ASTM_D_686_-_93_2002.pdf

Designation:D 686 93(Reapproved 2002)An American National StandardStandard Test Methods ofQualitative Examination of Mineral Filler and MineralCoating of Paper1This standard is issued under the fixed designation D 686;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 These test methods cover two procedures for the quali-tative determination and identification of the mineral constitu-ents of filled and coated papers.1.2 Due to the similarity in chemical composition andphysical size and shape of some of the various possibleconstituents contained in a given paper specimen,more pre-cise,quantitative methods may at times be required for positiveidentification.1.3 It is recommended that one become thoroughly familiarwith these test methods by analyzing paper samples of knownmineral component content.1.4 The test methods appear as follows:SectionsMethod AChemical Analysis4 to 11Method BMicroscopical Identification2 to 191.5 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.NOTE1These test methods are technically equivalent to TAPPI T421 83.2.Referenced Documents2.1 ASTM Standards:D 585 Practice for Sampling and Accepting a Single Lot ofPaper,Paperboard,Fiberboard,and Related Products2D 586 Test Method for Ash in Pulp,Paper,and PaperProducts2D 921 Test Method for Titanium Dioxide in Paper3D 1030Test Method for Fiber Analysis of Paper andPaperboard22.2TAPPI Standards:T 401Fiber analysis of paper and paperboard4T 438Zinc and cadmium in paper and pigments4Test Method AQualitative Chemical Analysis3.Significance and Use3.1 Qualitative chemical analyses of the mineral componentof a paper specimen,Test Method A,serve to identify the ionsof any such minerals.The results may then be interpreted interms of the minerals themselves.Direct identification of someof these minerals or their ions is frequently possible usingoptical microscopical examination,Test Method B.For addi-tional information,see the annex.3.2 The analysis can be considerably simplified if it isdesired only to establish the presence or absence of a particularfiller.3.3 A microscopical examination of the ash usually provesto be a useful adjunct to chemical analysis,and if possibleshould be attempted(see Sections 12 to 18).4.Apparatus4.1 Crucible,platinum,with lid,for use in 9.7.1 and inashing the sample that is being examined.Porcelain or silicacrucibles may be used if their weight does not change under theignition conditions.4.2 Muffle Furnace,electric,controlled to maintain a tem-perature of 525 6 25C.4.3 Laboratory Oven,electric,controlled to maintain atemperature of 150 6 3C.4.4 Blowpipe.4.5 Wire Loop,platinum.4.6 Spot Plate,black,glazed.1These test methods are under the jurisdiction of ASTM Committee D06 onPaper and Paper Products and are the direct responsibility of Subcommittee D06.92on Test Methods.Current edition approved Sept.15,1993.Published November 1993.Originallypublished as D 686 42T.Last previous edition D 686 88.2Annual Book of ASTM Standards,Vol 15.09.3Discontinued,see 1981 Annual Book of ASTM Standards,Part 20.4Available from the Technical Association of the Pulp and Paper Industry,Technology Park/Atlanta,P.O.Box 105113,Atlanta,GA 30348.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.4.7 Other ApparatusBeakers,250-mL;watch glass;volu-metric flasks,100-mL;filter funnels and fairly rapid,low-ashfilter paper,5and Bunsen burner.5.Reagents5.1 Acetic Acid,(Glacial,99.7%CH3-COOH,sp gr 1.05),approximately 1 N solution.Add approximately 11.5 mLglacial acetic acid to 50 mL water in a volumetric flask anddilute to 100-mL mark.5.2 Ammonium Chloride Solution(NH4OH,10%).5.3 Ammonium Hydroxide(sp gr 0.90)Concentrated am-monium hydroxide(NH4OH).5.4 Ammonium Oxalate Solution(NH4)2-C2O4H2O,3.5%).5.5 Ammonium Sulfate,(NH4)2SO4.5.6 Barium Chloride Solution(BaCl2,10%).5.7 Charcoal Black.5.8 Cobalt Nitrate SolutionDissolve 8 g of cobalt nitrate(Co(NO3)26H2O)in 100 mL of water.5.9 Diphenylthiocarbazone(Dithizone)SolutionDissolve10 mg dithizone in 100 mL carbon tetrachloride,(CCl4).5.10 Hydrochloric Acid(2 N,sp gr 1.19)Concentratedhydrochloric acid(HCl).Add 15 mL of concentrated HCl toapproximately 75 mLwater in a 100-mLvolumetric flask,cool,and dilute to 100-mL mark.5.11 Hydrogen Peroxide(30%H2O2),or a solution of 3%H2O2used in proportionately greater quantities.Extremecaution should be used when handling 30%H2O2solution asit is very active when in contact with skin.Eye protectionshould be worn.5.12 Iodine Solution(0.1 N).5.13