ASTM_D_1612_-_05.pdf

Designation:D 1612 05Standard 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.Scope*1.1 This test method covers a procedure for detecting thepresence of acetone in methanol in amounts greater than 0.003weight%.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications,test result(s)shall be rounded off“to the nearestunit”in the last right-hand digit used in expressing thespecification limit,in accordance with the rounding-off methodof Practice E 29.1.4 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 standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.5 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2E 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3.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,1This 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 May 15,2005.Published May 2005.Originallyapproved in 1958.Last previous edition approved in 1999 as D 1612 95(1999).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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.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 tes