ASTM E299-17a
(Test Method)Standard Test Method for Trace Amounts of Peroxides In Organic Solvents
Standard Test Method for Trace Amounts of Peroxides In Organic Solvents
SIGNIFICANCE AND USE
4.1 Dilute solutions of peroxides in various organic solvents frequently are used as catalysts or reaction initiators. Peroxides also can be formed through autoxidation in certain classes of compounds including ethers, acetals, dienes, and alkylaromatic hydrocarbons and present a potential safety hazard. This test method provides a procedure for determining the peroxide or active oxygen level.
SCOPE
1.1 This test method2,3 covers organic solvents containing active oxygen in the range from 5 to 80 μg/g (ppm) or higher. By using a special reaction-absorption cell, the test method can be extended to cover the range from 0 to 5 ppm. The test method can be used to determine numerous peroxide classes of varying reactivity such as hydroperoxides, diacyl peroxides, diaroyl peroxides, peresters, and ketone peroxides. The stable di-tert-alkyl peroxides do not react under the conditions of analysis.
1.2 Solvents that can be analyzed successfully include saturated and aromatic hydrocarbons, alcohols, ethers, ketones, and esters. In addition, the test method is applicable to olefinic solvents and to certain compounds that contain α, β, and conjugated unsaturation. Solid samples that are soluble in the acetic acid-chloroform solvent also can be analyzed.
1.3 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid practices, and safety precautions.
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address 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.
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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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: E299 − 17a
Standard Test Method for
1
Trace Amounts of Peroxides In Organic Solvents
This standard is issued under the fixed designation E299; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* mendations issued by the World Trade Organization Technical
2,3 Barriers to Trade (TBT) Committee.
1.1 This test method covers organic solvents containing
active oxygen in the range from 5 to 80 µg/g (ppm) or higher.
2. Referenced Documents
By using a special reaction-absorption cell, the test method can
4
2.1 ASTM Standards:
be extended to cover the range from 0 to 5 ppm. The test
D1193 Specification for Reagent Water
method can be used to determine numerous peroxide classes of
D6809 Guide for Quality Control and Quality Assurance
varying reactivity such as hydroperoxides, diacyl peroxides,
Procedures for Aromatic Hydrocarbons and Related Ma-
diaroyl peroxides, peresters, and ketone peroxides. The stable
terials
di-tert-alkyl peroxides do not react under the conditions of
E180 Practice for Determining the Precision of ASTM
analysis.
Methods for Analysis and Testing of Industrial and Spe-
1.2 Solvents that can be analyzed successfully include
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cialty Chemicals (Withdrawn 2009)
saturatedandaromatichydrocarbons,alcohols,ethers,ketones,
and esters. In addition, the test method is applicable to olefinic
3. Summary of Test Method
solvents and to certain compounds that contain α, β, and
3.1 A sample is dissolved in a mixture of acetic acid and
conjugated unsaturation. Solid samples that are soluble in the
chloroform. The solution is deaerated and potassium iodide
acetic acid-chloroform solvent also can be analyzed.
reagentsolutionisadded.Themixtureisallowedtoreactinthe
1.3 Review the current Safety Data Sheets (SDS) for de-
dark for 1 h, thereby releasing an equivalent amount of iodine.
tailed information concerning toxicity, first aid practices, and
The absorbance of the solution is measured at 470 nm and the
safety precautions.
amount of active oxygen present in the sample is determined
1.4 The values stated in SI units are to be regarded as
by reference to a calibration curve prepared from iodine.
standard. The values given in parentheses are for information
3.2 Forsamplescontaining0to5µg/g(ppm)activeoxygen,
only.
a special reaction-absorption cell is employed. The sample is
1.5 This standard does not purport to address the safety
de-aerated and the reaction is carried out within the cell.
concerns, if any, associated with its use. It is the responsibility
Absorbance measurements are made at 410 nm to increase the
of the user of this standard to establish appropriate safety,
sensitivity.
health, and environmental practices and determine the appli-
cability of regulatory limitations prior to use.
4. Significance and Use
1.6 This international standard was developed in accor-
4.1 Dilute solutions of peroxides in various organic solvents
dance with internationally recognized principles on standard-
frequently are used as catalysts or reaction initiators. Peroxides
ization established in the Decision on Principles for the
also can be formed through autoxidation in certain classes of
Development of International Standards, Guides and Recom-
compounds including ethers, acetals, dienes, and alkylaromatic
hydrocarbons and present a potential safety hazard. This test
method provides a procedure for determining the peroxide or
1
This test method is under the jurisdiction of ASTM Committee D16 on
active oxygen level.
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
bility of Subcommittee D16.12 on Caustics and Peroxides.
Current edition approved July 1, 2017. Published July 2017. Originally approved
4
in 1966. Last previous edition approved in 2017 as E299 – 17. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
E0299-17a. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
Banerjee, D. K., and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, Standards volume information, refer to the standard’s Document Summary page on
1964, pp. 792–796. the ASTM website.
3 5
Banerjee, D. K., and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, The last approved version of this historical standard is referenced on
1964, pp. 2367–2368. www.astm.org.
*A Summary of Changes section appear
...
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: E299 − 17 E299 − 17a
Standard Test Method for
1
Trace Amounts of Peroxides In Organic Solvents
This standard is issued under the fixed designation E299; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope*
2,3
1.1 This test method covers organic solvents containing active oxygen in the range from 5 to 80 μg/g (ppm) or higher. By
using a special reaction-absorption cell, the test method can be extended to cover the range from 0 to 5 ppm. The test method can
be used to determine numerous peroxide classes of varying reactivity such as hydroperoxides, diacyl peroxides, diaroyl peroxides,
peresters, and ketone peroxides. The stable di-tert-alkyl peroxides do not react under the conditions of analysis.
1.2 Solvents that can be analyzed successfully include saturated and aromatic hydrocarbons, alcohols, ethers, ketones, and
esters. In addition, the test method is applicable to olefinic solvents and to certain compounds that contain α,β, and conjugated
unsaturation. Solid samples that are soluble in the acetic acid-chloroform solvent also can be analyzed.
1.3 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid practices, and safety
precautions.
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address 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.
1.5 Review the current Safety Data Sheets (SDS) for detailed information concerning toxicity, first aid practices, and safety
precautions.
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.
2. Referenced Documents
4
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
5
(Withdrawn 2009)
3. Summary of Test Method
3.1 A sample is dissolved in a mixture of acetic acid and chloroform. The solution is deaerated and potassium iodide reagent
solution is added. The mixture is allowed to react in the dark for 1 h, thereby releasing an equivalent amount of iodine. The
absorbance of the solution is measured at 470 nm and the amount of active oxygen present in the sample is determined by reference
to a calibration curve prepared from iodine.
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 Feb. 1, 2017July 1, 2017. Published February 2017July 2017. Originally approved in 1966. Last previous edition approved in 20082017 as
E299 – 08.E299 – 17. DOI: 10.1520/E0299-17.10.1520/E0299-17a.
2
Banerjee, D. K., and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, 1964, pp. 792–796.
3
Banerjee, D. K., and Budke, C. C., Analytical Chemistry, ANCHAM, Vol 36, 1964, pp. 2367–2368.
4
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 Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
5
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
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E299 − 17a
3.2 For samples containing 0 to 5 μg/g (ppm) active oxygen, a special reaction-absorption cell is
...
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