ASTM D7639-10(2014)
(Test Method)Standard Test Method for Determination of Zirconium Treatment Weight or Thickness on Metal Substrates by X-Ray Fluorescence
Standard Test Method for Determination of Zirconium Treatment Weight or Thickness on Metal Substrates by X-Ray Fluorescence
SIGNIFICANCE AND USE
4.1 The procedure described in this test method is designed to provide a method by which the coating weight of zirconium treatments on metal substrates may be determined.
4.2 This test method is applicable for determination of the total coating weight and the zirconium coating weight of a zirconium-containing treatment.
SCOPE
1.1 This test method covers the use of X-ray fluorescence (XRF) spectrometry for the determination of the mass of zirconium (Zr) coating weight per unit area of metal substrates.
1.2 Coating treatments can also be expressed in units of linear thickness provided that the density of the coating is known, or provided that a calibration curve has been established for thickness determination using standards with treatment matching this of test specimens to be analyzed. For simplicity, the method will subsequently refer to the determination expressed as coating weight.
1.3 XRF is applicable for the determination of the coating weight as zirconium or total coating weight of a zirconium containing treatment, or both, on a variety of metal substrates.
1.4 The maximum measurable coating weight for a given coating is that weight beyond which the intensity of the characteristic X-ray radiation from the coating or the substrate is no longer sensitive to small changes in weight.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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: D7639 − 10 (Reapproved 2014)
Standard Test Method for
Determination of Zirconium Treatment Weight or Thickness
on Metal Substrates by X-Ray Fluorescence
This standard is issued under the fixed designation D7639; 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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method covers the use of X-ray fluorescence
(XRF) spectrometry for the determination of the mass of
3. Summary of Test Method
zirconium(Zr)coatingweightperunitareaofmetalsubstrates.
3.1 The test specimen is placed in the X-ray beam, and the
1.2 Coating treatments can also be expressed in units of
resultant peak intensity of the zirconium Ka line (at 0.0786 nm
linear thickness provided that the density of the coating is
or 15.747 keV) or the zirconium La line (at 0.606 nm or 2.042
known, or provided that a calibration curve has been estab-
keV) is measured. The intensity (in counts or counts per
lished for thickness determination using standards with treat-
second) is then compared to a previously prepared calibration
ment matching this of test specimens to be analyzed. For
curve or equation to obtain the coating weight of zirconium
simplicity, the method will subsequently refer to the determi- 2 2
treatment in mg/m or mg/ft (or µm or nm).
nation expressed as coating weight.
3.2 The exact relationship between the measured number of
1.3 XRF is applicable for the determination of the coating
counts and the corresponding coating weight (or coating
weight as zirconium or total coating weight of a zirconium
thickness) must be established for each individual combination
containing treatment, or both, on a variety of metal substrates.
of substrate and zirconium-containing treatment. Usually de-
1.4 The maximum measurable coating weight for a given termined by the treatment supplier, this relationship is estab-
coating is that weight beyond which the intensity of the lished by using primary standards having known amounts of
characteristic X-ray radiation from the coating or the substrate the same treatment applied to the same substrate composition
is no longer sensitive to small changes in weight. as the test specimens to be measured.
1.5 The values stated in SI units are to be regarded as
4. Significance and Use
standard. No other units of measurement are included in this
4.1 The procedure described in this test method is designed
standard.
to provide a method by which the coating weight of zirconium
1.6 This standard does not purport to address all of the
treatments on metal substrates may be determined.
safety concerns, if any, associated with its use. It is the
4.2 This test method is applicable for determination of the
responsibility of the user of this standard to establish appro-
total coating weight and the zirconium coating weight of a
priate safety and health practices and determine the applica-
zirconium-containing treatment.
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents
5.1 X-RayFluorescenceSpectrometer,capableofmeasuring
2.1 ASTM Standards:
the intensity of zirconium Ka or La line, and establish the
E177 Practice for Use of the Terms Precision and Bias in
relationship between peak intensity and coating weight. The
ASTM Test Methods
spectrometer’s design must include, as a minimum, the follow-
ing features:
This test method is under the jurisdiction of ASTM Committee D01 on Paint
5.1.1 SourceofX-RayExcitation,X-raytubewithexcitation
and Related Coatings, Materials, andApplications and is the direct responsibility of
above 2.55 keV if measuring the zirconium La line, or above
Subcommittee D01.53 on Coil Coated Metal.
18 keV if measuring the zirconium Ka line.
Current edition approved June 15, 2014. Published June 2014. Originally
5.1.2 X-Ray Detector, with high sensitivity and capable of
approved in 2010. Last previous edition approved in 2010 as D7639 – 10.
DOI:10.1520/D7639-10R14.
discriminating between zirconium La or Ka radiation and other
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
X-rays of higher or lower energies.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.1.2.1 In the case of wavelength dispersive X-ray fluores-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. cence(WDXRF),thiscanbeananalyzingcrystal(forexample,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7639 − 10 (2014)
fixed channel, goniometer) setup to detect the zirconium 6.7 The coated area of the test specimen should be larger
X-rays (La or Ka line). Germanium 111 has been found to be than the measured area.
acceptable for the Zirconium La line and LiF220 or LiF200 for
6.8 The calibration standards and test specimens should be
the zirconium Ka line.
measured over the X-ray port using the same rolling direction
5.1.2.2 In the case of energy dispersive X-ray fluorescence
of the metal. This is not necessary for instruments operating
(EDXRF), it can be a proportional counter, or a semiconductor
with a sample spinner.
such as a PIN diode or a silicon-drift detector.
5.1.3 Pulse-Height Analyzer, or other means of energy
7. Calibration Procedure
discrimination.
7.1 Set up the instrument calibration and operating param-
5.1.4 Optical Path, specified by manufacturer. A helium or
eters according to the chemical supplier and instrument manu-
vacuum path is recommended when measuring the zirconium
facturer’s recommendations.
La line in order to minimize the attenuation of the X-rays by
7.2 Establish calibration curve by carefully determining the
the air in the optical path. The zirconium Ka line has a higher
intensity of the emitted zirconium radiation from each of the
energy and its intensity will not be affected by air.
calibration standards (a minimum of five standards is recom-
5.1.5 Signal Conditioning and Data Handling System,
mended). Obtain three readings for each standard (measured
whereby a coating weight versus X-ray counts curve may be
across the standard’s surface if it is suspected that the zirco-
established within the system for the direct readout of coating
nium coating weight might be varying).
weight.
5.1.6 Sample Spinner (optional), to reduce the effects of 7.3 Construct a calibration by using the software and
algorithms supplied by the equipment manufacturer, establish-
coating weight variation across the test specimen.
ingtherelationshipbetweenzirconiumintensityandzirconium
treatment coating weight.
6. Calibration Standards and Test Specimens
7.4 When using drift correction monitors, determine the
6.1 Calibration Standards should be specimens for which
intensity of the drift correction monitor sample(s).
the coating weight has been well characterized by other
analytical procedures such as x-ray photoelectron
7.5 Immediately after completing the calibration, determine
spectroscopy, Auger emission spectroscopy, glow discharge
the zirconium coating weight of one or more calibration check
optical emission spectrometry, weigh-strip-weigh method, or
sample. Check samples can be stable, well-characterized ma-
other depth-profiling analytical technique.
terials. The differences between two measured values shall be
withintherepeatabilityofthistestmethod.Whenthisisnotthe
6.2 Blank (bare and untreated) Specimen (optional), should
case, the stability of the instrument and the repeatability of the
be of the same metal substrate on which the treatment coating
sample preparation should be investigated and corrective
weight is to be determined. It may be necessary to prepare
...
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: D7639 − 10 D7639 − 10 (Reapproved 2014)
Standard Test Method for
Determination of Zirconium Treatment Weight or Thickness
on Metal Substrates by X-Ray Fluorescence
This standard is issued under the fixed designation D7639; 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 test method covers the use of X-ray fluorescence (XRF) spectrometry for the determination of the mass of zirconium
(Zr) coating weight per unit area of metal substrates.
1.2 Coating treatments can also be expressed in units of linear thickness provided that the density of the coating is known, or
provided that a calibration curve has been established for thickness determination using standards with treatment matching this of
test specimens to be analyzed. For simplicity, the method will subsequently refer to the determination expressed as coating weight.
1.3 XRF is applicable for the determination of the coating weight as zirconium or total coating weight of a zirconium containing
treatment, or both, on a variety of metal substrates.
1.4 The maximum measurable coating weight for a given coating is that weight beyond which the intensity of the characteristic
X-ray radiation from the coating or the substrate is no longer sensitive to small changes in weight.
1.5 The values stated in SI units are regarded as the to be regarded as standard. No other units of measurement are included
in this standard.
1.6 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:
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Summary of Test Method
3.1 The test specimen is placed in the X-ray beam, and the resultant peak intensity of the zirconium Ka line (at 0.0786 nm or
15.747 keV) or the zirconium La line (at 0.606 nm or 2.042 keV) is measured. The intensity (in counts or counts per second) is
then compared to a previously prepared calibration curve or equation to obtain the coating weight of zirconium treatment in mg/m
or mg/ft (or μm or nm).
3.2 The exact relationship between the measured number of counts and the corresponding coating weight (or coating thickness)
must be established for each individual combination of substrate and zirconium-containing treatment. Usually determined by the
treatment supplier, this relationship is established by using primary standards having known amounts of the same treatment applied
to the same substrate composition as the test specimens to be measured.
4. Significance and Use
4.1 The procedure described in this test method is designed to provide a method by which the coating weight of zirconium
treatments on metal substrates may be determined.
This test method is under the jurisdiction of ASTM Committee D01 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.53 on Coil Coated Metal.
Current edition approved June 1, 2010June 15, 2014. Published June 2010June 2014. DOI:10.1520/D7639–10.Originally approved in 2010. Last previous edition approved
in 2010 as D7639 – 10. DOI:10.1520/D7639-10R14.
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
D7639 − 10 (2014)
4.2 This test method is applicable for determination of the total coating weight and the zirconium coating weight of a
zirconium-containing treatment.
5. Apparatus
5.1 X-Ray Fluorescence Spectrometer, capable of measuring the intensity of zirconium Ka or La line, and establish the
relationship between peak intensity and coating weight. The spectrometer’s design must include, as a minimum, the following
features:
5.1.1 Source of X-Ray Excitation, X-ray tube with excitation above 2.55 keV if measuring the zirconium La line, or above 18
keV if measuring the zirconium Ka line.
5.1.2 X-Ray Detector, with high sensitivity and capable of discriminating between zirconium La or Ka radiation and other
X-rays of higher or lower energies.
5.1.2.1 In the case of wavelength dispersive X-ray fluorescence (WDXRF), this can be an analyzing crystal (for example, fixed
channel, goniometer) setup to detect the zirconium X-rays (La or Ka line). Germanium 111 has been found to be acceptable for
the Zirconium La line and LiF220 or LiF200 for the zirconium Ka line.
5.1.2.2 In the case of energy dispersive X-ray fluorescence (EDXRF), it can be a proportional counter, or a semiconductor such
as a PIN diode or a silicon-drift detector.
5.1.3 Pulse-Height Analyzer, or other means of energy discrimination.
5.1.4 Optical Path, specified by manufacturer. A helium or vacuum path is recommended when measuring the zirconium La line
in order to minimize the attenuation of the X-rays by the air in the optical path. The zirconium Ka line has a higher energy and
its intensity will not be affected by air.
5.1.5 Signal Conditioning and Data Handling System, whereby a coating weight versus X-ray counts curve may be established
within the system for the direct readout of coating weight.
5.1.6 Sample Spinner (optional), to reduce the effects of coating weight variation across the test specimen.
6. Calibration Standards and Test Specimens
6.1 Calibration Standards should be specimens for which the coating weight has been well characterized by other analytical
procedures such as x-ray photoelectron spectroscopy, Auger emission spectroscopy, glow discharge optical emission spectrometry,
weigh-strip-weigh method, or other depth-profiling analytical technique.
6.2 Blank (bare and untreated) Specimen (optional), should be of the same metal substrate on which the treatment coating
weight is to be determined. It may be necessary to prepare a blank specimen from a treated specimen if an untreated specimen is
not available. To best imitate a bare, untreated blank, abrade a treated specimen that is from the same metal specimen as the test
specimen using a small abrasive pad.
NOTE 1—The first abrading is made parallel with the rolling direction of the metal, the second abrading is made perpendicular to the rolling direction
of the metal, and the third abrading is made parallel with the rolling direction of the metal. This procedure should be repeated until constant readings
are obtained. Always use the same side of the metal substrate from which the readings of the treated specimen will be taken.
6.3 Calibration Standards and Test Specimens shall be cut to the required size, if necessary, for measurement by the instrument.
6.4 All calibration standards and test specimens shall be flat in the area of measurement and free of burrs and distortions that
would prevent proper seating in the analysis chamber or the specimen holder, or proper seating of the handheld analyzer on the
standard’s surface.
6.5 The treatment on the substrate should be uniform in the area of measurement. If the coating weight might vary across the
surface, it is recommended to analyze the test specimen in three different areas and use the average reading as the result.
6.6 The area of measurement should be maintained free of foreign materials. The test specimen shall be handled only by the
edges that are outside of the area to be measured.
6.7 The coated
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