ASTM D3618-85a(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3618–85a(Reapproved1999)
Standard Test Method for
Detection of Lead in Paint and Dried Paint Films
This standard is issued under the fixed designation D 3618; 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.
1. Scope 4. Significance and Use
1.1 This test method is intended as a screening test to 4.1 The permissible level of heavy metals in certain coat-
determine if the solids in a paint contain more than 0.5 % lead. ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
The test described barely detects the presence of 0.4 % but methodprovidesafullydocumentedprocedurefordetermining
gives a definite positive result at the 0.5 % level. low concentrations of lead present in both water and solvent-
reducible coatings to determine compliance.
NOTE 1—This test method may be used to detect the presence of lead
at concentrations higher or lower than 0.5 % by making appropriate
5. Apparatus
changes in the specimen size and reagent quantities specified.
5.1 Burner, Meker-type.
1.2 Paints giving an unexpected positive or questionable
5.2 Crucibles, porcelain, high-form, 15-mL, with covers.
result should be analyzed quantitatively for lead, using Test
5.3 Filter Paper, ashless, medium texture.
Method D 3335.
5.4 Hot Plate, with variable surface temperature control
1.3 This standard does not purport to address all of the
over the range from 70 to 200°C.
safety concerns, if any, associated with its use. It is the
5.5 Muffle Furnace, maintained at 475 6 25°C.
responsibility of the user of this standard to establish appro-
5.6 Syringe, glass, 2-mL.
priate safety and health practices and determine the applica-
5.7 Volumetric Flasks, 50, 100, 1000-mL.
bility of regulatory limitations prior to use. Specific hazard
5.8 Paint Shaker.
statements are given in Section 7.
5.9 Paint Draw-Down Bar.
2. Referenced Documents
6. Reagents
2.1 ASTM Standards:
6.1 Purity of Reagents—Reagent grade chemicals shall be
D 1193 Specification for Reagent Water
used in all tests unless otherwise specified. Unless otherwise
D 2832 Guide for Determining Volatile and Nonvolatile
indicated, it is intended that all reagents shall conform to the
Content of Paint and Related Coatings
specifications of the Committee on Analytical Reagents of the
D 3335 Test Method for Low Concentrations of Lead,
American Chemical Society, where such specifications are
Cadmium, and Cobalt in Paint by Atomic Absorption
available. Other grades may be used, provided it is first
Spectroscopy
ascertained that the reagent is of sufficiently high purity to
permit its use without lessening the accuracy of the determi-
3. Summary of Test Method
nation.
3.1 The sample of liquid paint or dried film is prepared by
6.2 Purity of Water—Unless otherwise indicated, references
dry ashing a weighed specimen at 475 to 500°C. The ash is
to water shall be understood to mean reagent grade water
extracted with hot sodium hydroxide solution and a drop of the
conforming to Type II of Specification D 1193.
extract is transferred to filter paper. Lead present is oxidized to
6.3 Acetic Acid, glacial.
leadperoxidewithbrominewater,thentreatedwith“tetrabase”
6.4 Ammonium Hydroxide (1 + 1)—Mix 1 volume of con-
to produce a blue quinoidal salt. Known amounts of lead are
centrated ammonium hydroxide (NH OH, sp gr 0.90) with 1
added to standard paints that are concurrently tested to provide
volume of water.
a base for comparison.
6.5 Bromine Water, saturated.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
CurrenteditionapprovedMay31andSept.27,1985.PublishedNovember1985. listed by the American Chemical Society, see Analar Standards for Laboratory
Originally published as D 3618 – 77. Last previous edition D 3618 – 77 (1984). Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 06.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3618
6.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid 8.2 Weigh to 0.1 mg, 50 mg of paint solids into a porcelain
(HNO ). crucible or 50-mLglass beaker. For a liquid coating, determine
6.7 Lead Standard Stock Solution, Aqueous (1 mg/mL)— the specimen weight to be taken by the following equation:
Dissolve 1.600 g of lead nitrate (Pb(NO ) ) in 100 mL of
3 2
S 5 (1)
water, add 2 mL of nitric acid (sp gr 1.42), and dilute to 1 L.
C
6.8 Lead Standard Working Solution, Aqueous (0.2 mg/
where:
mL)—Pipet 10 mLof the aqueous lead standard stock solution
S 5 specimen weight, g, and
into a 50-mLvolumetric flask and dilute to volume with water.
C 5 nonvolatile content, %
6.9 Toluene, technical grade.
6.10 Lead Standard Stock Solution, Solvent-Based (1 mg/
NOTE 4—Crucibles or beakers used in this test method should be new
mL)—Dissolve 4.2 g of lead naphthenate (containing 24 %
or in very good condition. Otherwise, it is possible that some lead may be
lost and a false negative obtained.
lead) in 100 mL of toluene and dilute to 1 L.
8.3 Weigh 50 mg of solids from the appropriate standard
NOTE 2—Other toluene-soluble lead driers such as lead tallate, lead
paint (solvent-reducible or water-reducible) into each of two
linoleate, and lead octoate may also be used provided that the lead content
is accurately known and the appropriate weight is diluted to 100 mL to additional porcelain crucibles or 50-mL glass beakers. Using a
provide a toluene solution containing 1 mg/mL of lead.
2-mL glass syringe, add 1.0 mL of the appropriate 200-ppm
standard working solution (solvent-reducible or water-
6.11 Lead Standard Working Solution, Solvent-Based (0.2
reducible) to one of the crucibles or beakers, and 1.8 mLto the
mg/mL)—Pip
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