ASTM D5155-14e1
(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
5.1 These test methods are to 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 is also applicable 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 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: Method C of this test method is equivalent to Method B of ISO 14896.
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´1
Designation: D5155 − 14
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
ε NOTE—Editorially corrected Eq 2 in January 2016.
1. Scope* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 These test methods measure the isocyanate content of
D883Terminology Relating to Plastics
aromatic isocyanates used as polyurethane raw materials.
D1193Specification for Reagent Water
1.1.1 Test Method A—Unheatedtoluene-dibutylaminedeter-
E180Practice for Determining the Precision of ASTM
mines the toluene diisocyanate content, the amine equivalent
Methods for Analysis and Testing of Industrial and Spe-
and the isocyanate content of refined toluene-2,4-diisocyanate
3
cialty Chemicals (Withdrawn 2009)
and toluene-2,6-diisocyanate, or mixtures of the two. Other
E691Practice for Conducting an Interlaboratory Study to
isomers, if present, will be included in the determination. This
Determine the Precision of a Test Method
test method is also applicable to other isocyanates of suitable
2.2 ISO Standard:
reactivity and solubility.
ISO14896 Polyurethane Raw Materials-Determination of
1.1.2 Test Method B—Heated toluene-dibutylamine deter- Isocyanate Content
minestheamineequivalentandtheisocyanatecontentofcrude
3. Terminology
or modified isocyanates derived from toluene diisocyanate,
methylene di-(4-phenylisocyanate) and polymeric (methylene 3.1 Definitions—For definitions of terms that appear in this
phenylisocyanate). test method, refer to Terminology D883.
1.1.3 Test Method C—Unheated trichlorobenzene-toluene-
3.2 Definitions of Terms Specific to This Standard:
dibutylamine determines the amine equivalent and the isocya-
3.2.1 amine equivalent—the weight of sample that will
nate content of crude or modified isocyanates derived from combine with 1.0-g equivalent weight of dibutylamine.
toluene diisocyanate, methylene-di-(4-phenylisocyanate) and
3.2.2 assay—the percent by weight of toluene diisocyanate
polymeric (methylene phenylisocyanate).
present in the sample.
3.2.3 isocyanate (NCO) content—the percent by weight of
1.2 The values stated in SI units are to be regarded as
NCO groups present in the sample.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Methods
1.3 This standard does not purport to address all of the
4.1 All three test methods react the isocyanate sample with
safety concerns, if any, associated with its use. It is the
an excess amount of dibutylamine to form the corresponding
responsibility of the user of this standard to establish appro-
urea. The NCO content is determined from the amount of
priate safety and health practices and determine the applica-
dibutylamineconsumedinthereaction.Thetestmethodsdiffer
bility of regulatory limitations prior to use.
in the reaction conditions, or solvents used, or both.
4.1.1 Test Method A—The sample is added to an excess
NOTE 1—Method C of this test method is equivalent to Method B of
amount of dibutylamine in toluene and allowed to stand at
ISO14896.
room temperature for 15 min. The reaction mixture is diluted
1 2
These test methods are under the jurisdiction of ASTM Committee D20 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Materials - Plastics and Elastomers. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2014. Published November 2014. Originally the ASTM website.
3
approved in 1991. Last previous edition approved in 2010 as D5155-10. DOI: The last approved version of this historical standard is referenced on
10.1520/D5155-14. 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 − 14
with isopropyl alcohol, and the excess dibutylamine is back- neering controls and personal protective equipment, including
titrated with hydrochloric acid. respiratory, skin and eye protection, may be used to prevent
4.1.2 Test Method B—The sample is added to an excess over-exposure to diisocyanates. Consult the product suppliers’
amount of dibutylamine in toluene and stirred for 20 min. The Safety Data Sheet (SDS) for more de
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D5155 − 14 D5155 − 14
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1
ε NOTE—Editorially corrected Eq 2 in January 2016.
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 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 is also applicable 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 phenyli-
socyanate).
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 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—Method C of this test method is equivalent to Method B of ISO 14896.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1193 Specification for Reagent Water
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 ISO Standard:
ISO 14896 Polyurethane Raw Materials-Determination of Isocyanate Content
3. Terminology
3.1 Definitions—For definitions of terms that appear in this test method, refer to Terminology D883.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 amine equivalent—the weight of sample that will combine with 1.0-g equivalent weight of dibutylamine.
3.2.2 assay—the percent by weight of toluene diisocyanate present in the sample.
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 Nov. 1, 2014. Published November 2014. Originally approved in 1991. Last previous edition approved in 2010 as D5155 - 10. DOI:
10.1520/D5155-14.
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
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
1
---------------------- Page: 1 ----------------------
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D5155 − 14
3.2.3 isocyanate (NCO) content—the percent by weight of NCO groups present in the sample.
4. Summary of Test Methods
4.1 All three test methods react the isocyanate sample with an excess amount of dibutylamine to form the corresponding urea.
The NCO content is determined from the amount of dibutylamine consumed in the reaction. The test methods differ in the reaction
conditions, or solvents used, or both.
4.1.1 Test Method A—The sample is added to an excess amount of dibutylamine in toluene and allowed to stand at room
temperature for 15 min. The reaction mixture is diluted with isopropyl alcohol, and the excess dibutylamine is back-titrated with
hydrochloric acid.
4.1.2 Test Method B—The samp
...
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