ASTM D3335-85a(2020)
(Test Method)Standard Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy
Standard Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by Atomic Absorption Spectroscopy
SIGNIFICANCE AND USE
4.1 The permissible level of heavy metals in certain coatings is specified by governmental regulatory agencies. This test method provides a fully documented procedure for determining low concentrations of lead, cadmium, and cobalt present in both water and solvent-reducible coatings to determine compliance.
SCOPE
1.1 This test method covers the determination of lead2 contents between 0.01 and 5 %, cadmium contents between 50 and 150 ppm (mg/kg), and cobalt contents between 50 and 2000 ppm (mg/kg) present in the nonvolatile portion of liquid coatings or contained in dried films. There is no reason to believe that higher levels of all three elements could not be determined by this test method, provided that appropriate dilutions and adjustments in specimen size and reagent quantities are made.
1.2 Only pigmented coatings were used for evaluating this test method, but there is no reason to believe that varnishes and lacquers could not be analyzed successfully, provided that appropriate precautions are taken.
1.3 This test method is not applicable to the determination of lead in samples containing antimony pigments (low recoveries are obtained).
1.4 If lead is present in the sample to be analyzed in the form of an organic lead compound at a concentration greater than 0.1 %, small losses of lead may occur, resulting in slightly poorer precision than shown in Section 12.
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
1.7 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.
General Information
Relations
Standards Content (Sample)
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: D3335 − 85a (Reapproved 2020)
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 D3335; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 1.7 This international standard was developed in accor-
2 dance with internationally recognized principles on standard-
1.1 This test method covers the determination of lead
ization established in the Decision on Principles for the
contents between 0.01 and 5 %, cadmium contents between 50
Development of International Standards, Guides and Recom-
and 150 ppm (mg/kg), and cobalt contents between 50 and
mendations issued by the World Trade Organization Technical
2000 ppm (mg/kg) present in the nonvolatile portion of liquid
Barriers to Trade (TBT) Committee.
coatings or contained in dried films. There is no reason to
believe that higher levels of all three elements could not be
2. Referenced Documents
determined by this test method, provided that appropriate
2.1 ASTM Standards:
dilutions and adjustments in specimen size and reagent quan-
D1193 Specification for Reagent Water
tities are made.
D2832 GuideforDeterminingVolatileandNonvolatileCon-
1.2 Only pigmented coatings were used for evaluating this
tent of Paint and Related Coatings
test method, but there is no reason to believe that varnishes and
lacquers could not be analyzed successfully, provided that
3. Summary of Test Method
appropriate precautions are taken.
3.1 The specimen of liquid coating or dried film is prepared
1.3 This test method is not applicable to the determination
for analysis by dry ashing. The content of lead, cadmium, or
of lead in samples containing antimony pigments (low recov-
cobalt of an acid extract of the ash is determined by atomic
eries are obtained).
absorption spectroscopy.
1.4 If lead is present in the sample to be analyzed in the
4. Significance and Use
form of an organic lead compound at a concentration greater
4.1 The permissible level of heavy metals in certain coat-
than 0.1 %, small losses of lead may occur, resulting in slightly
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
poorer precision than shown in Section 12.
methodprovidesafullydocumentedprocedurefordetermining
1.5 The values stated in SI units are to be regarded as the
low concentrations of lead, cadmium, and cobalt present in
standard. The values given in parentheses are for information
both water and solvent-reducible coatings to determine com-
only.
pliance.
1.6 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5.1 Atomic Absorption Spectrophotometer, consisting of an
priate safety, health, and environmental practices and deter-
atomizer and either a single- or three-slot burner; gas pressure
mine the applicability of regulatory limitations prior to use.
regulating and metering devices for air and acetylene; lead,
Specific hazard statements are given in Section 7.
cadmium, and cobalt source lamps with a regulated constant-
current supply; a monochromator and associated optics; a
photosensitive detector connected to an electronic amplifier;
and a readout device.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Feb. 1, 2020. Published February 2020. Originally For referenced ASTM standards, visit the ASTM website, www.astm.org, or
approved in 1974. Last previous edition approved in 2014 as D3335 – 85a (2014). contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
DOI: 10.1520/D3335-85AR20. Standards volume information, refer to the standard’s Document Summary page on
Vandeberg, J. T., Swafford, H. D., and Scott, R. W., “Determination of Low the ASTM website.
Concentrations of Lead in Paint,” Journal of Paint Technology, Vol 47, No. 604, Both hollow cathode lamps and electrodeless discharge lamps have been found
May 1975. satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3335 − 85a (2020)
5.2 Muffle Furnace, capable of maintaining 500 6 10°C. 6.7 Lead Standard Stock Solution (1 mg/mL)—Dissolve
1.5980 g of lead nitrate (Pb(NO ) ) in 10 mL of water, add 10
3 2
5.3 Crucibles, wide-form, porcelain, glazed inside and out-
mL of HNO (sp gr 1.42), and dilute to 1 L.
side except for the outside bottom surface, approximately
30-mL capacity, 50-mm rim diameter and 31-mm height.
NOTE 1—10.00 mg/mL concentrations of cadmium, lead, silver and
zinc are available as SRM 2121; and the same concentration of cobalt,
5.4 Hot Plate, with variable surface temperature control
copper, iron and nickel as SRM 2124 from: Office of Standard Reference
over the range from 70 to 200°C.
Materials, Room B-311, Chemistry Building, NIST, Washington, DC
20234.
5.5 High-Silica Glass Beakers, 100 and 250-mL.
6.8 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
5.6 Volumetric Flasks, 50, 100, and 1000-mL.
(HNO ).
1 1
5.7 Dropping Bottles, ⁄4 or 7 or 15-mL ( ⁄2-oz) capacity.
6.9 Nitric Acid(1+1)—Add1volumeofHNO (spgr1.42)
5.8 Glass or Disposable Syringes, 5 or 10-mL capacity.
to 1 volume of water.
5.9 Pipets, 1, 2, 5, and 10-mL capacity.
7. Hazards
5.10 Paint Shaker.
7.1 Concentrated nitric acid is corrosive and may cause
5.11 Paint Draw-Down Bar.
severe burns of the skin or eyes; the vapor is irritating to
mucousmembranes.Usecareinhandlingthisacidicsubstance.
6. Reagents
Refer to suppliers’ Material Safety Data Sheet.
6.1 Purity of Reagents—Reagent grade chemicals shall be
7.2 Use only a rubber bulb aspirator for pipeting liquids.
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
8. Calibration and Standardization
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
8.1 Prepare 100-mL quantities of at least four standard
used, provided it is first ascertained that the reagent is of
solutions bracketing the expected lead, cadmium, or cobalt
sufficiently high purity to permit its use without lessening the
concentration in the sample to be tested.To suitable aliquots of
accuracy of the determination.
the 1 mg/mLstandard lead, cadmium, or cobalt solution, add 5
mL of HNO (sp gr 1.42) and 15 mL of 50 % ammonium
6.2 Purity of Water—Unless otherwise indicated, references
acetate solution. Dilute to 100 mL with water.
to water shall be understood to mean reagent grade water
conforming to Type II of Specification D1193.
8.2 Operational instructions for atomic absorption spectro-
photometers vary with different models. Consult the manufac-
6.3 Ammonium Acetate Solution (50 % weight/volume)—
turer’s literature for establishing optimum conditions for the
Dissolve 500 g of ammonium acetate (NH C H O ) in water
4 2 3 2
specific instrument used.
and dilute to 1 L.
8.3 Turn the instrument on and set the wavelength to the
6.4 Ammonium Acetate Diluting Solution—Add 50 mL of
283.3-nm lead line, the 228.8-nm cadmium line, or the
HNO (sp gr 1.42) to 150 mL of 50 % weight/volume
240.7-nm cobalt line. Apply the current recommended by the
ammonium acetate solution and dilute to 1 L.
manufacturer to the lead, cadmium, or cobalt source lamp.
6.5 Cadmium Standard Stock Solution (1 mg/mL)—
Allow the instrument to warm up for about 15 min and set the
Dissolve 2.1032 g of cadmium nitrate (Cd(NO ) )in10mLof
3 2
slit width. Adjust the air and acetylene pressure or flow rates
water, add 10 mL of HNO (sp gr 1.42), and dilute to 1 L.
and ignite the burner in accordance with the manufacturer’s
6.6 Cobalt Standard Stock Solution (1 mg/mL)—Dissolve
instructions.
4.9387 g of cobalt nitrate hexahydrate (Co(NO ) ·6H O) in 10
3 2 2
8.4 Aspirate water to rinse the atomizer chamber.Aspirate a
mL of water, add 10 mL of HNO (sp gr 1.42), and dilute to 1
standard solution and make any necessary readjustment in
L.
instrument parameters to obtain maximum absorption.
8.5 Aspirate each of the appropriate standard solutions and
The sole source of supply of No. 25007 crucibles, known to the committee at record the corresponding instrument readings. Aspirate water
this time is Coors Manufacturer. If you are aware of alternative suppliers, please
between each standard.
provide this information toASTM International Headquarters. Your comments will
receive careful consideration at a meeting of the responsible technical committee, 8.6 Construct a calibration curve on linear graph paper by
which you may attend.
plotting the absorbance versus concentration (micrograms per
The sole source of supply of Vycor beakers, known to the committee at this
millilitre) for each standard solution.Alternatively, the calibra-
time is Corning Glass Co., Houghton Park, Corning, NY1
...
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