ASTM F2853-10(2015)
(Test Method)Standard Test Method for Determination of Lead in Paint Layers and Similar Coatings or in Substrates and Homogenous Materials by Energy Dispersive X-Ray Fluorescence Spectrometry Using Multiple Monochromatic Excitation Beams
Standard Test Method for Determination of Lead in Paint Layers and Similar Coatings or in Substrates and Homogenous Materials by Energy Dispersive X-Ray Fluorescence Spectrometry Using Multiple Monochromatic Excitation Beams
SIGNIFICANCE AND USE
5.1 This test method may be used for quantitative determinations of Pb in painted and unpainted articles such as toys, children’s products, and other consumer products. Typical test time for quantification of Pb in homogenous samples is 1 to 3 min; and typical test time for quantification of Pb in paint is 4 to 8 min.
SCOPE
1.1 This test method uses energy dispersive X-ray fluorescence (EDXRF) spectrometry for detection and quantification of lead (Pb) in paint layers, similar coatings, or substrates and homogenous materials. The following material types were tested in the interlaboratory study for this standard test method: ABS plastic, polyethylene, polypropylene, PVC, glass, zinc alloy, wood, and fabric.
1.2 This technique may also be commonly referred to as High Definition X-ray Fluorescence (HDXRF) or Multiple Monochromatic Beam EDXRF (MMB-EDXRF).
1.3 This test method is applicable for the products and materials described in 1.1 for a Pb mass fraction range of 14 to 1200 mg/kg for uncoated samples and 30 to 450 mg/kg for coated samples, as specified in Table 1 and determined by an interlaboratory study using representative samples
1.4 Ensure that the analysis area of the sample is visually uniform in appearance and at least as large as the X-ray excitation beam at the point of sample excitation.
1.5 For coating analysis, this test method is limited to paint and similar coatings. Metallic coatings are not covered by this test method.
1.6 X-ray Nomenclature—This standard names X-ray lines using the IUPAC convention with the Siegbahn convention in parentheses.
1.7 There are no known ISO equivalent methods to this standard.
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.9 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.
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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: F2853 − 10 (Reapproved 2015)
Standard Test Method for
Determination of Lead in Paint Layers and Similar Coatings
or in Substrates and Homogenous Materials by Energy
Dispersive X-Ray Fluorescence Spectrometry Using Multiple
Monochromatic Excitation Beams
This standard is issued under the fixed designation F2853; 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.
1. Scope 1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method uses energy dispersive X-ray fluores-
responsibility of the user of this standard to establish appro-
cence (EDXRF) spectrometry for detection and quantification
priate safety, health, and environmental practices and deter-
of lead (Pb) in paint layers, similar coatings, or substrates and
mine the applicability of regulatory limitations prior to use.
homogenous materials. The following material types were
1.10 This international standard was developed in accor-
tested in the interlaboratory study for this standard test method:
dance with internationally recognized principles on standard-
ABS plastic, polyethylene, polypropylene, PVC, glass, zinc
ization established in the Decision on Principles for the
alloy, wood, and fabric.
Development of International Standards, Guides and Recom-
1.2 This technique may also be commonly referred to as
mendations issued by the World Trade Organization Technical
High Definition X-ray Fluorescence (HDXRF) or Multiple
Barriers to Trade (TBT) Committee.
Monochromatic Beam EDXRF (MMB-EDXRF).
2. Referenced Documents
1.3 This test method is applicable for the products and
materials described in 1.1 for a Pb mass fraction range of 14 to
2.1 ASTM Standards:
1200 mg/kg for uncoated samples and 30 to 450 mg/kg for
D883 Terminology Relating to Plastics
coated samples, as specified in Table 1 and determined by an
D6299 Practice for Applying Statistical Quality Assurance
interlaboratory study using representative samples
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.4 Ensure that the analysis area of the sample is visually
E135 Terminology Relating to Analytical Chemistry for
uniform in appearance and at least as large as the X-ray
Metals, Ores, and Related Materials
excitation beam at the point of sample excitation.
E691 Practice for Conducting an Interlaboratory Study to
1.5 For coating analysis, this test method is limited to paint
Determine the Precision of a Test Method
and similar coatings. Metallic coatings are not covered by this
F2576 Terminology Relating to Declarable Substances in
test method.
Materials
1.6 X-ray Nomenclature—This standard names X-ray lines
using the IUPAC convention with the Siegbahn convention in 3. Terminology
parentheses.
3.1 Definitions—Definitions of terms applying to XRF, plas-
1.7 There are no known ISO equivalent methods to this tics and declarable substances appear in Terminology D883,
standard. E135, and F2576.
1.8 The values stated in SI units are to be regarded as 3.2 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this 3.2.1 Compton scattering—the inelastic scattering of an
standard. X-ray photon through its interaction with the bound electrons
of an atom. This process is also referred to as incoherent
scattering.
This test method is under the jurisdiction of ASTM Committee F40 on
Declarable Substances in Materials and is the direct responsibility of Subcommittee
F40.01 on Test Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2015. Published October 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 2010. Last previous edition approved in 2010 as F2853 – 10 . Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/F2853-10R15. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F2853 − 10 (2015)
TABLE 1 Mass Fraction Ranges for Various Sample Types
Sample Type Homogenous Material Lead (Pb) Mass
or Substrate Type Fraction
Range, mg/kg
Uncoated Non-PVC Plastic, 14–1200
Glass or Ceramic
Uncoated Metal 66–600
Uncoated PVC 376–1150
Paint Layer Plastic or Metal 30–450
Paint Layer Fabric 79–200
Paint Layer Wood 58
3.2.2 fundamental parameters (FP) model—a model for aperture. Depending on the data acquisition mode (see 13.1 and
calibration of X-ray fluorescence response, including the cor- 13.2), one or more monochromatic X-ray beams are focused on
rection of matrix effects, based on the theory describing the the sample. The appropriate region of the fluorescence spec-
physical processes of the interactions of X-rays with matter. trum is processed by an FP method to obtain the analysis result,
that is, the Pb mass fraction in the sample.
3.2.3 homogenous material—materials are considered ho-
mogenous when the elemental composition as determined by
4.3 The apparatus is calibrated for each data acquisition
the technique in this test method is independent with respect to
mode. The calibration may be performed by the manufacturer
the measured location on the specimen and among separate
or by the user.
specimens prepared from the same material.
5. Significance and Use
3.2.4 low energy monochromatic beam—a focused mono-
5.1 This test method may be used for quantitative determi-
chromatic beam having its selected photon energy between 3
nations of Pb in painted and unpainted articles such as toys,
and 9 keV.
children’s products, and other consumer products. Typical test
3.2.5 medium energy monochromatic beam—a focused
time for quantification of Pb in homogenous samples is 1 to 3
monochromatic beam having its selected photon energy be-
min; and typical test time for quantification of Pb in paint is 4
tween 15 and 23 keV.
to 8 min.
3.2.6 monochromatic beam—an incident monochromatic
6. Interferences
beam on a sample having a selected photon energy with a
narrow energy bandwidth relative to the selected energy.
6.1 Spectral Interference—Spectral interferences result
Method precision is achieved with a monochromatic beam
from spectral overlaps among the X-ray lines that remain
having an energy bandwidth (Full Width Half Maximum) less
unresolved due to the limited energy resolution of the detector.
than 61.5 % relative to the selected energy and containing
For instance, the arsenic (As) K-L (Kα ) peak directly
2,3 1,2
more than 98 % flux of the spectrum of the excitation beam
overlaps the Pb L -M (Lα ) peak. The arsenic-Pb interfer-
3 4,5 1,2
which is incident on the sample.
ence may be minimized by a de-convolution algorithm, but the
precision of the Pb analysis may be affected. If the presence of
3.2.7 multiple monochromatic excitation beams—two or
arsenic is suspected, the user may further investigate the
more monochromatic beams.
arsenic interference. Interactions of photons and electrons
3.2.8 paint layer—a single paint layer or other similar
inside the detector result in additional peaks in the spectrum
surface-coating material on a substrate.
known as escape peaks and sum peaks. These peaks can
3.2.9 Rayleigh scattering—the elastic scattering of an X-ray
overlap with X-ray lines of interest, for example, the sum peak
photon through its interaction with the bound electrons of an
of iron (Fe) K-L (Kα ) can overlap with the Pb L -M (Lβ )
2,3 1,2 2 4 1
atom. This process is also referred to as coherent scattering.
peak.
3.2.10 substrate—the material beneath a paint layer. The
6.2 Substrate Interference—The presence of Pb in a sub-
substrate may or may not be homogenous.
strate can interfere with the determination of the Pb mass
3.3 Acronyms:
fraction of the paint layer. If the Pb signal of the paint layer and
3.3.1 EDXRF—energy dispersive X-ray fluorescence
substrate composite is dominated by the contribution from the
3.3.2 FP—fundamental parameters
substrate, the uncertainty of the FP analysis can be significant
3.3.3 HDXRF—high definition X-ray fluorescence
and the Pb measurement for the paint layer will exhibit a
3.3.4 MMB—multiple monochromatic beams
positive bias and may not meet the precision statement of this
test method. See Note 8 in Section 16.
4. Summary of Test Method
6.3 Matrix Effect—Matrix effects, also called interelement
4.1 The relevant samples include paint layers, their
effects, exist among all elements as the result of absorption of
substrates, and homogenous materials.
fluorescent X-rays (secondary X-rays) by atoms in the speci-
4.2 This technique uses one or more monochromatic exci- men. Absorption reduces the apparent sensitivity for the
tation beams to separately quantify the Pb mass fractions in element. In contrast, the atom that absorbs the X-rays may in
paint layers and substrates, and homogenous materials. The turn emit a fluorescent X-ray, increasing apparent sensitivity
area of the sample to be analyzed is placed against an X-ray for the second element. Mathematical methods may be used to
F2853 − 10 (2015)
compensate for matrix effects. A number of mathematical 8. Reagents and Materials
correction procedures are commonly utilized including full FP 4
8.1 Purity of Reagents —Reagent grade chemicals shall be
treatments and mathematical models based on influence coef-
used in all tests. Unless otherwise indicated, it is intended that
ficient algorithms.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
7. Apparatus
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
7.1 EDXRF Spectrometer —designed for X-ray fluores-
high purity to permit its use without lessening the accuracy of
cence analysis using multiple monochromatic excitation beams
the determination. Reagents used include materials used for
with an energy dispersive detector. Any EDXRF spectrometer
cleaning of samples.
may be used if it is capable of meeting method precision and
its design incorporates the following features: 8.2 Reagents:
8.2.1 Isopropanol or ethanol,
7.1.1 Source of X-ray Excitation—typically an X-ray tube,
8.2.2 Nitric acid (HNO ),
capable of exciting the Pb L lines in a sample. For instance, an
8.2.3 Hexane, and
X-ray tube with a zirconium, molybdenum, rhodium,
8.2.4 Deionized water (H O).
palladium, or silver target can be used.
8.3 Gloves—Disposable gloves are recommended for han-
7.1.2 X-ray Optics—X-ray optical elements capable of ac-
dling reference materials and other samples to minimize
cepting X-rays from a tube and directing monochromatic
contamination.
beams on the sample. Two or more X-ray optical elements are
necessary to provide multiple monochromatic beams. At least
8.4 Appropriate personal protective equipment for the han-
one optical element provides a low energy monochromatic
dling of reagents.
beam, and at least one optical element provides a medium
8.5 Uncoated Mode Calibration Standards—At least two
energy monochromatic beam.
standards are required for calibration, one a scattering standard,
7.1.3 X-Ray Detector—with energy resolution equal to or
and the other a Pb-containing homogenous material (see Note
better than 250 eV full width at half maximum of the
3). The scattering standard shall have a known density,
manganese (Mn) K-L (Kα ) line.
2,3 1,2
thickness, and composition. The other standard shall be a Pb
7.1.4 Digital Pulse Processor and Multi-channel
containing homogenous standard with a known Pb mass
Analyzer—a digital pulse processor for pulse shaping and
fraction. Refer to manufacturer’s recommendations.
conditioning, and a multi-channel analyzer for binning the
NOTE 1—Better performance is expected if the Pb mass fraction of the
pulses according to X-ray energy.
Pb containing calibration standard is within the upper half of the scope
7.1.5 Detector Aperture—an aperture in the beam path
range (see Section 1).
between the sample and the detector to limit the field of view
8.6 Paint Layer Mode Calibration Standards—A minimum
of the detector.
of four standards are needed for calibration (see Note 3). Two
standards shall be scattering standards, and the other two shall
7.2 The following spectrometer features and accessories are
be Pb containing paint layer-on-substrate standards. Refer to
optional:
manufacturer’s recommendations.
7.2.1 Beam Shutter—used to select a monochromatic beam
8.6.1 Scattering Standards—At least two scattering stan-
or select a combination of monochromatic beams.
dards are necessary due to the overlap of Compton and
7.2.2 Drift Correction Monitors—due to instability of the
Rayleigh scattering of the low energy beam. One scattering
measurement system, the sensitivity and background of the
standard shall have a known density, thickness, and composi-
spectrometer may drift with time. Drift correction monitors
tion. The other scattering standard shall be a thin paint layer,
may be used to compensate for this drift. The optimum drift
with a known mass per unit area, mounted on a thin polyester
correction monitor samples are permanent materials that are
film. An example of the polyester film is film used for liquid
stable with repeated exposure to X-rays.
cells having a thickness of 3.7 μm or similar.
8.6.2 Paint Layer Standards—At least two Pb-containing
7.3 Discussion—the data acquisition has two modes, one for
paint layer standards each with differing paint layer thicknesses
homogenous materials and one for paint layers. The uncoated
and known Pb mass fraction are required.
mode only requires one monochromatic beam for the excitation
of the Pb L shell. The paint layer mode requires a second and
NOTE 2—Better performance is expected if the Pb mass fraction of the
lower energy monochromatic beam with less penetration of the
two Pb containing paint layer standards are within the upper half of the
scope range (see Section 1).
sample to determine paint surface information and the Pb mass
NOTE 3—Additional calibration standards may be used for improved
fraction in the paint layer.
accuracy.
Reagent Chemicals, American Chemical Society Specifications, American
The sole source of supply of the apparatus known to the committee at this time Chemical Society, Washington
...
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: F2853 − 10 (Reapproved 2015)
Standard Test Method for
Determination of Lead in Paint Layers and Similar Coatings
or in Substrates and Homogenous Materials by Energy
Dispersive X-Ray Fluorescence Spectrometry Using Multiple
Monochromatic Excitation Beams
This standard is issued under the fixed designation F2853; 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.
1. Scope 1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method uses energy dispersive X-ray fluores-
responsibility of the user of this standard to establish appro-
cence (EDXRF) spectrometry for detection and quantification
priate safety, health, and environmental practices and deter-
of lead (Pb) in paint layers, similar coatings, or substrates and
mine the applicability of regulatory limitations prior to use.
homogenous materials. The following material types were
1.10 This international standard was developed in accor-
tested in the interlaboratory study for this standard test method:
dance with internationally recognized principles on standard-
ABS plastic, polyethylene, polypropylene, PVC, glass, zinc
ization established in the Decision on Principles for the
alloy, wood, and fabric.
Development of International Standards, Guides and Recom-
1.2 This technique may also be commonly referred to as
mendations issued by the World Trade Organization Technical
High Definition X-ray Fluorescence (HDXRF) or Multiple
Barriers to Trade (TBT) Committee.
Monochromatic Beam EDXRF (MMB-EDXRF).
2. Referenced Documents
1.3 This test method is applicable for the products and
materials described in 1.1 for a Pb mass fraction range of 14 to
2.1 ASTM Standards:
1200 mg/kg for uncoated samples and 30 to 450 mg/kg for
D883 Terminology Relating to Plastics
coated samples, as specified in Table 1 and determined by an
D6299 Practice for Applying Statistical Quality Assurance
interlaboratory study using representative samples
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
1.4 Ensure that the analysis area of the sample is visually
E135 Terminology Relating to Analytical Chemistry for
uniform in appearance and at least as large as the X-ray
Metals, Ores, and Related Materials
excitation beam at the point of sample excitation.
E691 Practice for Conducting an Interlaboratory Study to
1.5 For coating analysis, this test method is limited to paint
Determine the Precision of a Test Method
and similar coatings. Metallic coatings are not covered by this
F2576 Terminology Relating to Declarable Substances in
test method.
Materials
1.6 X-ray Nomenclature—This standard names X-ray lines
using the IUPAC convention with the Siegbahn convention in 3. Terminology
parentheses.
3.1 Definitions—Definitions of terms applying to XRF, plas-
1.7 There are no known ISO equivalent methods to this tics and declarable substances appear in Terminology D883,
standard. E135, and F2576.
1.8 The values stated in SI units are to be regarded as 3.2 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this 3.2.1 Compton scattering—the inelastic scattering of an
standard. X-ray photon through its interaction with the bound electrons
of an atom. This process is also referred to as incoherent
scattering.
This test method is under the jurisdiction of ASTM Committee F40 on
Declarable Substances in Materials and is the direct responsibility of Subcommittee
F40.01 on Test Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2015. Published October 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ɛ1
approved in 2010. Last previous edition approved in 2010 as F2853 – 10 . Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/F2853-10R15. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F2853 − 10 (2015)
TABLE 1 Mass Fraction Ranges for Various Sample Types
Sample Type Homogenous Material Lead (Pb) Mass
or Substrate Type Fraction
Range, mg/kg
Uncoated Non-PVC Plastic, 14–1200
Glass or Ceramic
Uncoated Metal 66–600
Uncoated PVC 376–1150
Paint Layer Plastic or Metal 30–450
Paint Layer Fabric 79–200
Paint Layer Wood 58
3.2.2 fundamental parameters (FP) model—a model for aperture. Depending on the data acquisition mode (see 13.1 and
calibration of X-ray fluorescence response, including the cor- 13.2), one or more monochromatic X-ray beams are focused on
rection of matrix effects, based on the theory describing the the sample. The appropriate region of the fluorescence spec-
physical processes of the interactions of X-rays with matter. trum is processed by an FP method to obtain the analysis result,
that is, the Pb mass fraction in the sample.
3.2.3 homogenous material—materials are considered ho-
mogenous when the elemental composition as determined by
4.3 The apparatus is calibrated for each data acquisition
the technique in this test method is independent with respect to
mode. The calibration may be performed by the manufacturer
the measured location on the specimen and among separate
or by the user.
specimens prepared from the same material.
5. Significance and Use
3.2.4 low energy monochromatic beam—a focused mono-
5.1 This test method may be used for quantitative determi-
chromatic beam having its selected photon energy between 3
nations of Pb in painted and unpainted articles such as toys,
and 9 keV.
children’s products, and other consumer products. Typical test
3.2.5 medium energy monochromatic beam—a focused
time for quantification of Pb in homogenous samples is 1 to 3
monochromatic beam having its selected photon energy be-
min; and typical test time for quantification of Pb in paint is 4
tween 15 and 23 keV.
to 8 min.
3.2.6 monochromatic beam—an incident monochromatic
6. Interferences
beam on a sample having a selected photon energy with a
narrow energy bandwidth relative to the selected energy.
6.1 Spectral Interference—Spectral interferences result
Method precision is achieved with a monochromatic beam
from spectral overlaps among the X-ray lines that remain
having an energy bandwidth (Full Width Half Maximum) less
unresolved due to the limited energy resolution of the detector.
than 61.5 % relative to the selected energy and containing
For instance, the arsenic (As) K-L (Kα ) peak directly
2,3 1,2
more than 98 % flux of the spectrum of the excitation beam
overlaps the Pb L -M (Lα ) peak. The arsenic-Pb interfer-
3 4,5 1,2
which is incident on the sample.
ence may be minimized by a de-convolution algorithm, but the
precision of the Pb analysis may be affected. If the presence of
3.2.7 multiple monochromatic excitation beams—two or
arsenic is suspected, the user may further investigate the
more monochromatic beams.
arsenic interference. Interactions of photons and electrons
3.2.8 paint layer—a single paint layer or other similar
inside the detector result in additional peaks in the spectrum
surface-coating material on a substrate.
known as escape peaks and sum peaks. These peaks can
3.2.9 Rayleigh scattering—the elastic scattering of an X-ray
overlap with X-ray lines of interest, for example, the sum peak
photon through its interaction with the bound electrons of an
of iron (Fe) K-L (Kα ) can overlap with the Pb L -M (Lβ )
2,3 1,2 2 4 1
atom. This process is also referred to as coherent scattering.
peak.
3.2.10 substrate—the material beneath a paint layer. The
6.2 Substrate Interference—The presence of Pb in a sub-
substrate may or may not be homogenous.
strate can interfere with the determination of the Pb mass
3.3 Acronyms:
fraction of the paint layer. If the Pb signal of the paint layer and
3.3.1 EDXRF—energy dispersive X-ray fluorescence
substrate composite is dominated by the contribution from the
3.3.2 FP—fundamental parameters
substrate, the uncertainty of the FP analysis can be significant
3.3.3 HDXRF—high definition X-ray fluorescence
and the Pb measurement for the paint layer will exhibit a
3.3.4 MMB—multiple monochromatic beams
positive bias and may not meet the precision statement of this
test method. See Note 8 in Section 16.
4. Summary of Test Method
6.3 Matrix Effect—Matrix effects, also called interelement
4.1 The relevant samples include paint layers, their
effects, exist among all elements as the result of absorption of
substrates, and homogenous materials.
fluorescent X-rays (secondary X-rays) by atoms in the speci-
4.2 This technique uses one or more monochromatic exci- men. Absorption reduces the apparent sensitivity for the
tation beams to separately quantify the Pb mass fractions in element. In contrast, the atom that absorbs the X-rays may in
paint layers and substrates, and homogenous materials. The turn emit a fluorescent X-ray, increasing apparent sensitivity
area of the sample to be analyzed is placed against an X-ray for the second element. Mathematical methods may be used to
F2853 − 10 (2015)
compensate for matrix effects. A number of mathematical 8. Reagents and Materials
correction procedures are commonly utilized including full FP
8.1 Purity of Reagents —Reagent grade chemicals shall be
treatments and mathematical models based on influence coef-
used in all tests. Unless otherwise indicated, it is intended that
ficient algorithms.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
7. Apparatus
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently
7.1 EDXRF Spectrometer —designed for X-ray fluores-
high purity to permit its use without lessening the accuracy of
cence analysis using multiple monochromatic excitation beams
the determination. Reagents used include materials used for
with an energy dispersive detector. Any EDXRF spectrometer
cleaning of samples.
may be used if it is capable of meeting method precision and
its design incorporates the following features: 8.2 Reagents:
8.2.1 Isopropanol or ethanol,
7.1.1 Source of X-ray Excitation—typically an X-ray tube,
8.2.2 Nitric acid (HNO ),
capable of exciting the Pb L lines in a sample. For instance, an 3
8.2.3 Hexane, and
X-ray tube with a zirconium, molybdenum, rhodium,
8.2.4 Deionized water (H O).
palladium, or silver target can be used. 2
8.3 Gloves—Disposable gloves are recommended for han-
7.1.2 X-ray Optics—X-ray optical elements capable of ac-
dling reference materials and other samples to minimize
cepting X-rays from a tube and directing monochromatic
contamination.
beams on the sample. Two or more X-ray optical elements are
necessary to provide multiple monochromatic beams. At least
8.4 Appropriate personal protective equipment for the han-
one optical element provides a low energy monochromatic
dling of reagents.
beam, and at least one optical element provides a medium
8.5 Uncoated Mode Calibration Standards—At least two
energy monochromatic beam.
standards are required for calibration, one a scattering standard,
7.1.3 X-Ray Detector—with energy resolution equal to or
and the other a Pb-containing homogenous material (see Note
better than 250 eV full width at half maximum of the
3). The scattering standard shall have a known density,
manganese (Mn) K-L (Kα ) line.
2,3 1,2
thickness, and composition. The other standard shall be a Pb
7.1.4 Digital Pulse Processor and Multi-channel
containing homogenous standard with a known Pb mass
Analyzer—a digital pulse processor for pulse shaping and
fraction. Refer to manufacturer’s recommendations.
conditioning, and a multi-channel analyzer for binning the
NOTE 1—Better performance is expected if the Pb mass fraction of the
pulses according to X-ray energy.
Pb containing calibration standard is within the upper half of the scope
7.1.5 Detector Aperture—an aperture in the beam path
range (see Section 1).
between the sample and the detector to limit the field of view
8.6 Paint Layer Mode Calibration Standards—A minimum
of the detector.
of four standards are needed for calibration (see Note 3). Two
standards shall be scattering standards, and the other two shall
7.2 The following spectrometer features and accessories are
be Pb containing paint layer-on-substrate standards. Refer to
optional:
manufacturer’s recommendations.
7.2.1 Beam Shutter—used to select a monochromatic beam
8.6.1 Scattering Standards—At least two scattering stan-
or select a combination of monochromatic beams.
dards are necessary due to the overlap of Compton and
7.2.2 Drift Correction Monitors—due to instability of the
Rayleigh scattering of the low energy beam. One scattering
measurement system, the sensitivity and background of the
standard shall have a known density, thickness, and composi-
spectrometer may drift with time. Drift correction monitors
tion. The other scattering standard shall be a thin paint layer,
may be used to compensate for this drift. The optimum drift
with a known mass per unit area, mounted on a thin polyester
correction monitor samples are permanent materials that are
film. An example of the polyester film is film used for liquid
stable with repeated exposure to X-rays.
cells having a thickness of 3.7 µm or similar.
8.6.2 Paint Layer Standards—At least two Pb-containing
7.3 Discussion—the data acquisition has two modes, one for
paint layer standards each with differing paint layer thicknesses
homogenous materials and one for paint layers. The uncoated
and known Pb mass fraction are required.
mode only requires one monochromatic beam for the excitation
of the Pb L shell. The paint layer mode requires a second and
NOTE 2—Better performance is expected if the Pb mass fraction of the
lower energy monochromatic beam with less penetration of the two Pb containing paint layer standards are within the upper half of the
scope range (see Section 1).
sample to determine paint surface information and the Pb mass
NOTE 3—Additional calibration standards may be used for improved
fraction in the paint layer.
accuracy.
Reagent Chemicals, American Chemical Society Specifications, American
The sole source of supply of the apparatus known to the committee at this time Chemical Society, Washington, D.C. For suggestions on the testing of reagents not
is X-Ray Optical Systems, Inc., 15 Tech Valley Drive, East Greenbush, N
...
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.
´1
Designation: F2853 − 10 F2853 − 10 (Reapproved 2015)
Standard Test Method for
Determination of Lead in Paint Layers and Similar Coatings
or in Substrates and Homogenous Materials by Energy
Dispersive X-Ray Fluorescence Spectrometry Using Multiple
Monochromatic Excitation Beams
This standard is issued under the fixed designation F2853; 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.
ε NOTE—Section 7.1.3 was changed editorially from “.≥ than 250 eV.” to correctly read “.equal to or better than 250
eV.” in July 2011.
1. Scope
1.1 This test method uses energy dispersive X-ray fluorescence (EDXRF) spectrometry for detection and quantification of lead
(Pb) in paint layers, similar coatings, or substrates and homogenous materials. The following material types were tested in the
interlaboratory study for this standard test method: ABS plastic, polyethylene, polypropylene, PVC, glass, zinc alloy, wood, and
fabric.
1.2 This technique may also be commonly referred to as High Definition X-ray Fluorescence (HDXRF) or Multiple
Monochromatic Beam EDXRF (MMB-EDXRF).
1.3 This test method is applicable for the products and materials described in 1.1 for a Pb mass fraction range of 14 to 1200
mg/kg for uncoated samples and 30 to 450 mg/kg for coated samples, as specified in Table 1 and determined by an interlaboratory
study using representative samples
1.4 Ensure that the analysis area of the sample is visually uniform in appearance and at least as large as the X-ray excitation
beam at the point of sample excitation.
1.5 For coating analysis, this test method is limited to paint and similar coatings. Metallic coatings are not covered by this test
method.
1.6 X-ray Nomenclature—This standard names X-ray lines using the IUPAC convention with the Siegbahn convention in
parentheses.
1.7 There are no known ISO equivalent methods to this standard.
1.8 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.9 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.
2. Referenced Documents
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
This test method is under the jurisdiction of ASTM Committee F40 on Declarable Substances in Materials and is the direct responsibility of Subcommittee F40.01 on
Test Methods.
Current edition approved July 1, 2010Oct. 1, 2015. Published July 2010October 2015. DOI:10.1520/F2853–10ε01. Originally approved in 2010. Last previous edition
ɛ1
approved in 2010 as F2853-10 . DOI:10.1520/F2853–10R15.
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
F2853 − 10 (2015)
TABLE 1 Mass Fraction Ranges for Various Sample Types
Sample Type Homogenous Material Lead (Pb) Mass
or Substrate Type Fraction
Range, mg/kg
Uncoated Non-PVC Plastic, 14–1200
Glass or Ceramic
Uncoated Metal 66–600
Uncoated PVC 376–1150
Paint Layer Plastic or Metal 30–450
Paint Layer Fabric 79–200
Paint Layer Wood 58
F2576 Terminology Relating to Declarable Substances in Materials
3. Terminology
3.1 Definitions—Definitions of terms applying to XRF, plastics and declarable substances appear in Terminology D883, E135,
and F2576.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 Compton scattering—the inelastic scattering of an X-ray photon through its interaction with the bound electrons of an
atom. This process is also referred to as incoherent scattering.
3.2.2 fundamental parameters (FP) model—a model for calibration of X-ray fluorescence response, including the correction of
matrix effects, based on the theory describing the physical processes of the interactions of X-rays with matter.
3.2.3 homogenous material—materials are considered homogenous when the elemental composition as determined by the
technique in this test method is independent with respect to the measured location on the specimen and among separate specimens
prepared from the same material.
3.2.4 low energy monochromatic beam—a focused monochromatic beam having its selected photon energy between 3 and 9
keV.
3.2.5 medium energy monochromatic beam—a focused monochromatic beam having its selected photon energy between 15 and
23 keV.
3.2.6 monochromatic beam—an incident monochromatic beam on a sample having a selected photon energy with a narrow
energy bandwidth relative to the selected energy. Method precision is achieved with a monochromatic beam having an energy
bandwidth (Full Width Half Maximum) less than 61.5 % relative to the selected energy and containing more than 98 % flux of
the spectrum of the excitation beam which is incident on the sample.
3.2.7 multiple monochromatic excitation beams—two or more monochromatic beams.
3.2.8 paint layer—a single paint layer or other similar surface-coating material on a substrate.
3.2.9 Rayleigh scattering—the elastic scattering of an X-ray photon through its interaction with the bound electrons of an atom.
This process is also referred to as coherent scattering.
3.2.10 substrate—the material beneath a paint layer. The substrate may or may not be homogenous.
3.3 Acronyms:
3.3.1 EDXRF—energy dispersive X-ray fluorescence
3.3.2 FP—fundamental parameters
3.3.3 HDXRF—high definition X-ray fluorescence
3.3.4 MMB—multiple monochromatic beams
4. Summary of Test Method
4.1 The relevant samples include paint layers, their substrates, and homogenous materials.
4.2 This technique uses one or more monochromatic excitation beams to separately quantify the Pb mass fractions in paint
layers and substrates, and homogenous materials. The area of the sample to be analyzed is placed against an X-ray aperture.
Depending on the data acquisition mode (see 13.1 and 13.2), one or more monochromatic X-ray beams are focused on the sample.
The appropriate region of the fluorescence spectrum is processed by an FP method to obtain the analysis result, that is, the Pb mass
fraction in the sample.
4.3 The apparatus is calibrated for each data acquisition mode. The calibration may be performed by the manufacturer or by
the user.
F2853 − 10 (2015)
5. Significance and Use
5.1 This test method may be used for quantitative determinations of Pb in painted and unpainted articles such as toys, children’s
products, and other consumer products. Typical test time for quantification of Pb in homogenous samples is 1 to 3 min; and typical
test time for quantification of Pb in paint is 4 to 8 min.
6. Interferences
6.1 Spectral Interference—Spectral interferences result from spectral overlaps among the X-ray lines that remain unresolved
due to the limited energy resolution of the detector. For instance, the arsenic (As) K-L (Kα ) peak directly overlaps the Pb
2,3 1,2
L -M (Lα ) peak. The arsenic-Pb interference may be minimized by a de-convolution algorithm, but the precision of the Pb
3 4,5 1,2
analysis may be affected. If the presence of arsenic is suspected, the user may further investigate the arsenic interference.
Interactions of photons and electrons inside the detector result in additional peaks in the spectrum known as escape peaks and sum
peaks. These peaks can overlap with X-ray lines of interest, for example, the sum peak of iron (Fe) K-L (Kα ) can overlap with
2,3 1,2
the Pb L -M (Lβ ) peak.
2 4 1
6.2 Substrate Interference—The presence of Pb in a substrate can interfere with the determination of the Pb mass fraction of
the paint layer. If the Pb signal of the paint layer and substrate composite is dominated by the contribution from the substrate, the
uncertainty of the FP analysis can be significant and the Pb measurement for the paint layer will exhibit a positive bias and may
not meet the precision statement of this test method. See Note 8 in Section 16.
6.3 Matrix Effect—Matrix effects, also called interelement effects, exist among all elements as the result of absorption of
fluorescent X-rays (secondary X-rays) by atoms in the specimen. Absorption reduces the apparent sensitivity for the element. In
contrast, the atom that absorbs the X-rays may in turn emit a fluorescent X-ray, increasing apparent sensitivity for the second
element. Mathematical methods may be used to compensate for matrix effects. A number of mathematical correction procedures
are commonly utilized including full FP treatments and mathematical models based on influence coefficient algorithms.
7. Apparatus
7.1 EDXRF Spectrometer —designed for X-ray fluorescence analysis using multiple monochromatic excitation beams with an
energy dispersive detector. Any EDXRF spectrometer may be used if it is capable of meeting method precision and its design
incorporates the following features:
7.1.1 Source of X-ray Excitation—typically an X-ray tube, capable of exciting the Pb L lines in a sample. For instance, an X-ray
tube with a zirconium, molybdenum, rhodium, palladium, or silver target can be used.
7.1.2 X-ray Optics—X-ray optical elements capable of accepting X-rays from a tube and directing monochromatic beams on
the sample. Two or more X-ray optical elements are necessary to provide multiple monochromatic beams. At least one optical
element provides a low energy monochromatic beam, and at least one optical element provides a medium energy monochromatic
beam.
7.1.3 X-Ray Detector—with energy resolution equal to or better than 250 eV full width at half maximum of the manganese (Mn)
K-L (Kα ) line.
2,3 1,2
7.1.4 Digital Pulse Processor and Multi-channel Analyzer—a digital pulse processor for pulse shaping and conditioning, and
a multi-channel analyzer for binning the pulses according to X-ray energy.
7.1.5 Detector Aperture—an aperture in the beam path between the sample and the detector to limit the field of view of the
detector.
7.2 The following spectrometer features and accessories are optional:
7.2.1 Beam Shutter—used to select a monochromatic beam or select a combination of monochromatic beams.
7.2.2 Drift Correction Monitors—due to instability of the measurement system, the sensitivity and background of the
spectrometer may drift with time. Drift correction monitors may be used to compensate for this drift. The optimum drift correction
monitor samples are permanent materials that are stable with repeated exposure to X-rays.
7.3 Discussion—the data acquisition has two modes, one for homogenous materials and one for paint layers. The uncoated mode
only requires one monochromatic beam for the excitation of the Pb L shell. The paint layer mode requires a second and lower
energy monochromatic beam with less penetration of the sample to determine paint surface information and the Pb mass fraction
in the paint layer.
The sole source of supply of the apparatus known to the committee at this time is X-Ray Optical Systems, Inc., 15 Tech Valley Drive, East Greenbush, NY 12061. 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.
F2853 − 10 (2015)
8. Reagents and Materials
8.1 Purity of Reagents —Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents 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. Reagents used include materials used for cleaning of samples.
8.2 Reagents:
8.2.1 Isopropanol or ethanol,
8.2.2 Nitric acid (HNO ),
8.2.3 Hexane, and
8.2.4 Deionized water (H O).
8.3 Gloves—Disposable gloves are recommended for handling reference materials and other samples to minimize contamina-
tion.
8.4 Appropriate personal protective equipment for the handling of reagents.
8.5 Uncoated Mode Calibration Standards—At least two standards are required for calibration, one a scattering standard, and
the other a Pb-containing homogenous material (see Note 3). The scattering standard shall have a known density, thickness, and
composition. The other standard shall be a Pb containing homogenous standard with a known Pb mass fraction. Refer to
manufacturer’s recommendations.
NOTE 1—Better performance is expected if the Pb mass fraction of the Pb containing calibration standard is within the upper half of the scope range
(see Section 1).
8.6 Paint Layer Mode Calibration Standards—A minimum of four standards are needed for calibration (see Note 3). Two
standards shall be scattering standards, and the other two shall be Pb containing paint layer-on-substrate standards. Refer to
manufacturer’s recommendations.
8.6.1 Scattering Standards—At least two scattering standards are necessary due to the overlap of Compton and Rayleigh
scattering of the low energy beam. One scattering standard shall have a known density, thickness, and composition. The other
scattering standard shall be a thin paint layer, with a known mass per unit area, mounted on a thin polyester film. An example of
the polyester film is film used for liquid cells having a thickness of 3.7 μm or similar.
8.6.2 Paint Layer Standards—At least two Pb-containing paint layer standards each with differing paint layer thicknesses and
known Pb mass fraction are required.
NOTE 2—B
...
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