ASTM D5799-19

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.  
1.5 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: 30-Nov-2019
• 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)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5799 − 19
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* fate solution using visual end-point detection. Interfering traces
of iron are complexed with sodium fluoride.
1.1 This test method covers the determination of peroxides
in butadiene.
4. Significance and Use
1.2 This test method covers the concentrations range of
4.1 Due to the inherent danger of peroxides in butadiene,
1 mg ⁄kg to 10 mg ⁄kg as available oxygen.
specification limits are usually set for their presence. This test
1.3 The values stated in SI units are to be regarded as
method will provide values that can be used to determine the
standard. No other units of measurement are included in this
peroxide content of a sample of commercial butadiene.
standard.
4.2 Butadiene polyperoxide is a very dangerous product of
1.4 This standard does not purport to address all of the
the reaction between butadiene and oxygen that can occur. The
safety concerns, if any, associated with its use. It is the
peroxide has been reported to be the cause of some violent
responsibility of the user of this standard to establish appro-
explosions in vessels that are used to store butadiene.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
5. Apparatus
1.5 This international standard was developed in accor-
5.1 Condensers, Liebig, with 24/40 standard-tapered
dance with internationally recognized principles on standard-
ground-glass joint connections.
ization established in the Decision on Principles for the
5.2 Cylinders, graduated, 100 mL capacity.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5.3 Flask, Erlenmeyer, 250 mL capacity, with 24/40
Barriers to Trade (TBT) Committee.
standard-tapered ground-glass connections with marking at
100 mL.
2. Referenced Documents
5.4 Heating Mantle, electric, for 250 mL Erlenmeyer flasks.
2
2.1 ASTM Standards:
5.5 Microburette, 10 mL capacity, graduated in 0.02 mL
D1265 Practice for Sampling Liquefied Petroleum (LP)
divisions.
Gases, Manual Method
5.6 Water Bath, a thermostatically controlled liquid bath
D3700 Practice for Obtaining LPG Samples Using a Float-
capable of maintaining a water temperature of 60 °C 6 1 °C.
ing Piston Cylinder
6. Reagents
3. Summary of Test Method
6.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 A known mass of the butadiene sample is placed in a
used in all tests. Unless otherwise indicated, it is intended that
flask and evaporated. The residue is then refluxed with acetic
all reagents shall conform to the specifications of the Commit-
acid and sodium iodide reagents. The peroxides react to
tee on Analytical Reagents of the American Chemical Society,
liberate iodine which is titrated with standard sodium thiosul-
3
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
1
This test method is under the jurisdiction of ASTM Committee D02 on
accuracy of the determination.
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, 2019. Published January 2020. Originally
3
approved in 1995. Last previous edition approved in 2014 as D5799 – 95 (2014). ACS Reagent Chemicals, Specifications and Procedures for Reagents and
DOI: 10.1520/D5799-19. 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 Conshohocken, PA 19428-2959. United States
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D5799 − 19
6.2 Purity of Water—Unless otherwise indicated, references 0.20 g 6 0.
...

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 − 95 (Reapproved 2014) D5799 − 19
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 Scope*
1.1 This test method covers the determination of peroxides in butadiene.
1.2 This test method covers the concentrations range of 11 mg ⁄kg to 1010 mg ppm by mass (ppmw) ⁄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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
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.
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-mL100 mL capacity.
5.3 Flask, Erlenmeyer, 250-mL250 mL capacity, with 24/40 standard-tapered ground-glass connections with marking at 100
mL.100 mL.
5.4 Heating Mantle, electric, for 250-mL250 mL Erlenmeyer flasks.
5.5 Microburette, 10-mL10 mL capacity, graduated in 0.02-mL0.02 mL divisions.
5.6 Water Bath, a thermostatically controlled liquid bath capable of maintaining a water temperature of 6060 °C 6 1°C.1 °C.
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 May 1, 2014Dec. 1, 2019. Published July 2014January 2020. Originally approved in 1995. Last previous edition approved in 20092014 as
D5799 – 95 (2009).(2014). DOI: 10.1520/D5799-95R14.10.1520/D5799-19.
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

---------------------- Page: 1 ----------------------
D5799 − 19
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 American Chemical Society, where
3
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to
...