ASTM D5799-23

Standard Test Method for Determination of Peroxides in Butadiene

SIGNIFICANCE AND USE
4.1 Due to the inherent danger of peroxides in butadiene, specification limits are usually set for their presence. This test method will provide values that can be used to determine the peroxide content of a sample of commercial butadiene.  
4.2 Butadiene polyperoxide is a very dangerous product of the reaction between butadiene and oxygen that can occur. The peroxide has been reported to be the cause of some violent explosions in vessels that are used to store butadiene.
SCOPE
1.1 This test method covers the determination of peroxides in butadiene.  
1.2 This test method covers the concentrations range of 1 mg/kg to 10 mg/kg as available oxygen.  
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 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.  
1.4.1 The user is advised to obtain LPG safety training for the safe operation of this test method procedure and related activities.  
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: Published
• Publication Date: 28-Feb-2023
• ICS: 71.080.10 - Aliphatic hydrocarbons
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.D0.04 - C4 and C5 Hydrocarbons

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: D5799 − 23
Standard Test Method for
1
Determination of Peroxides in Butadiene
This standard is issued under the fixed designation D5799; 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* acid and sodium iodide reagents. The peroxides react to
liberate iodine which is titrated with standard sodium thiosul-
1.1 This test method covers the determination of peroxides
fate solution using visual end-point detection. Interfering traces
in butadiene.
of iron are complexed with sodium fluoride.
1.2 This test method covers the concentrations range of
1 mg ⁄kg to 10 mg ⁄kg as available oxygen.
4. Significance and Use
1.3 The values stated in SI units are to be regarded as
4.1 Due to the inherent danger of peroxides in butadiene,
standard. No other units of measurement are included in this
specification limits are usually set for their presence. This test
standard.
method will provide values that can be used to determine the
peroxide content of a sample of commercial butadiene.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.2 Butadiene polyperoxide is a very dangerous product of
responsibility of the user of this standard to establish appro-
the reaction between butadiene and oxygen that can occur. The
priate safety, health, and environmental practices and deter-
peroxide has been reported to be the cause of some violent
mine the applicability of regulatory limitations prior to use.
explosions in vessels that are used to store butadiene.
1.4.1 The user is advised to obtain LPG safety training for
5. Apparatus
the safe operation of this test method procedure and related
activities.
5.1 Condensers, Liebig, with 24/40 standard-tapered
1.5 This international standard was developed in accor- ground-glass joint connections.
dance with internationally recognized principles on standard-
5.2 Cylinders, graduated, 100 mL capacity.
ization established in the Decision on Principles for the
5.3 Flask, Erlenmeyer, 250 mL capacity, with 24/40
Development of International Standards, Guides and Recom-
standard-tapered ground-glass connections with marking at
mendations issued by the World Trade Organization Technical
100 mL.
Barriers to Trade (TBT) Committee.
5.4 Heating Mantle, electric, for 250 mL Erlenmeyer flasks.
2. Referenced Documents
5.5 Microburette, 10 mL capacity, graduated in 0.02 mL
2
2.1 ASTM Standards:
divisions.
D1265 Practice for Sampling Liquefied Petroleum (LP)
5.6 Water Bath, a thermostatically controlled liquid bath
Gases, Manual Method
capable of maintaining a water temperature of 60 °C 6 1 °C.
D3700 Practice for Obtaining LPG Samples Using a Float-
ing Piston Cylinder
6. Reagents
3. Summary of Test Method
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
3.1 A known mass of the butadiene sample is placed in a
all reagents shall conform to the specifications of the Commit-
flask and evaporated. The residue is then refluxed with acetic
tee on Analytical Reagents of the American Chemical Society,
3
where such specifications are available. Other grades may be
1
This test method is under the jurisdiction of ASTM Committee D02 on
used, provided it is first ascertained that the reagent is of
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.D0.04 on C4 and C5 Hydrocarbons.
Current edition approved March 1, 2023. Published June 2023. Originally
3
approved in 1995. Last previous edition approved in 2019 as D5799 – 19. DOI: ACS Reagent Chemicals, Specifications and Procedures for Reagents and
10.1520/D5799-23. Standard-Grade Reference Materials, American Chemical Society, Washington,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by the American Chemical
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
...

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: D5799 − 19 D5799 − 23
Standard Test Method for
1
Determination of Peroxides in Butadiene
This standard is issued under the fixed designation D5799; 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 determination of peroxides in butadiene.
1.2 This test method covers the concentrations range of 1 mg ⁄kg to 10 mg ⁄kg as available oxygen.
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 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 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.
1.4.1 The user is advised to obtain LPG safety training for the safe operation of this test method procedure and related activities.
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:
D1265 Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
D3700 Practice for Obtaining LPG Samples Using a Floating Piston Cylinder
3. Summary of Test Method
3.1 A known mass of the butadiene sample is placed in a flask and evaporated. The residue is then refluxed with acetic acid and
sodium iodide reagents. The peroxides react to liberate iodine which is titrated with standard sodium thiosulfate solution using
visual end-point detection. Interfering traces of iron are complexed with sodium fluoride.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.D0.04 on C4 and C5 Hydrocarbons.
Current edition approved Dec. 1, 2019March 1, 2023. Published January 2020June 2023. Originally approved in 1995. Last previous edition approved in 20142019 as
D5799 – 95 (2014).D5799 – 19. DOI: 10.1520/D5799-19.10.1520/D5799-23.
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.
*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

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D5799 − 23
4. Significance and Use
4.1 Due to the inherent danger of peroxides in butadiene, specification limits are usually set for their presence. This test method
will provide values that can be used to determine the peroxide content of a sample of commercial butadiene.
4.2 Butadiene polyperoxide is a very dangerous product of the reaction between butadiene and oxygen that can occur. The
peroxide has been reported to be the cause of some violent explosions in vessels that are used to store butadiene.
5. Apparatus
5.1 Condensers, Liebig, with 24/40 standard-tapered ground-glass joint connections.
5.2 Cylinders, graduated, 100 mL capacity.
5.3 Flask, Erlenmeyer, 250 mL capacity, with 24/40 standard-tapered ground-glass connections with marking at 100 mL.
5.4 Heating Mantle, electric, for 250 mL Erlenmeyer flasks.
5.5 Microburette, 10 mL capacity, graduated in 0.02 mL divisions.
5.6 Water Bath, a thermostatically controlled liquid bath capable of maintaining a water temperature of 60 °C 6 1 °C.
6. Reagents
6.1 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 A
...