1、Designation:D579995(Reapproved 2014)Standard 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
2、 number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of peroxidesin butadiene.1.2 This test method covers the concentrations range of 1 to10 ppm by m
3、ass(ppmw)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 s
4、tandard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1265 Practice for Sampling Liquefied Petroleum(LP)Gases,Manual MethodD3700 Practice for Obtaining LPG Samples Using a Float
5、-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 vis
6、ual 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 co
7、ntent 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,Li
8、ebig,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 capaci
9、ty,graduated in 0.02-mLdivisions.5.6 Water Bath,a thermostatically controlled liquid bathcapable of maintaining a water temperature of 60 6 1C.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to
10、 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 determ
11、ination.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 mL of glacial acetic acid(CH3COOH).(Warning1This test method is under the jurisdiction of ASTM Committee D02 onPetr
12、oleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.D0.04 on C4 Hydrocarbons.Current edition approved May 1,2014.Published July 2014.Originally approvedin 1995.Last previous edition approved in 2009 as D5799 95(2009).DOI:10.1520/D5799-95R14.2For referenced
13、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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Socie
14、ty,Washington,DC.For Suggestions on the testing of reagents notlisted by the American Chemical Society,see Annual Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyright ASTM
15、International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 Poisonous and corrosive.Combustible.May be fatal if swal-lowed.Causes severe burns.Harmful if inhaled.)6.4 Carbon Dioxide,solid(dry ice).(WarningUse glovesto avoid frostbite when handling.)6.5 Potassium Di
16、chromate Solution,Standard(0.1 N)Dissolve 2.452 g of potassium dichromate(K2Cr2O7)in waterand dilute to 500 mL in a volumetric flask.(WarningAvoidcontact with eyes and skin and avoid breathing of dust.)6.6 Sodium Fluoride.6.7 Sodium Iodide.6.8 Sodium Thiosulfate Solution,Standard(0.1 N)Dissolve 12.5 g of sodium thiosulfate(Na2S2O3 5H2O)plus0.1 g of sodium carbonate(Na2CO3)in 500 mL of water(theNa2CO3is added to stabilize the Na2S2O3solution).Let thissolution stand a week or more before using.Sta