ASTM D49-83(2014)

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of the standard as published by ASTM is to be considered the official document.
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Designation: D49 − 83 (Reapproved 2008) D49 − 83 (Reapproved 2014)
Standard Test Methods of
Chemical Analysis of Red Lead
This standard is issued under the fixed designation D49; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
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
1.1 These test methods cover procedures for the chemical analysis of red lead having the approximate formula Pb O (probably
3 4
PbO ·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.
2. Referenced Documents
2.1 ASTM Standards:
D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese
D215 Practice for the Chemical Analysis of White Linseed Oil Paints (Withdrawn 2005)
D280 Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
D1193 Specification for Reagent Water
D1208 Test Methods for Common Properties of Certain Pigments
D1301 Test Methods for Chemical Analysis of White Lead Pigments
D1959 Test Method for Iodine Value of Drying Oils and Fatty Acids (Withdrawn 2006)
3. Treatment of Sample
3.1 If the pigment is lumpy or not finely ground, grind it to a fine powder and mix thoroughly. Large samples may be thoroughly
mixed and a representative portion taken and powdered if lumpy or not finely ground. The sample in all cases shall be thoroughly
mixed before taking portions for analysis. All samples shall be preserved in stoppered bottles or containers.
4. Purity of Reagents
4.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform
to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are
available. Other grades may be used provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Type II of
Specification D1193.
5. Moisture
5.1 Determine moisture content with a 2-g specimen in accordance with Method A of Test Methods D280. The specimen is dried
for 2 h at 105°C. The loss in weight is considered as moisture.
These test methods are under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility of
Subcommittee D01.31 on Pigment Specifications.
Current edition approved July 1, 2008Dec. 1, 2014. Published August 2008December 2014. Originally approved in 1917. Last previous edition approved in 20022008 as
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D49 - 83 (2002).D49 – 83 (2008 ). DOI: 10.1520/D0049-83R08E01.10.1520/D0049-83R0814.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Reagent Chemicals, American Chemical Society Specifications, , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D49 − 83 (2014)
6. Organic Color
6.1 Boil 2 g of the sample with 25 mL of 95 % ethyl alcohol, let settle, decant the supernatant liquid; boil the residue with 25
mL of distilled water and decant as before; boil the residue with 25 mL of diluted NH OH (1 + 4) and again decant. Boil another
2-g portion of the sample with 25 mL of chloroform, let settle, and decant the supernatant liquid. If any one of the above solutions
is colored, organic coloring matter is indicated. If the solutions remain colorless, organic colors are probably absent.
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 used,
taking into account the nature of the pigment involved (1,2,3).
7. Total Lead and Insoluble Matter
7.1 Treat 1 g of the sample with 15 mL of HNO (1 + 1) and sufficient H O to dissolve all PbO on warming. If any insoluble
3 2 2 2
matter is present, add 25 mL of water, boil, filter, and wash with hot water. The insoluble matter contains free SiO and should
be examined for BaSO and silicates, if appreciable.
7.2 To the original solution or filtrate from the insoluble matter add 20 mL of H SO (sp gr 1.84) and evaporate to SO fumes.
2 4 3
Cool, add 150 mL of water, and 150 mL of 95 % ethyl alcohol, let stand cold for 2 h, filter, on a Gooch crucible, wash with 95 %
alcohol, dry at 105 to 110°C, and weigh as PbSO . Calculate to PbO.
7.3 Red lead is rarely adulterated, but should the specimen contain soluble barium compounds, the PbSO obtained in 8.2 will
contain BaSO . In this case, precipitate the lead as sulfide from a slightly acid (HCl) solution, dissolve the PbS in hot diluted
HNO , and determine the lead as sulfate or chromate.
7.4 If the specimen contains significant amounts of calcium or magnesium, boil the HNO − H O solution (7.1) until all the
3 2 2
lead is converted into nitrate and then determine the lead as PbCrO .
7.5 If soluble barium, calcium, or magnesium are to be determined, precipitate the lead as sulfide from a slightly acid solution
(HCl), dissolve the PbS in hot diluted HNO , and determine the lead as sulfate. Boil the filtrate from the PbS to expel H S, add
3 2
a little bromine water to oxidize iron (if present), boil to expel bromine, and precipitate the barium with a few millilitres of H SO
2 4
(1 + 3). Filter and weigh as BaSO . Calculate to BaO or BaCO . To the filtrate from the BaSO add NH OH in slight excess, filter
4 3 4 4
off any precipitate of Fe(OH) + Al(OH) , wash with hot water. Manganese, if present, can be precipitated by adding bromine and
3 3
NH OH and warming. Filter, wash with hot water, ignite, and weigh as Mn O . Unite all the filtrates, make slightly acid with acetic
4 3 4
acid, heat to boiling and pass H S into the hot solution until saturated (20 to 30 min); add 5 g of NH Cl and let stand 5 h, filter
2 4
off any ZnS, wash with H S water, dissolve the ZnS in hot diluted HCl and determine the zinc by titration with K Fe(CN) . Or,
2 4 6
boil off the H S, filter out any separated sulfur and determine the zinc as Zn P O . Calcium may be determined in the filtrate from
2 2 2 7
the ZnS by expelling H S and then adding NH OH and ammonium oxalate. Titrate the calcium oxide precipitate using the
2 4
procedure described in 13.3 of Test Methods D50. In the filtrate from calcium determine magnesium by precipitating with sodium
phosphate solution, finally weighing as Mg P O .
2 2 7
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 when substances are present, other than oxides of lead, that liberate iodine under
conditions given, or substances such as metallic lead which reduce PbO to PbO without the liberation of iodine.
8.1 Solutions Required: (a) Red Lead Solution—Dissolve in 1-L beaker 600 g of crystallized sodium acetate and 48 g of KI 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 beaker an
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