Designation: D 6906 – 03
Standard Test Method for
Determination of Titanium Treatment Weight on Metal
Substrates by X-Ray Fluorescence1
This standard is issued under the fixed designation D 6906; 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
1.1 This test method covers the use of X-ray fluorescence
(XRF) 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2. Summary of Practice
2.1 Excitation—The measurement of titanium treatment
coating weights by XRF methods is based on the combined
interaction of the titanium coating and the substrate with an
intense beam of primary radiation. Since each element fluo-
resces 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.
2.2 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 in-
cludes the radiation detector with electronics for pulse ampli-
fication and pulse counting.
2.3 Basic Principle:
2.3.1 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.
2.3.2 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.
2.3.3 If a linear relationship exists, the coating weight and
number of counts of X-rays of a chromium 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. This is usually expressed in mg/ft2 or
mg/m2 of titanium or total coating weight.
2.3.4 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 treat-
ment 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.
2.3.5 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 2.3.3, 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.
3. Significance and Use
3.1 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.1 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 May 10, 2003. Published June 2003.
1
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
3.2 This test method is applicable for determination of the
total coating weight and the titanium coating weight of a
titanium-containing treatment.
4. Apparatus and Materials
4.1 Measuring Instrument,2 which is capable of determining
the coating weights of chromium-containing treatments on
metal substrates by X-ray fluorescence is required. The treat-
ment supplier should be consulted for the suitability of the
instrumentation to be used
4.2 Calibration Standard,3 necessary to calibrate the instru-
ment. The count value of this standard must be specified by the
treatment supplier.
4.3 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.
4.4 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.4
4.4.1 The first abrading is made parallel with the rolling
direction of the metal, the second abrading is made perpen-
dicular 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 read-
ings are obtained. Always use the same side of the metal
substrate from which the readings of the treated coupon will be
taken.
5. Test Specimens
5.1 All test specimens must be flat in the area of measure-
ment and free of burrs and distortions that would prevent
proper seating in the specimen holder.
5.2 The treatment on the substrate must be uniform in the
area of measurement.
5.3 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.
5.4 The coated area of the specimen must be larger than the
measuring area.
6. Procedure
6.1 Operate the instrument in accordance with the manufac-
turer’s instructions.
6.2 Set the instrument settings as follows:
Dial and arm titanium position
Seconds indicator pretreatment supplier
Multiplier switch pretreatment supplier
Response switch pretreatment supplier
Range pretreatment supplier
Milliamps adjust for calibration of output
pretreatment supplier
6.3 All specimens must be seated firmly and securely over
the measuring opening. The distance between the measuring
apparatus and specimen must be maintained the same as that
during the calibration. The blank and treated specimens must
be placed in the holder so that the rolling direction of the metal
is in the same orientation. Whenever a sample tray holder is a
part of the apparatus, the same opening of the slide must be
used for the blank and treated specimen unless the openings
have been determined to produce equivalent results. If it is
necessary to use a backer to hold the test specimen firmly
against the window, make sure that the backer is of untreated
coupons of the same metal as the specimen. The same backer
must be used for each set of measurements.
6.4 Insert the titanium calibration standard that has been
recommended by the treatment supplier into the instrument,
and obtain a count. Adjust the current with the control knob on
the probe until the count value is within 60.50 % of the counts
provided by the treatment supplier with each titanium calibra-
tion standard.
6.5 Obtain the counts of a blank.
6.6 Obtain the counts of the treated specimen.
6.7 Consult the instrument manufacturer’s instruction
manuals for calibrating and operating procedures if the X-ray
apparatus has a data handling system for direct readout of
coating weights.
7. Calculation
7.1 Use 7.2-7.5 for calculating the coating weight if an
automated data handling system is not available.
7.2 The average of a minimum of three readings of both the
blank and treated specimen is used to calculate the coating
weight.
7.3 Calculate the delta (D) counts by subtracting the counts
of the blank from the counts of the treated specimen.
7.4 The coating weight is calculated by dividing the D
counts by the conversion factor that is supplied by the
treatment supplier for the particular substrate and treatment
combination under study.
Coating weight ~weight/unit area! 5
D counts
conversion factor (1)
Other methods as recommended by the treatment supplier
may be used to calculate the coating weight.
7.5 The conversion factors supplied by the treatment sup-
plier are valid only for the instrument calibration procedure
recommended by the treatment supplier.
8. Precision and Bias
8.1 The precision and bias of this test method is being
determined and will be available on or before June 2008.
2 A measuring instrument such as a Portaspect, or equivalent, available from
Cianflone Scientific, 228 RIDC Park West Drive, Pittsburgh, PA 15275, has been
found suitable for this purpose.
3 The calibration standard may be a coupon of titanium base metal or other
titanium standard provided by the treatment supplier, or other titanium calibration
standard as agreed upon between the purchaser and the seller. A calibration standard
such as Brammer BS-T-22, Titanium Standard available from Brammer Standard
Company, Inc. 14603 Benfer Road, Houston TX 77069, or equivalent, has been
found suitable for this purpose.
4 An abrasive pad such as Scotchbritey No. 7447 General Purpose Hand Pad or
No. 96 General Purpose Commercial Scouring Pad, available from 3M, St. Paul,
Minnesota, or equivalent, has been found suitable for this purpose.
D 6906 – 03
2
9. Keywords
9.1 coating weight; non-chrome; titanium; treatment; X-ray
fluorescence
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D 6906 – 03
3
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