ASTM D1301-91(2003)

Standard Test Methods for Chemical Analysis of White Lead Pigments

SIGNIFICANCE AND USE
These test methods are suitable for determining the level of purity and for determining the levels of various impurities. They may be used to establish compliance with specification requirements.
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 Practice D 215.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address 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

• Status: Historical
• Publication Date: 30-Nov-2003
• 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 D1301-91(1999) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Dec-2003
• Replaced By: ASTM D1301-91(2008) - Standard Test Methods for Chemical Analysis of White Lead Pigments
• Effective Date: 01-Jul-2008
• Referred By: ASTM D81-87(2020) - Standard Specification for Basic Carbonate White Lead Pigment
• Effective Date: 01-Dec-2003
• Referred By: ASTM D34-08(2023) - Standard Guide for Chemical Analysis of White Pigments
• Effective Date: 01-Dec-2003
• Referred By: ASTM D49-83(2020) - Standard Test Methods of Chemical Analysis of Red Lead
• Effective Date: 01-Dec-2003

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D1301–91(Reapproved2003)
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 health practices and determine the applicability of regulatory
limitations prior to use.
1.1 These test methods cover procedures for the chemical
analysis of basic carbonate white lead and basic sulfate white
2. Referenced Documents
lead.
2.1 ASTM Standards:
NOTE 1—If it is necessary to separate these pigments from others, refer
C 25 Test Methods for Chemical Analysis of Limestone,
to Practice D 215.
Quicklime, and Hydrated Lime
1.2 The values stated in SI units are to be regarded as the
D 185 Test Methods for Coarse Particles in Pigments,
standard. The values given in parentheses are for information
Pastes, and Paints
only.
D 215 Practice for ChemicalAnalysis of White Linseed Oil
1.3 The analytical procedures appear in the following order:
Paints
Section D 280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
Preparation of Sample 6
D 1193 Specification for Reagent Water
Basic Carbonate White Lead:
Small Amounts of Iron 7 D 2371 Test Method for Pigment Content of Solvent-
Total Lead 8
Reducible Paints
Moisture and Other Volatile Matter 9
D 2372 Practice for Separation of Vehicle from Solvent-
Carbon Dioxide (Evolution Method) 10
Carbon Dioxide and Combined Water (Combustion Method) 11
Reducible Paints
Lead Carbonate 12
D 3280 Test Methods for Analysis of White Zinc Pigments
Total Matter Insoluble in Acetic Acid 13
E 11 Specification for Wire Cloth and Sieves for Testing
Total Matter Insoluble in Acid Ammonium Acetate 14
Total Impurities Other Than Moisture 15
Purposes
Coarse Particles 16
Basic Sulfate White Lead:
3. Significance and Use
Small Amounts of Iron 17
Total Lead 3.1 Thesetestmethodsaresuitablefordeterminingthelevel
Moisture and Other Volatile Matter 19
of purity and for determining the levels of various impurities.
Total Sulfate 20
They may be used to establish compliance with specification
Zinc Oxide 21
Basic Lead Oxide 22 requirements.
Total Impurities 23
Coarse Particles 24
4. Reagents
1.4 This standard does not purport to address the safety
4.1 Purity of Reagents—Reagent grade chemicals shall be
concerns, if any, associated with its use. It is the responsibility
used in all tests. Unless otherwise indicated, it is intended that
of the user of this standard to establish appropriate safety and
all reagents shall conform to specifications of the Committee
on Analytical Reagents of the American Chemical Society,
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee D01.31 on Pigment Specifications. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Current edition approved Dec. 1, 2003. Published December 2003. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1953. Last previous edition approved in 1991 as D 1301 – 91 (1999). the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D1301–91 (2003)
where such specifications are available. Other grades may be 6.4 Preserve all samples in stoppered bottles or containers.
used, provided it is first ascertained that the reagent is of
BASIC CARBONATE WHITE LEAD
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
7. Small Amounts of Iron
4.2 Purity of Water—Unless otherwise indicated, references
7.1 Reagents:
towatershallbeunderstoodtomeanreagentwaterconforming
7.1.1 Ammonium Hydroxide (sp gr 0.90). Warning—See
to Type II of Specification D 1193.
5.1.
4.3 Concentration of Reagents:
7.1.2 Hydrofluoric Acid (48 %). Warning—See 5.1.
4.3.1 Concentrated Acids and Ammonium Hydroxide—
7.1.3 Nitric Acid (sp gr 1.42). Warning—See 5.1.
When acids and ammonium hydroxide are specified by name
7.1.4 Sulfuric Acid (sp gr 1.84). Warning—See 5.1.
or chemical formula only, it shall be understood that concen-
7.2 Procedure:
trated reagents of the following specific gravities or concen-
7.2.1 Weigh to 10 mg about1gof specimen into a 400-mL
trations are intended:
beaker. Treat the sample with 10 mL of HNO (1 + 1) and
Acetic acid, CH COOH 99.5 % 3
Hydrochloric acid, HCl sp gr 1.19
dilute to about 200 mL with water. If insoluble matter remains
Hydrofluoric acid, HF 48 %
following treatment with HNO and dilution, filter and wash
Nitric acid, HNO sp gr 1.42
the residue with hot water until lead free. Evaporate the filtrate
Sulfuric acid, H SO sp gr 1.84
2 4
Ammonium hydroxide, NH OH sp gr 0.90
and washings to about 200 mL. Add 20 mL of H SO (1+1)
2 4
to precipitate the bulk of the lead (it is unnecessary to
The desired specific gravities or concentrations of all other
evaporate down). Cool, filter, and wash with diluted H SO
2 4
concentrated acids are stated whenever they are specified.
(1 + 99). Save the precipitate for determination of total lead
Warning—See Section 5.
(Section 8).
4.3.2 Diluted Acids and Ammonium Hydroxide—
7.2.2 Ignite the HNO -insoluble matter and treat with HF
Concentrations of diluted acids and ammonium hydroxide,
and H SO . Bring into solution, filter (any precipitate is
2 4
except when standardized, are specified as a ratio stating the
probably BaSO ), and add to the PbSO filtrate.
4 4
number of volumes of concentrated reagent to be diluted with
7.2.3 Colorimetrically determine iron in the combined fil-
a given number of volumes of water, as in the following
trates by the thiocyanate method, using the same amounts of
example: HCl (1 + 99) means 1 volume of concentrated HCl
reagents in preparing the reference standards. If copper is
(sp gr 1.19) diluted with 99 volumes of water.
present in the filtrate, as shown by the characteristic blue-green
5. Hazards
or yellow color, remove it by precipitating the iron with
NH OH,filtering,washing,redissolvingtheFe(OH) in10mL
5.1 The concentrated acids bases and other reagents used in 4 3
of HNO (1 + 1), and diluting to about 200 mLbefore proceed-
these test methods can be dangerous. Check their Material 3
ing with the thiocyanate method.
Safety Data Sheets, (MSDS) before use.
8. Total Lead
6. Preparation of Sample
6.1 Grind dry pigments, if lumpy or not finely ground, to a 8.1 Apparatus:
8.1.1 Gooch Crucible, prepared prior to use.
fine powder for analysis. Large samples may be thoroughly
mixed and a representative portion taken and powdered if 8.2 Reagents:
8.2.1 Acetic Acid (glacial)—Warning—See 5.1.
lumpy or not finely ground. Mix the sample in all cases
thoroughly and comminute before taking specimens for analy- 8.2.2 Ammonium Hydroxide (sp gr 0.90)—Warning—See
5.1.
sis.
6.2 In cases of pastes in oil, extract the oil from the pigment 8.2.3 Ethyl Alcohol (95 volume %)—Warning—See 5.1.
8.2.4 PotassiumDichromateSolution (100gK Cr O /L)—
as described in Test Method D 2371 or Practice D 2372, but
2 2 7
without straining. Warning—See 5.1.
6.3 Drypigmentsseparatedfrompaintsorpastesinoilinan 8.3 Procedure:
8.3.1 IgnitethePbSO precipitateandfilterpaperfrom7.2.1
oven at 95 to 98°C (203 to 210°F) for 2 h, grind to a fine
powder, pass through a No. 80 (180-µm) sieve (Note 2) to at or below 550°C (1020°F), and transfer the residue to a
400-mL beaker. (If preferred, a new 1-g specimen of pigment
remove skins, and mix thoroughly. Such pigments, after
weighing, should be moistened with a little ethyl alcohol may be weighed to 10 mg into a 400-mL beaker. Proceed to
8.3.2.)
(95 %) before adding reagents for analysis.
8.3.2 Moisten with water and add 5 mL of glacial acetic
NOTE 2—Detailed requirements for this sieve are given in Specification
acid.Warm to dissolve the material and dilute to about 200 mL
E11.
withwater.NeutralizethesolutionwithNH OHandthenmake
slightly acid with acetic acid, adding about 3 mLexcess. Filter
Reagent Chemicals, American Chemical Society Specifications, American
off any insoluble residue and wash thoroughly with hot water.
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, Described in Scott, Standard Methods of Chemical Analysis, Fifth Edition, D.
MD. Van Nostrand Co., New York, NY, 1939, p. 486.
D1301–91 (2003)
8.3.3 Unite the filtrate and washings, heat to boiling, and besidethefurnace,connecttheabsorptiontubestothenitrogen
add 15 mL of K Cr O solution. Stir and heat until the yellow supply, and pass a slow stream of nitrogen (about 30 mL/min)
2 2 7
precipitate assumes an orange color. Let settle and filter on a through them, to clear out any residual moisture and CO .
weighed Gooch crucible. Wash by decantation with hot water Accurately weigh the absorption bulbs and reconnect them in
until the washings are colorless. Finally transfer all the the train. Transfer1gofthe specimen, weighed to 10 mg, to a
precipitate from the beaker to the crucible
...