ASTM E222-17
(Test Method)Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
SIGNIFICANCE AND USE
4.1 Hydroxyl is an important functional group, and knowledge of its content is required in many intermediate and end use applications. The test methods described herein are for the determination of primary and secondary hydroxyl groups and can be used for the assay of compounds containing them.
SCOPE
1.1 These test methods cover the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic and alicyclic compounds and phenols.
1.2 Three test methods are given as follows:
Sections
Test Method A (Pressure Bottle Method)
8 – 14
Test Method B (Reflux Method)
16 – 22
Test Method C (Perchloric Acid Catalyzed Method)
24 – 30
1.2.1 Test Method A is recommended for general use. Test Method B is included to give a standard procedure for the method that has been used widely. Test Method C is recommended when the results are required in a minimum period of time or where ambient temperature for the reaction is desired.
1.2.2 The results obtained using Test Methods A and B will be essentially the same, but the results obtained using Test Method C will be higher (up to approximately 4 % relative) than those obtained using the other two methods.
1.2.3 Statements on precision are included with each test method. The precision of Test Methods A and C is consistent over a wide range of hydroxyl content (tested over hydroxyl number range of 250 to 1600), whereas Test Method B is less precise at the higher hydroxyl content level than it is at the lower hydroxyl content level. In general, Test Method A is approximately two-fold as precise as Test Method C. Test Method B has approximately the same precision as Test Method C at the lower hydroxyl content level but poorer precision at the higher hydroxyl content level.
1.2.4 The interferences are essentially the same for the three methods. Some compounds can be analyzed using Test Methods A or B but not using Test Method C because of interfering reactions of the strong acid catalyst with the compound being analyzed or the acetate product formed in the determination. However, because of its increased reactivity, Test Method C is applicable for determination of some compounds, particularly sterically hindered secondary alcohols, which react too slowly or not at all in Test Methods A and B.
Note 1: Other methods for determination of hydroxyl groups are given in Test Methods D1957, D2195, E326, E335, and E567.
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 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.
1.5 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. Specific hazards statements are given in Section 7.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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Designation: E222 − 17
Standard Test Methods for
1
Hydroxyl Groups Using Acetic Anhydride Acetylation
This standard is issued under the fixed designation E222; 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.
NOTE 1—Other methods for determination of hydroxyl groups are given
1. Scope*
in Test Methods D1957, D2195, E326, E335, and E567.
1.1 These test methods cover the determination of hydroxyl
1.3 The values stated in SI units are to be regarded as
groups attached to primary and secondary carbon atoms in
standard. No other units of measurement are included in this
aliphatic and alicyclic compounds and phenols.
standard.
1.2 Three test methods are given as follows:
1.4 Review the current appropriate Safety Data Sheets
Sections
(SDS) for detailed information concerning toxicity, first aid
Test Method A (Pressure Bottle Method) 8 – 14
Test Method B (Reflux Method) 16 – 22 procedures, and safety precautions.
Test Method C (Perchloric Acid Catalyzed Method) 24 – 30
1.5 This standard does not purport to address all of the
1.2.1 Test Method A is recommended for general use. Test
safety concerns, if any, associated with its use. It is the
Method B is included to give a standard procedure for the
responsibility of the user of this standard to establish appro-
method that has been used widely. Test Method C is recom-
priate safety, health, and environmental practices and deter-
mended when the results are required in a minimum period of
mine the applicability of regulatory limitations prior to use.
time or where ambient temperature for the reaction is desired.
Specific hazards statements are given in Section 7.
1.2.2 The results obtained using Test Methods A and B will
1.6 This international standard was developed in accor-
be essentially the same, but the results obtained using Test
dance with internationally recognized principles on standard-
Method C will be higher (up to approximately 4 % relative)
ization established in the Decision on Principles for the
than those obtained using the other two methods.
Development of International Standards, Guides and Recom-
1.2.3 Statements on precision are included with each test
mendations issued by the World Trade Organization Technical
method. The precision of Test Methods A and C is consistent
Barriers to Trade (TBT) Committee.
over a wide range of hydroxyl content (tested over hydroxyl
number range of 250 to 1600), whereas Test Method B is less
2. Referenced Documents
precise at the higher hydroxyl content level than it is at the
2
2.1 ASTM Standards:
lower hydroxyl content level. In general, Test Method A is
D1193 Specification for Reagent Water
approximately two-fold as precise as Test Method C. Test
D1957 Test Method for Hydroxyl Value of Fatty Oils and
Method B has approximately the same precision as Test
3
Acids (Withdrawn 2007)
Method C at the lower hydroxyl content level but poorer
3
D2195 Test Methods for Pentaerythritol (Withdrawn 2011)
precision at the higher hydroxyl content level.
D6809 Guide for Quality Control and Quality Assurance
1.2.4 The interferences are essentially the same for the three
Procedures for Aromatic Hydrocarbons and Related Ma-
methods. Some compounds can be analyzed using Test Meth-
terials
ods A or B but not using Test Method C because of interfering
E180 Practice for Determining the Precision of ASTM
reactions of the strong acid catalyst with the compound being
Methods for Analysis and Testing of Industrial and Spe-
analyzed or the acetate product formed in the determination.
3
cialty Chemicals (Withdrawn 2009)
However, because of its increased reactivity, Test Method C is
E200 Practice for Preparation, Standardization, and Storage
applicable for determination of some compounds, particularly
of Standard and Reagent Solutions for Chemical Analysis
sterically hindered secondary alcohols, which react too slowly
E203 Test Method for Water Using Volumetric Karl Fischer
or not at all in Test Methods A and B.
Titration
1 2
These test methods are 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 are the direct responsi- contact ASTM Customer Service at service@astm.org. 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 June 1, 2017. Published July 2017. Originally approved the ASTM website.
3
in 1963. Last previous edition approved in 2010 as E222 – 10. DOI: 10.1520/ The last
...
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: E222 − 10 E222 − 17
Standard Test Methods for
1
Hydroxyl Groups Using Acetic Anhydride Acetylation
This standard is issued under the fixed designation E222; 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 These test methods cover the determination of hydroxyl groups attached to primary and secondary carbon atoms in aliphatic
and alicyclic compounds and phenols.
1.2 Three test methods are given as follows:
Sections
Test Method A (Pressure Bottle Method) 8 – 14
Test Method B (Reflux Method) 15 – 21
Test Method B (Reflux Method) 16 – 22
Test Method C (Perchloric Acid Catalyzed Method) 22 – 28
Test Method C (Perchloric Acid Catalyzed Method) 24 – 30
1.2.1 Test Method A is recommended for general use. Test Method B is included to give a standard procedure for the method
that has been used widely. Test Method C is recommended when the results are required in a minimum period of time or where
ambient temperature for the reaction is desired.
1.2.2 The results obtained using Test Methods A and B will be essentially the same, but the results obtained using Test Method
C will be higher (up to approximately 4 % relative) than those obtained using the other two methods.
1.2.3 Statements on precision are included with each test method. The precision of Test Methods A and C is consistent over a
wide range of hydroxyl content (tested over hydroxyl number range of 250 to 1600), whereas Test Method B is less precise at the
higher hydroxyl content level than it is at the lower hydroxyl content level. In general, Test Method A is approximately two-fold
as precise as Test Method C. Test Method B has approximately the same precision as Test Method C at the lower hydroxyl content
level but poorer precision at the higher hydroxyl content level.
1.2.4 The interferences are essentially the same for the three methods. Some compounds can be analyzed using Test Methods
A or B but not using Test Method C because of interfering reactions of the strong acid catalyst with the compound being analyzed
or the acetate product formed in the determination. However, because of its increased reactivity, Test Method C is applicable for
determination of some compounds, particularly sterically hindered secondary alcohols, which react too slowly or not at all in Test
Methods A and B.
NOTE 1—Other methods for determination of hydroxyl groups are given in Test Methods D1957, D2195, E326, E335, and E567.
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 Review the current appropriate Material Safety Data Sheets (MSDS)(SDS) for detailed information concerning toxicity, first
aid procedures, and safety precautions.
1.5 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. Specific hazards statements are given in Section 77.
NOTE 1—Other methods for determination of hydroxyl groups are given in Test Methods D1957, D2195, E326, E335, and E567.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1
These test methods are under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and are the
direct responsibility of Subcommittee D16.15 on Industrial and Specialty General Standards.
Current edition approved March 1, 2010June 1, 2017. Published April 2010July 2017. Originally approved in 1963. Last previous edition approved in 20052010 as
ε1
E222 – 00 (2005)E222 – 10. . DOI: 10.1520/E0222-10.10.1520/E0222-17.
*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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E222 − 17
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for
...
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