ASTM D686-1993(2002) Standard Test Methods of Qualitative Examination of Mineral Filler and Mineral Coating of Paper《纸中矿物填料和矿物涂料的定性标准试验方法》.pdf
《ASTM D686-1993(2002) Standard Test Methods of Qualitative Examination of Mineral Filler and Mineral Coating of Paper《纸中矿物填料和矿物涂料的定性标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D686-1993(2002) Standard Test Methods of Qualitative Examination of Mineral Filler and Mineral Coating of Paper《纸中矿物填料和矿物涂料的定性标准试验方法》.pdf(12页珍藏版)》请在麦多课文档分享上搜索。
1、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
2、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 determ
3、ination 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 requir
4、ed 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 Analysis 4 to 11Method BMicroscopical Identification 2 to 191.5
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.NOTE 1These test me
6、thods 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
7、in Paper3D 1030 Test Method for Fiber Analysis of Paper andPaperboard22.2 TAPPI Standards:T 401 Fiber analysis of paper and paperboard4T 438 Zinc and cadmium in paper and pigments4Test Method AQualitative Chemical Analysis3. Significance and Use3.1 Qualitative chemical analyses of the mineral compon
8、entof 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. Fo
9、r 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 atte
10、mpted (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 te
11、m-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
12、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 Techni
13、cal 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; f
14、ilter 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 Solut
15、ion (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 SolutionDissolve8gofcobalt nitrate(Co(NO3)2
16、6H2O) 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 mL water in a 100-mL volumetric flask, c
17、ool,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)
18、.5.13 Lead Acetate PaperImmerse strips of filter paper ina saturated solution of lead acetate (Pb(C2H3O2)23H2O);withdraw from solution and allow to air dry.5.14 Lime Water, saturated solution. Dissolve about 0.2 g ofcalcium hydroxide (Ca(OH)2) in 100 mL of water and filter.5.15 Magnesium ReagentDiss
19、olve 0.5 g of para-nitrobenzeneazoresorcinol in 100 mL of sodium hydroxide(NaOH) solution (1 %).5.16 Microcosmic Salt SolutionDissolve5gofsodiumammonium phosphate (NaNH4HPO44H2O) in water anddilute to 100 mL.5.17 Morin (3,5,7,28,48-pentahydroxyflavanone)Saturated solution of morin in methyl alcohol.
20、5.18 Potassium Dichromate Solution (K2Cr2O7, 4%).5.19 Potassium Ferrocyanide SolutionDissolve 15 g of(K4Fe(CN)63H2O) in 1000 mL of water.5.20 Potassium Hydroxide Solution (2N)Dissolve 11.2 gof potassium hydroxide (KOH) in 75 mL water; cool and diluteto 100 mL.5.21 Sodium CarbonatePowdered sodium car
21、bonate(Na2CO3).5.22 Sodium Hydroxide Solution (2N). Dissolve 8 g(NaOH) in 75 mL water; cool and dilute to 100 mL.5.23 Sulfuric Acid (5 %, sp gr 1.84)Concentrated sulfuricacid (H2SO4). Add 3 mL of concentrated H2SO4to 75 mL ofwater, cool, dilute to 100 mL.6. Purity of Reagents6.1 Reagent grade chemic
22、als shall be used in all tests.Unless otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.6Other grades may be used, pro-vided it is first ascertained
23、that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.Test Method AQualitative Chemical Analysis7. Sampling7.1 Obtain a sample of the paper to be tested in accordancewith Methods D 585.8. Test Specimens8.1 From each test unit, for each co
24、mplete determination,cut test specimens of sufficient size to yield at least 0.15 g ofash.8.2 An additional specimen of each test unit should beavailable for testing without previous ashing.9. Procedure9.1 An outline scheme of the qualitative procedure is givenin Fig. 1.9.2 Sulfite, Sulfide, and Car
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