ASTM D5155-14
(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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Designation: D5155 − 14
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* 2. Referenced Documents
2
1.1 These test methods measure the isocyanate content of 2.1 ASTM Standards:
aromatic isocyanates used as polyurethane raw materials. D883Terminology Relating to Plastics
1.1.1 Test Method A—Unheatedtoluene-dibutylaminedeter- D1193Specification for Reagent Water
mines the toluene diisocyanate content, the amine equivalent E180Practice for Determining the Precision of ASTM
and the isocyanate content of refined toluene-2,4-diisocyanate Methods for Analysis and Testing of Industrial and Spe-
3
and toluene-2,6-diisocyanate, or mixtures of the two. Other cialty Chemicals (Withdrawn 2009)
isomers, if present, will be included in the determination. This E691Practice for Conducting an Interlaboratory Study to
test method is also applicable to other isocyanates of suitable Determine the Precision of a Test Method
reactivity and solubility. 2.2 ISO Standard:
1.1.2 Test Method B—Heated toluene-dibutylamine deter- ISO14896 Polyurethane Raw Materials-Determination of
minestheamineequivalentandtheisocyanatecontentofcrude Isocyanate Content
or modified isocyanates derived from toluene diisocyanate,
3. Terminology
methylene di-(4-phenylisocyanate) and polymeric (methylene
phenylisocyanate). 3.1 Definitions—For definitions of terms that appear in this
1.1.3 Test Method C—Unheated trichlorobenzene-toluene- test method, refer to Terminology D883.
dibutylamine determines the amine equivalent and the isocya-
3.2 Definitions of Terms Specific to This Standard:
nate content of crude or modified isocyanates derived from
3.2.1 amine equivalent—the weight of sample that will
toluene diisocyanate, methylene-di-(4-phenylisocyanate) and
combine with 1.0-g equivalent weight of dibutylamine.
polymeric (methylene phenylisocyanate).
3.2.2 assay—the percent by weight of toluene diisocyanate
1.2 The values stated in SI units are to be regarded as
present in the sample.
standard. No other units of measurement are included in this
3.2.3 isocyanate (NCO) content—the percent by weight of
standard.
NCO groups present in the sample.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Summary of Test Methods
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.
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
1
---------------------- Page: 1 ----------------------
D5155 − 14
4.1.1 Test Method A—The sample is added to an excess Diisocyanates can cause skin and respiratory sensitization
amount of dibutylamine in toluene and allowed to stand at (asthma) in some people. Once sensitized, further exposure to
room temperature for 15 min. The reaction mixture is diluted diisocyanates should be eliminated. A combination of engi-
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
...
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.
Designation: D5155 − 10 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. Scope 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 mayis also be applied 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.
3.2.3 isocyanate (NCO) content—the percent by weight of NCO groups 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 April 1, 2010Nov. 1, 2014. Published June 2010November 2014. Originally approved in 1991. Last previous edition approved in 20072010 as
D5155 - 07.D5155 - 10. DOI: 10.1520/D5155-10.10.1520/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 ----------------------
D5155 − 14
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 Me
...
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