ASTM D3335-85a(2009)

This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3335–85a(Reapproved2005) Designation:D3335–85a(Reapproved2009)
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 (´) 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
1.1 This test method covers the determination of lead 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 Ifleadispresentinthesampletobeanalyzedintheformofanorganicleadcompoundataconcentrationgreaterthan0.1 %,
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazard statements are given in Section 7.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 2832 Guide for Determining Volatile and Nonvolatile Content of Paint and Related Coatings
3. Summary of Test Method
3.1 The specimen of liquid coating or dried film is prepared for analysis by dry ashing.The content of lead, cadmium, or cobalt
of an acid extract of the ash is determined by atomic absorption spectroscopy.
4. 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.
5. Apparatus
5.1 Atomic Absorption Spectrophotometer , consisting of an atomizer and either a single- or three-slot burner; gas pressure
regulating and metering devices for air and acetylene; lead, 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.
5.2 Muffle Furnace, capable of maintaining 500 6 10°C.
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials .
Current edition approved Jan.June 1, 2005.2009. Published February 2005.June 2009. Originally approved in 1974. Last previous edition approved in 19992005 as
D3335–85a(1999). D 3335 – 85a (2005).
Vandeberg, J.T., Swafford, H. D., and Scott, R.W., “Determination of Low Concentrations of Lead in Paint,” Journal of Paint Technology,Vol 47, No. 604, May 1975.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Both hollow cathode lamps and electrodeless discharge lamps have been found satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3335–85a (2009)
5.3 Crucibles, wide-form, porcelain, glazed inside and outside except for the outside bottom surface, approximately 30-mL
capacity, 50-mm rim diameter and 31-mm height.
5.4 Hot Plate, with variable surface temperature control over the range from 70 to 200°C.
5.5 High-Silica Glass Beakers, 100 and 250-mL.
5.6 Volumetric Flasks, 50, 100, and 1000-mL.
1 1
5.7 Dropping Bottles, ⁄4 or 7 or 15-mL ( ⁄2-oz) capacity.
5.8 Glass or Disposable Syringes , 5 or 10-mL capacity.
5.9 Pipets, 1, 2, 5, and 10-mL capacity.
5.10 Paint Shaker.
5.11 Paint Draw-Down Bar.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent grade water
conforming to Type II of Specification D 1193.
6.3 Ammonium Acetate Solution (50 % weight/volume)—Dissolve 500 g of ammonium acetate (NH C H O ) in water and
4 2 3 2
dilute to 1 L.
6.4 Ammonium Acetate Diluting Solution— Add 50 mL of HNO (sp gr 1.42) to 150 mL of 50 % weight/volume ammonium
acetate solution and dilute to 1 L.
6.5 Cadmium Standard Stock Solution (1 mg/mL)—Dissolve 2.1032 g of cadmium nitrate (Cd(NO ) ) in 10 mL of water, add
3 2
10 mL of HNO (sp gr 1.42), and dilute to 1 L.
6.6 Cobalt Standard Stock Solution (1 mg/mL)—Dissolve 4.9387 g of cobalt nitrate hexahydrate (Co(NO ) ·6H O) in 10 mL
3 2 2
of water, add 10 mL of HNO (sp gr 1.42), and dilute to 1 L.
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 mL
3 2
of HNO (sp gr 1.42), and dilute to 1 L.
NOTE 1—10.00 mg/mLconcentrations of cadmium, lead, silver and zinc are available as SRM 2121; and the same concentration of cobalt, copper, iron
and nickel as SRM 2124 from: Office of Standard Reference Materials, Room B-311, Chemistry Building, NIST, Washington, DC 20234.
6.8 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
6.9 Nitric Acid (1 + 1) —Add 1 volume of HNO (sp gr 1.42) to 1 volume of water.
7. Hazards
7.1 Concentrated nitric acid is corrosive and may cause severe burns of the skin or eyes; the vapor is irritating to mucous
membranes. Use care in handling this acidic substance. Refer to suppliers’ Material Safety Data Sheet.
7.2 Use only a rubber bulb aspirator for pipeting liquids.
8. Calibration and Standardization
8.1 Prepare100-mLquantitiesofatleastfourstandardsolutionsbracketingtheexpectedlead,cadmium,orcobaltconcentration
in the sample to be tested. To suitable aliquots of the 1 mg/mL standard lead, cadmium, or cobalt solution, add 5 mL of HNO (sp
gr 1.42) and 15 mL of 50 % ammonium acetate solution. Dilute to 100 mL with water.
8.2 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the manufacturer’s
literature for establishing optimum conditions for the specific instrument used.
8.3 Turntheinstrumentonandsetthewavelengthtothe283.3-nmleadline,the228.8-nmcadmiumline,orthe240.7-nmcobalt
line. Apply the current recommended by the manufacturer to the lead, cadmium, or cobalt source lamp. Allow the instrument to
warm up for about 15 min and set the slit width. Adjust the air and acetylene pressure or flow rates and ignite the burner in
accordance with the manufacturer’s instructions.
8.4 Aspirate water to rinse the atomizer chamber. Aspirate a standard solution and make any necessary readjustment in
instrument parameters to obtain maximum absorption.
The sole source of supply of No. 25007 crucibles, known to the committee at this time is Coors Manufacturer. If you are aware of alternative suppliers, please provide
this information toASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,1which you may
attend.
ThesolesourceofsupplyofVycorbeakers,knowntothecommitteeatthistimeisCorningGlassCo.,HoughtonPark,Corning,NY14831.Ifyouareawareofalternative
suppliers, please provide this information to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical
committee,1which you may attend.
Reagent Chemicals, American Chemical Society Specifications , American
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