ASTM_D_4563_-_02_2015.pdf

Designation:D456302(Reapproved 2015)Standard Test Method forDetermination by Atomic Absorption Spectroscopy ofTitanium Dioxide Content of Pigments Recovered FromWhole Paint1This standard is issued under the fixed designation D4563;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.Scope1.1 This test method covers the atomic absorption(AA)analysis of titanium dioxide content in pigments recoveredfrom whole paint.It is applicable to quality control situationswhere the same type of product is repeatedly analyzed.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 the safetyconcerns,if any,associated with its use.It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.Specific hazard statements are given inSection 7.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1394 Test Methods for Chemical Analysis of White Tita-nium PigmentsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E288 Specification for Laboratory Glass Volumetric Flasks3.Summary of Test Method3.1 The specimen is prepared for analysis by ashing at450C followed by digestion with sulfuric acid and ammoniumsulfate as in Test Methods D1394.The titanium content isdetermined by atomic absorption spectroscopy using a speci-men similar to that previously analyzed by the AluminumReduction Method in Test Methods D1394.3.2 By utilizing the pigment analyzed in Test MethodsD1394 as an atomic absorption standard,several hundred TiO2determinations can be made.The AA technique is much fasterthan the technique in Test Methods D1394 for multipledeterminations and uses only acids.This keeps reagents andtime to a minimum.4.Significance and Use4.1 This test method may be used in quality control labo-ratories when the repeated analysis of titanium dioxide insimilar paints may be required.Reagents and time are kept toa minimum when this test method is used in place of wetchemical analysis such as in Test Methods D1394.However,reproducibility and repeatability are not as good as in TestMethods D1394.5.Apparatus5.1 Atomic Absorption Spectrophotometer,consisting of5.1.1 Atomizer and nitrous oxide burner,5.1.2 Gas-pressure regulator and metering devices for ni-trous oxide and acetylene,5.1.3 Titanium hollow cathode lamp with regulatedconstant-current supply,5.1.4 Monochromator and associated optics,5.1.5 Photosensitive detector connected to an electronicamplifier,5.1.6 Readout device.5.2 Muffle Furnace,capable of maintaining 450 6 25C.5.3 Circulating Oven,maintained at 105 6 2C.5.4 Porcelain Dishes,90-mm diameter.5.5 Plastic Disposable Syringe,10-mL capacity.5.6 Agate Mortar and Pestle,95-mm outside diameter.5.7 Wide-Mouth Erlenmeyer Flask,500-mL capacity.5.8 Hot Plate,with variable surface temperature controlfrom 10C above ambient to 370C accurate to within 65C.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved June 1,2015.Published June 2015.Originallyapproved in 1986.Last previous edition approved in 2008 as D4563 02(2008).DOI:10.1520/D4563-02R15.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.9 Burner.5.10 Volumetric Flask,1000 mL,plastic(see SpecificationE288).5.11 Paint Shaker.5.12 Weighing Bottles,wide-mouth,with an external-fittingcap,and no larger than necessary for required amount ofsample.5.13 Desiccator.6.Reagents6.1 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.4Other grades may beused,provided it is first ascertained that the reagent is ofsufficient high purity to permit its use without reducing theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D