ASTM D4764-88(1993)e1
(Test Method)Standard Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint
Standard Test Method for Determination by X-ray Fluorescence Spectroscopy of Titanium Dioxide Content in Paint
SCOPE
1.1 This test method covers the determination of titanium dioxide content in liquid paint. This test method is applicable to both water-reducible and solvent-reducible paints.
1.2 The values stated in SI units ae to be regarded as the standard. The values given in parentheses are for information only.
1.3 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. Specific hazards statements are given in Section 7.
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e1
Designation: D 4764 – 88 (Reapproved 1993)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determination by X-ray Fluorescence Spectroscopy of
Titanium Dioxide Content in Paint
This standard is issued under the fixed designation D 4764; 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.
e NOTE—Keywords were added editorially in April 1993.
1. Scope mined by comparing the ratio of the intensities of titanium and
bromine peaks in the test paint and the standard. Differences in
1.1 This test method covers the determination of titanium
the nonvolatile content of the paints are taken into account in
dioxide content in liquid paint. This test method is applicable
the calculation of results.
to both water-reducible and solvent-reducible paints.
1.2 This standard does not purport to address all of the
4. Significance and Use
safety problems, if any, associated with its use. It is the
4.1 Titanium dioxide pigments are components with high
responsibility of the user of this standard to establish appro-
refractive index that significantly influence the opacity, color,
priate safety and health practices and determine the applica-
durability, and other properties of coatings. This test method
bility of regulatory limitations prior to use. Specific hazards
for determining titanium dioxide content is quicker and easier
statements are given in Section 7.
to use than Test Methods D 1394, a wet chemical analysis
2. Referenced Documents method for pigments. It is conveniently applicable to single
samples and to large numbers of samples. Only a single
2.1 ASTM Standards:
relatively stable reagent used to prepare standards and paints
D 476 Specification for Titanium Dioxide Pigments
3 under test need be stored. Drawdown specimens used as
D 1193 Specifications for Reagent Water
standards, once prepared, can be stored indefinitely and used
D 1394 Test Methods for Chemical Analysis of White
2 repeatedly.
Titanium Pigments
D 2369 Test Method for Volatile Content of Coatings
5. Apparatus
D 3925 Practice for Sampling Liquid Paints and Related
4 5.1 X-ray Fluorescence Spectrometer, suitable for measure-
Pigmented Coatings
ment of the baseline corrected intensity of the Ka lines of
D 3980 Practice for Interlaboratory Testing of Paint and
4 titanium and of bromine. For spectrometers equipped with a
Related Materials
tungsten or chromium target and a lithium fluoride (200)
E 180 Practice for Determining the Precision Data of
analyzing crystal, these lines are observed at 2u angles of
ASTM Methods for Analysis and Testing of Industrial
86.09° and 29.97°, respectively.
Chemicals
NOTE 1—Follow the recommendations of the manufacturer of the
3. Summary of Test Method
instrument used. Use operating conditions that ensure that the count rate
for bromine and titanium are within the linear response range of the
3.1 Paint containing a known amount of titanium dioxide is
detector. Although the base operating conditions and count rate may be
used as the reference standard. A solution of tetraethylammo-
different for different instruments, these differences will not affect the
nium bromide in 2-ethoxyethanol is added to the standard paint
outcome of the analysis.
and to each paint being analyzed. Drawdown films of the
5.2 Paint Shaker.
standard and test paint are made on thin plastic sheets. The
5.3 Film Applicator, to produce a 3-mil (75-μm) wet film
intensities of key X-ray fluorescence peaks of titanium and
thickness.
bromine are measured. The titanium dioxide content is deter-
5.4 Plastic Sheet, with no interfering X-ray fluorescence
peaks and not attacked by paint solvent.
1 5.5 Perforated Suction Plate, or other flat surface.
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 5.6 Vials and caps,20mL.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Feb. 26, 1988. Published April 1988.
Annual Book of ASTM Standards, Vol 06.03.
3 6
Annual Book of ASTM Standards, Vol 11.01. Leneta P-121-10N dull black plastic panels 6 ⁄2 by 17 in. by 10 mils (165 by
Annual Book of ASTM Standards, Vol 06.01. 432 by 0.25 mm) in size, available from Leneta Co., 15 Whitney Rd., Mahwah, NJ
Annual Book of ASTM Standards, Vol 15.05. 07430, have been found suitable for this purpose.
D 4764
6. Reagents titanium dioxide, and each test paint using the following
procedure. Into a 20-mL vial weigh approximately 7.00 g of
6.1 Purity of Reagents—Reagent grade chemicals shall be
paint to 1 mg. Pipet 2 mL of TEAB internal standard solution
used in all tests, unless otherwise specified. It is intended that
(see 6.4) into the paint and thoroughly mix.
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Societywhere
TABLE 1 Instrument Conditions
such specifications are available. Other grades may be used,
Ti Ka Br Ka
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of Analyzer crystal LiF LiF
Counter Flow or Scintillation Scintillation
the determination.
Collimator Fine Coarse
6.2 Purity of Water—Unless otherwise indicated, references
Order First First
to water shall be understood to mean reagent water that Tube KV/mA 10/5 60/24
Time, s 20 20
conforms to the requirements of Type II of Specification
Peak, 2u,° 86.09 29.97
D 1193.
Background, 2u,° 85.00 29.00
6.3 2-ethoxyethanol, purified grade.
6.4 Tetraethylammonium Bromide, internal standard
8.2 Place a plastic sheet on the perforated suction plate. On
solution—Into a 100-mL volumetric flask weigh approxi-
the plastic sheet make a 3.0-mil (75-μm) thick drawdown of the
mately 10.80 g of tetraethylammonium bromide (TEAB) to 1
liquid paint. Air dry the drawdown film overnight. Cut from the
mg. Dissolve the TEAB in 2-ethoxyethanol, fill the flask to the
drawdown on the plastic sheet a disk of a size appropriate for
mark with 2-ethoxyethanol, and mix thoroughly. (TEAB dis-
the specimen holder of the spectrometer.
solved in 2-ethoxyethanol can be used as an internal standard
8.3 Determine the percent nonvolatile content of each paint
for both water-reducible and solvent-reducible paint. However,
at 110°C in accordance with Test Method D 2369 if the
water may be substituted for 2-ethoxyethanol, if only water-
information is not already available.
reducible paint is to be analyzed.)
9. Procedure
7. Hazards
9.1 Turn on the spectrometer and allow it to stabilize
7.1 As exposure to excessive quantities of x-radiation is
thoroughly before beginning collection of results. With th
...
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