ASTM D49-83(1996)e1
(Test Method)Standard Test Methods of Chemical Analysis of Red Lead
Standard Test Methods of Chemical Analysis of Red Lead
SCOPE
1.1 These methods cover procedures for the chemical analysis of red lead having the approximate formula Pb3O4 (probably PbO2[dot]2PbO).
1.2 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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 49 – 83 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods of
Chemical Analysis of Red Lead
This standard is issued under the fixed designation D 49; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Keywords and References were added editorially in May 1996.
1. Scope 4. Purity of Reagents
1.1 These test methods cover procedures for the chemical 4.1 Reagent grade chemicals shall be used in all tests.
analysis of red lead having the approximate formula Pb O Unless otherwise indicated, it is intended that all reagents shall
3 4
(probably PbO ·2PbO). conform to the specifications of the Committee on Analytical
1.2 This standard does not purport to address all of the Reagents of the American Chemical Society where such
safety concerns, if any, associated with its use. It is the specifications are available. Other grades may be used pro-
responsibility of the user of this standard to establish appro- vided it is first ascertained that the reagent is of sufficiently
priate safety and health practices and determine the applica- high purity to permit its use without lessening the accuracy of
bility of regulatory limitations prior to use. the determination.
4.2 Unless otherwise indicated, references to water shall be
2. Referenced Documents
understood to mean reagent water conforming to Type II of
2.1 ASTM Standards: Specification D 1193.
D 50 Test Methods for Chemical Analysis of Yellow, Or-
5. Moisture
ange, Red, and Brown Pigments Containing Iron and
Manganese 5.1 Determine moisture content with a 2-g specimen in
D 215 Practice for Chemical Analysis of White Linseed Oil accordance with Method A of Test Method D 280. The speci-
Paints men is dried for2hat 105°C. The loss in weight is considered
D 280 Test Methods for Hygroscopic Moisture (and Other as moisture.
Matter Volatile Under the Test Conditions) in Pigments
4 6. Organic Color
D 1193 Specification for Reagent Water
D 1208 Test Methods for Common Properties of Certain 6.1 Boil2gofthe sample with 25 mL of 95 % ethyl alcohol,
let settle, decant the supernatant liquid; boil the residue with 25
Pigments
D 1301 Test Methods for Chemical Analysis of White Lead mL of distilled water and decant as before; boil the residue
with 25 mL of diluted NH OH (1 + 4) and again decant. Boil
Pigments
D 1959 Test Method for Iodine Value of Drying Oils and another 2-g portion of the sample with 25 mL of chloroform,
let settle, and decant the supernatant liquid. If any one of the
Fatty Acids
above solutions is colored, organic coloring matter is indicated.
3. Treatment of Sample
If the solutions remain colorless, organic colors are probably
3.1 If the pigment is lumpy or not finely ground, grind it to absent.
a fine powder and mix thoroughly. Large samples may be
NOTE 1—If it is desired to test for organic colors resistant to the above
thoroughly mixed and a representative portion taken and
reagents, the test procedures described in the following books may be
powdered if lumpy or not finely ground. The sample in all
used, taking into account the nature of the pigment involved (1,2,3).
cases shall be thoroughly mixed before taking portions for
7. Total Lead and Insoluble Matter
analysis. All samples shall be preserved in stoppered bottles or
containers.
7.1 Treat1gofthe sample with 15 mL of HNO (1 + 1) and
sufficient H O to dissolve all PbO on warming. If any
2 2 2
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
Reagent Chemicals, American Chemical Society Specifications, American
and Related Coatings, Materials, and Applications and are the direct responsibility
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
of Subcommittee D 01.31 on Pigment Specifications.
listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Dec. 20, 1983. Published January 1984. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 49 – 17 T. Last previous edition D 49 – 82. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.03. MD.
3 6
Annual Book of ASTM Standards, Vol 06.01. The boldface numbers in parentheses refer to a list of references at the end of
Annual Book of ASTM Standards, Vol 11.01. these test methods.
D49
insoluble matter is present, add 25 mL of water, boil, filter, and in 25 mL of the acetic acid (1 + 3), warming gently and stirring
wash with hot water. The insoluble matter contains free SiO until a clear solution is obtained. Cool this solution to room
and should be examined for BaSO and silicates, if appreciable. temperature, dilute to 50 mL with the acetic acid solution
7.2 To the original solution or filtrate from the insoluble (1 + 3), and mix thoroughly.
matter add 20 mL of H SO (sp gr 1.84) and evaporate to SO 8.2 Sodium Thiosulfate Solution (0.1N)—Dissolve 24.83 g
2 4 3
fumes. Cool, add 150 mL of water, and 150 mL of 95 % ethyl of sodium thiosulfate (Na S O ·5H O), freshly pulverized and
2 2 3 2
alcohol, let stand cold for 2 h, filter, on a Gooch crucible, wash dried between filter paper, and dilute with water to 1 litre at the
with 95 % alcohol, dry at 105 to 110°C, and weigh as PbSO . temperature at which the titrations are to be made. The solution
Calculate to PbO. is best made with well-boiled water free from CO , or let stand
7.3 Red lead is rarely adulterated, but should the specimen 8 to 14 days before standardizing, as described in Section 5 of
contain soluble barium compounds, the PbSO obtained in 8.2 Test Method D 1959.
will contain BaSO . In this case, precipitate the lead as sulfide 8.3 Starch Solution—Stir 2 to3gof potato starch with 100
from a slightly acid (HCl) solution, dissolve the PbS in hot mL of salicylic acid solution (1 %), and boil the mixture until
diluted HNO , and determine the lead as sulfate or chromate. the starch is practically dissolved, then dilute to 1 L (Note 3),
7.4 If the specimen contains significant amounts of calcium or prepare as described in 7.8.2 of Test Method D 1959.
or magnesium, boil the HNO −H O solution (7.1) until all
3 2 2
NOTE 3—Lead Peroxide—If the pigment contains an appreciable
the lead is converted into nitrate and then determine the lead as
amount of nitrite (nitrate has no effect on the method), leach out
PbCrO .
4 water-soluble matter as below, dry the residue and determine PbO as
7.5 If soluble barium, calcium, or magnesium are to be
above, calculating to basis of original specimen.
determined, precipitate the lead as sulfide from a slightly acid
9. Procedure
solution (HCl), dissolve the PbS in hot diluted HNO , and
determine the lead as sulfate. Boil the filtrate from the PbS to 9.1 Weigh1gofthe finely ground sample, transfer to a
200-mL Erlenmeyer flask, add 20 mL of water; then add as
expel H S, add a little bromine water to oxidize iron (if
present), boil to expel bromine, and precipitate the barium with quickly as possible 40 mL of the “red lead solution” at room
temperature. If the sample is red lead that has been extracted
a few millilitres of H SO (1 + 3). Filter and weigh as BaSO .
2 4 4
Calculate to BaO or BaCO . To the filtrate from the BaSO add from a paint or paste, in place of the water use 10 mL of a
3 4
mixture of 7 parts by volume of chloroform and 3 parts by
NH OH in slight excess, filter off any precipitate of
F
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.