ASTM D3335-85a(2014)
(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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.
General Information
Relations
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2014)
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 priate safety and health practices and determine the applica-
2 bility of regulatory limitations prior to use. Specific hazard
1.1 This test method covers the determination of lead
statements are given in Section 7.
contents between 0.01 and 5 %, cadmium contents between 50
and 150 ppm (mg/kg), and cobalt contents between 50 and
2. Referenced Documents
2000 ppm (mg/kg) present in the nonvolatile portion of liquid
2.1 ASTM Standards:
coatings or contained in dried films. There is no reason to
D1193 Specification for Reagent Water
believe that higher levels of all three elements could not be
D2832 GuideforDeterminingVolatileandNonvolatileCon-
determined by this test method, provided that appropriate
tent of Paint and Related Coatings
dilutions and adjustments in specimen size and reagent quan-
tities are made.
3. Summary of Test Method
1.2 Only pigmented coatings were used for evaluating this
3.1 The specimen of liquid coating or dried film is prepared
test method, but there is no reason to believe that varnishes and
for analysis by dry ashing. The content of lead, cadmium, or
lacquers could not be analyzed successfully, provided that
cobalt of an acid extract of the ash is determined by atomic
appropriate precautions are taken.
absorption spectroscopy.
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
5. Apparatus
standard. The values given in parentheses are for information
5.1 Atomic Absorption Spectrophotometer, consisting of an
only.
atomizer and either a single- or three-slot burner; gas pressure
1.6 This standard does not purport to address all of the
regulating and metering devices for air and acetylene; lead,
safety concerns, if any, associated with its use. It is the
cadmium, and cobalt source lamps with a regulated constant-
responsibility of the user of this standard to establish appro-
current supply; a monochromator and associated optics; a
photosensitive detector connected to an electronic amplifier;
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and a readout device.
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 July 1, 2014. Published July 2014. Originally approved For referenced ASTM standards, visit the ASTM website, www.astm.org, or
in 1974. Last previous edition approved in 2009 as D3335 – 85a (2009). DOI: contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
10.1520/D3335-85AR14. 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 (2014)
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, NY14831. If you are aware of
tionresultsmaybestoredintheinstrument,ifsoequipped,and
alternative suppliers, please provide this information to ASTM Headquarters. Your
comments will receive careful consideration at a meeting of the res
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 (Reapproved 2009) D3335 − 85a (Reapproved 2014)
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
1.1 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 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 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:
D1193 Specification for Reagent Water
D2832 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.
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 June 1, 2009July 1, 2014. Published June 2009July 2014. Originally approved in 1974. Last previous edition approved in 20052009 as
D3335 – 85a (2005).(2009). DOI: 10.1520/D3335-85AR09.10.1520/D3335-85AR14.
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 referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3335 − 85a (2014)
5. Apparatus
5.1 Atomic Absorption Spectrophotometer , 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.
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 D1193.
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 of
3 2
HNO (sp gr 1.42), and dilute to 1 L.
NOTE 1—10.00 mg/mL concentrations 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’suppliers’ Material Safety Data Sheet.
Both hollow cathode lamps and electrodeless discharge lamps have been found satisfactory for this purpose.
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 to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee, which you
may attend.
The sole source of supply of Vycor beakers, known to the committee at this time is Corning Glass Co., Houghton Park, Corning, NY 14831. If you are aware of alternative
suppliers, please provide this information to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,
which you may attend.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D3335 − 85a (2014)
7.2 Use only a rubber bulb aspirator for pipeting liquids.
8. Calibration and Standardization
8.1 Prepare 100-mL quantities of at least four standard solutions bracketing the expected lead, cadmium, or cobalt concentration
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 Turn the instrument on and set the wavelength to the 283.3-nm lead line, the 228.8-nm cadmium line, or the 240.7-nm cobalt
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.
8.5 Aspir
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.