ASTM D5155-10
(Test Method)Standard Test Methods for Polyurethane Raw Materials Determination of the Isocyanate Content of Aromatic Isocyanates
Standard Test Methods for Polyurethane Raw Materials Determination of the Isocyanate Content of Aromatic Isocyanates
SIGNIFICANCE AND USE
These test methods can be used for research or for quality control to characterize isocyanates used in polyurethane products.
SCOPE
1.1 These test methods measure the isocyanate content of aromatic isocyanates used as polyurethane raw materials.
1.1.1 Test Method A—Unheated toluene-dibutylamine determines the toluene diisocyanate content, the amine equivalent and the isocyanate content of refined toluene-2,4-diisocyanate and toluene-2,6-diisocyanate, or mixtures of the two. Other isomers, if present, will be included in the determination. This test method may also be applied to other isocyanates of suitable reactivity and solubility.
1.1.2 Test Method B—Heated toluene-dibutylamine determines the amine equivalent and the isocyanate content of crude or modified isocyanates derived from toluene diisocyanate, methylene di-(4-phenylisocyanate) and polymeric (methylene phenylisocyanate).
1.1.3 Test Method C—Unheated trichlorobenzene-toluene-dibutylamine determines the amine equivalent and the isocyanate content of crude or modified isocyanates derived from toluene diisocyanate, methylene-di-(4-phenylisocyanate) and polymeric (methylene phenylisocyanate).
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.
Note 1—Method C of this test method is equivalent to Method B of ISO 14896.
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Designation: D5155 − 10
StandardTest Methods for
Polyurethane Raw Materials: Determination of the
1
Isocyanate Content of Aromatic Isocyanates
This standard is issued under the fixed designation D5155; 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 E180Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
1.1 These test methods measure the isocyanate content of
3
cialty Chemicals (Withdrawn 2009)
aromatic isocyanates used as polyurethane raw materials.
E691Practice for Conducting an Interlaboratory Study to
1.1.1 Test Method A—Unheatedtoluene-dibutylaminedeter-
Determine the Precision of a Test Method
mines the toluene diisocyanate content, the amine equivalent
and the isocyanate content of refined toluene-2,4-diisocyanate 2.2 ISO Standard:
ISO14896Polyurethane Raw Materials-Determination of
and toluene-2,6-diisocyanate, or mixtures of the two. Other
isomers, if present, will be included in the determination. This Isocyanate Content
testmethodmayalsobeappliedtootherisocyanatesofsuitable
reactivity and solubility. 3. Terminology
1.1.2 Test Method B—Heated toluene-dibutylamine deter-
3.1 Definitions—For definitions of terms that appear in this
minestheamineequivalentandtheisocyanatecontentofcrude
test method, refer to Terminology D883.
or modified isocyanates derived from toluene diisocyanate,
3.2 Definitions of Terms Specific to This Standard:
methylene di-(4-phenylisocyanate) and polymeric (methylene
3.2.1 amine equivalent—the weight of sample that will
phenylisocyanate).
combine with 1.0-g equivalent weight of dibutylamine.
1.1.3 Test Method C—Unheated trichlorobenzene-toluene-
3.2.2 assay—the percent by weight of toluene diisocyanate
dibutylamine determines the amine equivalent and the isocya-
present in the sample.
nate content of crude or modified isocyanates derived from
toluene diisocyanate, methylene-di-(4-phenylisocyanate) and
3.2.3 isocyanate (NCO) content—the percent by weight of
polymeric (methylene phenylisocyanate).
NCO groups present in the sample.
1.2 This standard does not purport to address all of the
4. Summary of Test Methods
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 All three test methods react the isocyanate sample with
priate safety and health practices and determine the applica-
an excess amount of dibutylamine to form the corresponding
bility of regulatory limitations prior to use.
urea. The NCO content is determined from the amount of
dibutylamineconsumedinthereaction.Thetestmethodsdiffer
NOTE 1—Method C of this test method is equivalent to Method B of
ISO14896. in the reaction conditions, or solvents used, or both.
4.1.1 Test Method A—The sample is added to an excess
2. Referenced Documents
amount of dibutylamine in toluene and allowed to stand at
2
room temperature for 15 min. The reaction mixture is diluted
2.1 ASTM Standards:
with isopropyl alcohol, and the excess dibutylamine is back-
D883Terminology Relating to Plastics
titrated with hydrochloric acid.
D1193Specification for Reagent Water
4.1.2 Test Method B—The sample is added to an excess
amount of dibutylamine in toluene and stirred for 20 min. The
1
These test methods are under the jurisdiction of ASTM Committee D20 on resulting solution is then heated rapidly to 100°C, removed
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular
from the heat, and allowed to stand for 30 min. The reaction
Materials - Plastics and Elastomers.
mixture is diluted with isopropyl alcohol, and the excess
Current edition approved April 1, 2010. Published June 2010. Originally
dibutylamine is back-titrated with hydrochloric acid.
approved in 1991. Last previous edition approved in 2007 as D5155-07. DOI:
10.1520/D5155-10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. 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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D5155 − 10
4.1.3 Test Method C—The sample is added to an excess 9. Test Conditions
amount of dibutylamine in toluene and trichlorobenzene. The
9.1 Since isocyanates react with moisture, keep the labor
...
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:D5155–07 Designation:D5155–10
Standard Test Methods for
Polyurethane Raw Materials: Determination of the
1
Isocyanate Content of Aromatic Isocyanates
This standard is issued under the fixed designation D5155; 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 isocyanate content of aromatic isocyanates used as polyurethane raw materials.
1.1.1 Test Method A—Unheated toluene-dibutylamine determines the amount of toluene diisocyanate content, the amine
equivalent and the isocyanate content of refined toluene-2,4-diisocyanate and toluene-2,6-diisocyanate, or mixtures of the two.
Other isomers, if present, will be included in the determination. This test method may also be applied to other isocyanates of
suitable reactivity and solubility.
1.1.2 Test Method B—Heated toluene-dibutylamine determines the amine equivalent of crude or modified isocyanates derived
from toluene diisocyanate, methylenebis-(4-phenylisocyanate), and polymethylene polyphenylisocyanate. —Heated toluene-
dibutylamine determines the amine equivalent and the isocyanate content of crude or modified isocyanates derived from toluene
diisocyanate, methylene di-(4-phenylisocyanate) and polymeric (methylene phenylisocyanate).
1.1.3 Test Method C—Unheatedtrichlorobenzene-toluene-dibutylaminedeterminestheisocyanatecontentofcrudeormodified
isocyanates derived from toluene diisocyanate, methylene-bis-(4-phenylisocyanate), and polymethylene polyphenylisocyanate.
This test method can also be used to assay isomer mixtures of toluene diisocyanate and methylene-bis-(phenylisocyanate).
—Unheated trichlorobenzene-toluene-dibutylamine determines the amine equivalent and the isocyanate content of crude or
modified isocyanates derived from toluene diisocyanate, methylene-di-(4-phenylisocyanate) and polymeric (methylene phenyl-
isocyanate).
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. For specific warning and precautionary statements, see Note 2.
NOTE 1—Method C of this test method is equivalent to Method B of ISO14896.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
E180 PracticeforDeterminingthePrecisionofASTMMethodsforAnalysisandTestingofIndustrialandSpecialtyChemicals
Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 ISO Standard:
ISO14896 Polyurethane Raw Materials-Determination of Isocyanate Content
3. Terminology
3.1Definitions:
3.1.1polyurethane—apolymerpreparedbythereactionofanorganicdiisocyanateorpolyisocyanatewithcompoundscontaining
hydroxyl groups.
3.1.1.1Discussion—Polyurethanesorurethanes,astheyaresometimescalled,maybethermosetting,thermoplastic,rigidorsoft
and flexible, or cellular or solid (see Terminology
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. These test methods were recommended to ASTM by the Society of the Plastics Industry Polyurethane Raw Materials Analysis Committee.
Current edition approved April 1, 2007. Published April 2007. Originally approved in 1991. Last previous edition approved in 2001 as D5155-01. DOI:
10.1520/D5155-07.on Cellular Materials - Plastics and Elastomers.
CurrenteditionapprovedApril1,2010.PublishedJune2010.Originallyapprovedin1991.Lastpreviouseditionapprovedin2007asD5155-07.DOI:10.1520/D5155-10.
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.
*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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D5155–10
3.1 Defi
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