ASTM E1899-16

Standard Test Method for Hydroxyl Groups Using Reaction with <emph type="ital">p</emph >-Toluenesulfonyl Isocyanate (TSI) and Potentiometric Titration with Tetrabutylammonium Hydroxide

SIGNIFICANCE AND USE
5.1 Hydroxyl is an important functional group and knowledge of its content is required in many intermediate and end use applications. This test method is for the determination of primary and secondary hydroxyl groups and can be used for the assay of compounds containing them.  
5.2 This test method has the following advantages over other hydroxyl number methods: It is rapid (10 min), pyridine-free, ambient temperature, small sample size, applicable to extremely low hydroxyl numbers (
SCOPE
1.1 This test method covers the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic and cyclic compounds and phenols. It is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms. This test method is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols, and rigid polyols. Other available test methods listed in Note 1 are not suitable for many of the sample types listed above.  
1.1.1 This test method is currently recommended for neutral refined products. Successful application has been made, however, to some in-process samples that contain an excess of acidic species. Proper validation must be performed, of course, to show that the acidic species either does not interfere, or that the acidic species interference has been obviated.
Note 1: Other methods for determination of hydroxyl groups are given in Test Methods D817, D871, D1957, D2195, D4252, D4273, D4274, E222, E326, and E335.  
1.2 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 hazards see Section 9.

General Information

• Status: Historical
• Publication Date: 31-Mar-2016
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.12 - Caustics and Peroxides

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1899 − 16
Standard Test Method for
Hydroxyl Groups Using Reaction with p-Toluenesulfonyl
Isocyanate (TSI) and Potentiometric Titration with
1
Tetrabutylammonium Hydroxide
This standard is issued under the fixed designation E1899; 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* Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
1.1 This test method covers the determination of hydroxyl
Barriers to Trade (TBT) Committee.
groups attached to primary and secondary carbon atoms in
aliphatic and cyclic compounds and phenols. It is not suitable
2. Referenced Documents
for determination of hydroxyl groups attached to tertiary
2
2.1 ASTM Standards:
carbon atoms. This test method is applicable to polyacetals,
D817 Test Methods of Testing Cellulose Acetate Propionate
temperature sensitive materials, high solids polymer polyols,
and Cellulose Acetate Butyrate
and rigid polyols. Other available test methods listed in Note 1
D871 Test Methods of Testing Cellulose Acetate
are not suitable for many of the sample types listed above.
D1193 Specification for Reagent Water
1.1.1 This test method is currently recommended for neutral
D1957 Test Method for Hydroxyl Value of Fatty Oils and
refined products. Successful application has been made,
3
Acids (Withdrawn 2007)
however, to some in-process samples that contain an excess of
3
D2195 Test Methods for Pentaerythritol (Withdrawn 2011)
acidic species. Proper validation must be performed, of course,
D4252 Test Methods for Chemical Analysis of Alcohol
to show that the acidic species either does not interfere, or that
Ethoxylates and Alkylphenol Ethoxylates
the acidic species interference has been obviated.
D4273 Test Method for Polyurethane Raw Materials: Deter-
NOTE 1—Other methods for determination of hydroxyl groups are given
mination of Primary Hydroxyl Content of Polyether Poly-
in Test Methods D817, D871, D1957, D2195, D4252, D4273, D4274,
ols
E222, E326, and E335.
D4274 Test Methods for Testing Polyurethane Raw Materi-
1.2 Review the current appropriate Safety Data Sheets
als: Determination of Hydroxyl Numbers of Polyols
(SDS) for detailed information concerning toxicity, first aid
E180 Practice for Determining the Precision of ASTM
procedures, and safety precautions.
Methods for Analysis and Testing of Industrial and Spe-
3
1.3 The values stated in SI units are to be regarded as
cialty Chemicals (Withdrawn 2009)
standard. No other units of measurement are included in this E222 Test Methods for Hydroxyl Groups Using Acetic
standard.
Anhydride Acetylation
E300 Practice for Sampling Industrial Chemicals
1.4 This standard does not purport to address all of the
E326 Test Method for Hydroxyl Groups by Phthalic Anhy-
safety concerns, if any, associated, with its use. It is the
3
dride Esterification (Withdrawn 2001)
responsibility of the user of this standard to establish appro-
E335 Test Method for Hydroxyl Groups by Pyromellitic
priate safety, health, and environmental practices and deter-
3
Dianhydride Esterification (Withdrawn 2002)
mine the applicability of regulatory limitations prior to use.
For specific hazards see Section 9.
3. Terminology
1.5 This international standard was developed in accor-
3.1 Definitions:
dance with internationally recognized principles on standard-
3.1.1 hydroxyl number (OH#)—the milligrams of potassium
ization established in the Decision on Principles for the
hydroxide equivalent to the hydroxyl content of 1 g of sample.
1 2
This test method is under the jurisdiction of ASTM Committee D16 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi- contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
bility of Subcommittee D16.12 on Caustics and Peroxides. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2016. Published May 2016. Originally the ASTM website.
3
approved in 1997. Last previous edition approved in 2008 as E1899 – 08. DOI: The last approved version of this historical standard is referenced on
10.1520/E1899-16. 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 ----------------------
E1899 − 16
refined products, the analyst must first validate this test method
on a case by case bas
...

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: E1899 − 08 E1899 − 16
Standard Test Method for
Hydroxyl Groups Using Reaction with p-Toluenesulfonyl
Isocyanate (TSI) and Potentiometric Titration with
1
Tetrabutylammonium Hydroxide
This standard is issued under the fixed designation E1899; 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*
1.1 This test method covers the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic
and cyclic compounds and phenols. It is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms. This
test method is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols, and rigid polyols. Other
available test methods listed in Note 1 are not suitable for many of the sample types listed above.
1.1.1 This test method is currently recommended for neutral refined products. Successful application has been made, however,
to some in-process samples that contain an excess of acidic species. Proper validation must be performed, of course, to show that
the acidic species either does not interfere, or that the acidic species interference has been obviated.
NOTE 1—Other methods for determination of hydroxyl groups are given in Test Methods D817, D871, D1957, D2195, D4252, D4273, D4274, E222,
E326, and E335.
1.2 Review the current appropriate Material Safety Data Sheets (MSDS)(SDS) for detailed information concerning toxicity, first
aid procedures, and safety precautions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 hazards see Section 9.
For specific hazards see Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D817 Test Methods of Testing Cellulose Acetate Propionate and Cellulose Acetate Butyrate
D871 Test Methods of Testing Cellulose Acetate
D1193 Specification for Reagent Water
3
D1957 Test Method for Hydroxyl Value of Fatty Oils and Acids (Withdrawn 2007)
3
D2195 Test Methods for Pentaerythritol (Withdrawn 2011)
D4252 Test Methods for Chemical Analysis of Alcohol Ethoxylates and Alkylphenol Ethoxylates
D4273 Test Method for Polyurethane Raw Materials: Determination of Primary Hydroxyl Content of Polyether Polyols
D4274 Test Methods for Testing Polyurethane Raw Materials: Determination of Hydroxyl Numbers of Polyols
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E222 Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
E300 Practice for Sampling Industrial Chemicals
3
E326 Test Method for Hydroxyl Groups by Phthalic Anhydride Esterification (Discontinued 2001) (Withdrawn 2001)
3
E335 Test Method for Hydroxyl Groups by Pyromellitic Dianhydride Esterification (Withdrawn 2002)
1
This test method is under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and is the direct responsibility of Subcommittee E15.01 on
General Standards.
Current edition approved April 1, 2008April 1, 2016. Published May 2008May 2016. Originally approved in 1997. Last previous edition approved in 20022008 as
E1899 – 02.E1899 – 08. DOI: 10.1520/E1899-08.10.1520/E1899-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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 ----------------------
E1899 − 16
3. Terminology
3.1 Definitions:
3.1.1 hydroxyl number (OH#)—the milligrams of potassium hydroxide equivalent to the hydroxyl content of 1 g of sample.
3.1.1.1 Discussion—
In the case of a pure compound, the hydroxyl num
...