1、Designation: D1301 91 (Reapproved 2014)Standard Test Methods forChemical Analysis of White Lead Pigments1This standard is issued under the fixed designation D1301; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 These test methods cover procedures for
3、 the chemicalanalysis of basic carbonate white lead and basic sulfate whitelead.NOTE 1If it is necessary to separate these pigments from others, referto Practice D215.1.2 The analytical procedures appear in the following order:SectionPreparation of Sample 6Basic Carbonate White Lead:Small Amounts of
4、 Iron 7Total Lead 8Moisture and Other Volatile Matter 9Carbon Dioxide (Evolution Method) 10Carbon Dioxide and Combined Water (Combustion Method) 11Lead Carbonate 12Total Matter Insoluble in Acetic Acid 13Total Matter Insoluble in Acid Ammonium Acetate 14Total Impurities Other Than Moisture 15Coarse
5、Particles 16Basic Sulfate White Lead:Small Amounts of Iron 17Total LeadMoisture and Other Volatile Matter 19Total Sulfate 20Zinc Oxide 21Basic Lead Oxide 22Total Impurities 23Coarse Particles 241.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are f
6、or informationonly.1.4 This standard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Refe
7、renced Documents2.1 ASTM Standards:2C25 Test Methods for Chemical Analysis of Limestone,Quicklime, and Hydrated LimeD185 Test Methods for Coarse Particles in PigmentsD215 Practice for the Chemical Analysis of White LinseedOil Paints (Withdrawn 2005)3D280 Test Methods for Hygroscopic Moisture (and Ot
8、herMatter Volatile Under the Test Conditions) in PigmentsD1193 Specification for Reagent WaterD2371 Test Method for Pigment Content of Solvent-Reducible PaintsD2372 Practice for Separation of Vehicle From Solvent-Reducible PaintsD3280 Test Methods for Analysis of White Zinc PigmentsE11 Specification
9、 for Woven Wire Test Sieve Cloth and TestSieves3. Significance and Use3.1 These test methods are suitable for determining the levelof purity and for determining the levels of various impurities.They may be used to establish compliance with specificationrequirements.4. Reagents4.1 Purity of ReagentsR
10、eagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to specifications of the Committeeon Analytical Reagents of the American Chemical Society,1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Relat
11、ed Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.31 on Pigment Specifications.Current edition approved Dec. 1, 2014. Published December 2014. Originallyapproved in 1953. Last previous edition approved in 2008 as D1301 91 (2008).DOI: 10.1520/D1301-91R14.2F
12、or 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.3The last approved version of this historical standard is refer
13、enced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use w
14、ithout lessening theaccuracy of the determination.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Type II of Specification D1193.4.3 Concentration of Reagents:4.3.1 Concentrated Acids and Ammonium HydroxideWhen acids and ammoni
15、um hydroxide are specified by nameor chemical formula only, it shall be understood that concen-trated reagents of the following specific gravities or concen-trations are intended:Acetic acid, CH3COOH 99.5 %Hydrochloric acid, HCl sp gr 1.19Hydrofluoric acid, HF 48 %Nitric acid, HNO3sp gr 1.42Sulfuric
16、 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.WarningSee Section 5.4.3.2 Diluted Acids and Ammonium HydroxideConcentrations of diluted acids and ammonium hydroxide,excep
17、t when standardized, are specified as a ratio stating thenumber of volumes of concentrated reagent to be diluted witha given number of volumes of water, as in the followingexample: HCl (1 + 99) means 1 volume of concentrated HCl(sp gr 1.19) diluted with 99 volumes of water.5. Hazards5.1 The concentr
18、ated acids bases and other reagents used inthese test methods can be dangerous. Check their MaterialSafety Data Sheets, (MSDS) before use.6. 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 representa
19、tive portion taken and powdered iflumpy or not finely ground. Mix the sample in all casesthoroughly and comminute before taking specimens for analy-sis.6.2 In cases of pastes in oil, extract the oil from the pigmentas described in Test Method D2371 or Practice D2372, butwithout straining.6.3 Dry pig
20、ments separated from paints or pastes in oil in anoven at 95 to 98C (203 to 210F) for 2 h, grind to a finepowder, pass through a No. 80 (180-m) sieve (Note 2)toremove skins, and mix thoroughly. Such pigments, afterweighing, should be moistened with a little ethyl alcohol(95 %) before adding reagents
21、 for analysis.NOTE 2Detailed requirements for this sieve are given in SpecificationE11.6.4 Preserve all samples in stoppered bottles or containers.BASIC CARBONATE WHITE LEAD7. Small Amounts of Iron7.1 Reagents:7.1.1 Ammonium Hydroxide (sp gr 0.90). WarningSee5.1.7.1.2 Hydrofluoric Acid (48 %). Warni
22、ngSee 5.1.7.1.3 Nitric Acid (sp gr 1.42). WarningSee 5.1.7.1.4 Sulfuric Acid (sp gr 1.84). WarningSee 5.1.7.2 Procedure:7.2.1 Weigh to 10 mg about1gofspecimen into a 400-mLbeaker.Treat the sample with 10 mLof HNO3(1 + 1) and diluteto about 200 mL with water. If insoluble matter remainsfollowing trea
23、tment with HNO3and dilution, filter and washthe residue with hot water until lead free. Evaporate the filtrateand washings to about 200 mL. Add 20 mL of H2SO4(1+1)to precipitate the bulk of the lead (it is unnecessary toevaporate down). Cool, filter, and wash with diluted H2SO4(1 + 99). Save the pre
24、cipitate for determination of total lead(Section 8).7.2.2 Ignite the HNO3-insoluble matter and treat with HFand H2SO4. Bring into solution, filter (any precipitate isprobably BaSO4), and add to the PbSO4filtrate.7.2.3 Colorimetrically determine iron in the combined fil-trates by the thiocyanate meth
25、od,5using the same amounts ofreagents in preparing the reference standards. If copper ispresent in the filtrate, as shown by the characteristic blue-greenor yellow color, remove it by precipitating the iron withNH4OH, filtering, washing, redissolving the Fe(OH)3in 10 mLof HNO3(1 + 1), and diluting t
26、o about 200 mL beforeproceeding with the thiocyanate method.8. Total Lead8.1 Apparatus:8.1.1 Gooch Crucible, prepared prior to use.8.2 Reagents:8.2.1 Acetic Acid (glacial)WarningSee 5.1.8.2.2 Ammonium Hydroxide (sp gr 0.90)WarningSee5.1.8.2.3 Ethyl Alcohol (95 volume %)WarningSee 5.1.8.2.4 Potassium
27、 Dichromate Solution (100 g K2Cr2O7/L)WarningSee 5.1.8.3 Procedure:8.3.1 Ignite the PbSO4precipitate and filter paper from 7.2.1at or below 550C (1020F), and transfer the residue to a400-mL beaker. (If preferred, a new 1-g specimen of pigmentmay be weighed to 10 mg into a 400-mL beaker. Proceed to8.
28、3.2.)8.3.2 Moisten with water and add 5 mL of glacial aceticacid. Warm to dissolve the material and dilute to about 200 mL4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemi
29、cal 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), Rockville,MD.5Described in Scott, Standard Methods of Chemical Analysis, Fifth Edition, D.Van Nostrand Co.,
30、New York, NY, 1939, p. 486.D1301 91 (2014)2with water. Neutralize the solution with NH4OH and then makeslightly acid with acetic acid, adding about 3 mL excess. Filteroff any insoluble residue and wash thoroughly with hot water.8.3.3 Unite the filtrate and washings, heat to boiling, andadd 15 mL of
31、K2Cr2O7solution. Stir and heat until the yellowprecipitate assumes an orange color. Let settle and filter on aweighed Gooch crucible. Wash by decantation with hot wateruntil the washings are colorless. Finally transfer all theprecipitate from the beaker to the crucible and wash with ethylalcohol (95
32、 %). Dry at 105 6 2C (220 6 4F) for 1 h. Coolin a desiccator and weigh as PbCrO4.8.4 Calculation:PbO, % 5 P 30.691/S! 3100where:P = PbCrO4precipitate, g,S = specimen, g, and0.691 = PbO/PbCrO4= 223.19323.18.9. Moisture and Other Volatile Matter9.1 ProcedureDetermine moisture and other volatile mat-te
33、r in accordance with Method A of Test Methods D280.10. Carbon Dioxide (Evolution Method)10.1 ApparatusKnorr type of CO2evolution apparatuswith dropping funnel, condenser, and suitable purifying train.NOTE 3A description of a suitable purifying train, is found in theCarbon Dioxide Standard Method sec
34、tion of Test Methods C25.10.2 Reagent:10.2.1 Nitric Acid (1 + 19).10.3 ProcedureTransfer about 2 g of the sample, weighedto 10 mg, to a clean, dry evolution flask. Connect the evolutionflask to the absorption train, which previously has been flushedfree of any CO2, and add 100 mL of HNO3, (1 + 19) t
35、hrougha separatory funnel. When all of the HNO3has been introducedinto the flask, close the stopcock from the separatory funnel.Heat the solution in the flask to gentle boiling and boil for 5min. Turn off the heat and aspirate CO2free air through thesystem for 20 min. Remove the absorbing tube from
36、thesystem, seal, cool in a desiccator, and weigh. The increase inweight is CO2.10.4 CalculationCalculate the percent of carbon dioxideas follows:CO2,%5 C1/S1! 3100where:C1=CO2,g,andS1= specimen, g.11. Carbon Dioxide and Combined Water (CombustionMethod)11.1 ApparatusCombustion Train, consisting of t
37、he fol-lowing parts connected in the order specified; tank of purifiedcompressed nitrogen, purifying jars including a CO2absorp-tion jar, drying tube, combustion tube, tube furnace providedwith suitable controls to maintain the temperature from 450 to550C (840 to 1020F), absorption bulb for water, a
38、nd anabsorption bulb for CO2.11.2 Procedure:11.2.1 Heat the furnace, without the combustion tube, from450 to 550C (840 to 1022F). Connect the combustion tubebeside the furnace, connect the absorption tubes to the nitrogensupply, and pass a slow stream of nitrogen (about 30 mL/min)through them, to cl
39、ear out any residual moisture and CO2.Accurately weigh the absorption bulbs and reconnect them inthe train. Transfer1gofthespecimen, weighed to 10 mg, to acombustion boat that has been previously ignited and cooled.11.2.2 With the nitrogen still flowing, disconnect the trainand place the boat contai
40、ning the specimen in the middle of thetube with the aid of a hooked wire. Flush the combustion tubethoroughly with nitrogen and reconnect with the train. Placethe tube in the furnace.11.2.3 Continue the combustion for 30 min, or until thewater that condenses in the inlet arm of the first absorption
41、bulbhas been completely swept into the bulb. Disconnect theabsorption bulbs from the combustion tube, after closing allstopcocks, place in a desiccator to cool, and then weigh.11.3 Calculation:Carbon dioxide, % 5 100 3 C1Combined water, % 5 100W12 MCombined water as PbOH!2,%5 100 W12 M! 313.39where:
42、C1=CO2,g,W1= total water, g,M = free moisture, %, and13.39 = Pb(OH)2/H2O = 241.2018.015.12. Lead Carbonate12.1 CalculationCalculate the percent of PbCO3from theCO2content, as follows:PbCO3,%5 C136.071/S23100where:C1=CO2(10.4 or 11.3), g,S2= specimen weight used in the CO2determination, g,and6.071 =
43、PbCO3/CO2= 267.2044.01.13. Total Matter Insoluble in Acetic Acid13.1 ApparatusGooch Crucible, prepared and weighedprior to use.13.2 ReagentAcetic Acid (3 + 2).13.3 ProcedureTransfer 10 g of the sample, weighed to 10mg, to a 250-mL beaker and add 40 mL of acetic acid (2 + 3).Heat until solution is co
44、mplete and filter through a previouslyprepared and weighed Gooch crucible. Wash thoroughly withhot water, dry at 105 6 2C (220 6 4F) for 1 h, cool, andweigh.13.4 CalculationCalculate the percent of total matterinsoluble in acetic acid as:R/S3! 3100D1301 91 (2014)3where:R = residue, g, andS3= specime
45、n, g.14. Total Matter Insoluble in Acid Ammonium Acetate14.1 ApparatusGooch Crucible, prepared and weighedprior to use.14.2 ReagentAcid Ammonium Acetate SolutionMix 150mL of acetic acid (3 + 2) with 100 mL of water and then with95 mL of NH4OH (sp gr 0.90).14.3 ProcedureTransfer about 10 g of the sam
46、ple,weighed to 10 mg, to a 250-mL beaker. Add 40 mL of acidammonium acetate solution and heat until solution is complete.Filter through a previously prepared and weighed Goochcrucible and wash thoroughly with hot water. Dry at 105 to110C for 1 h, cool, and weigh.14.4 CalculationCalculate the percent
47、 of total matterinsoluble in acid ammonium acetate as:R/S4! 3100where:R1= residue, g, andS4= specimen, g.15. Total Impurities Other Than Moisture15.1 Calculations:15.1.1 Calculate the percent of total impurities other thanmoisture as:100 2 L1C1H1M!where:L = PbO % (8.4),C =CO2%(10.4 or 11.3),H = comb
48、ined water, % (11.3), andM = free moisture, % (9.1).15.1.2 In the case of extracted pigments where directdetermination of combined water cannot be madeconveniently, calculate the impurities other than moisture as:100 (L + 1.205 D + M) where L, D, are as defined in 15.1.1 and1.025 = 2 CO2+H2O/2 CO2=
49、106.03588.02.16. Coarse Particles16.1 ProcedureDetermine coarse particles in accordancewith Test Methods D185.BASIC SULFATE WHITE LEAD17. Small Amounts of Iron17.1 ProcedureDetermine small amounts of iron in accor-dance with Section 7.18. Total Lead18.1 ProcedureDetermine total lead in accordance withSection 88.19. Moisture and Other Volatile Matter19.1 ProcedureDetermine moisture and other volatilematter in accordance with Method A of Test Methods D280.20. Total Sulfate20.1 ApparatusGooch Crucible, ignited and weigh
