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ASTM D5799-95(2000)e1

(Test Method)

Standard Test Method for Determination of Peroxides in Butadiene

Standard Test Method for Determination of Peroxides in Butadiene

SCOPE
1.1 This procedure covers the determination of peroxides in butadiene.  
1.2 This test method covers the concentrations range of 1 to 10 ppm by mass (ppmw) as available oxygen.  
1.3 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.

General Information

Status
Historical
Publication Date
09-Nov-2000
ICS
71.080.10 - Aliphatic hydrocarbons
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.D0.04 - C4 and C5 Hydrocarbons
Current Stage
Ref Project

Relations

Replaces
ASTM D5799-95 - Standard Test Method for Determination of Peroxides in Butadiene
Effective Date
10-Nov-2000
Replaced By
ASTM D5799-95(2004) - Standard Test Method for Determination of Peroxides in Butadiene
Effective Date
01-Nov-2004
Referred By
ASTM D5274-00(2019) - Standard Guide for Analysis of 1,3–Butadiene Product
Effective Date
10-Nov-2000

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ASTM D5799-95(2000)e1 - Standard Test Method for Determination of Peroxides in ButadieneASTM D5799-95(2000)e1 - Standard Test Method for Determination of Peroxides in Butadiene
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ASTM D5799-95(2000)e1 - Standard Test Method for Determination of Peroxides in Butadiene
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
e1
Designation:D5799–95 (Reapproved 2000)
Standard Test Method for
Determination of Peroxides in Butadiene
This standard is issued under the fixed designation D 5799; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Warning notes were placed in the text editorially in November 2000.
1. Scope 5. Apparatus
1.1 This procedure covers the determination of peroxides in 5.1 Condensers, Liebig, with 24/40 standard-tapered
butadiene. ground-glass joint connections.
1.2 This test method covers the concentrations range of 1 to 5.2 Cylinders, graduated, 100-mL capacity.
10 ppm by mass (ppmw) as available oxygen. 5.3 Flask, Erlenmeyer, 250-mL capacity, with 24/40
1.3 This standard does not purport to address all of the standard-tapered ground-glass connections with marking at
safety concerns, if any, associated with its use. It is the 100 mL.
responsibility of the user of this standard to establish appro- 5.4 Heating Mantle, electric for 250-mL Erlenmeyer flasks.
priate safety and health practices and determine the applica- 5.5 Microburette, 10-mL capacity, graduated in 0.02-mL
bility of regulatory limitations prior to use. divisions.
5.6 Water Bath, a thermostatically controlled liquid bath
2. Referenced Documents
capable of maintaining a water temperature of 60 6 1°C (140
2.1 ASTM Standards:
6 2°F).
D 1265 Practice for Sampling Liquefied Petroleum (LP)
6. Reagents
Gases–Manual Method
D 3700 Practice for Containing Hydrocarbons Fluid 6.1 Purity of Reagents—Reagent grade chemicals shall be
Samples Using a Floating Piston Cylinder used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
3. Summary of Test Method
tee onAnalytical Reagents of theAmerican Chemical Society,
3.1 A known mass of the butadiene sample is placed in a where such specifications are available. Other grades may be
flask and evaporated. The residue is then refluxed with acetic
used, provided it is first ascertained that the reagent is of
acid and sodium iodide reagents. The peroxides react to sufficiently high purity to permit its use without lessening the
liberate iodine which is titrated with standard sodium thiosul-
accuracy of the determination.
fatesolutionusingvisualend-pointdetection.Interferingtraces 6.2 Purity of Water—Unless otherwise indicated, references
of iron are complexed with sodium fluoride.
to water shall be understood to mean deionized or distilled
water.
4. Significance and Use
6.3 Acetic Acid, 94 % by volume. Mix 60 mL of water with
4.1 Due to the inherent danger of peroxides in butadiene,
940 mL of glacial acetic acid (CH COOH). (Warning—
specification limits are usually set for their presence. This test
Poisonous and corrosive. Combustible. May be fatal if swal-
method will provide values that can be used to determine the
lowed. Causes severe burns. Harmful if inhaled.)
peroxide content of a sample of commercial butadiene.
6.4 Carbon Dioxide,solid(dryice).(Warning—Usegloves
4.2 Butadiene polyperoxide is a very dangerous product of
to avoid frostbite when handling.)
the reaction between butadiene and oxygen that can occur. The
6.5 Potassium Dichromate Solution, Standard (0.1 N)—
peroxide has been reported to be the cause of some violent
Dissolve 2.452 g of potassium dichromate (K Cr O ) in water
2 2 7
explosions in vessels that are used to store butadiene.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on Reagent Chemicals, American Chemical Society Specifications, American
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Chemical Society, Washington, DC. For suggestions on the testing of reagents not
D02.D on Hydrocarbons for Chemical and Special Uses. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Oct. 10, 1995. Published December 1995. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 05.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 05.02. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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.
D5799
and dilute to 500 mL in a volumetric flask.(Warning—Avoid Immediately add 100 mL of water through the top of the
contact with eyes and skin and avoid breathing of dust.) condenser followed by several pellets of dry ice.
8.7 Maintaining an inert atmosphere with CO pellets,
6.6 Sodium Fluoride.
remove the flask from the condenser and allow to cool to
6.7 Sodium Iodide.
ambient temperature. Cold water may be used to assist in this
6.8 Sodium Thiosulfate Solution, Standard (0.1 N)—
step. Titrate the liberated iodine with 0.1 N sodium thiosulfate
Dissolve 12.5 g of sodium thiosulfate (Na S O 3 5H O) plus
2 2 3 2
until a clear endpoint is reached.
0.1 g of sodium carbonate (Na CO ) in 500
...

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4.1 This guide is intended to provide information on the possible composition of 1,3-butadiene products and possible ways to test them. Since there are currently not enough ASTM standards for determining all components of interest, this guide provides information on other potentially available test methods.  
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