ASTM E1228-09
(Test Method)Standard Test Method for Assay of Peroxy Esters-Catalyzed Iodometric Procedure
Standard Test Method for Assay of Peroxy Esters-Catalyzed Iodometric Procedure
SIGNIFICANCE AND USE
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 E 298, E 475, and E 755.
1.2 Review the current material safety data sheets (MSDS) 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.
General Information
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Designation: E1228 − 09
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* E755 Test Method for Dicumyl Peroxide, Assay (Liquid
Chromatography)
1.1 This test method covers the assay of organic peroxides
of the peroxy ester type.
3. Terminology
NOTE 1—Other test methods for the assay of organic peroxides are
3.1 Definitions:
given in Test Methods E298, E475, and E755.
3.1.1 active oxygen—the oxidizing power present in organic
1.2 Review the current material safety data sheets (MSDS)
peroxides expressed as oxygen (equivalent weight 8.00).
for detailed information concerning toxicity, first aid
4. Summary of Test Method
procedures, and safety precautions.
4.1 Asample is dissolved in a mixture of isopropyl alcohol,
1.3 The values stated in SI units are to be regarded as the
acetic acid, and cupric chloride.Asolution of potassium iodide
standard. No other units of measurement are included in this
isaddedandthemixtureisbrieflyheated,thenallowedtoreact
test method.
in the dark at room temperature for 30 min. The cupric ion
1.4 This standard does not purport to address all of the
catalyzes the reduction of the peroxide and the liberated iodine
safety concerns, if any, associated with its use. It is the
is titrated with standard sodium thiosulfate solution.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. Specific hazards
5.1 Peroxy esters are widely used as chemical
statements are given in Section 9.
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
E180 Practice for Determining the Precision of ASTM
6.1 Conjugated diolefins interfere under the conditions of
Methods for Analysis and Testing of Industrial and Spe-
3 analysis by absorbing iodine.
cialty Chemicals (Withdrawn 2009)
E200 Practice for Preparation, Standardization, and Storage
7. Apparatus
of Standard and Reagent Solutions for ChemicalAnalysis
7.1 Iodine Flasks, 250-mL capacity, with stoppers.
E298 Test Methods for Assay of Organic Peroxides
E475 Test Method for Assay of Di-tert-Butyl Peroxide
NOTE 2—All glassware should be cleaned thoroughly with dichromate
cleaning solution before use.
Using Gas Chromatography
7.2 Beakers, 1-mL capacity, glass or PTFE.
1
This test method is under the jurisdiction of ASTM Committee D16 on
7.3 Buret, 50-mL capacity, graduated in 0.1-mL subdivi-
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
sions.
Subcommittee D16.15 on Industrial and Specialty General Standards.
Current edition approved April 1, 2009. Published April 2009. Originally
7.4 Water Bath, maintained at 60°C.
ε1
approved in 1988. Last previous edition approved in 2003 as E1228 – 94 (2003) .
DOI: 10.1520/E1228-09.
8. Reagents
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
8.1 Purity of Reagents—Reagent grade chemicals shall be
Standards volume information, refer to the standard’s Document Summary page on
used in all tests. Unless otherwise indicated, it is intended that
the ASTM website.
3 all reagents shall conform to the Specifications of the Com-
The last approved version of this historical standard is referenced on
www.astm.org. mittee on Analytical Reagents of the American Chemical
*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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E1228 − 09
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Society, where such specifications are available. Other grades thesampletothepreparedflaskandimmediatelyrestopperand
may be used, provided it is first ascertained that the reagent is mix. The approximate sample weight may be calculated as
of sufficiently high purity to permit its use without lessening follows:
the accuracy of the determination.
3.5 M
Sample mass, g 5 (2)
8.2 Purity of Water—Unless otherwise indicated, references 2C 31000
to water shall be understood to mean Type II or III reagent
where:
water conforming to Specification D1193.
M = molecular weight of compound, and
8.3 Acetic Acid,
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
´1
Designation:E1228–94 (Reapproved 2003) Designation:E1228–09
Standard Test Method for
1
Assay of Peroxy Esters—Catalyzed Iodometric Procedure
This standard is issued under the fixed designation E 1228; 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
´ NOTE—“Between Days Variability” was dropped from the title of 13.1.2 editorially in October 2003.
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 E755E 298, E 475, and E 755.
1.2 Reviewthecurrentmaterialsafetydatasheets(MSDS)fordetailedinformationconcerningtoxicity,firstaidprocedures,and
safety precautions.
1.3The values stated in SI units are to be regarded as the standard.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
E 180 Practice for Determining the Precision ofASTM Methods forAnalysis andTesting of Industrial and Specialty Chemicals
E 200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
E 298 Test Methods for Assay of Organic Peroxides
E 475 Test Method for Assay of Di-tert-Butyl Peroxide byUsing Gas Chromatographic AnalysisChromatography
E 755 Test Method for Assay of Dicumyl Peroxide by Liquid Chromatography Test Method for Dicumyl Peroxide, Assay
(Liquid Chromatography)
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 Asample is dissolved in a mixture of isopropyl alcohol, acetic acid, and cupric chloride.Asolution 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.
6. Interferences
6.1 Conjugated diolefins interfere under the conditions of analysis by absorbing iodine.
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 Dec. 15, 1994. Published February 1995. Originally published as E1228–88. Last previous edition E1228–88. on General Standards.
´1
Current edition approved April 1, 2009. Published April 2009. Originally approved in 1988. Last previous edition approved in 2003 as E 1228 - 94(2003) .
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website. .
*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 ----------------------
E1228–09
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
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the Specifications of the Committee on Analytical Reagents of the American Chemical Society, where
3
such specifications are
...
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