ASTM D4764-01(2023)

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.
Designation: D4764 − 01 (Reapproved 2023)
Standard Test Method for
Determination by X-ray Fluorescence Spectroscopy of
Titanium Dioxide Content in Paint
This standard is issued under the fixed designation D4764; 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 E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
1.1 This test method covers the determination of titanium
cialty Chemicals (Withdrawn 2009)
dioxide content in liquid paint. This test method is applicable
to both water-reducible and solvent-reducible paints.
3. Summary of Test Method
1.2 The values stated in SI units are to be regarded as the
3.1 Paint containing a known amount of titanium dioxide is
standard. The values given in parentheses are for information
used as the reference standard. A solution of tetraethylammo-
only.
nium bromide in 2-ethoxyethanol is added to the standard paint
1.3 This standard does not purport to address all of the
and to each paint being analyzed. Drawdown films of the
safety concerns, if any, associated with its use. It is the
standard and test paint are made on thin plastic sheets. The
responsibility of the user of this standard to establish appro-
intensities of key X-ray fluorescence peaks of titanium and
priate safety, health, and environmental practices and deter-
bromine are measured. The titanium dioxide content is deter-
mine the applicability of regulatory limitations prior to use.
mined by comparing the ratio of the intensities of titanium and
Specific hazards statements are given in Section 7.
bromine peaks in the test paint and the standard. Differences in
1.4 This international standard was developed in accor-
the nonvolatile content of the paints are taken into account in
dance with internationally recognized principles on standard-
the calculation of results.
ization established in the Decision on Principles for the
4. Significance and Use
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4.1 Titanium dioxide pigments are components with high
Barriers to Trade (TBT) Committee.
refractive index that significantly influence the opacity, color,
durability, and other properties of coatings. This test method
2. Referenced Documents
for determining titanium dioxide content is quicker and easier
2.1 ASTM Standards: to use than Test Methods D1394, a wet chemical analysis
D1193 Specification for Reagent Water method for pigments. It is conveniently applicable to single
D1394 Test Methods for Chemical Analysis of White Tita- samples and to large numbers of samples. Only a single
nium Pigments relatively stable reagent used to prepare standards and paints
D2369 Test Method for Volatile Content of Coatings under test need be stored. Drawdown specimens used as
D3925 Practice for Sampling Liquid Paints and Related standards, once prepared, can be stored indefinitely and used
Pigmented Coatings repeatedly.
D3980 Practice for Interlaboratory Testing of Paint and
5. Apparatus
Related Materials (Withdrawn 1998)
5.1 X-ray Fluorescence Spectrometer, suitable for measure-
ment of the baseline corrected intensity of the Kα lines of
This test method is under the jurisdiction of ASTM Committee D01 on Paint
titanium and of bromine. For spectrometers equipped with a
and Related Coatings, Materials, and Applications and is the direct responsibility of
tungsten or chromium target and a lithium fluoride (200)
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
analyzing crystal, these lines are observed at 2θ angles of
Current edition approved Feb. 1, 2023. Published February 2023. Originally
86.09° and 29.97°, respectively.
approved in 1988. Last previous edition approved in 2016 as D4764 – 01 (2016).
DOI: 10.1520/D4764-01R23.
2 NOTE 1—Follow the recommendations of the manufacturer of the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
instrument used. Use operating conditions that ensure that the count rate
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
for bromine and titanium are within the linear response range of the
Standards volume information, refer to the standard’s Document Summary page on
detector. Although the base operating conditions and count rate may be
the ASTM website.
The last approved version of this historical standard is referenced on www.ast- different for different instruments, these differences will not affect the
m.org. outcome of the analysis.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4764 − 01 (2023)
5.2 Paint Shaker. become familiar with established safe exposure factors by a
careful study of the National Bureau of Standards Handbook
5.3 Film Applicator, to produce a 75 μm (3 mil) wet film
“X-ray Recommendations of the International Roentgen Ray
thickness.
Committee on X-ray Protection,” the manufacturer’s instruc-
5.4 Plastic Sheet, with no interfering X-ray fluorescence
tion manual, and other standard publications on the subject.
peaks and not attacked by paint solvent.
Inquiries should be made of state agencies as to existing
requirements.
5.5 Perforated Suction Plate, or other flat surface.
5.6 Vials and caps, 20 mL.
8. Specimen Preparation
8.1 Thoroughly mix and sample each paint in accordance
6. Reagents
with Practice D3925. Prepare duplicate specimens of the
6.1 Purity of Reagents—Reagent grade chemicals shall be
standard paint, which contains a known concentration of
used in all tests, unless otherwise specified. It is intended that
titanium dioxide, and each test paint using the following
all reagents conform to the specifications of the Committee on
procedure. Into a 20 mL vial weigh approximately 7.00 g of
Analytical Reagents of the American Chemical Society where
paint to 1 mg. Pipet 2 mL of TEAB internal standard solution
such specifications are available. Other grades may be used,
(see 6.4) into the paint and thoroughly mix.
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
the determination.
TABLE 1 Instrument Conditions
6.2 Purity of Water—Unless otherwise indicated, references
Ti Kα Br Kα
to water shall be understood to mean reagent water that
Analyzer crystal LiF LiF
conforms to the requirements of Type II of Specification
Counter Flow or Scintillation Scintillation
Collimator Fine Coarse
D1193.
Order First First
Tube KV/mA 10/5 60/24
6.3 2-ethoxyethanol, purified grade.
Time, s 20 20
6.4 Tetraethylammonium Bromide, internal standard
Peak, 2θ,° 86.09 29.97
Background, 2θ,° 85.00 29.00
solution—Into a 100 mL volumetric flask weigh approximately
10.80 g of tetraethylammonium bromide (TEAB) to 1 mg.
Dissolve the TEAB in 2-ethoxyethanol, fill the flask to the
mark with 2-ethoxyethanol, and mix thoroughly. (TEAB dis-
8.2 Place a plastic sheet on the perforated suction plate. On
solved in 2-ethoxyethanol can be used as an internal standard
the plastic sheet make a 3.0 mil (75 μm) thick drawdown of the
for both water-reducible and solvent-reducible paint. However,
liquid paint. Air dry the drawdown film overnight. Cut from the
water may be substituted for 2-ethoxyethanol, if only water-
drawdown on the plastic sheet a disk of a size appropriate for
reducible paint is to be analyzed.)
the specimen holder of the spectrometer.
7. Hazards
8.3 Determine the percent nonvolatile content of e
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