ASTM D5381-93(2014)

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

SIGNIFICANCE AND USE
5.1 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.  
5.2 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.

General Information

• Status: Historical
• Publication Date: 30-Jun-2014
• ICS: 87.060.10 - Pigments and extenders
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

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: D5381 − 93 (Reapproved 2014)
Standard Guide for
X-Ray Fluorescence (XRF) Spectroscopy of Pigments and
1
Extenders
This standard is issued under the fixed designation D5381; 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 3. Radiation Concerns
3.1 Modern XRF instrumentation has been designed to
1.1 This guide covers the general considerations for proper
minimize exposure of laboratory personnel to X-ray radiation
use of X-ray fluorescence (XRF) spectroscopy. Because many
during instrument use. However, most laboratories use dosim-
differences exist between XRF instruments, no detailed oper-
etry to monitor personnel who are normally present around the
ating instructions are provided. The analyst should follow the
XRF instrument while it is in operation. Such dosimetry
instructions provided by the manufacturer for his instrument.
devices are normally read on a monthly basis.
1.2 The analyst is encouraged to consult the chemical
3.2 After XRF instrument maintenance (especially where
literature, various trade journals, pigment supplier
the X-ray tube, detector, or shielding has been moved or
publications, etc., as well as the instrument manuals from the
replaced), an X-ray survey of all areas around the instrument
manufacturer.
(while in operation) is recommended. The results of such a
1.3 XRF is commonly employed to determine the elements
survey should be documented and stored for future reference.
present in inorganic pigments and extenders, often in concert
3.3 It is recommended that the laboratory check its compli-
with other analysis techniques. Organic pigments cannot nor-
ance with all applicable local, state, and federal requirements.
mally be identified solely by XRF. On occasion, organic
Many companies also have policies concerning use of X-ray
pigments contain heavier elements that can distinguish be-
equipment in their laboratories.
tween major classes of these pigments or may serve to
3.4 It is common laboratory practice to post placards on all
distinguish one of the two distinct pigments. However, the
entrances to the laboratories containing X-ray equipment that
analyst should be wary of a qualitative pigment identification
indicate its presence.
solely by XRF technique.
4. Summary of the Guide
1.4 This standard does not purport to address all of the
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-
paint and paint components is provided. Knowledge of the
priate safety and health practices and determine the applica-
elements present in a sample can be used to infer the identity
bility of regulatory limitations prior to use. For specific hazard
of pigments and extenders that may be present. The absence of
information see Section 3 on Radiation Concerns.
specific pigments and extenders can be proven by the absence
of their constituent elements. The presence or absence of toxic
2. Referenced Documents
elements can be demonstrated. Analysis consists of irradiating
2 the test specimen with monochromatic X-rays and determining
2.1 ASTM Standards:
the energy or wavelength of the fluorescent X-ray emitted by
D3925 Practice for Sampling Liquid Paints and Related
the specimen. Since different elements emit X-rays with
Pigmented Coatings
different energy and wavelength under these conditions, the
element content of the specimen can be determined by exami-
nation of the X-ray spectrum. The spectrum is recorded either
1
This guide is under the jurisdiction of ASTM Committee D01 on Paint and
on chart paper or magnetic media. Identification of the con-
Related Coatings, Materials, and Applications and is the direct responsibility of
stituent elements is accomplished by comparing the peaks in
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
thespectrumwithknowntabulateddata,usingeithermanualor
Current edition approved July 1, 2014. Published July 2014. Originally approved
in 1993. Last previous edition approved in 2009 as D5381 – 93 (2009). DOI:
computer-assisted procedures.
10.1520/D5381-93R014.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5. Significance and Use
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1 The identification of pigments in a sample of liquid
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. paint or paint film is often important for regulatory purposes.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box
...

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: D5381 − 93 (Reapproved 2009) D5381 − 93 (Reapproved 2014)
Standard Guide for
X-Ray Fluorescence (XRF) Spectroscopy of Pigments and
1
Extenders
This standard is issued under the fixed designation D5381; 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
1.1 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D3925 Practice for Sampling Liquid Paints and Related Pigmented Coatings
3. Radiation Concerns
3.1 Modern XRF instrumentation has been designed to minimize exposure of laboratory personnel to X-ray radiation during
instrument use. However, most laboratories use dosimetry to monitor personnel who are normally present around the XRF
instrument while it is in operation. Such dosimetry devices are normally read on a monthly basis.
3.2 After XRF instrument maintenance (especially where the X-ray tube, detector, or shielding has been moved or replaced),
an X-ray survey of all areas around the instrument (while in operation) is recommended. The results of such a survey should be
documented and stored for future reference.
3.3 It is recommended that the laboratory check its compliance with all applicable local, state, and federal requirements. Many
companies also have policies concerning use of X-ray equipment in their laboratories.
3.4 It is common laboratory practice to post placards on all entrances to the laboratories containing X-ray equipment that
indicate its presence.
4. Summary of the Guide
4.1 A general guide for qualitative elemental analysis of paint and paint components is provided. Knowledge of the elements
present in a sample can be used to infer the identity of pigments and extenders that may be present. The absence of specific
pigments and extenders can be proven by the absence of their constituent elements. The presence or absence of toxic elements can
be demonstrated. Analysis consists of irradiating the test specimen with monochromatic X-rays and determining the energy or
1
This guide 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 Feb. 1, 2009July 1, 2014. Published February 2009July 2014. Originally approved in 1993. Last previous edition approved in 200332009 as
D5381 – 93 (2003).(2009). DOI: 10.1520/D5381-93R09.10.1520/D5381-93R014.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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
1

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D5381 − 93 (2014)
wavelength of the fluorescent X-ray emitted by the specimen. Since different elements emit X-rays with different energy and
wavelength under these
...