ASTM D4764-01(2012)
(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
SIGNIFICANCE AND USE
4.1 Titanium dioxide pigments are components with high refractive index that significantly influence the opacity, color, durability, and other properties of coatings. This test method for determining titanium dioxide content is quicker and easier to use than Test Methods D1394, a wet chemical analysis method for pigments. It is conveniently applicable to single samples and to large numbers of samples. Only a single relatively stable reagent used to prepare standards and paints under test need be stored. Drawdown specimens used as standards, once prepared, can be stored indefinitely and used repeatedly.
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 are 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.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4764 − 01 (Reapproved 2012)
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This test method covers the determination of titanium 3.1 Paint containing a known amount of titanium dioxide is
dioxide content in liquid paint. This test method is applicable used as the reference standard. A solution of tetraethylammo-
to both water-reducible and solvent-reducible paints. niumbromidein2-ethoxyethanolisaddedtothestandardpaint
and to each paint being analyzed. Drawdown films of the
1.2 The values stated in SI units are to be regarded as the
standard and test paint are made on thin plastic sheets. The
standard. The values given in parentheses are for information
intensities of key X-ray fluorescence peaks of titanium and
only.
bromine are measured. The titanium dioxide content is deter-
1.3 This standard does not purport to address all of the
mined by comparing the ratio of the intensities of titanium and
safety concerns, if any, associated with its use. It is the
brominepeaksinthetestpaintandthestandard.Differencesin
responsibility of the user of this standard to establish appro-
the nonvolatile content of the paints are taken into account in
priate safety and health practices and determine the applica-
the calculation of results.
bility of regulatory limitations prior to use. Specific hazards
4. Significance and Use
statements are given in Section 7.
4.1 Titanium dioxide pigments are components with high
2. Referenced Documents
refractive index that significantly influence the opacity, color,
2.1 ASTM Standards: durability, and other properties of coatings. This test method
D1193Specification for Reagent Water for determining titanium dioxide content is quicker and easier
D1394Test Methods for Chemical Analysis of White Tita- to use than Test Methods D1394, a wet chemical analysis
nium Pigments method for pigments. It is conveniently applicable to single
D2369Test Method for Volatile Content of Coatings samples and to large numbers of samples. Only a single
D3925Practice for Sampling Liquid Paints and Related relatively stable reagent used to prepare standards and paints
Pigmented Coatings under test need be stored. Drawdown specimens used as
standards, once prepared, can be stored indefinitely and used
D3980Practice for Interlaboratory Testing of Paint and
Related Materials (Withdrawn 1998) repeatedly.
E180Practice for Determining the Precision of ASTM
5. Apparatus
Methods for Analysis and Testing of Industrial and Spe-
5.1 X-ray Fluorescence Spectrometer, suitable for measure-
cialty Chemicals (Withdrawn 2009)
ment of the baseline corrected intensity of the Kα lines of
titanium and of bromine. For spectrometers equipped with a
1 tungsten or chromium target and a lithium fluoride (200)
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of analyzing crystal, these lines are observed at 2θ angles of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
86.09° and 29.97°, respectively.
CurrenteditionapprovedJune1,2012.PublishedJuly2012.Originallyapproved
in 1988. Last previous edition approved in 2006 as D4764–01 (2006). DOI:
NOTE 1—Follow the recommendations of the manufacturer of the
10.1520/D4764-01R12.
instrument used. Use operating conditions that ensure that the count rate
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
for bromine and titanium are within the linear response range of the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
detector. Although the base operating conditions and count rate may be
Standards volume information, refer to the standard’s Document Summary page on
different for different instruments, these differences will not affect the
the ASTM website.
outcome of the analysis.
The last approved version of this historical standard is referenced on
www.astm.org. 5.2 Paint Shaker.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4764 − 01 (2012)
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-
4 tion manual, and other standard publications on the subject.
5.4 Plastic Sheet, with no interfering X-ray fluorescence
Inquiries should be made of state agencies as to existing
peaks and not attacked by paint solvent.
requirements.
5.5 Perforated Suction Plate, or other flat surface.
8. Specimen Preparation
5.6 Vials and caps, 20 mL.
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 theAmerican 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
D1193.
Collimator Fine Coarse
Order First First
6.3 2-ethoxyethanol, purified grade.
Tube KV/mA 10/5 60/24
Time, s 20 20
6.4 Tetraethylammonium Bromide, internal standard
Peak, 2θ,° 86.09 29.97
solution—Intoa100-mLvolumetricflaskweighapproximately
Background, 2θ,° 85.00 29.00
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-
solved in 2-ethoxyethanol can be used as an internal standard
8.2 Place a plastic sheet on the perforated suction plate. On
forbothwater-reducibleandsolvent-reduciblepaint.However,
theplasticsheetmakea3.0-mil(75-µm)thickdrawdownofthe
water may be substituted for 2-ethoxyethanol, if only water-
liquidpaint.Airdrythedrawdownfilmovernight.Cutfromthe
reducible paint is to be analyzed.)
drawdown on the plastic sheet a disk of a size appropriate for
7. Hazards the specimen holder of the spectrometer.
8.3 Determine the percent nonvolatile content of each paint
7.1 As exposure to excessive quantities of x-radiation is
injurious to health, X-ray producing equipment can be danger- at 110°C in accordance with Test Method D2369 if the
information is not already available.
ous to both the operator and persons in the immediate vicinity
unlesssa
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