Standard Guide for X-Ray Fluorescence (XRF) Spectroscopy of Pigments and Extenders

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 problems, 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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Historical
Publication Date
31-Dec-1992
Current Stage
Ref Project

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ASTM D5381-93(1998) - Standard Guide for X-Ray Fluorescence (XRF) Spectroscopy of Pigments and Extenders
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5381 – 93 (Reapproved 1998)
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 etry to monitor personnel who are normally present around the
XRF instrument while it is in operation. Such dosimetry
1.1 This guide covers the general considerations for proper
devices are normally read on a monthly basis.
use of X-ray fluorescence (XRF) spectroscopy. Because many
3.2 After XRF instrument maintenance (especially where
differences exist between XRF instruments, no detailed oper-
the X-ray tube, detector, or shielding has been moved or
ating instructions are provided. The analyst should follow the
replaced), an X-ray survey of all areas around the instrument
instructions provided by the manufacturer for his instrument.
(while in operation) is recommended. The results of such a
1.2 The analyst is encouraged to consult the chemical
survey should be documented and stored for future reference.
literature, various trade journals, pigment supplier publica-
3.3 It is recommended that the laboratory check its compli-
tions, etc., as well as the instrument manuals from the
ance with all applicable local, state, and federal requirements.
manufacturer.
Many companies also have policies concerning use of X-ray
1.3 XRF is commonly employed to determine the elements
equipment in their laboratories.
present in inorganic pigments and extenders, often in concert
3.4 It is common laboratory practice to post placards on all
with other analysis techniques. Organic pigments cannot nor-
entrances to the laboratories containing X-ray equipment that
mally be identified solely by XRF. On occasion, organic
indicate its presence.
pigments contain heavier elements that can distinguish be-
tween major classes of these pigments or may serve to
4. Summary of the Guide
distinguish one of the two distinct pigments. However, the
4.1 A general guide for qualitative elemental analysis of
analyst should be wary of a qualitative pigment identification
paint and paint components is provided. Knowledge of the
solely by XRF technique.
elements present in a sample can be used to infer the identity
1.4 This standard does not purport to address all of the
of pigments and extenders that may be present. The absence of
safety concerns, if any, associated with its use. It is the
specific pigments and extenders can be proven by the absence
responsibility of the user of this standard to establish appro-
of their constituent elements. The presence or absence of toxic
priate safety and health practices and determine the applica-
elements can be demonstrated. Analysis consists of irradiating
bility of regulatory limitations prior to use. For specific hazard
the test specimen with monochromatic X-rays and determining
information see Section 3 on Radiation Concerns.
the energy or wavelength of the fluorescent X-ray emitted by
2. Referenced Documents the specimen. Since different elements emit X-rays with
different energy and wavelength under these conditions, the
2.1 ASTM Standards:
element content of the specimen can be determined by exami-
D 3925 Practice for Sampling Liquid Paints and Related
2 nation of the X-ray spectrum. The spectrum is recorded either
Pigmented Coatings
on chart paper or magnetic media. Identification of the con-
3. Radiation Concerns stituent elements is accomplished by comparing the peaks in
thespectrumwithknowntabulateddata,usingeithermanualor
3.1 Modern XRF instrumentation has been designed to
computer-assisted procedures.
minimize exposure of laboratory personnel to X-ray radiation
during instrument use. However, most laboratories use dosim-
5. Significance and Use
5.1 The identification of pigments in a sample of liquid
This guide is under the jurisdiction of ASTM Committee D-1 on Paint and
paint or paint film is often important for regulatory purposes.
Related Coatings, Materials, and Applications and is the direct responsibility of
Many inorganic pigments or extenders utilized in past paint
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
formulation are now regulated by federal, state, or municipal
Current edition approved April 15, 1993. Published June 1993.
health authorities. XRF is one of the more common and
Annual Book of ASTM Standards, Vol 06.01.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org)
...

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