ASTM D1301-91(2020)

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: D1301 − 91 (Reapproved 2020)
Standard Test Methods for
Chemical Analysis of White Lead Pigments
This standard is issued under the fixed designation D1301; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.1 These test methods cover procedures for the chemical
mendations issued by the World Trade Organization Technical
analysis of basic carbonate white lead and basic sulfate white
Barriers to Trade (TBT) Committee.
lead.
NOTE 1—If it is necessary to separate these pigments from others, refer
2. Referenced Documents
to Practice D215.
2.1 ASTM Standards:
1.2 Theanalyticalproceduresappearinthefollowingorder:
C25Test Methods for Chemical Analysis of Limestone,
Section
Quicklime, and Hydrated Lime
Preparation of Sample 6
D185Test Methods for Coarse Particles in Pigments
Basic Carbonate White Lead:
D215Practice for the Chemical Analysis of White Linseed
Small Amounts of Iron 7
Oil Paints (Withdrawn 2005)
Total Lead 8
Moisture and Other Volatile Matter 9
D280Test Methods for Hygroscopic Moisture (and Other
Carbon Dioxide (Evolution Method) 10
Matter Volatile Under the Test Conditions) in Pigments
Carbon Dioxide and Combined Water (Combustion Method) 11
D1193Specification for Reagent Water
Lead Carbonate 12
Total Matter Insoluble in Acetic Acid 13
D2371 Test Method for Pigment Content of Solvent-
Total Matter Insoluble in Acid Ammonium Acetate 14
Reducible Paints
Total Impurities Other Than Moisture 15
D2372Practice for Separation of Vehicle From Solvent-
Coarse Particles 16
Basic Sulfate White Lead:
Reducible Paints
Small Amounts of Iron 17
D3280Test Methods for Analysis of White Zinc Pigments
Total Lead
E11Specification forWovenWireTest Sieve Cloth andTest
Moisture and Other Volatile Matter 19
Total Sulfate 20
Sieves
Zinc Oxide 21
Basic Lead Oxide 22
3. Significance and Use
Total Impurities 23
Coarse Particles 24
3.1 Thesetestmethodsaresuitablefordeterminingthelevel
1.3 The values stated in SI units are to be regarded as the
of purity and for determining the levels of various impurities.
standard. The values given in parentheses are for information
They may be used to establish compliance with specification
only.
requirements.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Reagents
responsibility of the user of this standard to establish appro-
4.1 Purity of Reagents—Reagent grade chemicals shall be
priate safety, health, and environmental practices and deter-
used in all tests. Unless otherwise indicated, it is intended that
mine the applicability of regulatory limitations prior to use.
all reagents shall conform to specifications of the Committee
1.5 This international standard was developed in accor-
on Analytical Reagents of the American Chemical Society,
dance with internationally recognized principles on standard-
1 2
These test methods are under the jurisdiction of ASTM Committee D01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Paint and Related Coatings, Materials, and Applications and are the direct contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
responsibility of Subcommittee D01.31 on Pigment Specifications. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2020. Published June 2020. Originally the ASTM website.
approved in 1953. Last previous edition approved in 2014 as D1301–91(2014). The last approved version of this historical standard is referenced on
DOI: 10.1520/D1301-91R20. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1301 − 91 (2020)
NOTE2—DetailedrequirementsforthissievearegiveninSpecification
where such specifications are available. Other grades may be
E11.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the 6.4 Preserve all samples in stoppered bottles or containers.
accuracy of the determination.
BASIC CARBONATE WHITE LEAD
4.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming
7. Small Amounts of Iron
to Type II of Specification D1193.
7.1 Reagents:
4.3 Concentration of Reagents:
7.1.1 Ammonium Hydroxide (sp gr 0.90). Warning—See
4.3.1 Concentrated Acids and Ammonium Hydroxide—
5.1.
When acids and ammonium hydroxide are specified by name
7.1.2 Hydrofluoric Acid (48%). Warning—See 5.1.
or chemical formula only, it shall be understood that concen-
7.1.3 Nitric Acid (sp gr 1.42). Warning—See 5.1.
trated reagents of the following specific gravities or concen-
7.1.4 Sulfuric Acid (sp gr 1.84). Warning—See 5.1.
trations are intended:
7.2 Procedure:
Acetic acid, CH COOH 99.5 %
7.2.1 Weigh to 10 mg about1gof specimen into a 400-mL
Hydrochloric acid, HCl sp gr 1.19
beaker.Treatthesamplewith10mLofHNO (1+1)anddilute
Hydrofluoric acid, HF 48 %
Nitric acid, HNO sp gr 1.42
3 to about 200 mL with water. If insoluble matter remains
Sulfuric acid, H SO sp gr 1.84
2 4
following treatment with HNO and dilution, filter and wash
Ammonium hydroxide, NH OH sp gr 0.90
the residue with hot water until lead free. Evaporate the filtrate
The desired specific gravities or concentrations of all other
and washings to about 200 mL. Add 20 mL of H SO (1+1)
2 4
concentrated acids are stated whenever they are specified.
to precipitate the bulk of the lead (it is unnecessary to
Warning—See Section 5.
evaporate down). Cool, filter, and wash with diluted H SO
2 4
4.3.2 Diluted Acids and Ammonium Hydroxide—
(1+99). Save the precipitate for determination of total lead
Concentrations of diluted acids and ammonium hydroxide,
(Section 8).
except when standardized, are specified as a ratio stating the
7.2.2 Ignite the HNO -insoluble matter and treat with HF
number of volumes of concentrated reagent to be diluted with
and H SO . Bring into solution, filter (any precipitate is
2 4
a given number of volumes of water, as in the following
probably BaSO ), and add to the PbSO filtrate.
4 4
example: HCl (1+99) means 1 volume of concentrated HCl
7.2.3 Colorimetrically determine iron in the combined fil-
(sp gr 1.19) diluted with 99 volumes of water.
trates by the thiocyanate method, using the same amounts of
reagents in preparing the reference standards. If copper is
5. Hazards
presentinthefiltrate,asshownbythecharacteristicblue-green
5.1 The concentrated acids bases and other reagents used in
or yellow color, remove it by precipitating the iron with
these test methods can be dangerous. Check their Material
NH OH,filtering,washing,redissolvingtheFe(OH) in10mL
4 3
Safety Data Sheets, (MSDS) before use.
of HNO (1+1), and diluting to about 200 mL before
proceeding with the thiocyanate method.
6. Preparation of Sample
8. Total Lead
6.1 Grind dry pigments, if lumpy or not finely ground, to a
fine powder for analysis. Large samples may be thoroughly
8.1 Apparatus:
mixed and a representative portion taken and powdered if
8.1.1 Gooch Crucible, prepared prior to use.
lumpy or not finely ground. Mix the sample in all cases
8.2 Reagents:
thoroughly and comminute before taking specimens for analy-
8.2.1 Acetic Acid (glacial)—Warning—See 5.1.
sis.
8.2.2 Ammonium Hydroxide (sp gr 0.90)—Warning—See
6.2 Incasesofpastesinoil,extracttheoilfromthepigment
5.1.
as described in Test Method D2371 or Practice D2372, but
8.2.3 Ethyl Alcohol (95 volume %)—Warning—See 5.1.
without straining.
8.2.4 Potassium Dichromate Solution (100 g K Cr O /L)—
2 2 7
Warning—See 5.1.
6.3 Drypigmentsseparatedfrompaintsorpastesinoilinan
oven at 95 to 98°C (203 to 210°F) for 2 h, grind to a fine
8.3 Procedure:
powder, pass through a No. 80 (180-µm) sieve (Note 2)to
8.3.1 IgnitethePbSO precipitateandfilterpaperfrom7.2.1
remove skins, and mix thoroughly. Such pigments, after
at or below 550°C (1020°F), and transfer the residue to a
weighing, should be moistened with a little ethyl alcohol
400-mL beaker. (If preferred, a new 1-g specimen of pigment
(95%) before adding reagents for analysis.
may be weighed to 10 mg into a 400-mL beaker. Proceed to
8.3.2.)
8.3.2 Moisten with water and add 5 mL of glacial acetic
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
acid.Warmtodissolvethematerialanddilutetoabout200mL
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma- Described in Scott, Standard Methods of Chemical Analysis, Fifth Edition, D.
copeial Convention, Inc. (USPC), Rockville, MD. Van Nostrand Co., New York, NY, 1939, p. 486.
D1301 − 91 (2020)
withwater.NeutralizethesolutionwithNH OHandthenmake 550°C (840 to 1020°F), absorption bulb for water, and an
slightly acid with acetic acid, adding about 3 mLexcess. Filter absorption bulb for CO .
off any insoluble residue and wash thoroughly with hot water.
11.2 Procedure:
8.3.3 Unite the filtrate and washings, heat to boiling, and
11.2.1 Heat the furnace, without the combustion tube, from
add 15 mLof K Cr O solution. Stir and heat until the yellow
2 2 7
450 to 550°C (840 to 1022°F). Connect the combustion tube
precipitate assumes an orange col
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