ASTM D3335-85a(2005)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3335–85a(Reapproved2005)
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 bility of regulatory limitations prior to use. Specific hazard
2 statements are given in Section 7.
1.1 This test method covers the determination of lead
contents between 0.01 and 5 %, cadmium contents between 50
2. Referenced Documents
and 150 ppm (mg/kg), and cobalt contents between 50 and
2.1 ASTM Standards:
2000 ppm (mg/kg) present in the nonvolatile portion of liquid
D 1193 Specification for Reagent Water
coatings or contained in dried films. There is no reason to
D 2832 Guide for Determining Volatile and Nonvolatile
believe that higher levels of all three elements could not be
Content of Paint and Related Coatings
determined by this test method, provided that appropriate
dilutions and adjustments in specimen size and reagent quan-
3. Summary of Test Method
tities are made.
3.1 The specimen of liquid coating or dried film is prepared
1.2 Only pigmented coatings were used for evaluating this
for analysis by dry ashing. The content of lead, cadmium, or
test method, but there is no reason to believe that varnishes and
cobalt of an acid extract of the ash is determined by atomic
lacquers could not be analyzed successfully, provided that
absorption spectroscopy.
appropriate precautions are taken.
1.3 This test method is not applicable to the determination
4. Significance and Use
of lead in samples containing antimony pigments (low recov-
4.1 The permissible level of heavy metals in certain coat-
eries are obtained).
ingsisspecifiedbygovernmentalregulatoryagencies.Thistest
1.4 If lead is present in the sample to be analyzed in the
methodprovidesafullydocumentedprocedurefordetermining
form of an organic lead compound at a concentration greater
low concentrations of lead, cadmium, and cobalt present in
than 0.1 %, small losses of lead may occur, resulting in slightly
both water and solvent-reducible coatings to determine com-
poorer precision than shown in Section 12.
pliance.
1.5 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
5. Apparatus
only.
5.1 Atomic Absorption Spectrophotometer, consisting of an
1.6 This standard does not purport to address all of the
atomizer and either a single- or three-slot burner; gas pressure
safety concerns, if any, associated with its use. It is the
regulating and metering devices for air and acetylene; lead,
responsibility of the user of this standard to establish appro-
cadmium, and cobalt source lamps with a regulated constant-
priate safety and health practices and determine the applica-
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. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Jan. 1, 2005. Published February 2005. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1974. Last previous edition approved in 1999 as D 3335 – 85a (1999). 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 (2005)
copper, iron and nickel as SRM 2124 from: Office of Standard Reference
5.2 Muffle Furnace, capable of maintaining 500 6 10°C.
Materials, Room B-311, Chemistry Building, NIST, Washington, DC
5.3 Crucibles, wide-form, porcelain, glazed inside and out-
20234.
side except for the outside bottom surface, approximately
6.8 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
30-mL capacity, 50-mm rim diameter and 31-mm height.
5.4 Hot Plate, with variable surface temperature control (HNO ).
6.9 Nitric Acid (1 + 1)—Add 1 volume of HNO (sp gr
over the range from 70 to 200°C.
5.5 High-Silica Glass Beakers, 100 and 250-mL. 1.42) to 1 volume of water.
5.6 Volumetric Flasks, 50, 100, and 1000-mL.
1 1
7. Hazards
5.7 Dropping Bottles, ⁄4 or 7 or 15-mL ( ⁄2-oz) capacity.
5.8 Glass or Disposable Syringes, 5 or 10-mL capacity.
7.1 Concentrated nitric acid is corrosive and may cause
5.9 Pipets, 1, 2, 5, and 10-mL capacity.
severe burns of the skin or eyes; the vapor is irritating to
5.10 Paint Shaker.
mucousmembranes.Usecareinhandlingthisacidicsubstance.
5.11 Paint Draw-Down Bar.
Refer to suppliers’ Material Safety Data Sheet.
7.2 Use only a rubber bulb aspirator for pipeting liquids.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be
8. Calibration and Standardization
used in all tests. Unless otherwise indicated, it is intended that
8.1 Prepare 100-mL quantities of at least four standard
all reagents shall conform to the specifications of the Commit-
solutions bracketing the expected lead, cadmium, or cobalt
tee onAnalytical Reagents of theAmerican Chemical Society,
concentration in the sample to be tested.To suitable aliquots of
where such specifications are available. Other grades may be
the 1 mg/mLstandard lead, cadmium, or cobalt solution, add 5
used, provided it is first ascertained that the reagent is of
mL of HNO (sp gr 1.42) and 15 mL of 50 % ammonium
sufficiently high purity to permit its use without lessening the
acetate solution. Dilute to 100 mL with water.
accuracy of the determination.
8.2 Operational instructions for atomic absorption spectro-
6.2 Purity of Water—Unless otherwise indicated, references
photometers vary with different models. Consult the manufac-
to water shall be understood to mean reagent grade water
turer’s literature for establishing optimum conditions for the
conforming to Type II of Specification D 1193.
specific instrument used.
6.3 Ammonium Acetate Solution (50 % weight/volume)—
8.3 Turn the instrument on and set the wavelength to the
Dissolve 500 g of ammonium acetate (NH C H O ) in water
4 2 3 2
283.3-nm lead line, the 228.8-nm cadmium line, or the
and dilute to 1 L.
240.7-nm cobalt line. Apply the current recommended by the
6.4 Ammonium Acetate Diluting Solution—Add 50 mL of
manufacturer to the lead, cadmium, or cobalt source lamp.
HNO (sp gr 1.42) to 150 mL of 50 % weight/volume ammo-
Allow the instrument to warm up for about 15 min and set the
nium acetate solution and dilute to 1 L.
slit width. Adjust the air and acetylene pressure or flow rates
6.5 Cadmium Standard Stock Solution (1 mg/mL)—
and ignite the burner in accordance with the manufacturer’s
Dissolve 2.1032 g of cadmium nitrate (Cd(NO ) )in10mLof
3 2
instructions.
water, add 10 mL of HNO (sp gr 1.42), and dilute to 1 L.
8.4 Aspirate water to rinse the atomizer chamber.Aspirate a
6.6 Cobalt Standard Stock Solution (1 mg/mL)—Dissolve
standard solution and make any necessary readjustment in
4.9387 g of cobalt nitrate hexahydrate (Co(NO ) ·6H O) in 10
3 2 2
instrument parameters to obtain maximum absorption.
mL of water, add 10 mL of HNO (sp gr 1.42), and dilute to 1
8.5 Aspirate each of the appropriate standard solutions and
L.
record the corresponding instrument readings. Aspirate water
6.7 Lead Standard Stock Solution (1 mg/mL)—Dissolve
between each standard.
1.5980 g of lead nitrate (Pb(NO ) ) in 10 mLof water, add 10
3 2
8.6 Construct a calibration curve on linear graph paper by
mL of HNO (sp gr 1.42), and dilute to 1 L.
plotting the absorbance versus concentration (micrograms per
NOTE 1—10.00 mg/mL concentrations of cadmium, lead, silver and millilitre) for each standard solution.Alternatively, the calibra-
zinc are available as SRM 2121; and the same concentration of cobalt,
tionresultsmaybestoredintheinstrument,ifsoequipped,and
readings made directly in concentration.
The sole source of supply of No. 25007 crucibles, known to the committee at
9. Procedure
this time is Coors Manufacturer. If you are aware of alternative suppliers, please
provide this information toASTM International Headquarters. Your comments will 9.1 If the sample is a liquid coating, mix it until homoge-
receive careful consideration at a meeting of the responsible technical
neous, preferably on a mechanical shaker. Determine the
committee, which you
...