ASTM D49-83(2020)

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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-May-2020
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.31 - Pigment Specifications

Relations

• Replaces: ASTM D49-83(2014) - Standard Test Methods of Chemical Analysis of Red Lead
• Effective Date: 01-Jun-2020
• Refers: ASTM D1301-91(2020) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Jun-2020
• Refers: ASTM D1208-96(2019) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Jun-2019
• Refers: ASTM D1301-91(2014) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Dec-2014
• Refers: ASTM D1208-96(2012) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Nov-2012
• Refers: ASTM D280-01(2012) - Standard Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
• Effective Date: 01-Nov-2012
• Refers: ASTM D50-90(2011) - Standard Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese
• Effective Date: 01-Jun-2011
• Refers: ASTM D1301-91(2008) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Jul-2008
• Refers: ASTM D1208-96(2007) - Standard Test Methods for Common Properties of Certain Pigments
• Effective Date: 01-Jun-2007
• Refers: ASTM D280-01(2007) - Standard Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
• Effective Date: 01-Feb-2007
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D50-90(2005) - Standard Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese
• Effective Date: 01-Sep-2005
• Refers: ASTM D1301-91(2003) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Dec-2003
• Refers: ASTM D280-81(1995) - Standard Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
• Effective Date: 10-May-2001
• Refers: ASTM D280-01 - Standard Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments
• Effective Date: 10-May-2001

Overview

ASTM D49-83(2020), titled Standard Test Methods of Chemical Analysis of Red Lead, establishes standardized procedures for the chemical analysis of red lead pigments with the approximate formula Pb₃O₄. Developed by ASTM International, this standard ensures reliable and consistent methods for qualifying the composition and properties of red lead, a key industrial compound. The document outlines protocols for preparing samples, using appropriate reagent grades, and executing specific analyses to determine parameters such as moisture content, organic coloring matter, total lead, insoluble matter, and several other chemical constituents. Adherence to these methods supports quality control and regulatory compliance in industries utilizing red lead.

Key Topics

• Sample Preparation: Detailed instructions are provided for grinding red lead pigments to a fine powder and thoroughly mixing samples before analysis to ensure accuracy.
• Reagent Standards: Only reagent-grade chemicals, as specified by the American Chemical Society, must be used to maintain analytical precision.
• Moisture Content Determination: Methods for quantifying the moisture within red lead pigments involve controlled drying and weighing.
• Organic Coloring Matter: Step-by-step procedures identify the presence of organic dyes or colorants in pigment samples.
• Lead Content Analysis: The standard specifies how to determine both total lead and lead in its various chemical oxide states, critical for product certification.
• Measurement of Additional Constituents: The analysis covers insoluble matter, zinc, matter soluble in water, total silica, carbon dioxide, sulfates, and iron oxide, ensuring comprehensive chemical profiling.
• Calculation Procedures: Formulas are provided for calculating the percentages of lead dioxide and tetra lead oxide, supporting precise results for quality and regulatory purposes.

Applications

The ASTM D49-83(2020) standard is essential for:

• Paint and Pigment Manufacturing: Ensures the quality and consistency of red lead pigments used in protective and anti-corrosive paints for steel structures, bridges, and marine equipment.
• Material Quality Control: Analytical laboratories use these methods to certify pigment purity, confirm product specifications, and support compliance with safety and environmental regulations.
• Industrial Research: The standard aids researchers in evaluating raw material suitability and investigating pigment degradation or contamination.
• Regulatory Compliance: The document supports industries in meeting international guidelines as referenced by the World Trade Organization Technical Barriers to Trade (TBT) Committee. This is crucial for companies involved in cross-border trade, as compliance with recognized standards can streamline acceptance in various global markets.

Related Standards

Businesses and laboratories using ASTM D49-83(2020) may also reference these relevant standards for complementary procedures:

• ASTM D50: Test Methods for Chemical Analysis of Yellow, Orange, Red, and Brown Pigments Containing Iron and Manganese.
• ASTM D280: Test Methods for Hygroscopic Moisture (and Other Matter Volatile Under the Test Conditions) in Pigments.
• ASTM D1193: Specification for Reagent Water.
• ASTM D1208: Test Methods for Common Properties of Certain Pigments.
• ASTM D1301: Test Methods for Chemical Analysis of White Lead Pigments.

Conclusion

Adopting ASTM D49-83(2020) for the chemical analysis of red lead ensures that manufacturers, laboratories, and regulatory bodies can achieve reliable, reproducible, and internationally accepted results. By following these standard test methods, stakeholders uphold the highest levels of product quality, consumer safety, and regulatory compliance in the use of red lead pigments.

Keywords: chemical analysis, red lead, lead dioxide, tetra lead oxide, ASTM D49, pigment analysis, quality control, industrial standards, lead pigment testing, regulatory compliance.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D49 − 83 (Reapproved 2020)
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.
1. Scope D1301Test Methods for Chemical Analysis of White Lead
Pigments
1.1 These test methods cover procedures for the chemical
D1959Test Method for Iodine Value of Drying Oils and
analysis of red lead having the approximate formula Pb O
3 4
Fatty Acids (Withdrawn 2006)
(probably PbO ·2PbO).
1.2 The values stated in SI units are to be regarded as
3. Treatment of Sample
standard. No other units of measurement are included in this
3.1 If the pigment is lumpy or not finely ground, grind it to
standard.
a fine powder and mix thoroughly. Large samples may be
1.3 This standard does not purport to address all of the
thoroughly mixed and a representative portion taken and
safety concerns, if any, associated with its use. It is the
powdered if lumpy or not finely ground. The sample in all
responsibility of the user of this standard to establish appro-
cases shall be thoroughly mixed before taking portions for
priate safety, health, and environmental practices and deter-
analysis.All samples shall be preserved in stoppered bottles or
mine the applicability of regulatory limitations prior to use.
containers.
1.4 This international standard was developed in accor-
4. Purity of Reagents
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4.1 Reagent grade chemicals shall be used in all tests.
Development of International Standards, Guides and Recom-
Unlessotherwiseindicated,itisintendedthatallreagentsshall
mendations issued by the World Trade Organization Technical
conform to the specifications of the Committee on Analytical
Barriers to Trade (TBT) Committee.
Reagents of the American Chemical Society where such
specifications are available. Other grades may be used pro-
2. Referenced Documents
vided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
2.1 ASTM Standards:
the determination.
D50TestMethodsforChemicalAnalysisofYellow,Orange,
Red, and Brown Pigments Containing Iron and Manga-
4.2 Unless otherwise indicated, references to water shall be
nese
understood to mean reagent water conforming to Type II of
D215Practice for the Chemical Analysis of White Linseed
Specification D1193.
Oil Paints (Withdrawn 2005)
D280Test Methods for Hygroscopic Moisture (and Other 5. Moisture
Matter Volatile Under the Test Conditions) in Pigments
5.1 Determine moisture content with a 2-g specimen in
D1193Specification for Reagent Water
accordance with Method A of Test Methods D280. The
D1208Test Methods for Common Properties of Certain
specimen is dried for2hat 105°C. The loss in weight is
Pigments
considered as moisture.
6. Organic Color
These test methods are under the jurisdiction of ASTM Committee D01 on
6.1 Boil2gofthesamplewith25mLof95%ethylalcohol,
Paint and Related Coatings, Materials, and Applications and are the direct
letsettle,decantthesupernatantliquid;boiltheresiduewith25
responsibility of Subcommittee D01.31 on Pigment Specifications.
mL of distilled water and decant as before; boil the residue
Current edition approved June 1, 2020. Published June 2020. Originally
approvedin1917.Lastpreviouseditionapprovedin2014asD49–83(2014).DOI:
10.1520/D0049-83R20.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or ACS Reagent Chemicals, Specifications and Procedures for Reagents and
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standard-Grade Reference Materials, American Chemical Society, Washington,
Standards volume information, refer to the standard’s Document Summary page on DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
the ASTM website. Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
The last approved version of this historical standard is referenced on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
www.astm.org. copeial Convention, Inc. (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D49 − 83 (2020)
with 25 mL of diluted NH OH (1+4) and again decant. Boil Methods D50. In the filtrate from calcium determine magne-
another 2-g portion of the sample with 25 mL of chloroform, sium by precipitating with sodium phosphate solution, finally
let settle, and decant the supernatant liquid. If any one of the weighing as Mg P O .
2 2 7
abovesolutionsiscolored,organiccoloringmatterisindicated.
If the solutions remain colorless, organic colors are probably
8. Lead Peroxide (PbO ) and True Red Lead (Pb O )
2 3 4
absent. NOTE 2—Method of Diehl (4) modified by Topf (5)—not applicable
whensubstancesarepresent,otherthanoxidesoflead,thatliberateiodine
NOTE 1—If it is desired to test for organic colors resistant to the above
under conditions given, or substances such as metallic lead which reduce
reagents, the test procedures described in the following books may be
PbO to PbO without the liberation of iodine.
used, taking into account the nature of the pigment involved (1,2,3).
8.1 Solutions Required: (a) Red Lead Solution—Dissolve in
7. Total Lead and Insoluble Matter
1-Lbeaker 600 g of crystallized sodiumacetate and 48 g of KI
in about 500 mL of acetic acid (1+3) (made by mixing 150
7.1 Treat1gofthesamplewith15mLofHNO (1+1)and
mL of glacial acetic acid with 450 mL of water). Warm the
sufficient H O to dissolve all PbO on warming. If any
2 2 2
beakerandcontentsonasteambath,stirringoccasionally,until
insolublematterispresent,add25mLofwater,boil,filter,and
a clear solution is obtained. Cool this solution to room
wash with hot water. The insoluble matter contains free SiO
temperature, dilute to exactly 1000 mL with the acetic acid
and should be examined for BaSO and silicates, if appre-
(1+3) and mix thoroughly. If preferred, the red lead solution
ciable.
may be prepared separately for each titration, as follows:
7.2 To the original solution or filtrate from the insoluble
Dissolve30gofthecrystallizedsodiumacetateand2.4gofKI
matter add 20 mLof H SO (sp gr 1.84) and evaporate to SO
2 4 3
in25mLoftheaceticacid(1+3),warminggentlyandstirring
fumes. Cool, add 150 mLof water, and 150 mLof 95% ethyl
until a clear solution is obtained. Cool this solution to room
alcohol,letstand coldfor2h,filter,onaGoochcrucible,wash
temperature, dilute to 50 mL with the acetic acid solution
with 95% alcohol, dry at 105 to 110°C, and weigh as PbSO .
(1+3), and mix thoroughly.
Calculate to PbO.
8.2 Sodium Thiosulfate Solution (0.1N)—Dissolve 24.83 g
7.3 Red lead is rarely adulterated, but should the specimen
of sodium thiosulfate (Na S O ·5H O), freshly pulverized and
contain soluble barium compounds, the PbSO obtained in 8.2 2 2 3 2
driedbetweenfilterpaper,anddilutewithwaterto1litreatthe
will contain BaSO . In this case, precipitate the lead as sulfide
temperatureatwhichthetitrationsaretobemade.Thesolution
from a slightly acid (HCl) solution, dissolve the PbS in hot
isbestmadewithwell-boiledwaterfreefromCO ,orletstand
diluted HNO , and determine the lead as sulfate or chromate. 2
8 to 14 days before standardizing, as described in Section 5 of
7.4 If the specimen contains significant amounts of calcium
Test Method D1959.
or magnesium, boil the HNO −H O solution (7.1) until all
3 2 2
theleadisconvertedintonitrateandthendeterminetheleadas 8.3 Starch Solution—Stir2to3gof potato starch with 100
PbCrO . mL of salicylic acid solution (1%), and boil the mixture until
the starch is practically dissolved, then dilute to 1 L (Note 3),
7.5 If soluble barium, calcium, or magnesium are to be
or prepare as described in 7.8.2 of Test Method D1959.
determined, precipitate the lead as sulfide from a sl
...