ASTM D3280-1985(2004)e1 Standard Test Methods for Analysis of White Zinc Pigments《锌白颜料的分析方法》.pdf
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1、Designation: D 3280 85 (Reapproved 2004)e1Standard Test Methods forAnalysis of White Zinc Pigments1This standard is issued under the fixed designation D 3280; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.e1NOTEEditorial corrections were made in 3.2.2, 7.1.2, and E
3、q 2 in August 2006.1. Scope1.1 These test methods cover procedures for the analysis ofwhite zinc pigments.1.2 The analytical procedures appear in the following order:SectionPreparation of Sample 6Zinc OxideTotal Zinc, Using Diphenylamine as Internal Indicator 7Total Zinc, Using Uranyl Acetate as Ext
4、ernal Indicator 8Total Impurities 9Total Sulfur 10Moisture and Other Volatile Matter 11Leaded Zinc OxideTotal Lead 12Total Zinc 13Total Sulfur 14Total Impurities 15Moisture and Other Volatile Matter 16Water-Soluble Salts 17Zinc SulfideZinc Oxide 18Zinc Sulfide 19Water-Soluble Salts 20Moisture and Ot
5、her Volatile Matter 21Barium Sulfate 22Titanium Dioxide 231.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is there
6、sponsibility 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:2D 280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Cond
7、itions) in PigmentsD 1193 Specification for Reagent WaterD 1394 Test Methods for Chemical Analysis of WhiteTitanium PigmentsE11 Specification for Wire Cloth and Sieves for TestingPurposes3. Summary of Test Methods3.1 Zinc Oxide:3.1.1 Total ZincDetermined using diphenylamine as aninternal indicator a
8、nd also using uranyl acetate as an externalindicator. Total impurities are calculated.3.1.2 Total SulfurDetermined as BaSO4and calculated tosulfur.3.1.3 Moisture and Volatile MatterDetermined in accor-dance with Method A of Test Methods D 280.3.2 Leaded Zinc Oxide:3.2.1 Total LeadDetermined as PbSO4
9、and calculated topercent PbO.3.2.2 Total ZincDetermined on the filtrate from procedurein 13.2.1 in accordance with methods in Sections 7 or 8.3.2.3 Total SulfurDetermined as BaSO4and calculated topercent SO3.3.2.4 Total ImpuritiesCalculated from compositionaldata.3.2.5 Moisture and Other Volatile Ma
10、tterDetermined inaccordance with Method A of Test Methods D 280.3.2.6 Water Soluble SaltsDetermined gravimetrically.3.3 Zinc Sulfide:3.3.1 Total ZincDetermined using uranyl acetate externalindicator in accordance with Section 9.3.3.2 Zinc SulfideDetermined in accordance with Sec-tions 8 or 9 and cal
11、culating ZnO to ZnS.3.3.3 Water Soluble SaltsDetermined in accordance withSection 18.3.3.4 MoistureDetermined in accordance with Method Aof Test Methods D 280.3.3.5 Barium SulfateThe sample is treated with N2SO4and Na2CO3and the residue of BaCO3is dissolved in NCl and(NH4)2SO4added to precipitate Ba
12、SO4, which is weighed.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.31 on Pigment Specifications.Current edition approved Nov. 1, 2004. Published November 2004. Origi
13、nallyapproved in 1973. Last previous edition approved in 1999 as D 3280 85 (1999).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 pag
14、e onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.3.6 Titanium DioxideDetermined in accordance withTest Methods D 1394.4. Significance and Use4.1 White zinc pigments find considerable use in whitepaints, and as s
15、uch it is useful to formulators and users to beable to monitor the amounts of these pigments in whole paints.It is also of interest to raw material suppliers and paintproducers to check the specifications of each pigment.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all te
16、sts. 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.3Other grades may beused, provided it is first ascertained that the reagent is ofsuff
17、iciently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II reagent gradewater conforming to Specification D 1193.5.3 Concentration of Reagents:5.3.1 Concentrated Acids
18、 and Ammonium HydroxideWhen acids and ammonium hydroxide are specified by nameor chemical formula only it should be understood that concen-trated reagents of the following specific gravities or concen-trations are intended:Acetic acid, HC2H3O299.5 %Hydrochloric acid, HCl sp gr 1.19Hydrofluoric acid,
19、 HF 48 %Nitric acid, HNO3sp gr 1.42Sulfuric acid, H2SO4sp gr 1.84Ammonium hydroxide, NH4OH sp gr 0.90The desired specific gravities or concentrations of all otherconcentrated acids are stated whenever they are specified.5.3.2 Diluted Acids and Ammonium HydroxideConcentrations of diluted acids and am
20、monium hydroxide,except when standardized, are specified as a ratio stating thenumber of volumes of the concentrated reagents to be dilutedwith a given number of volumes of water, as in the followingexample: HCl (1+99) means 1 volume of concentrated HCl (spgr 1.19) diluted with 99 volumes of water.6
21、. Preparation of Sample6.1 Grind dry pigments, if lumpy or not finely ground, to afine powder for analysis. Large samples may be thoroughlymixed and a representative portion taken and powdered iflumpy or not finely ground. Mix the sample in all casesthoroughly before taking specimens for analysis.6.
22、2 Separate pigments from paints or pastes, grind to a finepowder, pass through a 180-m (No. 80) sieve (Note 1)toremove any skins, thoroughly mix, and oven dry at 105C.Moisten such pigments after weighing with a little alcoholbefore adding reagents for analysis.NOTE 1Detailed requirements for this si
23、eve are given in SpecificationE11.6.3 Preserve all samples in stoppered bottles or containers.ZINC OXIDE7. Total Zinc, Using Diphenylamine as Internal Indicator7.1 Reagents:7.1.1 Diphenylamine Indicator Solution (10 g/L)Dissolve1 g of diphenylamine in 100 mL of H2SO4.7.1.2 Potassium Ferrocyanide (1
24、mL = 0.008 g Zn)Dissolve 35 g of K4Fe(CN)63H2O in water and dilute to 1 Land add 0.3 g of potassium ferricyanide (K3Fe(CN)6). Stan-dardize the solution by titrating against zinc (320 to 340 mg),following the procedure described in 7.2. Calculate the gramsof zinc equivalent to 1.00 mL of the solution
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