ASTM_D_4423_-_10_2015.pdf

Designation:D442310(Reapproved 2015)Standard Test Method forDetermination of Carbonyls in C4Hydrocarbons1This standard is issued under the fixed designation D4423;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.Scope1.1 This test method covers the determination of carbonyls(ketones and aldehydes)in C4hydrocarbons.This test methodwas tested on polymerization-grade 1,3-butadiene.1.2 The applicable range for this test method is 0 mg kg to50 mgkg carbonyls calculated as acetaldehyde.1.3 Other C4hydrocarbons and their mixtures besidespolymerization-grade 1,3-butadiene could be tested using thissame test method.However,the precision section of this testmethod covers only carbonyls in applicable range as listed in1.2,as found in polymerization-grade 1,3-butadiene.1.4 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system,kidney and liver damage.Mercury,orits vapor,may be hazardous to health and corrosive tomaterials.Caution should be taken when handling mercury andmercury containing products.See the applicable product Ma-terial Safety Data Sheet(MSDS)for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information.Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D484 Specification for Hydrocarbon Dry Cleaning Solvents(Withdrawn 1982)3D1193 Specification for Reagent WaterE1 Specification for ASTM Liquid-in-Glass Thermometers3.Summary of Test Method3.1 A measured amount of sample is added to an alcoholichydroxylamine hydrochloride solution that has been adjustedto a given coloration using either alcoholic acid or base.Thecarbonyls will react with the hydroxylamine hydrochloridereleasing an equivalent amount of hydrochloric acid which isthen back-titrated to the original coloration.Ablank containingonly methanol and sample is titrated and the samples resultsare calculated using the blank adjustment.Results are reportedas milligrams per kilogram carbonyls as acetaldehyde.4.Significance and Use4.1 Thedeterminationofthecarbonylcontentofpolymerization-grade 1,3-butadiene is necessary,since in somepolymerization reactions,the presence of carbonyls in excessover some specified amount can have a deleterious effect uponthe polymer properties or the reaction itself,or both.5.Apparatus5.1 Bunsen ValvesA device constructed so that when usedwith an Erlenmeyer flask,the sample vapors can exit the flaskwhile protecting the flasks liquid contents.See Fig.1 fordetails.5.2 Cooling CoilPrepare a cooling coil by winding about10 cm to 15 cm of seamless copper tubing(about 6 mmdiameter)on a short length of pipe(about 1.5 cm to 2.0 cmdiameter),allowing sufficient length of tubing at the end of thecoil to connect it to the sample source.Attach a valve at a pointthat would not extend more than 8 cm above the surface of thecooling bath liquid.To the valve,attach a 6 cm to 8 cm length1This 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 Hydrocarbons.Current edition approved April 1,2015.Published May 2015.Originallyapproved in 1984.Last previous edition approved in 2010 as D4423 10.DOI:10.1520/D4423-10R15.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 piece of tubing bent downward so that the hydrocarbon liquidcan be directed into the receiving container.5.3 Dewar FlaskThe Dewar flask must be of sufficientvolume to completely immerse the main portion of the coolingcoil except for the extremities necessary for receiving anddelivering the sample through the coil.5.4 Erlenmeyer Flasks,250 mL capacity.5.5 Volumetric Flasks,1 L capacity.These flasks should beClass A glassware.5.6 GraduatedCylinders100 mLcapacity,glasscylinders,graduated in 1 mL or 2 mL divisions.5.7 Microburets,2.00 mL or 5.00 mL capacit