ASTM_D_686_-_93_2007.pdf

Designation:D686 93(Reapproved 2007)An American National StandardStandard Test Methods ofQualitative Examination of Mineral Filler and MineralCoating of Paper1This standard is issued under the fixed designation D686;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 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 AQualitative Chemical Analysis4 to 11Method BMicroscopical Identification12 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 TAPPIT 421.2.Referenced Documents2.1 ASTM Standards:2D585 Practice for Sampling and Accepting a Single Lot ofPaper,Paperboard,Fiberboard,and Related ProductD586 Test Method for Ash in Pulp,Paper,and PaperProducts3 3D921Discontinued 1980;Method of Test for TitaniumDioxide in Paper3D1030 Test Method for Fiber Analysis of Paper and Paper-board2.2TAPPI Standards:4T 401Fiber analysis of paper and paperboardT 438Zinc and cadmium in paper and pigmentsT 421Qualitative(Including Optical Microscopic)Analy-sis of Mineral Filler and Mineral Coating of Paper3.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 Annex A1.3.2 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 12-18).Test Method AQualitative Chemical Analysis4.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.1These test methods are under the jurisdiction of ASTM Committee D06 onPaper and Paper Products and are the direct responsibility of Subcommittee D06.92on Standard Documents Relating to Paper and Paper Products.Current edition approved Dec.1,2007.Published December 2007.Originallyapproved in 1942.Last previous edition approved in 2002 as D 686 93(2002).DOI:10.1520/D0686-93R07.2For 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.3Withdrawn.4Available from Technical Association of the Pulp and Paper Industry(TAPPI),15 Technology Parkway South,Norcross,GA 30092,http:/www.tappi.org.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.NOTICE:This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International(www.astm.org)for the latest information4.6 Spot Plate,black,glazed.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)Solu