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ASTM E222-23

(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 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded in accordance with the rounding off methods of Practice E29.  
1.5 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.  
1.7 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.

General Information

Status
Published
Publication Date
31-Mar-2023
ICS
71.040.40 - Chemical analysis
Technical Committee
D16 - Aromatic, Industrial, Specialty and Related Chemicals
Drafting Committee
D16.12 - Caustics and Peroxides
Current Stage
Ref Project

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ASTM E222-23 - Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride AcetylationASTM E222-23 - Standard Test Methods for Hydroxyl Groups Using Acetic Anhydride Acetylation
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Standards Content (Sample)

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.
Designation: E222 − 23
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 In determining the conformance of the test results using
Sections
this method to applicable specifications, results shall be
Test Method A (Pressure Bottle Method) 8 – 14
rounded in accordance with the rounding off methods of
Test Method B (Reflux Method) 16 – 22
Test Method C (Perchloric Acid Catalyzed Method) 24 – 30
Practice E29.
1.2.1 Test Method A is recommended for general use. Test
1.5 Review the current appropriate Safety Data Sheets
Method B is included to give a standard procedure for the
(SDS) for detailed information concerning toxicity, first aid
method that has been used widely. Test Method C is recom-
procedures, and safety precautions.
mended when the results are required in a minimum period of
1.6 This standard does not purport to address all of the
time or where ambient temperature for the reaction is desired.
safety concerns, if any, associated with its use. It is the
1.2.2 The results obtained using Test Methods A and B will
responsibility of the user of this standard to establish appro-
be essentially the same, but the results obtained using Test
priate safety, health, and environmental practices and deter-
Method C will be higher (up to approximately 4 % relative)
mine the applicability of regulatory limitations prior to use.
than those obtained using the other two methods.
Specific hazards statements are given in Section 7.
1.2.3 Statements on precision are included with each test
1.7 This international standard was developed in accor-
method. The precision of Test Methods A and C is consistent
dance with internationally recognized principles on standard-
over a wide range of hydroxyl content (tested over hydroxyl
ization established in the Decision on Principles for the
number range of 250 to 1600), whereas Test Method B is less
Development of International Standards, Guides and Recom-
precise at the higher hydroxyl content level than it is at the
mendations issued by the World Trade Organization Technical
lower hydroxyl content level. In general, Test Method A is
Barriers to Trade (TBT) Committee.
approximately two-fold as precise as Test Method C. Test
Method B has approximately the same precision as Test
2. Referenced Documents
Method C at the lower hydroxyl content level but poorer
2
precision at the higher hydroxyl content level. 2.1 ASTM Standards:
D1193 Specification for Reagent Water
1.2.4 The interferences are essentially the same for the three
methods. Some compounds can be analyzed using Test Meth- D1957 Test Method for Hydroxyl Value of Fatty Oils and
3
Acids (Withdrawn 2007)
ods A or B but not using Test Method C because of interfering
3
reactions of the strong acid catalyst with the compound being D2195 Test Methods for Pentaerythritol (Withdrawn 2011)
D6809 Guide for Quality Control and Quality Assurance
analyzed or the acetate product formed in the determination.
However, because of its increased reactivity, Test Method C is Procedures for Aromatic Hydrocarbons and Related Ma-
terials
applicable for determination of some compounds, particularly
sterically hindered secondary alcohols, which react too slowly E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
or not at all in Test Methods A and B.
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 April 1, 2023. Published June 2023. Originally th
...

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 − 17 E222 − 23
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) 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
These test methods are under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and are the direct responsibility of
Subcommittee D16.12 on Caustics and Peroxides.
Current edition approved June 1, 2017April 1, 2023. Published July 2017June 2023. Originally approved in 1963. Last previous edition approved in 20102017 as
E222 – 10.E222 – 17. DOI: 10.1520/E0222-17.10.1520/E0222-23.
*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 ----------------------
E222 − 23
1.4 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded in
accordance with the rounding off methods of Practice E29.
1.5 Review the current appropriate Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid procedures, and
safety precautions.
1.6 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific hazards statements are given in Section 7.
1.7 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3
D1957 Test Method for Hydroxyl Value of Fatty Oils and Acids (Wit
...

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1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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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ASTM
ASTM E1641-23(Test Method)
Standard Test Method for Decomposition Kinetics by Thermogravimetry Using the Ozawa/Flynn/Wall Method

SIGNIFICANCE AND USE
5.1 Thermogravimetry provides a rapid method for determining the temperature-decomposition profile of a material.  
5.2 This test method can be used for estimating lifetimes of materials, using Practice E1877 provided that a relationship has been established between the thermal endurance test results and actual lifetime tests.
SCOPE
1.1 This test method describes the determination of the kinetic parameters, Arrhenius activation energy, and pre-exponential factor by thermogravimetry, based on the assumption that the decomposition obeys first-order kinetics using the Ozawa/Flynn/Wall isoconversional method (1, 2).2  
1.2 This test method is generally applicable to materials with well-defined decomposition profiles, namely, a smooth, continuous mass change with a single maximum rate.  
1.3 This test method is normally applicable to decomposition occurring in the range from 400 K to 1300 K (nominally 100 °C to 1000 °C). The temperature range may be extended depending on the instrumentation used.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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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ASTM
ASTM E2403-23(Test Method)
Standard Test Method for Sulfated Ash of Organic Materials by Thermogravimetry

SIGNIFICANCE AND USE
5.1 The sulfated ash value indicates the level of known metal-containing additives or impurities in an organic material. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates. Tin and zinc are converted to their oxides.  
5.2 This test method may be used for research and development, specification acceptance, and quality assurance purposes.
SCOPE
1.1 This test method describes the determination of sulfated ash content (sometimes called residue-on-ignition) of organic materials by thermogravimetry. This test method converts common metals found in organic materials (such as sodium, potassium, lithium, calcium, magnesium, zinc, and tin) into their sulfate salts permitting estimation of their total content as sulfates or oxides. The range of this test method is from 0.1 % to 100 % metal content.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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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