ASTM_D_5194_-_13.pdf

Designation:D519413Standard Test Method forTrace Chloride in Liquid Aromatic Hydrocarbons1This standard is issued under the fixed designation D5194;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 totalchloride(organic and inorganic)in liquid aromatic hydrocar-bons and cyclohexane.1.2 The test method is applicable to samples with chlorideconcentrations of 1 to 25 mg/kg.1.3 Bromides and iodides,if present,will be calculated aschlorides.1.4 Materials,such as styrene,that are polymerized bysodium biphenyl reagent cannot be analyzed by this testmethod.1.5 In determining the conformance of the test results usingthis method to applicable specifications,results shall berounded off in accordance with the rounding-off method ofPractice E29.1.6 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.7 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.For a specifichazard statement,see Section 7.2.Referenced Documents2.1 ASTM Standards:2D891 Test Methods for Specific Gravity,Apparent,of LiquidIndustrial ChemicalsD1193 Specification for Reagent WaterD1555M Test Method for Calculation of Volume and Weightof Industrial Aromatic Hydrocarbons and CyclohexaneMetricD3437 Practice for Sampling and Handling Liquid CyclicProductsD3505 Test Method for Density or Relative Density of PureLiquid ChemicalsD4052 Test Method for Density,Relative Density,and APIGravity of Liquids by Digital Density MeterD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2.2 Other Documents:3OSHA Regulations,29 CFR paragraphs 1910.1000 and1910.12003.Summary of Test Method3.1 A known amount of hydrocarbon sample is transferredinto a separatory funnel containing toluene.Sodium biphenylreagent is added to convert organic halogens into inorganichalides.The excess reagent is decomposed with water and thephases are separated.The aqueous phase is acidified,washed,and concentrated.Acetone is added and the solution is titratedwith silver nitrate solution.4.Significance and Use4.1 Organic and inorganic chlorine compounds can have adeleterious effect on equipment and reactions in processesinvolving aromatic hydrocarbons.4.2 Maximum chloride levels are often specified for processstreams and for aromatic hydrocarbon products.5.Apparatus5.1 Titrator,potentiometric,recording,+2000 mV range,1mV resolution with dispenser having a volume readout of 0.00to 9.99 mL or 0.00 to 99.99 mL and 0.01%resolution.5.2 Electrode,glass,reference.5.3 Electrode,silver,billet type.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved July 1,2013.Published July 2013.Originally approvedin 1991.Last previous edition approved in 2011 as D5194 11a.DOI:10.1520/D5194-13.2For 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.3Available from U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.*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 States1 6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Types II or III of Specification D1193.6.3 Acetone,99.9%purity.6.4 Congo Red Paper.6.5 Detergent,residue free.6.6 Isobutanol,99.9%minimum purity.6.7 Isooctane.6.8 Nitric Acid,concentrated.6.9 Nitric Acid,5-M.Dilute 160 mLconcentrated nitric acidto 500 mL with water.6.10 Potassium Chloride,primary s