ASTM E1228-17

Standard Test Method for Assay of Peroxy Esters—Catalyzed Iodometric Procedure

SIGNIFICANCE AND USE
5.1 Peroxy esters are widely used as chemical intermediates, catalysts, and initiators. This test method provides a procedure for assaying peroxy esters to determine if they are suitable for their intended use.
SCOPE
1.1 This test method covers the assay of organic peroxides of the peroxy ester type.  
Note 1: Other test methods for the assay of organic peroxides are given in Test Methods E298, E475, and E755.  
1.2 Review the current 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 the standard. No other units of measurement are included in this test method.  
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. Specific hazards statements are given in Section 9.  
1.5 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: Historical
• Publication Date: 31-May-2017
• ICS: 71.080.70 - Esters
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E1228 − 17
Standard Test Method for
1
Assay of Peroxy Esters—Catalyzed Iodometric Procedure
This standard is issued under the fixed designation E1228; 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.
3
1. Scope* cialty Chemicals (Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage
1.1 This test method covers the assay of organic peroxides
of Standard and Reagent Solutions for Chemical Analysis
of the peroxy ester type.
E298 Test Methods for Assay of Organic Peroxides
NOTE 1—Other test methods for the assay of organic peroxides are
E475 Test Method for Assay of Di-tert-Butyl Peroxide
given in Test Methods E298, E475, and E755.
Using Gas Chromatography
1.2 Review the current safety data sheets (SDS) for detailed
E755 Test Method for Dicumyl Peroxide, Assay (Liquid
3
information concerning toxicity, first aid procedures, and safety
Chromatography) (Withdrawn 2016)
precautions.
3. Terminology
1.3 The values stated in SI units are to be regarded as the
3.1 Definitions:
standard. No other units of measurement are included in this
test method. 3.1.1 active oxygen—the oxidizing power present in organic
peroxides expressed as oxygen (equivalent weight 8.00).
1.4 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 Method
responsibility of the user of this standard to establish appro-
4.1 A sample is dissolved in a mixture of isopropyl alcohol,
priate safety, health, and environmental practices and deter-
acetic acid, and cupric chloride. A solution of potassium iodide
mine the applicability of regulatory limitations prior to use.
is added and the mixture is briefly heated, then allowed to react
Specific hazards statements are given in Section 9.
in the dark at room temperature for 30 min. The cupric ion
1.5 This international standard was developed in accor-
catalyzes the reduction of the peroxide and the liberated iodine
dance with internationally recognized principles on standard-
is titrated with standard sodium thiosulfate solution.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Significance and Use
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5.1 Peroxy esters are widely used as chemical
intermediates, catalysts, and initiators. This test method pro-
2. Referenced Documents vides a procedure for assaying peroxy esters to determine if
2 they are suitable for their intended use.
2.1 ASTM Standards:
D1193 Specification for Reagent Water
6. Interferences
D6809 Guide for Quality Control and Quality Assurance
6.1 Conjugated diolefins interfere under the conditions of
Procedures for Aromatic Hydrocarbons and Related Ma-
analysis by absorbing iodine.
terials
E180 Practice for Determining the Precision of ASTM
7. Apparatus
Methods for Analysis and Testing of Industrial and Spe-
7.1 Iodine Flasks, 250-mL capacity, with stoppers.
NOTE 2—All glassware should be cleaned thoroughly with dichromate
1
cleaning solution before use.
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
7.2 Beakers, 1-mL capacity, glass or PTFE.
bility of Subcommittee D16.12 on Caustics and Peroxides.
Current edition approved June 1, 2017. Published July 2017. Originally approved
7.3 Buret, 50-mL capacity, graduated in 0.1-mL subdivi-
in 1988. Last previous edition approved in 2009 as E1228 – 09. DOI: 10.1520/
sions.
E1228-17.
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
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. 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 ----------------------
E1228 − 17
be discarded and the analysis repeated if a significantly higher blank
7.4 Water Bath, maintained at 60°C.
value is obtained.)
8. Reagents
10.3 Sparge the solution with a rapid flow of nitrogen for 2
8.1 Purity of Reagents—Reagent grade chemicals shall be min, then stopper the flask and reserve.
used in all tests. Unless otherwise indicated, it is intended that
10.4 Accurately weigh a sample containing 3 to 4 meq
...

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: E1228 − 09 E1228 − 17
Standard Test Method for
1
Assay of Peroxy Esters—Catalyzed Iodometric Procedure
This standard is issued under the fixed designation E1228; 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 assay of organic peroxides of the peroxy ester type.
NOTE 1—Other test methods for the assay of organic peroxides are given in Test Methods E298, E475, and E755.
1.2 Review the current 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 the standard. No other units of measurement are included in this test
method.
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. Specific hazards statements are given in Section 9.
1.5 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
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
3
(Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
E298 Test Methods for Assay of Organic Peroxides
E475 Test Method for Assay of Di-tert-Butyl Peroxide Using Gas Chromatography
3
E755 Test Method for Dicumyl Peroxide, Assay (Liquid Chromatography) (Withdrawn 2016)
3. Terminology
3.1 Definitions:
3.1.1 active oxygen—the oxidizing power present in organic peroxides expressed as oxygen (equivalent weight 8.00).
4. Summary of Test Method
4.1 A sample is dissolved in a mixture of isopropyl alcohol, acetic acid, and cupric chloride. A solution of potassium iodide is
added and the mixture is briefly heated, then allowed to react in the dark at room temperature for 30 min. The cupric ion catalyzes
the reduction of the peroxide and the liberated iodine is titrated with standard sodium thiosulfate solution.
5. Significance and Use
5.1 Peroxy esters are widely used as chemical intermediates, catalysts, and initiators. This test method provides a procedure for
assaying peroxy esters to determine if they are suitable for their intended use.
1
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the direct
responsibility of Subcommittee D16.15 on Industrial and Specialty General Standards.
Current edition approved April 1, 2009June 1, 2017. Published April 2009July 2017. Originally approved in 1988. Last previous edition approved in 20032009 as
ε1
E1228 – 94 (2003)E1228 – 09. . DOI: 10.1520/E1228-09.10.1520/E1228-17.
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 ----------------------
E1228 − 17
6. Interferences
6.1 Conjugated diolefins interfere under the conditions of analysis by absorbing iodine.
7. Apparatus
7.1 Iodine Flasks, 250-mL capacity, with stoppers.
NOTE 2—All glassware should be cleaned thoroughly with dichromate cleaning solution before use.
7.2 Beakers, 1-mL capacity, glass or PTFE.
7.3 Buret, 50-mL capacity, graduated in 0.1-mL subdivisions.
7.4 Water Bath, maintained at 60°C.
8. Reagents
...