ASTM_D_1612_-_95_1999.pdf

Designation:D 1612 95(Reapproved 1999)Standard Test Method forAcetone in Methanol1This standard is issued under the fixed designation D 1612;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 a procedure for detecting thepresence of acetone in methanol in amounts greater than 0.003weight%.1.2 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.1.3 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Summary of Test Method3.1 The specimen is reacted with Nesslers reagent and theturbidity that is produced is compared to a standard containingthe equivalent of 0.003 weight%of acetone.4.Significance and Use4.1 This test method can be used to detect residual amountsof carbonyl compounds in synthetic and natural methanol.Thecarbonyl compounds are quantified by comparison to a knownstandard of acetone solution.4.2 Carbonyl compounds may be present as a result ofcontamination during storage,distribution,or manufacture.This test method may be used in assessing compliance with aspecification.5.Apparatus5.1 Volumetric Pipets,1,4,and 5-mL capacity.5.2 Test Tubes,matched for color,1.5 by 15 cm.6.Reagents6.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.3Other grades may be used,pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.6.2 Unless otherwise indicated,references to water shall beunderstood to mean reagent water conforming to Type IV ofSpecification D 1193.It is essential that the reagent water befree of ammonia.6.3 Acetone StandardPipet 6.0 mL of acetone into a 1-Lvolumetric flask and dilute with water to the 1-L mark.Take1.0 mL of the resulting solution and make up to 1 L with waterin a volumetric flask.Five millilitres of this solution contain0.024 mg of acetone.Under conditions outlined for this testmethod,the standard made up for comparison is equivalent toa methanol specimen containing 0.003 weight%of acetone.6.4 Nesslers Reagent:6.4.1 Solution ADissolve 270 g of sodium hydroxide(NaOH)pellets in water and dilute to 1 L.6.4.2 Solution BDissolve 36 g of potassium iodide(KI)crystals and 13.6 g of mercuric chloride(HgCl2)powder inwater and dilute to 500 mL.To prepare the Nesslers reagent,mix three parts of Solution A with 5 parts of Solution B andallow to stand until clear before using.7.Procedure7.1 Carefully pipet 1 mL of the sample and 4 mL of waterinto one of the matched test tubes and mix thoroughly.Carefully pipet 5 mL of the acetone standard into a secondmatched test tube.Pipet 5 mLof the Nesslers reagent into eachof the tubes containing the specimen and the acetone standard.Quickly mix the contents of each tube and allow both to standfor 5 min.At the end of the 5-min standing period,compare theturbidity of the specimen to the turbidity of the acetonestandard.8.Report8.1 If the turbidity of the specimen is less than that of theacetone standard,report the acetone content is“less than 0.0031This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved Feb.15,1995.Published April 1995.Originallypublished as D 1612 58 T.Last previous edition D 1612 90.2Annual Book of ASTM Standards,Vol 11.01.3Reagent 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,100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.weight%.”If the turbidity of the specimen is greater than thatof the acetone standard,report the acetone content as“greaterthan 0.003 weight%.”9.Precision and Bias9.1 PrecisionBecause of the“pass-fail”nature of thisprocedure,there is no precision statement.9.2 BiasAny material or contaminant that will react withNesslers reagent will affect the results.9.2.1 The results are reported“less t