ASTM D3335-85a(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3335–85a (Reapproved 1999)
Standard Test Method for
Low Concentrations of Lead, Cadmium, and Cobalt in Paint
by Atomic Absorption Spectroscopy
This standard is issued under the fixed designation D 3335; 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 D 2832 Guide for Determining Volatile and Nonvolatile
2 Content of Paint and Related Coatings
1.1 This test method covers the determination of lead
contents between 0.01 and 5 %, cadmium contents between 50
3. Summary of Test Method
and 150 ppm (mg/kg), and cobalt contents between 50 and
3.1 The specimen of liquid coating or dried film is prepared
2000 ppm (mg/kg) present in the nonvolatile portion of liquid
for analysis by dry ashing. The content of lead, cadmium, or
coatings or contained in dried films. There is no reason to
cobalt of an acid extract of the ash is determined by atomic
believe that higher levels of all three elements could not be
absorption spectroscopy.
determined by this test method, provided that appropriate
dilutions and adjustments in specimen size and reagent quan-
4. Significance and Use
tities are made.
4.1 The permissible level of heavy metals in certain coat-
1.2 Only pigmented coatings were used for evaluating this
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
test method, but there is no reason to believe that varnishes and
methodprovidesafullydocumentedprocedurefordetermining
lacquers could not be analyzed successfully, provided that
low concentrations of lead, cadmium, and cobalt present in
appropriate precautions are taken.
both water and solvent-reducible coatings to determine com-
1.3 This test method is not applicable to the determination
pliance.
of lead in samples containing antimony pigments (low recov-
eries are obtained).
5. Apparatus
1.4 If lead is present in the sample to be analyzed in the
5.1 Atomic Absorption Spectrophotometer, consisting of an
form of an organic lead compound at a concentration greater
atomizer and either a single- or three-slot burner; gas pressure
than 0.1 %, small losses of lead may occur, resulting in slightly
regulating and metering devices for air and acetylene; lead,
poorer precision than shown in Section 12.
cadmium, and cobalt source lamps with a regulated constant-
1.5 This standard does not purport to address all of the
current supply; a monochromator and associated optics; a
safety concerns, if any, associated with its use. It is the
photosensitive detector connected to an electronic amplifier;
responsibility of the user of this standard to establish appro-
and a readout device.
priate safety and health practices and determine the applica-
5.2 Muffle Furnace, capable of maintaining 500 6 10°C.
bility of regulatory limitations prior to use. Specific hazard
5.3 Crucibles, wide-form, porcelain, glazed inside and out-
statements are given in Section 7.
side except for the outside bottom surface, approximately
30-mL capacity, 50-mm rim diameter and 31-mm height.
2. Referenced Documents
5.4 Hot Plate, with variable surface temperature control
2.1 ASTM Standards:
3 over the range from 70 to 200°C.
D 1193 Specification for Reagent Water
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 Annual Book of ASTM Standards, Vol 06.01.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Both hollow cathode lamps and electrodeless discharge lamps have been found
Current edition approved July 16 and Nov. 29, 1985. Published January 1986. satisfactory for this purpose.
Originally published as D 3335 – 74. Last previous edition D 3335 – 84. The sole source of supply of No. 25007 crucibles, known to the committee at
Vandeberg, J. T., Swafford, H. D., and Scott, R. W., “Determination of Low this time is Coors Manufacturer. If you are aware of alternative suppliers, please
Concentrations of Lead in Paint,” Journal of Paint Technology, Vol 47, No. 604, provide this informtion toASTM Headquarters.Your comments will receive careful
May 1975. consideration at a meeting of the responsible technical committee, which you may
Annual Book of ASTM Standards, Vol 11.01. attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3335
5.5 High-Silica Glass Beakers, 100 and 250-mL. 7. Hazards
5.6 Volumetric Flasks, 50, 100, and 1000-mL.
7.1 Concentrated nitric acid is corrosive and may cause
1 1
5.7 Dropping Bottles, ⁄4 or ⁄2-oz (7 or 15-mL) capacity. severe burns of the skin or eyes; the vapor is irritating to
5.8 Glass or Disposable Syringes, 5 or 10-mL capacity. mucousmembranes.Usecareinhandlingthisacidicsubstance.
Refer to suppliers’ Material Safety Data Sheet.
5.9 Pipets, 1, 2, 5, and 10-mL capacity.
7.2 Use only a rubber bulb aspirator for pipeting liquids.
5.10 Paint Shaker.
5.11 Paint Draw-Down Bar.
8. Calibration and Standardization
8.1 Prepare 100-mL quantities of at least four standard
6. Reagents
solutions bracketing the expected lead, cadmium, or cobalt
6.1 Purity of Reagents—Reagent grade chemicals shall be
concentration in the sample to be tested.To suitable aliquots of
used in all tests. Unless otherwise indicated, it is intended that
the 1 mg/mLstandard lead, cadmium, or cobalt solution, add 5
all reagents shall conform to the specifications of the Commit-
mL of HNO (sp gr 1.42) and 15 mL of 50 % ammonium
tee onAnalytical Reagents of theAmerican Chem-ical Society,
acetate solution. Dilute to 100 mL with water.
where such specifications are available. Other grades may be
8.2 Operational instructions for atomic absorption spectro-
used, provided it is first ascertained that the reagent is of
photometers vary with different models. Consult the manufac-
sufficiently high purity to permit its use without lessening the
turer’s literature for establishing optimum conditions for the
accuracy of the determination.
specific instrument used.
6.2 Purity of Water—Unless otherwise indicated, references 8.3 Turn the instrument on and set the wavelength to the
to water shall be understood to mean reagent grade water 283.3-nm lead line, the 228.8-nm cadmium line, or the
conforming to Type II of Specification D 1193. 240.7-nm cobalt line. Apply the current recommended by the
manufacturer to the lead, cadmium, or cobalt source lamp.
6.3 Ammonium Acetate Solution (50 % weight/volume)—
Allow the instrument to warm up for about 15 min and set the
Dissolve 500 g of ammonium acetate (NH C H O ) in water
4 2 3 2
slit width. Adjust the air and acetylene pressure or flow rates
and dilute to 1 L.
and ignite the burner in accordance with the manufacturer’s
6.4 Ammonium Acetate Diluting Solution—Add 50 mL of
instructions.
HNO (sp gr 1.42) to 150 mL of 50 % weight/volume ammo-
8.4 Aspirate water to rinse the atomizer chamber.Aspirate a
nium acetate solution and dilute to 1 L.
standard solution and make any necessary readjustment in
6.5 Cadmium Standard Stock Solution (1 mg/mL)—
instrument parameters to obtain maximum absorption.
Dissolve 2.1032 g of cadmium nitrate (Cd(NO ) )in10mLof
3 2
8.5 Aspirate each of the appropriate standard solutions and
water, add 10 mL of HNO (sp gr 1.42), and dilute to 1 L.
record the corresponding instrument readings. Aspirate water
6.6 Cobalt Standard Stock Solution (1 mg/mL)—Dissolve
between each standard.
4.9387 g of cobalt nitrate hexahydrate (Co(NO ) ·6H O) in 10
3 2 2
8.6 Construct a calibration curve on linear graph paper by
mL of water, add 10 mL of HNO (sp gr 1.42), and dilute to 1
plotting the absorbance versus concentration (micrograms per
L.
millilitre) for each standard solution.Alternatively, the calibra-
6.7 Lead Standard Stock Solution (1 mg/mL)—Dissolve
tionresultsmaybestoredintheinstrument,ifsoequipped,and
1.5980 g of lead nitrate (Pb(NO ) ) in 10 mLof water, add 10
3 2
readings made directly in concentration.
mL of HNO (sp gr 1.42), and dilute to 1 L.
9. Procedure
NOTE 1—10.00 mg/mL concentrations of cadmium, lead, silver and
9.1 If the sample is a liquid coating, mix it until homoge-
zinc are available as SRM 2121; and the same concentration of cobalt,
copper, iron and nickel as SRM 2124 from: Office of Standard Reference neous, preferably on a mechanical shaker. Determine the
Materials, Room B-311, Chemistry Building, NIST, Washington, DC
nonvolatile content in accordance with Guide D 2832.
20234.
9.2 Prepare at least two replicate specimens by weighing by
diffe
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