorbanceofthe782-cm band
Methods for Analysis and Testing of Industrial and Spe-
is measured from an infrared spectrum of an undiluted sample
cialty Chemicals
and then converted to percent 2,6-isomer from a previously
3
2.2 ISO Standard:
established calibration curve.
ISO15064 Plastics—Aromatic Isocyanates for Use in the
5. Significance and Use
Production of Polyurethanes—Determination of the Iso-
mer Ratio in Toluenediisocyanate
5.1 These test methods can be used for research or for
quality control to determine the isomer ratios of toluene
1 diisocyanates.
These test methods are under the jurisdiction of ASTM Committee D20 on
5.2 The isomer ratio of a toluene diisocyanate relates to its
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
Materials—Plastics and Elastomers.
reactivity.
Current edition approved Sept. 1, 2006. Published September 2006. Originally
´1
approved in 1959. Last previous edition approved in 2006 as D4660-00(2006) .
6. Apparatus
DOI: 10.1520/D4660-06.
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-isomer
the ASTM website.
−1
3
doublet at 810 cm .
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036.
*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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D4660–06
6.2 Cells, sealed sodium chloride (NaCl) liquid absorption of each mixture is to be 3.5 to 4.0 g. Carefully shake the
cells with 0.2-mm (Test MethodA) and 0.1-mm (Test Method mixtures.Fromtheweightsofpure2,4-and2,6-TDI,calculate
B) path lengths. The actual thicknesses of the cells are to be the weight ratios (2,4-TDI to 2,6-TDI) of the mixtures,
known to 60.002 mm. expressed to four significant figures.
6.3 Glassware, 25-mL, glass-stoppered, volumetric flasks,
NOTE 3—Dry carefully all glassware since the diisocyanates react
0.80-mL pipet, and an all-glass syringe.
readily with moisture.
10.1.1 Approximate
...
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