ASTM F2853-10
(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
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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Designation:F2853–10
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 priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.1 This test method uses energy dispersive X-ray fluores-
cence (EDXRF) spectrometry for detection and quantification
2. Referenced Documents
of lead (Pb) in paint layers, similar coatings, or substrates and
2.1 ASTM Standards:
homogenous materials. The following material types were
D883 Terminology Relating to Plastics
testedintheinterlaboratorystudyforthisstandardtestmethod:
D6299 Practice for Applying Statistical Quality Assurance
ABS plastic, polyethylene, polypropylene, PVC, glass, zinc
and Control Charting Techniques to Evaluate Analytical
alloy, wood, and fabric.
Measurement System Performance
1.2 This technique may also be commonly referred to as
E135 Terminology Relating to Analytical Chemistry for
High Definition X-ray Fluorescence (HDXRF) or Multiple
Metals, Ores, and Related Materials
Monochromatic Beam EDXRF (MMB-EDXRF).
E691 Practice for Conducting an Interlaboratory Study to
1.3 This test method is applicable for the products and
Determine the Precision of a Test Method
materials described in 1.1 for a Pb mass fraction range of 14 to
F2576 Terminology Relating to Declarable Substances in
1200 mg/kg for uncoated samples and 30 to 450 mg/kg for
Materials
coated samples, as specified in Table 1 and determined by an
interlaboratory study using representative samples
3. Terminology
1.4 Ensure that the analysis area of the sample is visually
3.1 Definitions—Definitions of terms applying to XRF,
uniform in appearance and at least as large as the X-ray
plastics and declarable substances appear in Terminology
excitation beam at the point of sample excitation.
D883, E135, and F2576.
1.5 For coating analysis, this test method is limited to paint
3.2 Definitions of Terms Specific to This Standard:
and similar coatings. Metallic coatings are not covered by this
3.2.1 Compton scattering—the inelastic scattering of an
test method.
X-ray photon through its interaction with the bound electrons
1.6 X-ray Nomenclature—This standard names X-ray lines
of an atom. This process is also referred to as incoherent
using the IUPAC convention with the Siegbahn convention in
scattering.
parentheses.
3.2.2 fundamental parameters (FP) model—a model for
1.7 There are no known ISO equivalent methods to this
calibration of X-ray fluorescence response, including the cor-
standard.
rection of matrix effects, based on the theory describing the
1.8 The values stated in SI units are to be regarded as
physical processes of the interactions of X-rays with matter.
standard. No other units of measurement are included in this
3.2.3 homogenous material—materials are considered ho-
standard.
mogenous when the elemental composition as determined by
1.9 This standard does not purport to address all of the
the technique in this test method is independent with respect to
safety concerns, if any, associated with its use. It is the
the measured location on the specimen and among separate
responsibility of the user of this standard to establish appro-
specimens prepared from the same material.
This test method is under the jurisdiction of ASTM Committee F40 on
Declarable Substances in Materials and is the direct responsibility of Subcommittee For referenced ASTM standards, visit the ASTM website, www.astm.org, or
F40.01 on Test Methods. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved July 1, 2010. Published July 2010. DOI:10.1520/ Standards volume information, refer to the standard’s Document Summary page on
F2853–10. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F2853–10
TABLE 1 Mass Fraction Ranges for Various Sample Types
Sample Type Homogenous Material Lead (Pb) Mass Fraction
or Substrate Type 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
3.2.4 low energy monochromatic beam—a focused mono- 5. Significance and Use
chromatic beam having its selected photon energy between 3
5.1 This test method may be used for quantitative determi-
and 9 keV.
nations of Pb in painted and unpainted articles such as toys,
3.2.5 medium energy monochromatic beam—a focused
children’s products, and other consumer products. Typical test
monochromatic beam having its selected photon energy be-
time for quantification of Pb in homogenous samples is 1 to 3
tween 15 and 23 keV.
min; and typical test time for quantification of Pb in paint is 4
3.2.6 monochromatic beam—an incident monochromatic
to 8 min.
beam on a sample having a selected photon energy with a
narrow energy bandwidth relative to the selected energy.
6. Interferences
Method precision is achieved with a monochromatic beam
having an energy bandwidth (Full Width Half Maximum) less
6.1 Spectral Interference—Spectral interferences result
than 61.5 % relative to the selected energy and containing
from spectral overlaps among the X-ray lines that remain
more than 98 % flux of the spectrum of the excitation beam
unresolved due to the limited energy resolution of the detector.
which is incident on the sample.
For instance, the arsenic (As) K-L (Ka ) peak directly
2,3 1,2
3.2.7 multiple monochromatic excitation beams—two or
overlaps the Pb L -M (La ) peak. The arsenic-Pb interfer-
3 4,5 1,2
more monochromatic beams.
ence may be minimized by a de-convolution algorithm, but the
3.2.8 paint layer—a single paint layer or other similar
precision of the Pb analysis may be affected. If the presence of
surface-coating material on a substrate.
arsenic is suspected, the user may further investigate the
3.2.9 Rayleigh scattering—theelasticscatteringofanX-ray
arsenic interference. Interactions of photons and electrons
photon through its interaction with the bound electrons of an
inside the detector result in additional peaks in the spectrum
atom. This process is also referred to as coherent scattering.
known as escape peaks and sum peaks. These peaks can
3.2.10 substrate—the material beneath a paint layer. The
overlap with X-ray lines of interest, for example, the sum peak
substrate may or may not be homogenous.
of iron (Fe) K-L (Ka ) can overlap with the Pb L -M (Lb )
2,3 1,2 2 4 1
3.3 Acronyms:
peak.
3.3.1 EDXRF—energy dispersive X-ray fluorescence
6.2 Substrate Interference—The presence of Pb in a sub-
3.3.2 FP—fundamental parameters
strate can interfere with the determination of the Pb mass
3.3.3 HDXRF—high definition X-ray fluorescence
fractionofthepaintlayer.IfthePbsignalofthepaintlayerand
3.3.4 MMB—multiple monochromatic beams
substrate composite is dominated by the contribution from the
substrate, the uncertainty of the FP analysis can be significant
4. Summary of Test Method
and the Pb measurement for the paint layer will exhibit a
4.1 The relevant samples include paint layers, their sub-
positive bias and may not meet the precision statement of this
strates, and homogenous materials.
test method. See Note 8 in Section 16.
4.2 This technique uses one or more monochromatic exci-
6.3 Matrix Effect—Matrix effects, also called interelement
tation beams to separately quantify the Pb mass fractions in
effects, exist among all elements as the result of absorption of
paint layers and substrates, and homogenous materials. The
fluorescent X-rays (secondary X-rays) by atoms in the speci-
area of the sample to be analyzed is placed against an X-ray
men. Absorption reduces the apparent sensitivity for the
aperture.Dependingonthedataacquisitionmode(see13.1and
element. In contrast, the atom that absorbs the X-rays may in
13.2),oneormoremonochromaticX-raybeamsarefocusedon
turn emit a fluorescent X-ray, increasing apparent sensitivity
the sample. The appropriate region of the fluorescence spec-
for the second element. Mathematical methods may be used to
trumisprocessedbyanFPmethodtoobtaintheanalysisresult,
compensate for matrix effects. A number of mathematical
that is, the Pb mass fraction in the sample.
4.3 The apparatus is calibrated for each data acquisition correction procedures are commonly utilized including full FP
treatments and mathematical models based on influence coef-
mode. The calibration may be performed by the manufacturer
or by the user. ficient algorithms.
F2853–10
7. Apparatus all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
7.1 EDXRF Spectrometer —designed for X-ray fluores-
such specifications are available. Other grades may be used,
cenceanalysisusingmultiplemonochromaticexcitationbeams
provided it is first ascertained that the reagent is of sufficiently
with an energy dispersive detector. Any EDXRF spectrometer
high purity to permit its use without lessening the accuracy of
may be used if it is capable of meeting method precision and
the determination. Reagents used include materials used for
its design incorporates the following features:
cleaning of samples.
7.1.1 Source of X-ray Excitation—typically an X-ray tube,
8.2 Reagents:
capable of exciting the Pb Llines in a sample. For instance, an
X-ray tube with a zirconium, molybdenum, rhodium, palla- 8.2.1 Isopropanol or ethanol,
dium, or silver target can be used. 8.2.2 Nitric acid (HNO ),
7.1.2 X-ray Optics—X-ray optical elements capable of ac-
8.2.3 Hexane, and
cepting X-rays from a tube and directing monochromatic
8.2.4 Deionized water (H O).
beams on the sample. Two or more X-ray optical elements are
8.3 Gloves—Disposable gloves are recommended for han-
necessary to provide multiple monochromatic beams. At least
dling reference materials and other samples to minimize
one optical element provides a low energy monochromatic
contamination.
beam, and at least one optical element provides a medium
8.4 Appropriate personal protective equipment for the han-
energy monochromatic beam.
dling of reagents.
7.1.3 X-Ray Detector—withenergyresolution$250eVfull
8.5 Uncoated Mode Calibration Standards—At least two
width at half maximum of the manganese (Mn) K-L (Ka )
2,3 1,2
standardsarerequiredforcalibration,oneascatteringstandard,
line.
and the other a Pb-containing homogenous material (see Note
7.1.4 Digital Pulse Processor and Multi-channel
3). The scattering standard shall have a known density,
Analyzer—a digital pulse processor for pulse shaping and
thickness, and composition. The other standard shall be a Pb
conditioning, and a multi-channel analyzer for binning the
containing homogenous standard with a known Pb mass
pulses according to X-ray energy.
fraction. Refer to manufacturer’s recommendations.
7.1.5 Detector Aperture—an aperture in the beam path
between the sample and the detector to limit the field of view
NOTE 1—Better performance is expected if the Pb mass fraction of the
of the detector. Pb containing calibration standard is within the upper half of the scope
range (see Section 1).
7.2 The following spectrometer features and accessories are
optional:
8.6 Paint Layer Mode Calibration Standards—Aminimum
7.2.1 Beam Shutter—used to select a monochromatic beam
of four standards are needed for calibration (see Note 3). Two
or select a combination of monochromatic beams.
standards shall be scattering standards, and the other two shall
7.2.2 Drift Correction Monitors—due to instability of the
be Pb containing paint layer-on-substrate standards. Refer to
measurement system, the sensitivity and background of the
manufacturer’s recommendations.
spectrometer may drift with time. Drift correction monitors
8.6.1 Scattering Standards—At least two scattering stan-
may be used to compensate for this drift. The optimum drift
dards are necessary due to the overlap of Compton and
correction monitor samples are permanent materials that are
Rayleigh scattering of the low energy beam. One scattering
stable with repeated exposure to X-rays.
standard shall have a known density, thickness, and composi-
7.3 Discussion—the data acquisition has two modes, one
tion. The other scattering standard shall be a thin paint layer,
for homogenous materials and one for paint layers. The
with a known mass per unit area, mounted on a thin polyester
uncoated mode only requires one monochromatic beam for the
film. An example of the polyester film is film used for liquid
excitation of the Pb L shell. The paint layer mode requires a
cells having a thickness of 3.7 µm or similar.
second and lower energy monochromatic beam with less
8.6.2 Paint Layer Standards—At least two Pb-containing
penetration of the sample to determine paint surface informa-
paintlayerstandardseachwithdifferingpaintlayerthicknesses
tion and the Pb mass fraction in the paint layer.
and known Pb mass fraction are required.
8. Reagents and Materials
NOTE 2—Better performance is expected if the Pb mass fraction of the
8.1 Purity of Reagents —Reagent grade chemicals shall be two Pb containing paint layer standards are within the upper half of the
scope range (see Section 1).
used in all tests. Unless otherwise indicated, it is intended that
NOTE 3—Additional calibration standards may be used for improved
accuracy.
The sole source of supply of the apparatus known to the committee at this time
8.7 Reference Materials:
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
8.7.1 Homogeneous reference materials are available from
International Headquarters. Your comments will receive careful consideration at a
commercial sources. At the time of this publication, there are
meeting of the responsible technical committee, which you may attend.
4 no commercially available paint layer reference materials.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, D.C. For suggestions on the testing of reagents not 8.8 Quality Control Samples:
listed by the American Chemical Society, see Annular Standards for Laboratory
8.8.1 To ensure the quality of the results, quality con
...
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