ASTM_D_2192_-_06_2012.pdf

Designation:D219206(Reapproved 2012)Standard Test Method forPurity of Aldehydes and Ketones1This standard is issued under the fixed designation D2192;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 the purityof certain commercially available aldehydes and ketones.1.2 In addition to all aldehydes and ketones,all compoundssuch as vinyl alkyl ethers,acetals,and ketals,that hydrolyzeunder the conditions of the reaction to form free carbonylgroups,react with the reagent and consequently interfere.Water,alcohols,saturated esters,and hydrocarbons do not reactwith the reagent,but large amounts of inert organic solvents areundesirable because of the effect on the indicator.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 E29.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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 7.1.6 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:2D268 Guide for Sampling and Testing Volatile Solvents andChemical Intermediates for Use in Paint and RelatedCoatings and MaterialD1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE200 Practice for Preparation,Standardization,and Storageof Standard and Reagent Solutions for Chemical AnalysisE222 Test Methods for Hydroxyl Groups Using AceticAnhydride Acetylation3.Summary of Test Method3.1 Hydroxylamine hydrochloride is converted in part tofree hydroxylamine by reaction with a known amount ofaqueous triethanolamine.NH2OHHCl1HOCH2CH2!3N(1)NH2OH1HOCH2CH2!3NHClThe free hydroxylamine reacts with the aldehyde or ketoneto form the corresponding oxime.RR1C 5 01NH2OHRR1C 5 H 5 NOH1H2O,(2)where:R=alkyl group andR1=alkyl group or hydrogen.The amount of hydroxylamine consumed,which is deter-mined by titration of the excess base with standard sulfuricacid,is a measure of the aldehyde or ketone originally present.3.2 Since the determination is based on an acidimetrictitration,a suitable correction must be applied if the sample isnot neutral to bromophenol blue indicator.4.Significance and Use4.1 This test method provides a measurement of purity(assay)of aldehydes and ketones.The results of these mea-surements can be used for specification acceptance.4.2 The precision of this test method is applicable only tomaterial having a purity of 98 to 100%.5.Apparatus5.1 Pressure Bottle,200 to 350-mL capacity,with lever typeclosure and made of heat-resistant glass.5.2 Container for Pressure BottleA suitable safety deviceto contain the pressure bottle.A metal container with a hinged1This 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 1,2012.Published July 2012.Originally approvedin 1963.Last previous edition approved in 2006 as D2192 06.DOI:10.1520/D2192-06R12.2For 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.*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 top and perforated bottom,a strong synthetic fabric or canvasbag,or a safety shield may be used.5.3 Ampoule,1 or 2-mL capacity.5.4 Weighing Pipet,Lunge or similar type.5.5 Burets,50-mL capacity.5.6 Transfer Pipet,50-mL capacity.5.7 Glass Rod,8-mm,several pieces approximately 1 in.long.5.8 Boiling Water Bath.6.Reagents and Materials6.1 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 t