ASTM D4563-86(1996)
(Test Method)Standard Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered From Whole Paint
Standard Test Method for Determination by Atomic Absorption Spectroscopy of Titanium Dioxide Content of Pigments Recovered From Whole Paint
SCOPE
1.1 This test method covers the atomic absorption (AA) analysis of titanium dioxide content in pigments recovered from whole paint. It is applicable to quality control situations where the same type of product is repeatedly analyzed.
1.2 This standard does not purport to address 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 hazard statements are given in Section 7.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 4563 – 86 (Reapproved 1996)
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 Atomic Absorption Spectroscopy of
Titanium Dioxide Content of Pigments Recovered From
Whole Paint
This standard is issued under the fixed designation D 4563; 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 4. Significance and Use
1.1 This test method covers the atomic absorption (AA) 4.1 This test method may be used in quality control labo-
analysis of titanium dioxide content in pigments recovered ratories when the repeated analysis of titanium dioxide in
from whole paint. It is applicable to quality control situations similar paints may be required. Reagents and time are kept to
where the same type of product is repeatedly analyzed. a minimum when this test method is used in place of wet
1.2 This standard does not purport to address the safety chemical analysis such as in Test Methods D 1394. However,
concerns, if any, associated with its use. It is the responsibility reproducibility and repeatability are not as good as in Test
of the user of this standard to establish appropriate safety and Methods D 1394.
health practices and determine the applicability of regulatory
5. Apparatus
limitations prior to use. Specific hazard statements are given in
Section 7. 5.1 Atomic Absorption Spectrophotometer, consisting of
5.1.1 Atomizer and nitrous oxide burner,
2. Referenced Documents
5.1.2 Gas-pressure regulator and metering devices for ni-
2.1 ASTM Standards: trous oxide and acetylene,
D 1193 Specification for Reagent Water 5.1.3 Titanium hollow cathode lamp with regulated
D 1394 Test Methods for Chemical Analysis of White constant-current supply,
Titanium Pigments 5.1.4 Monochromator and associated optics,
E 180 Practice for Determining the Precision Data of 5.1.5 Photosensitive detector connected to an electronic
ASTM Methods for Analysis and Testing of Industrial amplifier,
Chemicals 5.1.6 Readout device.
E 288 Specification for Volumetric Flasks 5.2 Muffle Furnace, capable of maintaining 450 6 25 °C.
5.3 Circulating Oven, maintained at 105 6 2°C.
3. Summary of Test Method
5.4 Porcelain Dishes, 90-mm diameter.
3.1 The specimen is prepared for analysis by ashing at 5.5 Plastic Disposable Syringe, 10-mL capacity.
450°C followed by digestion with sulfuric acid and ammonium
5.6 Agate Mortar and Pestle, 95-mm outside diameter.
sulfate as in Test Methods D 1394. The titanium content is 5.7 Wide-Mouth Erlenmeyer Flask, 500-mL capacity.
determined by atomic absorption spectroscopy using a speci-
5.8 Hot Plate, with variable surface temperature control
men similar to that previously analyzed by the Aluminum from 10°C above ambient to 370°C accurate to within 65°C.
Reduction Method in Test Methods D 1394.
5.9 Burner.
3.2 By utilizing the pigment analyzed in Test Methods 5.10 Volumetric Flask, 1000 mL, plastic (see Specification
D 1394 as an atomic absorption standard, several hundred TiO E 288).
determinations can be made. The AA technique is much faster
5.11 Paint Shaker.
than the technique in Test Methods D 1394 for multiple 5.12 Weighing Bottles, wide-mouth, with an external-fitting
determinations and uses only acids. This keeps reagents and
cap, and no larger than necessary for required amount of
time to a minimum. sample.
5.13 Desiccator.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
6. Reagents
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. 6.1 Purity of Reagents—Reagent grade chemicals shall be
Current edition approved Jan. 31, 1986. Published March 1986.
used in all tests. Unless otherwise indicated, it is intended that
Annual Book of ASTM Standards, Vol 11.01.
all reagents shall conform to the specifications of the Commit-
Annual Book of ASTM Standards, Vol 06.01.
tee on Analytical Reagents of the American Chemical Society,
Annual Book of ASTM Standards, Vol 15.05.
Annual Book of ASTM Standards, Vol 14.02.
D 4563
where such specifications are available. Other grades may be 8.3.1 Expanding the scale of a spectrophotometer increases
used, provided it is first ascertained that the reagent is of the noise level of the readout system. Therefore, if expanding
sufficient high purity to permit its use without reducing the the scale to make the readout indicate 60 % TiO has this
accuracy of the determination. effect, do not use any expansion. For instance, it is not
6.2 Purity of Water—Unless otherwise indicated, references necessary to make the instrument read 60 for 60 % TiO
to water shall be understood to mean reagent water conforming standard. It may read 30. If 60 % equals 30, a pigment giving
to Type II of Specification D 1193. a reading of 25 would have a TiO content of 50 %.
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
PIGMENT CONTENT
monium hydroxide (NH OH).
6.4 Ammonium Sulfate (NH ) SO ).
4 2 4
9. Procedure
6.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
9.1 Mix the samples until homogenous, preferably on a
chloric acid (HCl).
mechanical shaker. If air bubbles become entrapped in the
6.6 Hydrofluoric Acid (HF)—Approximately 49 %.
sample, stir by hand.
6.7 Standard Pigment Solution.
9.2 Draw approximately5gofthe paint under test into a
6.7.1 Following the procedure in Section 9 recover the
10-mL syringe and weigh to 1 mg. Transfer, by dropwise
pigment from a paint that is similar to the unknown specimen.
addition, between 2.0 and 4.0 g of the specimen to a tared
Analyze the extracted pigment for TiO content in accordance
porcelain dish containing either 2 mL of water (for water-borne
with the Aluminum Reduction Method in Test Methods D 1394
paint) or 2 mL of toluene (for solvent-borne paint). Reweigh
and record the percent TiO found in the pigment.
the syringe to 1 mg. Swirl the dish during the addition of the
6.7.2 Following the procedure in 12.1-12.5 take a specimen
paint and continue to swirl until the specimen is completely
of the pigment extracted in 6.7.1 into solution. Store this
dispersed. If a water-borne paint tends to agglomerate or form
solution for no more than 3 months in a plastic bottle marked
lumps that cannot be dispersed, a drop or two of concentrated
with the percent TiO as determined in 6.7.1.
NH OH may help the dispersement. If the lumps persist,
6.8 Sulfuric Acid (sp gr 1.84), concentrated sulfuric acid
discard the specimen, and prepare a new one. Prepare a
(H SO ).
2 4
duplicate specimen in the same manner.
6.9 Toluene.
9.3 Dry the specimens at 110°C for 30 min and then drive
7. Hazards
off the remaining solvent or water at the lowest temperature
possible using a Meker burner (under a hood). Do not leave the
7.1 Concentrated Hydrofluoric Acid—Make certain to ob-
dishes on the burners after the flames have subsided.
serve manufacturer’s recommended precautions for handling.
9.4 Transfer the dried specimens to a muffle furnace and
7.2 Warning—Nitrous oxide and acetylene can cause ex-
heat at 450 6 25°C for at least 1 h and until no further char is
plosions, if not used properly. See the supplier’s manual of
evident. Leave the furnace door slightly open after first
instructions for the atomic absorption instrument for proper
inserting the dishes to allow smoke and possibly flames to
operation with these gases.
escape making certain the furnace is well vented.
8. Calibration and Standardization
9.5 Remove the dishes from the muffle furnace, cool in a
8.1 Operational instructions for atomic absorption spectro-
desiccator, and weigh.
photometers vary with different models. Consult the manufac-
9.6 Grind the pigment to pass through an 80-mesh screen.
turer’s literature for establishing optimum conditions for the
10. Calculation
specific instrument used.
8.2 Turn the instrument on and set the wavelength to the
10.1 Calculate the percent pigment content
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.