ASTM D1301-91(1999)

Standard Test Methods for Chemical Analysis of White Lead Pigments

SCOPE
1.1 These test methods cover procedures for the chemical analysis of basic carbonate white lead and basic sulfate white lead.  Note 1-If it is necessary to separate these pigments from others, refer to Methods D215.
1.2 The analytical procedures appear in the following order:  Section Preparation of Sample 6 Basic Carbonate White Lead: Small Amounts of Iron 7 Total Lead 8 Moisture and Other Volatile Matter 9 Carbon Dioxide (Evolution Method) 10 Carbon Dioxide and Combined Water (Combustion 11 Method) Lead Carbonate 12 Total Matter Insoluble in Acetic Acid 13 Total Matter Insoluble in Acid Ammonium Acetate 14 Total Impurities Other Than Moisture 15 Coarse Particles 16 Basic Sulfate White Lead: Small Amounts of Iron 17 Total Lead 18 Moisture and Other Volatile Matter 19 Total Sulfate 20 Zinc Oxide 21 Basic Lead Oxide 22 Total Impurities 23 Coarse Particles 24
1.3 This standard does not purport to address the safety problems 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

• Status: Historical
• Publication Date: 09-Jul-1999
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.31 - Pigment Specifications

Relations

• Replaced By: ASTM D1301-91(2003) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Dec-2003
• Referred By: ASTM D49-83(2020) - Standard Test Methods of Chemical Analysis of Red Lead
• Effective Date: 10-Jul-1999
• Referred By: ASTM D34-08(2023) - Standard Guide for Chemical Analysis of White Pigments
• Effective Date: 10-Jul-1999
• Referred By: ASTM D81-87(2020) - Standard Specification for Basic Carbonate White Lead Pigment
• Effective Date: 10-Jul-1999

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D 1301 – 91 (Reapproved 1999)
Standard Test Methods for
Chemical Analysis of White Lead Pigments
This standard is issued under the fixed designation D 1301; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D 185 Test Methods for Coarse Particles in Pigments,
Pastes, and Paints
1.1 These test methods cover procedures for the chemical
D 215 Practice for Chemical Analysis of White Linseed Oil
analysis of basic carbonate white lead and basic sulfate white
Paints
lead.
D 280 Test Methods for Hygroscopic Moisture (and Other
NOTE 1—If it is necessary to separate these pigments from others, refer 3
Matter Volatile Under the Test Conditions) in Pigments
to Test Methods D 215.
D 1193 Specification for Reagent Water
1.2 The analytical procedures appear in the following order:
D 2371 Test Method for Pigment Content of Solvent-
Section
Reducible Paints
D 2372 Practice for Separation of Vehicle from Solvent-
Preparation of Sample 6
Reducible Paints
Basic Carbonate White Lead:
Small Amounts of Iron 7 D 3280 Test Methods for Analysis of White Zinc Pigments
Total Lead 8
E 11 Specification for Wire-Cloth Sieves for Testing Pur-
Moisture and Other Volatile Matter 9
poses
Carbon Dioxide (Evolution Method) 10
Carbon Dioxide and Combined Water (Combustion Method) 11
Lead Carbonate 12
3. Significance and Use
Total Matter Insoluble in Acetic Acid 13
3.1 These test methods are suitable for determining the level
Total Matter Insoluble in Acid Ammonium Acetate 14
Total Impurities Other Than Moisture 15
of purity and for determining the levels of various impurities.
Coarse Particles 16
They may be used to establish compliance with specification
Basic Sulfate White Lead:
requirements.
Small Amounts of Iron 17
Total Lead
Moisture and Other Volatile Matter 19 4. Reagents
Total Sulfate 20
4.1 Purity of Reagents—Reagent grade chemicals shall be
Zinc Oxide 21
Basic Lead Oxide 22 used in all tests. Unless otherwise indicated, it is intended that
Total Impurities 23
all reagents shall conform to specifications of the Committee
Coarse Particles 24
on Analytical Reagents of the American Chemical Society,
1.3 This standard does not purport to address the safety
where such specifications are available. Other grades may be
concerns, if any, associated with its use. It is the responsibility
used, provided it is first ascertained that the reagent is of
of the user of this standard to establish appropriate safety and
sufficiently high purity to permit its use without lessening the
health practices and determine the applicability of regulatory
accuracy of the determination.
limitations prior to use.
4.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean reagent water conforming
2. Referenced Documents
to Type II of Specification D 1193.
2.1 ASTM Standards:
C 25 Test Methods for Chemical Analysis of Limestone,
Annual Book of ASTM Standards, Vol 06.03.
Quicklime, and Hydrated Lime
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 06.01.
Annual Book of ASTM Standards, Vol 14.02.
1 7
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 D01.31 on Pigment Specifications. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved Feb. 22, 1991. Published April 1991. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 1301 – 53 T. Last previous edition D 1301 – 86. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 04.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 1301
4.3 Concentration of Reagents: dilute to about 200 mL with water. If insoluble matter remains
4.3.1 Concentrated Acids and Ammonium Hydroxide— following treatment with HNO and dilution, filter and wash
When acids and ammonium hydroxide are specified by name the residue with hot water until lead free. Evaporate the filtrate
or chemical formula only, it shall be understood that concen- and washings to about 200 mL. Add 20 mL of H SO (1+1)
2 4
trated reagents of the following specific gravities or concen- to precipitate the bulk of the lead (it is unnecessary to
trations are intended: evaporate down). Cool, filter, and wash with diluted H SO
2 4
(1 + 99). Save the precipitate for determination of total lead
Acetic acid, CH COOH 99.5 %
Hydrochloric acid, HCl sp gr 1.19
(Section 8).
Hydrofluoric acid, HF 48 %
7.2.2 Ignite the HNO -insoluble matter and treat with HF
Nitric acid, HNO sp gr 1.42
Sulfuric acid, H SO sp gr 1.84 and H SO . Bring into solution, filter (any precipitate is
2 4 2 4
Ammonium hydroxide, NH OH sp gr 0.90
probably BaSO ), and add to the PbSO filtrate.
4 4
7.2.3 Colorimetrically determine iron in the combined fil-
The desired specific gravities or concentrations of all other
trates by the thiocyanate method, using the same amounts of
concentrated acids are stated whenever they are specified.
reagents in preparing the reference standards. If copper is
Warning—See Section 5.
present in the filtrate, as shown by the characteristic blue-green
4.3.2 Diluted Acids and Ammonium Hydroxide—
or yellow color, remove it by precipitating the iron with
Concentrations of diluted acids and ammonium hydroxide,
NH OH, filtering, washing, redissolving the Fe(OH) in 10 mL
except when standardized, are specified as a ratio stating the 4 3
of HNO (1 + 1), and diluting to about 200 mL before proceed-
number of volumes of concentrated reagent to be diluted with 3
ing with the thiocyanate method.
a given number of volumes of water, as in the following
example: HCl (1 + 99) means 1 volume of concentrated HCl
8. Total Lead
(sp gr 1.19) diluted with 99 volumes of water.
8.1 Apparatus:
5. Hazards
8.1.1 Gooch Crucible, prepared prior to use.
8.2 Reagents:
5.1 The concentrated acids bases and other reagents used in
these test methods can be dangerous. Check their Material 8.2.1 Acetic Acid (glacial)—Warning—See 5.1.
Safety Data Sheets, (MSDS) before use. 8.2.2 Ammonium Hydroxide (sp gr 0.90)—Warning—See
5.1.
6. Preparation of Sample
8.2.3 Ethyl Alcohol (95 volume %)—Warning—See 5.1.
6.1 Grind dry pigments, if lumpy or not finely ground, to a
8.2.4 Potassium Dichromate Solution (100 g K Cr O /L)—
2 2 7
fine powder for analysis. Large samples may be thoroughly
Warning—See 5.1.
mixed and a representative portion taken and powdered if
8.3 Procedure:
lumpy or not finely ground. Mix the sample in all cases
8.3.1 Ignite the PbSO precipitate and filter paper from 7.2.1
thoroughly and comminute before taking specimens for analy-
at or below 1020°F (550°C), and transfer the residue to a
sis.
400-mL beaker. (If preferred, a new 1-g specimen of pigment
6.2 In cases of pastes in oil, extract the oil from the pigment
may be weighed to 10 mg into a 400-mL beaker. Proceed to
as described in Test Methods D 2371 or D 2372, but without
8.3.2.)
straining.
8.3.2 Moisten with water and add 5 mL of glacial acetic
6.3 Dry pigments separated from paints or pastes in oil in an
acid. Warm to dissolve the material and dilute to about 200 mL
oven at 203 to 210°F (95 to 98°C) for 2 h, grind to a fine
with water. Neutralize the solution with NH OH and then make
powder, pass through a No. 80 (180-μm) sieve (Note 2) to
slightly acid with acetic acid, adding about 3 mL excess. Filter
remove skins, and mix thoroughly. Such pigments, after
off any insoluble residue and wash thoroughly with hot water.
weighing, should be moistened with a little ethyl alcohol
8.3.3 Unite the filtrate and washings, heat to boiling, and
(95 %) before adding reagents for analysis.
add 15 mL of K Cr O solution. Stir and heat until the yellow
2 2 7
precipitate assumes an orange color. Let settle and filter on a
NOTE 2—Detailed requirements for this sieve are given in Specification
weighed Gooch crucible. Wash by decantation with hot water
E11.
until the washings are colorless. Finally transfer all the
6.4 Preserve all samples in stoppered bottles or containers.
precipitate from the beaker to the crucible and wash with ethyl
BASIC CARBONATE WHITE LEAD alcohol (95 %). Dry at 220 6 4°F (105 6 2°C) for 1 h. Cool
in a desiccator and weigh as PbCrO .
7. Small Amounts of Iron
8.4 Calculation:
7.1 Reagents:
PbO, % 5 ~P 3 0.691 / S! 3 100
7.1.1 Ammonium Hydroxide (sp gr 0.90). Warning—See
5.1.
where:
7.1.2 Hydrofluoric Acid (48 %). Warning—See 5.1. P 5 PbCrO precipitate, g,
7.1.3 Nitric Acid (sp gr 1.42). Warning—See 5.1. S 5 specimen, g, and
7.1.4 Sulfuric Acid (sp gr 1.84). Warning—See 5.1.
7.2 Procedure:
7.2.1 Weigh to 10 mg about1gof specimen into a 400-mL
Described in Scott, Standard Methods of Chemical Analysis, Fifth Edition, D.
beaker. Treat the sample with 10 mL of HNO (1 + 1) and Van Nostrand Co., New York, NY, 1939, p. 486.
D 1301
absorption bulbs from the combustion tube, after closing all
0.691 5 PbO/PbCrO 5 223.19/323.18.
stopcocks, place in a desiccator to cool, and then weigh.
9. Moisture and Other Vo
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