ASTM D7639-10(2018)

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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-Aug-2018
• ICS: 25.220.40 - Metallic coatings
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.53 - Coil Coated Metal

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: D7639 − 10 (Reapproved 2018)
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the use of X-ray fluorescence
E177 Practice for Use of the Terms Precision and Bias in
(XRF) spectrometry for the determination of the mass of
ASTM Test Methods
zirconium(Zr)coatingweightperunitareaofmetalsubstrates.
E691 Practice for Conducting an Interlaboratory Study to
1.2 Coating treatments can also be expressed in units of
Determine the Precision of a Test Method
linear thickness provided that the density of the coating is
known, or provided that a calibration curve has been estab-
3. Summary of Test Method
lished for thickness determination using standards with treat-
3.1 The test specimen is placed in the X-ray beam, and the
ment matching this of test specimens to be analyzed. For
resultant peak intensity of the zirconium Ka line (at 0.0786 nm
simplicity, the method will subsequently refer to the determi-
or 15.747 keV) or the zirconium La line (at 0.606 nm or 2.042
nation expressed as coating weight.
keV) is measured. The intensity (in counts or counts per
1.3 XRF is applicable for the determination of the coating second) is then compared to a previously prepared calibration
weight as zirconium or total coating weight of a zirconium curve or equation to obtain the coating weight of zirconium
2 2
treatment in mg/m or mg/ft (or µm or nm).
containing treatment, or both, on a variety of metal substrates.
3.2 The exact relationship between the measured number of
1.4 The maximum measurable coating weight for a given
counts and the corresponding coating weight (or coating
coating is that weight beyond which the intensity of the
thickness) must be established for each individual combination
characteristic X-ray radiation from the coating or the substrate
of substrate and zirconium-containing treatment. Usually de-
is no longer sensitive to small changes in weight.
termined by the treatment supplier, this relationship is estab-
1.5 The values stated in SI units are to be regarded as
lished by using primary standards having known amounts of
standard. No other units of measurement are included in this
the same treatment applied to the same substrate composition
standard.
as the test specimens to be measured.
1.6 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4.1 The procedure described in this test method is designed
priate safety, health, and environmental practices and deter-
to provide a method by which the coating weight of zirconium
mine the applicability of regulatory limitations prior to use.
treatments on metal substrates may be determined.
1.7 This international standard was developed in accor-
4.2 This test method is applicable for determination of the
dance with internationally recognized principles on standard-
total coating weight and the zirconium coating weight of a
ization established in the Decision on Principles for the
zirconium-containing treatment.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5. Apparatus
Barriers to Trade (TBT) Committee.
5.1 X-RayFluorescenceSpectrometer,capableofmeasuring
the intensity of zirconium Ka or La line, and establish the
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.53 on Coil Coated Metal. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2018. Published September 2018. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2010. Last previous edition approved in 2014 as D7639 – 10 (2014). Standards volume information, refer to the standard’s Document Summary page on
DOI:10.1520/D7639-10R18. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7639 − 10 (2018)
relationship between peak intensity and coating weight. The thespecimenholder,orproperseatingofthehandheldanalyzer
spectrometer’s design must include, as a minimum, the follow- on the standard’s surface.
ing features:
6.5 The treatment on the substrate should be uniform in the
5.1.1 SourceofX-RayExcitation,X-raytubewithexcitation
area of measurement. If the coating weight might vary across
above 2.55 keV if measuring the zirconium La line, or above
the surface, it is recommended to analyze the test specimen in
18 keV if measuring the zirconium Ka line.
three different areas and use the average reading as the result.
5.1.2 X-Ray Detector, with high sensitivity and capable of
6.6 The area of measurement should be maintained free of
discriminating between zirconium La or Ka radiation and other
foreign materials. The test specimen shall be handled only by
X-rays of higher or lower energies.
the edges that are outside of the area to be measured.
5.1.2.1 In the case of wavelength dispersive X-ray fluores-
cence(WDXRF),thiscanbeananalyzingcrystal(forexample, 6.7 The coated area of the test specimen should be larger
than the measured area.
fixed channel, goniometer) setup to detect the zirconium
X-rays (La or Ka line). Germanium 111 has been found to be
6.8 The calibration standards and test specimens should be
acceptable for the Zirconium La line and LiF220 or LiF200 for
measured over the X-ray port using the same rolling direction
the zirconium Ka line.
of the metal. This is not necessary for instruments operating
5.1.2.2 In the case of energy dispersive X-ray fluorescence
with a sample spinner.
(EDXRF), it can be a proportional counter, or a semiconductor
such as a PIN diode or a silicon-drift detector.
7. Calibration Procedure
5.1.3 Pulse-Height Analyzer, or other means of energy
7.1 Set up the instrument calibration and operating param-
discrimination.
eters according to the chemical supplier and instrument manu-
5.1.4 Optical Path, specified by manufacturer. A helium or
facturer’s recommendations.
vacuum path is recommended when measuring the zirconium
7.2 Establish calibration curve by carefully determining the
La line in order to minimize the attenuation of the X-rays by
intensity of the emitted zirconium radiation from each of the
the air in the optical path. The zirconium Ka line has a higher
calibration standards (a minimum of five standards is recom-
energy and its intensity will not be affected by air.
mended). Obtain three readings for each standard (measured
5.1.5 Signal Conditioning and Data Handling System,
across the standard’s surface if it is suspected that the zirco-
whereby a coating weight versus X-ray counts curve may be
nium coating weight might be varying).
established within the system for the direct readout of coating
weight.
7.3 Construct a calibration by using the software and
5.1.6 Sample Spinner (optional), to reduce the effects of
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
7.5 Immediately after completing the calibration, determine
analytical procedures such as x-ray photoelectron
the zirconium coating weight of one or more calibration check
spectroscopy, Auger emission spectroscopy, gl
...

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 (Reapproved 2014) D7639 − 10 (Reapproved 2018)
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 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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 15, 2014Sept. 1, 2018. Published June 2014September 2018. Originally approved in 2010. Last previous edition approved in 20102014 as
D7639 – 10. DOI:10.1520/D7639-10R14.10 (2014). DOI:10.1520/D7639-10R18.
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’sstandard’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 (2018)
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 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 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 measurem
...