ASTM_D_3969_-_01_2012.pdf

Designation:D396901(Reapproved 2012)Standard Test Method forZirconium in Paint Driers by EDTA Method1This standard is issued under the fixed designation D3969;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 titrimetric determination ofzirconium in zirconium driers used in the coatings industry andutilizes the disodium salt of ethylenediaminetetraacetic aciddihydrate(EDTA).1.2 This test method is limited to the determination of thezirconium content of a liquid zirconium drier that does notcontain other drier elements.The test method is not applicableto drier blends and does not differentiate hafnium fromzirconium.1.3 All cations that can be titrated with EDTAin acid mediainterfere and must not be present in the sample.1.4 This test method has been tested for concentrations of 6and 12%zirconium,but there is no reason to believe that it isnot suitable for higher or lower zirconium concentrations,provided specimen size is adjusted proportionately.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 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.2.Referenced Documents2.1 ASTM Standards:2D600 Specification for Liquid Paint DriersD1193 Specification for Reagent WaterE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E300 Practice for Sampling Industrial Chemicals3.Summary of Test Method3.1 The zirconium drier is digested with concentrated sul-furic acid and 30%hydrogen peroxide to destroy all organicmatter.The diluted solution is boiled with an excess of EDTA,the pH adjusted,and the excess titrated with bismuth nitrateusing xylenol orange as the indicator.4.Significance and Use4.1 The amount of zirconium drier used in oxidizing-typecoatings significantly affects their drying properties.This testmethod may be used to confirm the stated content of a pureliquid zirconium drier manufactured for use by the coatingsindustry.5.Apparatus5.1 Centrifuge,capable of developing 1000 to 2000 g.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 ofsufficiently high purity to permit its use without lessening 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 D1193.6.3 Ammonium Hydroxide(sp gr 0.90)Concentrated,am-monium hydroxide(NH4OH).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 1,2012.Published July 2012.Originally approvedin 1980.Last previous edition approved in 2006 as D3969 01(2006).DOI:10.1520/D3969-01R12.2For 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.4Reagent 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.4 Bismuth Nitrate,Standard Solution(0.05 M)Dissolve24.25 g of bismuth nitrate(Bi(NO3)5H2O)in 20 to 30 mL ofconcentrated nitric acid(use a magnetic stirrer if possible).After solution is complete,dilute to 1 L with water.NOTE1Add the water very slowly to the acid solution,while coolingthe flask in an ice bath to prevent splattering.6.5 EDTA,Standard Solution(0.05 M)Dissolve 18.61 g ofEDTA in 300 to 500 mL of water and dilute to 1 L.Store in apolyethylene or borosilicate glass bottle.6.6 Eriochrome Black-T IndicatorTriturate 0.100 g