ASTM D5381-93(2003)
(Guide)Standard Guide for X-Ray Fluorescence (XRF) Spectroscopy of Pigments and Extenders
Standard Guide for X-Ray Fluorescence (XRF) Spectroscopy of Pigments and Extenders
SIGNIFICANCE AND USE
The identification of pigments in a sample of liquid paint or paint film is often important for regulatory purposes. Many inorganic pigments or extenders utilized in past paint formulation are now regulated by federal, state, or municipal health authorities. XRF is one of the more common and convenient methods employed to characterize the pigment composition of a paint formulation.
XRF techniques, in general, do not provide the ability to identify the chemical nature of organic pigments. There are instances where XRF techniques, used in tandem with other analytical methods, such as solid state Carbon 13 Nuclear Magnetic Resonance (C-13 NMR), can identify the organic pigments utilized in coatings. However, XRF provides only an elemental sketch of the inorganic pigmentation. The chemical composition of the pigments is inferred by the analyst from the samples, color, elemental information, and common sense. Small impurities are often found in pigments, so the relative XRF intensities also serve to guide the analyst in proposing the probable pigment present.
SCOPE
1.1 This guide covers the general considerations for proper use of X-ray fluorescence (XRF) spectroscopy. Because many differences exist between XRF instruments, no detailed operating instructions are provided. The analyst should follow the instructions provided by the manufacturer for his instrument.
1.2 The analyst is encouraged to consult the chemical literature, various trade journals, pigment supplier publications, etc., as well as the instrument manuals from the manufacturer.
1.3 XRF is commonly employed to determine the elements present in inorganic pigments and extenders, often in concert with other analysis techniques. Organic pigments cannot normally be identified solely by XRF. On occasion, organic pigments contain heavier elements that can distinguish between major classes of these pigments or may serve to distinguish one of the two distinct pigments. However, the analyst should be wary of a qualitative pigment identification solely by XRF technique.
1.4 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. For specific hazard information see Section 3 on Radiation Concerns.
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Designation:D5381–93(Reapproved2003)
Standard Guide for
X-Ray Fluorescence (XRF) Spectroscopy of Pigments and
Extenders
This standard is issued under the fixed designation D 5381; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Radiation Concerns
1.1 This guide covers the general considerations for proper 3.1 Modern XRF instrumentation has been designed to
use of X-ray fluorescence (XRF) spectroscopy. Because many minimize exposure of laboratory personnel to X-ray radiation
differences exist between XRF instruments, no detailed oper- during instrument use. However, most laboratories use dosim-
ating instructions are provided. The analyst should follow the etry to monitor personnel who are normally present around the
instructions provided by the manufacturer for his instrument. XRF instrument while it is in operation. Such dosimetry
1.2 The analyst is encouraged to consult the chemical devices are normally read on a monthly basis.
literature, various trade journals, pigment supplier publica- 3.2 After XRF instrument maintenance (especially where
tions, etc., as well as the instrument manuals from the the X-ray tube, detector, or shielding has been moved or
manufacturer. replaced), an X-ray survey of all areas around the instrument
1.3 XRF is commonly employed to determine the elements (while in operation) is recommended. The results of such a
present in inorganic pigments and extenders, often in concert survey should be documented and stored for future reference.
with other analysis techniques. Organic pigments cannot nor- 3.3 It is recommended that the laboratory check its compli-
mally be identified solely by XRF. On occasion, organic ance with all applicable local, state, and federal requirements.
pigments contain heavier elements that can distinguish be- Many companies also have policies concerning use of X-ray
tween major classes of these pigments or may serve to equipment in their laboratories.
distinguish one of the two distinct pigments. However, the 3.4 It is common laboratory practice to post placards on all
analyst should be wary of a qualitative pigment identification entrances to the laboratories containing X-ray equipment that
solely by XRF technique. indicate its presence.
1.4 This standard does not purport to address all of the
4. Summary of the Guide
safety concerns, if any, associated with its use. It is the
4.1 A general guide for qualitative elemental analysis of
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- paint and paint components is provided. Knowledge of the
elements present in a sample can be used to infer the identity
bility of regulatory limitations prior to use. For specific hazard
information see Section 3 on Radiation Concerns. of pigments and extenders that may be present. The absence of
specific pigments and extenders can be proven by the absence
2. Referenced Documents
of their constituent elements. The presence or absence of toxic
2.1 ASTM Standards: elements can be demonstrated. Analysis consists of irradiating
D 3925 Practice for Sampling Liquid Paints and Related the test specimen with monochromatic X-rays and determining
Pigmented Coatings the energy or wavelength of the fluorescent X-ray emitted by
the specimen. Since different elements emit X-rays with
different energy and wavelength under these conditions, the
This guide is under the jurisdiction of ASTM Committee D01 on Paint and
element content of the specimen can be determined by exami-
Related Coatings, Materials, and Applications and is the direct responsibility of
nation of the X-ray spectrum. The spectrum is recorded either
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Dec. 1, 2003. Published December 2003. Originally
on chart paper or magnetic media. Identification of the con-
approved in 1993. Last previous edition approved in 1993 as D 5381 – 93 (1998).
stituent elements is accomplished by comparing the peaks in
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
thespectrumwithknowntabulateddata,usingeithermanualor
contact ASTM Customer Service at service@astm.org. ForAnnual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on computer-assisted procedures.
the ASTM website.
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D5381–93 (2003)
5. Significance and Use 7.1.2 Solid samples may be in powder form, supported
tablets(briquettes),orpaintchips.Ifpaintchipscontainseveral
5.1 The identification of pigments in a sample of liquid
distinct paint l
...
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