ASTM_D_5799_-_19.pdf

Designation:D579919Standard Test Method forDetermination of Peroxides in Butadiene1This standard is issued under the fixed designation D5799;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope*1.1 This test method covers the determination of peroxidesin butadiene.1.2 This test method covers the concentrations range of1 mg kg to 10 mgkg as available oxygen.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D1265 Practice for Sampling Liquefied Petroleum(LP)Gases,Manual MethodD3700 Practice for Obtaining LPG Samples Using a Float-ing Piston Cylinder3.Summary of Test Method3.1 A known mass of the butadiene sample is placed in aflask and evaporated.The residue is then refluxed with aceticacid and sodium iodide reagents.The peroxides react toliberate iodine which is titrated with standard sodium thiosul-fate solution using visual end-point detection.Interfering tracesof iron are complexed with sodium fluoride.4.Significance and Use4.1 Due to the inherent danger of peroxides in butadiene,specification limits are usually set for their presence.This testmethod will provide values that can be used to determine theperoxide content of a sample of commercial butadiene.4.2 Butadiene polyperoxide is a very dangerous product ofthe reaction between butadiene and oxygen that can occur.Theperoxide has been reported to be the cause of some violentexplosions in vessels that are used to store butadiene.5.Apparatus5.1 Condensers,Liebig,with 24/40 standard-taperedground-glass joint connections.5.2 Cylinders,graduated,100 mL capacity.5.3 Flask,Erlenmeyer,250 mL capacity,with 24/40standard-tapered ground-glass connections with marking at100 mL.5.4 Heating Mantle,electric,for 250 mL Erlenmeyer flasks.5.5 Microburette,10 mL capacity,graduated in 0.02 mLdivisions.5.6 Water Bath,a thermostatically controlled liquid bathcapable of maintaining a water temperature of 60 C 6 1 C.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.D0.04 on C4 and C5 Hydrocarbons.Current edition approved Dec.1,2019.Published January 2020.Originallyapproved in 1995.Last previous edition approved in 2014 as D5799 95(2014).DOI:10.1520/D5799-19.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3ACS Reagent Chemicals,Specifications and Procedures for Reagents andStandard-Grade Reference Materials,American Chemical Society,Washington,DC.For suggestions on the testing of reagents not listed by the American ChemicalSociety,see Analar Standards for Laboratory Chemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeia and National Formulary,U.S.Pharma-copeial Convention,Inc.(USPC),Rockville,MD.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean deionized or distilledwater.6.3 Acetic Acid,94%by volume.Mix 60 mL of water with940 m