Standard Test Method for Determination of Titanium Treatment Weight on Metal Substrates by Wavelength Dispersive 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 titanium treatments on metal substrates may be determined.  
4.2 This test method is applicable for determination of the total coating weight and the titanium coating weight of a titanium-containing treatment.
SCOPE
1.1 This test method covers the use of wavelength dispersive X-ray fluorescence (WDXRF) techniques for determination of the coating weight of titanium treatments on metal substrates. These techniques are applicable for determination of the coating weight as titanium or total coating weight of a titanium containing treatment, or both, on a variety of metal substrates.  
1.2 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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Publication Date
30-Nov-2016
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ASTM D6906-12a(2016) - Standard Test Method for Determination of Titanium Treatment Weight on Metal Substrates by Wavelength Dispersive X-Ray Fluorescence
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REDLINE ASTM D6906-12a(2016) - Standard Test Method for Determination of Titanium Treatment Weight on Metal Substrates by Wavelength Dispersive X-Ray Fluorescence
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D6906 − 12a (Reapproved 2016)
Standard Test Method for
Determination of Titanium Treatment Weight on Metal
Substrates by Wavelength Dispersive X-Ray Fluorescence
This standard is issued under the fixed designation D6906; 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 can discriminate between the energy levels of fluorescing
radiations in the secondary beam. The detection system in-
1.1 This test method covers the use of wavelength disper-
cludes the radiation detector with electronics for pulse ampli-
sive X-ray fluorescence (WDXRF) techniques for determina-
fication and pulse counting.
tion of the coating weight of titanium treatments on metal
substrates. These techniques are applicable for determination
3.3 Basic Principle:
of the coating weight as titanium or total coating weight of a
3.3.1 A relationship exists between the treatment coating
titanium containing treatment, or both, on a variety of metal
weight and secondary radiation intensity. This relationship is
substrates.
usually linear within the desired coating weights of the
titanium treatments on metal substrates. The measurements are
1.2 This standard does not purport to address all of the
based on primary standards of known coating weights and
safety concerns, if any, associated with its use. It is the
instrument calibration that correlates the secondary radiation
responsibility of the user of this standard to establish appro-
intensity with the coating weight quantitatively.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 3.3.2 The coating weight is determined by measurement of
the fluorescent X-rays of the coating. The detection system is
2. Referenced Documents
set to count the number of X-rays in an energy region that is
characteristic of X-rays from the element of interest. The
2.1 ASTM Standards:
element of interest in this practice is titanium.
E177 Practice for Use of the Terms Precision and Bias in
3.3.3 If a linear relationship exists, the coating weight and
ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to number of counts of X-rays of a titanium treatment on a
particular substrate can be expressed by a conversion factor
Determine the Precision of a Test Method
that represents the number of counts for a particular coating
3. Summary of Practice
weight unit/unit area. This is usually expressed in mg/ft or
mg/m of titanium or total coating weight.
3.1 Excitation—The measurement of titanium treatment
3.3.4 The exact relationship between the measured number
coatingweightsbyWDXRFmethodsisbasedonthecombined
of counts and the corresponding coating weight must be
interaction of the titanium coating and the substrate with an
established for each individual combination of substrate and
intense beam of primary radiation. Since each element fluo-
titanium-containingtreatment.Usuallydeterminedbythetreat-
resces at an energy characteristic of the particular element, this
ment supplier, this relationship is established by using primary
interaction results in the generation of X-rays of defined
energy. The primary radiation may be generated by an X-ray standardshavingknownamountsofthesametreatmentapplied
to the same substrate composition as the specimens to be
tube or derived from a radioisotope.
measured.
3.2 Detection—The secondary beam (fluorescent X-rays of
3.3.5 Some X-ray apparatuses have a data handling system
the elements and scattered radiation) is read by a detector that
whereby a coating weight versus X-ray counts curve may be
established within the system for the direct readout of coating
This test method is under the jurisdiction of ASTM Committee D01 on Paint
weight. If such apparatus does not permit the entry of a
and Related Coatings, Materials, andApplications and is the direct responsibility of
conversion factor as described in 3.3.3, it is calibrated using a
Subcommittee D01.53 on Coil Coated Metal.
bare, untreated specimen and a minimum of three specimens
Current edition approved Dec. 1, 2016. Published December 2016. Originally
with known coating weights of the treatment and substrate
approved in 2003. Last previous edition approved in 2012 as D6906 – 12a. DOI:
10.1520/D6906-12AR16.
combination of interest. The coating weight to be measured
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
mustbewithintherangeoftheseknowncoatingweights.More
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
than three known specimens must be used if the relationship of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. X-ray counts to coating weight is not linear over the range to
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6906 − 12a (2016)
be measured. The treatment supplier should be consulted for 7.2 Set the instrument settings as follows:
recommendations for establishing the curve in the instrument
Dial and arm titanium position
Seconds indicator pretreatment supplier
for the particular treatment and substrate combination of
Multiplier switch pretreatment supplier
interest.
Response switch pretreatment supplier
Range pretreatment supplier
4. Significance and Use
Milliamps adjust for calibration of output
pretreatment supplier
4.1 The procedure described in this test method is designed
7.3 All specimens must be seated firmly and securely over
to provide a method by which the coating weight of titanium
the measuring opening. The distance between the measuring
treatments on metal substrates may be determined.
apparatus and specimen must be maintained the same as that
4.2 This test method is applicable for determination of the
during the calibration. The blank and treated specimens must
total coating weight and the titanium coating weight of a
be placed in the holder so that the rolling direction of the metal
titanium-containing treatment.
is in the same orientation. Whenever a sample tray holder is a
part of the apparatus, the same opening of the slide must be
5. Apparatus and Materials
used for the blank and treated specimen unless the openings
5.1 Measuring Instrument, which is capable of determining
have been determined to produce equivalent results. If it is
the coating weights of titanium-containing treatments on metal
necessary to use a backer to hold the test specimen firmly
substrates by X-ray fluorescence is required. The treatment
against the window, make sure that the backer is of untreated
supplier should be consulted for the suitability of the instru-
coupons of the same metal as the specimen. The same backer
mentation to be used
must be used for each set of measurements.
5.2 Calibration Standard, necessary to calibrate the instru-
7.4 Insert the titanium calibration standard that has been
ment.The count value of this standard must be specified by the
recommended by the treatment supplier into the instrument,
treatment supplier.
and obtain a count.Adjust the current with the control knob on
5.3 Treated Coupon, on which the coating weight is to be
the probe until the count value is within a single significant
determined must be cut to the required size for the instrument
figure rounded approximation of 63 times the square root of
from the treated substrate.
the counts provided by the treatment supplier with each
5.4 Blank (Bare and Untreated) Coupon should be a sample
titanium calibration standard.
of the same metal su
...


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: D6906 − 12a D6906 − 12a (Reapproved 2016)
Standard Test Method for
Determination of Titanium Treatment Weight on Metal
Substrates by Wavelength Dispersive X-Ray Fluorescence
This standard is issued under the fixed designation D6906; 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 wavelength dispersive X-ray fluorescence (WDXRF) techniques for determination of the
coating weight of titanium treatments on metal substrates. These techniques are applicable for determination of the coating weight
as titanium or total coating weight of a titanium containing treatment, or both, on a variety of metal substrates.
1.2 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 Practice
3.1 Excitation—The measurement of titanium treatment coating weights by WDXRF methods is based on the combined
interaction of the titanium coating and the substrate with an intense beam of primary radiation. Since each element fluoresces at
an energy characteristic of the particular element, this interaction results in the generation of X-rays of defined energy. The primary
radiation may be generated by an X-ray tube or derived from a radioisotope.
3.2 Detection—The secondary beam (fluorescent X-rays of the elements and scattered radiation) is read by a detector that can
discriminate between the energy levels of fluorescing radiations in the secondary beam. The detection system includes the radiation
detector with electronics for pulse amplification and pulse counting.
3.3 Basic Principle:
3.3.1 A relationship exists between the treatment coating weight and secondary radiation intensity. This relationship is usually
linear within the desired coating weights of the titanium treatments on metal substrates. The measurements are based on primary
standards of known coating weights and instrument calibration that correlates the secondary radiation intensity with the coating
weight quantitatively.
3.3.2 The coating weight is determined by measurement of the fluorescent X-rays of the coating. The detection system is set
to count the number of X-rays in an energy region that is characteristic of X-rays from the element of interest. The element of
interest in this practice is titanium.
3.3.3 If a linear relationship exists, the coating weight and number of counts of X-rays of a titanium treatment on a particular
substrate can be expressed by a conversion factor that represents the number of counts for a particular coating weight unit/unit area.
2 2
This is usually expressed in mg/ft or mg/m of titanium or total coating weight.
3.3.4 The exact relationship between the measured number of counts and the corresponding coating weight must be established
for each individual combination of substrate and titanium-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 specimens to be measured.
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 Nov. 1, 2012Dec. 1, 2016. Published January 2013December 2016. Originally approved in 2003. Last previous edition approved in 2012 as
D6906 – 12.12a. DOI: 10.1520/D6906-12A.10.1520/D6906-12AR16.
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’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
D6906 − 12a (2016)
3.3.5 Some X-ray apparatuses have a 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. If such apparatus does not permit the entry of a conversion
factor as described in 3.3.3, it is calibrated using a bare, untreated specimen and a minimum of three specimens with known coating
weights of the treatment and substrate combination of interest. The coating weight to be measured must be within the range of these
known coating weights. More than three known specimens must be used if the relationship of X-ray counts to coating weight is
not linear over the range to be measured. The treatment supplier should be consulted for recommendations for establishing the
curve in the instrument for the particular treatment and substrate combination of interest.
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 titanium
treatments on metal substrates may be determined.
4.2 This test method is applicable for determination of the total coating weight and the titanium coating weight of a
titanium-containing treatment.
5. Apparatus and Materials
5.1 Measuring Instrument, which is capable of determining the coating weights of titanium-containing treatments on metal
substrates by X-ray fluorescence is required. The treatment supplier should be consulted for the suitability of the instrumentation
to be used
5.2 Calibration Standard, necessary to calibrate the instrument. The count value of this standard must be specified by the
treatment supplier.
5.3 Treated Coupon, on which the coating weight is to be determined must be cut to the required size for the instrument from
the treated substrate.
5.4 Blank (Bare and Untreated) Coupon should be a sample of the same metal substrate on which the treatment coating weight
is to be determined. It may be necessary to prepare a blank coupon from a treated sample if an untreated coupon is not available.
To best imitate a bare, untreated blank, abrade a treated coupon that is from the same metal specimen as the test specimen using
a small abrasive pad.
5.4.1 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 coupon will be taken.
6. Test Specimens
6.1 All test specimens must be flat in the area of measurement and free of burrs and distortions that would prevent proper seating
in the specimen holder.
6.2 The treatment on the substrate must be uniform in the area of measurement.
6.3 The area of measurement must be maintained free of foreign materials. The specimen must be handled only by the edges
that are outside of the area to be measured.
6.4 The coated area of the specimen must be larger than the measuring area.
7. Procedure
7.1 Operate the instr
...

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