ASTM D49-83(2008)e1
(Test Method)Standard Test Methods of Chemical Analysis of Red Lead
Standard Test Methods of Chemical Analysis of Red Lead
ABSTRACT
These test methods cover procedures for the chemical analysis of red lead having the approximate formula Pb3O4 (probably PbO2·2PbO). The pigment sample shall be ground to fine powder (if lumpy or not finely ground) and shall be thoroughly mixed before taking portions for analysis. Reagent grade chemicals shall be used in all tests. The methods of determining moisture, organic coloring matter, and total lead and insoluble matter contents are given. The solutions required for the chemical analysis of lead peroxide (lead dioxide) and true red lead (tetra lead oxide) includes red lead solution, sodium thiosulfate solution, and starch solution. The formula for calculating the contents of lead peroxide and true red lead, and the procedures for determining the amounts of zinc, matter soluble in water, total silica, carbon dioxide, soluble sulfates, and iron oxide are detailed.
SCOPE
1.1 These test methods cover procedures for the chemical analysis of red lead having the approximate formula Pb3O4 (probably PbO2·2PbO).
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D49 − 83 (Reapproved2008)
Standard Test Methods of
Chemical Analysis of Red Lead
ThisstandardisissuedunderthefixeddesignationD49;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—The units statement in subsection 1.2 was corrected editorially in July 2008.
1. Scope 3. Treatment of Sample
3.1 If the pigment is lumpy or not finely ground, grind it to
1.1 These test methods cover procedures for the chemical
a fine powder and mix thoroughly. Large samples may be
analysis of red lead having the approximate formula Pb O
3 4
thoroughly mixed and a representative portion taken and
(probably PbO ·2PbO).
powdered if lumpy or not finely ground. The sample in all
1.2 The values stated in SI units are to be regarded as
cases shall be thoroughly mixed before taking portions for
standard. No other units of measurement are included in this
analysis.All samples shall be preserved in stoppered bottles or
standard.
containers.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4. Purity of Reagents
responsibility of the user of this standard to establish appro-
4.1 Reagent grade chemicals shall be used in all tests.
priate safety and health practices and determine the applica-
Unlessotherwiseindicated,itisintendedthatallreagentsshall
bility of regulatory limitations prior to use.
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society where such
2. Referenced Documents
specifications are available. Other grades may be used pro-
vided it is first ascertained that the reagent is of sufficiently
2.1 ASTM Standards:
high purity to permit its use without lessening the accuracy of
D50TestMethodsforChemicalAnalysisofYellow,Orange,
the determination.
Red, and Brown Pigments Containing Iron and Manga-
nese
4.2 Unless otherwise indicated, references to water shall be
D215Practice for the Chemical Analysis of White Linseed
understood to mean reagent water conforming to Type II of
Oil Paints (Withdrawn 2005)
Specification D1193.
D280Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments 5. Moisture
D1193Specification for Reagent Water
5.1 Determine moisture content with a 2-g specimen in
D1208Test Methods for Common Properties of Certain
accordance with Method A of Test Methods D280. The
Pigments
specimen is dried for2hat 105°C. The loss in weight is
D1301Test Methods for Chemical Analysis of White Lead
considered as moisture.
Pigments
D1959Test Method for Iodine Value of Drying Oils and
6. Organic Color
Fatty Acids (Withdrawn 2006)
6.1 Boil2gofthesamplewith25mLof95%ethylalcohol,
letsettle,decantthesupernatantliquid;boiltheresiduewith25
mL of distilled water and decant as before; boil the residue
These test methods are under the jurisdiction of ASTM Committee D01 on
with 25 mL of diluted NH OH (1+4) and again decant. Boil
Paint and Related Coatings, Materials, and Applications and are the direct
another 2-g portion of the sample with 25 mL of chloroform,
responsibility of Subcommittee D01.31 on Pigment Specifications.
let settle, and decant the supernatant liquid. If any one of the
Current edition approved July 1, 2008. Published August 2008. Originally
approvedin1917.Lastpreviouseditionapprovedin2002asD49-83(2002).DOI:
10.1520/D0049-83R08E01.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Reagent Chemicals, American Chemical Society Specifications , American
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Standards volume information, refer to the standard’s Document Summary page on listed by the American Chemical Society, see Analar Standards for Laboratory
the ASTM website. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
The last approved version of this historical standard is referenced on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
www.astm.org. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D49 − 83 (2008)
abovesolutionsiscolored,organiccoloringmatterisindicated. 8. Lead Peroxide (PbO ) and True Red Lead (Pb O )
2 3 4
NOTE 2—Method of Diehl (4) modified by Topf (5)—not applicable
If the solutions remain colorless, organic colors are probably
whensubstancesarepresent,otherthanoxidesoflead,thatliberateiodine
absent.
under conditions given, or substances such as metallic lead which reduce
PbO to PbO without the liberation of iodine.
NOTE 1—If it is desired to test for organic colors resistant to the above
reagents, the test procedures described in the following books may be
5 8.1 Solutions Required: (a) Red Lead Solution—Dissolve in
used, taking into account the nature of the pigment involved (1,2,3).
1-Lbeaker 600 g of crystallized sodiumacetate and 48 g of KI
7. Total Lead and Insoluble Matter in about 500 mL of acetic acid (1+3) (made by mixing 150
mL of glacial acetic acid with 450 mL of water). Warm the
7.1 Treat1gofthesamplewith15mLofHNO (1+1)and
beakerandcontentsonasteambath,stirringoccasionally,until
sufficient H O to dissolve all PbO on warming. If any
2 2 2
a clear solution is obtained. Cool this solution to room
insolublematterispresent,add25mLofwater,boil,filter,and
temperature, dilute to exactly 1000 mL with the acetic acid
wash with hot water. The insoluble matter contains free SiO
(1+3) and mix thoroughly. If preferred, the red lead solution
and should be examined for BaSO and silicates, if appre-
may be prepared separately for each titration, as follows:
ciable.
Dissolve30gofthecrystallizedsodiumacetateand2.4gofKI
7.2 To the original solution or filtrate from the insoluble
in25mLoftheaceticacid(1+3),warminggentlyandstirring
matter add 20 mLof H SO (sp gr 1.84) and evaporate to SO
2 4 3
until a clear solution is obtained. Cool this solution to room
fumes. Cool, add 150 mLof water, and 150 mLof 95% ethyl
temperature, dilute to 50 mL with the acetic acid solution
alcohol,letstand coldfor2h,filter,onaGoochcrucible,wash
(1+3), and mix thoroughly.
with 95% alcohol, dry at 105 to 110°C, and weigh as PbSO .
8.2 Sodium Thiosulfate Solution (0.1N)—Dissolve 24.83 g
Calculate to PbO.
of sodium thiosulfate (Na S O ·5H O), freshly pulverized and
2 2 3 2
7.3 Red lead is rarely adulterated, but should the specimen
driedbetweenfilterpaper,anddilutewithwaterto1litreatthe
contain soluble barium compounds, the PbSO obtained in 8.2
temperatureatwhichthetitrationsaretobemade.Thesolution
will contain BaSO . In this case, precipitate the lead as sulfide
isbestmadewithwell-boiledwaterfreefromCO ,orletstand
from a slightly acid (HCl) solution, dissolve the PbS in hot
8 to 14 days before standardizing, as described in Section 5 of
diluted HNO , and determine the lead as sulfate or chromate.
Test Method D1959.
7.4 If the specimen contains significant amounts of calcium
8.3 Starch Solution—Stir2to3gof potato starch with 100
or magnesium, boil the HNO −H O solution (7.1) until all
3 2 2
mL of salicylic acid solution (1%), and boil the mixture until
theleadisconvertedintonitrateandthendeterminetheleadas
the starch is practically dissolved, then dilute to 1 L (Note 3),
PbCrO .
or prepare as described in 7.8.2 of Test Method D1959.
7.5 If soluble barium, calcium, or magnesium are to be
NOTE 3—Lead Peroxide—If the pigment contains an appreciable
determined, precipitate the lead as sulfide from a slightly acid
amount of nitrite (nitrate has no effect on the method), leach out
solution (HCl), dissolve the PbS in hot diluted HNO , and
water-soluble matter as below, dry the residue and determine PbO as
determine the lead as sulfate. Boil the filtrate from the PbS to
above
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