ASTM D49-83(2014)
(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 (Reapproved 2014)
Standard Test Methods of
1
Chemical Analysis of Red Lead
ThisstandardisissuedunderthefixeddesignationD49;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope thoroughly mixed and a representative portion taken and
powdered if lumpy or not finely ground. The sample in all
1.1 These test methods cover procedures for the chemical
cases shall be thoroughly mixed before taking portions for
analysis of red lead having the approximate formula Pb O
3 4
analysis.All samples shall be preserved in stoppered bottles or
(probably PbO ·2PbO).
2
containers.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Purity of Reagents
standard.
4.1 Reagent grade chemicals shall be used in all tests.
1.3 This standard does not purport to address all of the
Unlessotherwiseindicated,itisintendedthatallreagentsshall
safety concerns, if any, associated with its use. It is the
conform to the specifications of the Committee on Analytical
responsibility of the user of this standard to establish appro-
Reagents of the American Chemical Society where such
4
priate safety and health practices and determine the applica-
specifications are available. Other grades may be used pro-
bility of regulatory limitations prior to use.
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
2. Referenced Documents
the determination.
2
2.1 ASTM Standards:
4.2 Unless otherwise indicated, references to water shall be
D50TestMethodsforChemicalAnalysisofYellow,Orange,
understood to mean reagent water conforming to Type II of
Red, and Brown Pigments Containing Iron and Manga-
Specification D1193.
nese
D215Practice for the Chemical Analysis of White Linseed
5. Moisture
3
Oil Paints (Withdrawn 2005)
5.1 Determine moisture content with a 2-g specimen in
D280Test Methods for Hygroscopic Moisture (and Other
accordance with Method A of Test Methods D280. The
Matter Volatile Under the Test Conditions) in Pigments
specimen is dried for2hat 105°C. The loss in weight is
D1193Specification for Reagent Water
considered as moisture.
D1208Test Methods for Common Properties of Certain
Pigments
6. Organic Color
D1301Test Methods for Chemical Analysis of White Lead
6.1 Boil2gofthesamplewith25mLof95%ethylalcohol,
Pigments
letsettle,decantthesupernatantliquid;boiltheresiduewith25
D1959Test Method for Iodine Value of Drying Oils and
3
mL of distilled water and decant as before; boil the residue
Fatty Acids (Withdrawn 2006)
with 25 mL of diluted NH OH (1+4) and again decant. Boil
4
3. Treatment of Sample
another 2-g portion of the sample with 25 mL of chloroform,
let settle, and decant the supernatant liquid. If any one of the
3.1 If the pigment is lumpy or not finely ground, grind it to
a fine powder and mix thoroughly. Large samples may be abovesolutionsiscolored,organiccoloringmatterisindicated.
If the solutions remain colorless, organic colors are probably
1
absent.
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
NOTE 1—If it is desired to test for organic colors resistant to the above
responsibility of Subcommittee D01.31 on Pigment Specifications.
reagents, the test procedures described in the following books may be
Current edition approved Dec. 1, 2014. Published December 2014. Originally
ε1
approved in 1917. Last previous edition approved in 2008 as D49–83(2008 ).
DOI: 10.1520/D0049-83R0814.
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
3
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
1
---------------------- Page: 1 ----------------------
D49 − 83 (2014)
5
used, taking into account the nature of the pigment involved (1,2,3).
8.1 Solutions Required: (a) Red Lead Solution—Dissolve in
1-Lbeaker
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D49 − 83 (Reapproved 2008) D49 − 83 (Reapproved 2014)
Standard Test Methods of
1
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.
1
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).
2
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
2.1 ASTM Standards:
D50 Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese
3
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
3
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
4
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.
1
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
ε1
D49 - 83 (2002).D49 – 83 (2008 ). DOI: 10.1520/D0049-83R08E01.10.1520/D0049-83R0814.
2
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
4
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
1
---------------------- Page: 1 ----------------------
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)
...
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