ASTM_D_1721_-_97_2007.pdf

Designation:D 1721 97(Reapproved 2007)Standard Test Method forPermanganate Time of Tricresyl Phosphate1This standard is issued under the fixed designation D 1721;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the detection in tricresyl phos-phate of the presence of impurities that reduce potassiumpermanganate.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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 specific hazardstatements,see Section 6.1.4 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent Water3.Significance and Use3.1 Impurities such as phenols,if present in tricresyl phos-phate,will react with potassium permanganate,reducing it tomanganese dioxide.In the permanganate test,the color of thetest solution is observed at the end of a 30-min period,and ifthe pink color is still present,the sample is consideredsubstantially free of oxidizable impurities.3.2 The results of this measurement can be used for speci-fication acceptance.4.Apparatus4.1 Graduated Cylinders,glass-stoppered,100-mL capac-ity.5.Reagents5.1 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.5.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type IV of Specification D 1193.5.3 Potassium Permanganate Solution(0.316 g/L)Dissolve 0.316 g of potassium permanganate(KMnO4)inwater and dilute to 1 L with freshly boiled water(Note 1).Thesolution should be stored in brown bottles and be freshlyprepared weekly as required.NOTE1Clean glassware is essential to the stability of the KMnO4solution.Clean graduated cylinders and permanganate storage and han-dling equipment with concentrated hydrochloric acid(HCl,sp gr 1.19)toremove residual manganese oxide(MnO2)which catalyzes reduction ofKMnO4.Remove the acid with not less than ten rinsings with water.6.Hazards6.1 Tricresyl phosphate is hazardous through inhalation orskin absorption.Take care in handling the material.Avoid eyeand skin contact and inhalation of vapors.6.2 Orthoisomer of tricresyl phosphate is considered toxic.Trace amounts may be present in tricresyl phosphate speci-mens.7.Procedure7.1 Weigh 10 6 0.1 g of the sample to be tested into a100-mLglass-stoppered graduated cylinder.To this,add 50 mLof the KMnO4solution.Vigorously shake the mixture for 21This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved June 1,2007.Published June 2007.Originallyapproved in 1960.Last previous edition approved in 2001 as D 1721 97(2001).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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.min,noting the time when the shaking begins.Allow the test tostand for a period of 28 min following the shaking period andobserve the color.8.Report8.1 If the color of the permanganate solution is still pink,report the sample as“passing.”If no pink color is present,report the sample as“not passing.”9.Precision and Bias9.1 PrecisionNo statement is made about the precision ofassessing this test method,since the results of the test methodare pass-fail.9.2 BiasBias cannot be determined for this test methodbecause there is no available material