ASTM D3618-05(2010)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3618 − 05 (Reapproved2010)
Standard Test Method for
Detection of Lead in Paint and Dried Paint Films
This standard is issued under the fixed designation D3618; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope extracted with hot sodium hydroxide solution and a drop of the
extract is transferred to filter paper. Lead present is oxidized to
1.1 This test method is intended as a screening test to
leadperoxidewithbrominewater,thentreatedwith“tetrabase”
determine if the solids in a paint contain more than 0.5 % lead.
to produce a blue quinoidal salt. Known amounts of lead are
The test described barely detects the presence of 0.4 % but
added to standard paints that are concurrently tested to provide
gives a definite positive result at the 0.5 % level.
a base for comparison.
NOTE 1—This test method may be used to detect the presence of lead
4. Significance and Use
at concentrations higher or lower than 0.5 % by making appropriate
changes in the specimen size and reagent quantities specified.
4.1 The permissible level of heavy metals in certain coat-
1.2 The values stated in SI units are to be regarded as
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
standard. No other units of measurement are included in this
methodprovidesafullydocumentedprocedurefordetermining
standard.
low concentrations of lead present in both water and solvent-
reducible coatings to determine compliance.
1.3 Paints giving an unexpected positive or questionable
result should be analyzed quantitatively for lead, using Test
5. Apparatus
Method D3335.
5.1 Burner, Meker-type.
1.4 This standard does not purport to address all of the
5.2 Crucibles, porcelain, high-form, 15-mL, with covers.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.3 Filter Paper, ashless, medium texture.
priate safety and health practices and determine the applica-
5.4 Hot Plate, with variable surface temperature control
bility of regulatory limitations prior to use. Specific hazard
over the range from 70 to 200°C.
statements are given in Section 7.
5.5 Muffle Furnace, maintained at 475 6 25°C.
2. Referenced Documents
5.6 Syringe, glass, 2-mL.
2.1 ASTM Standards:
5.7 Volumetric Flasks, 50, 100, 1000-mL.
D1193 Specification for Reagent Water
5.8 Paint Shaker.
D2832 GuideforDeterminingVolatileandNonvolatileCon-
tent of Paint and Related Coatings
5.9 Paint Draw-Down Bar.
D3335 Test Method for Low Concentrations of Lead,
6. Reagents
Cadmium, and Cobalt in Paint by Atomic Absorption
Spectroscopy 6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests unless otherwise specified. Unless otherwise
3. Summary of Test Method
indicated, it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the
3.1 The sample of liquid paint or dried film is prepared by
American Chemical Society, where such specifications are
dry ashing a weighed specimen at 475 to 500°C. The ash is
available. Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to
This test method is under the jurisdiction of ASTM Committee D01 on Paint
permit its use without lessening the accuracy of the determi-
and Related Coatings, Materials, andApplications and is the direct responsibility of
nation.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Dec. 1, 2010. Published December 2010. Originally
approved in 1977. Last previous edition approved in 2005 as D3618 – 05. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D3618-05R10. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
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D3618 − 05 (2010)
6.2 Purity of Water—Unless otherwise indicated, references 8. Procedure
to water shall be understood to mean reagent grade water
8.1 If the sample is a liquid coating, mix it until homoge-
conforming to Type II of Specification D1193.
neous, preferably on a mechanical shaker. Determine the
6.3 Acetic Acid, glacial.
nonvolatile content in accordance with Guide D2832.
6.4 Ammonium Hydroxide(1+1) —Mix 1 volume of con-
NOTE 3—Recover dried paint films from previously coated substrates
centrated ammonium hydroxide (NH OH, sp gr 0.90) with 1 (being careful not to remove any underlying material from the substrate)
or prepare in the laboratory from liquid samples. For the laboratory
volume of water.
preparation, flow some of the well-mixed sample onto a clean glass plate.
6.5 Bromine Water, saturated.
The use of a paint draw-down bar is recommended to obtain a uniform
film thickness not exceeding 2 mils (50 µm). Allow to dry in an oven at
6.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
105°C for a minimum of 1 h. Scrape the dried film off the glass plate,
(HNO ).
3 preferably with a single edge razor blade.
6.7 Lead Standard Stock Solution, Aqueous (1 mg/mL)—
8.2 Weigh to 0.1 mg, 50 mg of paint solids into a porcelain
Dissolve1.600gofleadnitrate(Pb(NO ) )in100mLofwater,
3 2 crucible or 50-mLglass beaker. For a liquid coating, determine
add 2 mL of nitric acid (sp gr 1.42), and dilute to 1 L.
the specimen weight to be taken by the following equation:
6.8 Lead Standard Working Solution, Aqueous (0.2 mg/
S 5 (1)
mL)—Pipet 10 mLof the aqueous lead standard stock solution
C
into a 50-mLvolumetric flask and dilute to volume with water.
where:
6.9 Toluene, technical grade.
S = specimen weight, g, and
6.10 Lead Standard Stock Solution, Solvent-Based (1 mg/ C = nonvolatile content, %
mL)—Dissolve 4.2 g of lead naphthenate (containing 24 % NOTE 4—Crucibles or beakers used in this test method should be new
or in very good condition. Otherwise, it is possible that some lead may be
lead) in 100 mL of toluene and dilute to 1 L.
lost and a false negative obtained.
NOTE 2—Other toluene-soluble lead driers such as lead tallate, lead
8.3 Weigh 50 mg of solids from the appropriate standard
linoleate, and lead octoate may
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