ASTM D718-1986(2014) Standard Test Methods for Analysis of Aluminum Silicate Pigment《分析硅酸铝颜料的标准试验方法》.pdf

1、Designation: D718 86 (Reapproved 2014)Standard Test Methods forAnalysis of Aluminum Silicate Pigment1This standard is issued under the fixed designation D718; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the analysis of aluminumsilicate pigment.1.2 The values stated in SI units are to be regarded as thestand

3、ard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address the safetyconcerns associated with its use. It is the responsibility of theuser of this standard to establish appropriate safety and healthpractices and determine the applicability of regulator

4、y limita-tions prior to use.2. Referenced Documents2.1 ASTM Standards:2D234 Specification for Raw Linseed Oil (Withdrawn 2007)3D280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Conditions) in PigmentsD717 Test Methods for Analysis of Magnesium SilicatePigmentD1193 S

5、pecification for Reagent WaterD1208 Test Methods for Common Properties of CertainPigmentsD2448 Test Method for Water-Soluble Salts in Pigments byMeasuring the Specific Resistance of the Leachate of thePigmentE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3. Significance and Use3.1 T

6、hese test methods may be used to confirm the statedaluminum oxide and SiO2content of aluminum silicate forquality control.4. Apparatus4.1 Platinum Crucible.4.2 Electric furnace (or gas burner), capable of 1050 to1100C.4.3 Volumetric flask, 100 and 250 mL.4.4 Colorimeter, with transmission range from

7、 400 to 550nm.4.5 High Silica Crucible.5. Purity of Reagents5.1 Reagent grade chemicals 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,4where suchspecif

8、ications are available. Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Unless otherwise indicated, references to water shall beunderstood to mean Type II of Specificat

9、ion D1193.SILICON DIOXIDE6. Procedure6.1 Determine the silicon dioxide content in accordancewith Test Methods D717.ALUMINUM OXIDE7. Reagents7.1 Ammonium Acetate (20 %)Dissolve 200 g of ammo-nium acetate (NH4C2H3O2) in 1 L of distilled water.7.2 Ammonium Chloride Solution (20 g/L)Dissolve 20 gof ammo

10、nium chloride (NH4Cl) in water and dilute to 1 L.7.3 Ammonium Hydroxide (sp gr 0.90Concentrated am-monium hydroxide (NH4OH).1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee

11、D01.31 on Pigment Specifications.Current edition approved Dec. 1, 2014. Published December 2014. Originallyapproved in 1943. Last previous edition approved in 2008 as D718 86 (2008).DOI: 10.1520/D0718-86R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer

12、 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, American

13、Chemical 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),

14、Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17.4 Diphenylamine Indicator Solution (1 g/100 mL)Dissolve1gofdiphenylamine in 100 mL of concentratedsulfuric acid (H2SO4, sp gr 1.84).7.5 Hydrochloric Acid (sp gr 1.19)Conce

15、ntrated hydro-chloric acid (HCl).7.6 Hydrochloric Acid (1+3)Mix 1 volume of concen-trated HCl (sp gr 1.19) with 3 volumes of water.7.7 Hydrofluoric Acid (48 %)Concentrated hydrofluoricacid (HF).7.8 Hydrogen Peroxide (H2O2, 3 %, freshly prepared)Mix 1 volume of H2O2(30 %) with 9 volumes of distilledw

16、ater.7.9 Hydroxylamine Hydrochloride (10 %)Dissolve 10 gof NH2OH HCl in 100 mL of distilled water. Prepare freshweekly.7.10 Iron StandardDissolve 0.1 g of analytical grade ironwire in 10 mL of HCl (1+1) and dilute to 1 L. Each millilitrecontains 0.1 mg of Fe.7.11 Mercuric Chloride Solution (HgCl2),

17、saturated.7.12 Methyl Red Indicator SolutionDissolve 0.2 g ofmethyl red in 100 mL of methanol, ethanol, or isopropanol.7.13 Potassium Dichromate, Standard Solution (0.05 N)Dissolve 2.457 g of potassium dichromate (K2Cr2O7)inwater and dilute to 1 L. Standardize against National Bureau ofStandards sta

18、ndard sample No. 27b of Sibley iron ore, usingsuch an amount as to give approximately the same titration asthe sample to be analyzed.7.14 Phosphoric Acid (H3PO4, 85 %)Concentrated phos-phoric acid.7.15 Potassium Pyrosulfate (K2S2O7).7.16 o-Phenanthroline (0.1 %)Dissolve 1.0 g ofo-phenanthroline in 1

19、 L of hot distilled water.7.17 Stannous Chloride Solution (5 g/100 mL)Dissolve 5g of stannous chloride (SnCl3,2H2O) in 10 mL of concentratedHCl (sp gr 1.19) and dilute to 100 mL with water. Add scrapsof iron-free granulated tin, and boil until the solution is clear.Keep the solution in a closed drop

20、ping bottle containingmetallic tin.7.18 Sulfuric Acid (1+1)Add carefully 1 volume of con-centrated sulfuric acid (H2SO4, sp gr 1.84) to 1 volume ofdistilled water.7.19 Sulfuric Acid (1+9)Add carefully 1 volume of con-centrated H2SO4(sp gr 1.84) to 9 volumes of distilled water.8. Procedure8.1 If an a

21、ppreciable residue remains after the treatmentwith HF in accordance with 7.4 of Test Methods D717, fuse theresidue with a small amount of K2S2O7until it is dissolved.Leach the pyrosulfate melt out of the crucible with water andcombine the solution with the filtrate reserved in accordancewith 7.3 or

22、Test Methods D717.8.2 Bring the volume of the combined solution to 250 mL,and, if necessary, add HCl in order to ensure a total of 10 to 15mL of HCl, add a few drops of methyl red indicator solution,and heat to boiling. Add concentrated NH4OH (sp gr 0.90)dropwise until 1 drop changes the color of th

23、e solution to adistinct yellow. Reheat the solution containing the precipitatedhydroxides to boiling, boil for 1 or 2 min, and filter. Wash theprecipitate once by decantation and then slightly on the filterwith hot NH4Cl.8.3 Transfer the precipitate and paper to the original beakerin which the preci

24、pitation was made. Dissolve the precipitate inhot HCl (1+3), dilute to 100 mL, and precipitate again asdescribed in 8.2. After filtering, wash the precipitate ten timeswith small portions of hot NH4Cl solution. Transfer theprecipitate to a weighed platinum crucible, heat slowly untilthe paper is cha

25、rred, and finally ignite to constant weight at1050 to 1100C in an electric furnace or over a burner, takingcare to avoid reduction. Weigh the precipitate asAl2O3+TiO2+Fe2O3.8.4 Fuse the combined oxides from 8.3 with9to10gofK2S2O7in a platinum crucible, starting at low temperature andincreasing the h

26、eat gradually until the oxides have all dis-solved. Take up the melt with 5 mL of H2SO4(1+1) in 150 mLof water and warm to effect solution. Transfer the solution to a250-mL volumetric flask, dilute to volume, and mix well.Reserve for TiO2and Fe2O3determinations.8.5 Determine the percent of TiO2as fo

27、llows: Pipet analiquot containing 0.2 to 3.0 mg of TiO2into a 100-mLvolumetric flask. For samples containing 0.5 to 3 % TiO2,a20-mL aliquot is suitable. Add 5 mL of H2O2(3 %), dilute tovolume with H2SO4(1+9) and mix well. Obtain the colorimet-ric reading in a suitable colorimeter using a filter with

28、transmission limits of 400 to 450 nm or at 410 nm with a prismor grating spectrometer. Compare the readings to a curveplotted from a set of TiO2standards similarly treated and readon the same instrument.8.6 Determine the percent of Fe2O3as follows: Pipet a25-mL aliquot into a 100-mL volumetric flask

29、. Add thefollowing in the order given, mixing well after each addition:2mLofNH2OH HCl (10 %), 10 mL of NH4C2H3O2(20 %),and 10 mL of o-phenanthroline (0.1 %). Roll a small piece ofcongo red paper into a ball and introduce into the flask. Addconcentrated NH4OH dropwise until indicator turns red and 1d

30、rop in excess. Dilute to volume and let stand for 10 to 20 min.Obtain the colorimetric reading in a suitable colorimeter usinga filter with transmission limits 485 to 550 nm, or at 510 nmwith a prism or grating spectrometer. Compare the readings toa curve plotted from a set of Fe2O3standards similar

31、ly treatedand read on the same instrument.8.7 Alternatively the Fe2O3may be determined by titrationas follows: Fuse1gofsample with 10 g of K2S2O7in ahigh-silica crucible starting at low temperature and increasingthe heat gradually until the crucible glows with a dull red colorand decomposition is ju

32、dged to be complete. Leach the meltwith 10 mL of concentrated HCl in 100 mL of water and digestat low heat to disintegrate the cake. Filter and wash free ofchlorides with hot water. Save filtrate. Ignite the insolubleresidue in a platinum crucible. Treat with 5 mL of H2SO4(1+1)and 15 mL of HF (48 %)

33、, and heat until fumes of H2SO4D718 86 (2014)2appear. Bring the residue into solution with the addition of afew drops more of H2SO4(1+1) and combine the solution withthe bulk of the iron. Add 5 mL of HCl to the combinedsolutions and evaporate to 50-mL volume.8.8 To the hot solution add SnCl2solution

34、, dropwise, whilestirring, until the solution is decolorized, and then add 2 to 3drops more. Cool the solution to room temperature, wash downthe inside of the beaker with water, and add at one stroke 10mL of cool HgCl2solution (saturated). Stir the solutionvigorously for 1 min, add 5 mL of phosphori

35、c acid (85 %) and3 drops of diphenylamine indicator solution. Titrate with 0.05N K2Cr2O7solution to an intense deep-blue end point thatremains unchanged on further addition of K2Cr2O7solution.8.9 Calculate the percent of Fe2O3as follows:Fe2O3% 5 N 3V 30.0798!/S# 3100 (1)where:S = sample used, g,V =K

36、2Cr2O7, mL, andN = normality of the K2Cr2O7.8.10 Calculate the percent of Al2O3as follows:Al2O3,%5 100P/S! 2 C (2)where:P = weight of combined oxides Al2O3+TiO2+Fe2O3,S = specimen weight, g, andC =Fe2O3+TiO2,%.LOSS ON IGNITION9. Procedure9.1 Determine loss on ignition in accordance with TestMethods

37、D1208.MOISTURE AND OTHER VOLATILE MATTER10. Procedure10.1 Determine moisture and other volatile matter in accor-dance with Test Methods D280.COARSE PARTICLES(Total Residue Retained on a No. 325 (45-m) Sieve)11. Apparatus11.1 SieveANo. 325 (45-m) 76 mm (3-in.) diameter highform sieve conforming to Sp

38、ecification E11, shall be used.11.2 Stirring Apparatus, consisting of:11.2.1 Mixing CupA stainless steel cup, about 178 mm (7in.) deep, and slightly tapered from an outside diameter at thetop of about 102 mm (4 in.) to about 70 mm (234 in.) at thebottom, such as is characteristic of a usual malted-m

39、ilk typemixing cup.11.2.2 Mechanically Operated Stirring Device, in which asuitably mounted electric motor turns a vertical shaft at a speedof not less than 10 000 r/min without load. The shaft shall beequipped with a replaceable stirring button not more than 25mm (1 in.) in diameter, and of such le

40、ngth that the stirringbutton shall operate not less than 19.0 mm (34 in.) nor morethan 38 mm (112 in.) above the bottom of the dispersion cup.A common malted milk-type mixer of high quality meets thisspecification.12. Procedure12.1 Dry a No. 325 (45-m) sieve in an oven at 105 6 2C,cool, and weigh ac

41、curately. Transfer 100 6 0.5 g of thespecimen to the mixing cup containing approximately 250 mLof water to which has been added about 2 drops of 0.5 %solution sodium silicate, and stir for about 10 min at highspeed. Pour the resulting slurry slowly through the sieve andwash out the mixing cup carefu

42、lly (a polyethylene squeeze-type wash bottle is very convenient) to ensure completetransfer of the specimen to the sieve. Spray the sieve surfacegently with a low pressure fan-shaped spray (tap water at about5 psig (30 kPa) back pressure) and continue washing until allthe pigment has been washed thr

43、ough and the water passing thesieve is clear. Dry the sieve for1hat105to110C, cool andweigh.12.2 Calculation:Percent of coarse particles (3)5increase in weight of sieve/specimen weight! 3100MATTER SOLUBLE IN WATER13. Procedure13.1 Determine the matter soluble in water by Test MethodD2448.COLOR14. St

44、andard Pigment14.1 Standard Extender Pigment.14.2 Standard Zinc Oxide.15. Procedure15.1 Carefully weigh out the proportion of the standardextender pigment and standard zinc oxide mutually agreedupon, and rub up to a fairly stiff paste with a glass muller on aglass plate or stone slab with raw linsee

45、d oil conforming toSpecification D234. Note the volume of the oil required.Prepare a similar paste with the sample using the same weightof pigment, volume of oil, and number of strokes of the glassmuller as used in the preparation of the paste of the standardpigments. Spread the pastes adjacently on

46、 a microscope slide,draw a scraper lightly across them to present them on an evenplane, and judge the color immediately.PRECISION AND BIAS16. Precision and Bias16.1 Data are not available to determine the precision andbias of these methods. There are no plans at present to obtainsuch information. Th

47、e methods have been in use for severalyears and are considered acceptable.D718 86 (2014)317. Keywords17.1 aluminum oxide in aluminum silicate pigment; alumi-num silicate pigment, analysis of; pigment, aluminum silicateASTM International takes no position respecting the validity of any patent rights

48、asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any tim

49、e by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address