ASTM D1301-91(2008)
(Test Method)Standard Test Methods for Chemical Analysis of White Lead Pigments
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 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 Method)11 Lead Carbonate12 Total Matter Insoluble in Acetic Acid13 Total Matter Insoluble in Acid Ammonium Acetate14 Total Impurities Other Than Moisture15 Coarse Particles16 Basic Sulfate White Lead: Small Amounts of Iron17 Total Lead Moisture and Other Volatile Matter19 Total Sulfate20 Zinc Oxide21 Basic Lead Oxide22 Total Impurities23 Coarse Particles24
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved2008)
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 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
C25Test Methods for Chemical Analysis of Limestone,
to Practice D215.
Quicklime, and Hydrated Lime
1.2 Theanalyticalproceduresappearinthefollowingorder:
D185Test Methods for Coarse Particles in Pigments
Section D215Practice for the Chemical Analysis of White Linseed
Oil Paints (Withdrawn 2005)
Preparation of Sample 6
D280Test Methods for Hygroscopic Moisture (and Other
Basic Carbonate White Lead:
Matter Volatile Under the Test Conditions) in Pigments
Small Amounts of Iron 7
Total Lead 8
D1193Specification for Reagent Water
Moisture and Other Volatile Matter 9
D2371 Test Method for Pigment Content of Solvent-
Carbon Dioxide (Evolution Method) 10
Carbon Dioxide and Combined Water (Combustion Method) 11 Reducible Paints
Lead Carbonate 12
D2372Practice for Separation of Vehicle From Solvent-
Total Matter Insoluble in Acetic Acid 13
Reducible Paints
Total Matter Insoluble in Acid Ammonium Acetate 14
Total Impurities Other Than Moisture 15 D3280Test Methods for Analysis of White Zinc Pigments
Coarse Particles 16
E11Specification forWovenWireTest Sieve Cloth andTest
Basic Sulfate White Lead:
Sieves
Small Amounts of Iron 17
Total Lead
3. Significance and Use
Moisture and Other Volatile Matter 19
Total Sulfate 20
3.1 Thesetestmethodsaresuitablefordeterminingthelevel
Zinc Oxide 21
Basic Lead Oxide 22
of purity and for determining the levels of various impurities.
Total Impurities 23
They may be used to establish compliance with specification
Coarse Particles 24
requirements.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 4. Reagents
only.
4.1 Purity of Reagents—Reagent grade chemicals shall be
1.4 This standard does not purport to address the safety
used in all tests. Unless otherwise indicated, it is intended that
concerns, if any, associated with its use. It is the responsibility
all reagents shall conform to specifications of the Committee
of the user of this standard to establish appropriate safety and
on Analytical Reagents of the American Chemical Society,
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
CurrenteditionapprovedJuly1,2008.PublishedJuly2008.Originallyapproved the ASTM website.
in 1953. Last previous edition approved in 2003 as D1301–91(2003). DOI: The last approved version of this historical standard is referenced on
10.1520/D1301-91R08. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D1301 − 91 (2008)
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
theresiduewithhotwateruntilleadfree.Evaporatethefiltrate
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
Reagent Chemicals, American Chemical Society Specifications, American
acid.Warmtodissolvethematerialanddilutetoabout200mL
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 (2008)
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 color. Let settle and filter on a
besidethefurnace,connecttheabsorptiontubestothenitrogen
weighed Gooch crucible. Wash by decantation with hot water
supply, and pass a slow stream of nitrogen (about 30 mL/min)
until the washings are colorless. Finally transfer
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.