ASTM D4563-02(2008)
(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
SIGNIFICANCE AND USE
This test method may be used in quality control laboratories when the repeated analysis of titanium dioxide in similar paints may be required. Reagents and time are kept to a minimum when this test method is used in place of wet chemical analysis such as in Test Methods D 1394. However, reproducibility and repeatability are not as good as in Test Methods D 1394.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
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Designation: D4563 − 02 (Reapproved2008)
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 D4563; 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 determined by atomic absorption spectroscopy using a speci-
men similar to that previously analyzed by the Aluminum
1.1 This test method covers the atomic absorption (AA)
Reduction Method in Test Methods D1394.
analysis of titanium dioxide content in pigments recovered
from whole paint. It is applicable to quality control situations 3.2 By utilizing the pigment analyzed in Test Methods
where the same type of product is repeatedly analyzed. D1394 as an atomic absorption standard, several hundred TiO
determinations can be made. TheAAtechnique is much faster
1.2 The values stated in SI units are to be regarded as
than the technique in Test Methods D1394 for multiple
standard. No other units of measurement are included in this
determinations and uses only acids. This keeps reagents and
standard.
time to a minimum.
1.3 This standard does not purport to address the safety
concerns, if any, associated with its use. It is the responsibility
4. Significance and Use
of the user of this standard to establish appropriate safety and
4.1 This test method may be used in quality control labo-
health practices and determine the applicability of regulatory
ratories when the repeated analysis of titanium dioxide in
limitations prior to use. Specific hazard statements are given in
similar paints may be required. Reagents and time are kept to
Section 7.
a minimum when this test method is used in place of wet
chemical analysis such as in Test Methods D1394. However,
2. Referenced Documents
2 reproducibility and repeatability are not as good as in Test
2.1 ASTM Standards:
Methods D1394.
D1193 Specification for Reagent Water
D1394 Test Methods for Chemical Analysis of White Tita-
5. Apparatus
nium Pigments
E180 Practice for Determining the Precision of ASTM 5.1 Atomic Absorption Spectrophotometer, consisting of
Methods for Analysis and Testing of Industrial and Spe- 5.1.1 Atomizer and nitrous oxide burner,
cialty Chemicals (Withdrawn 2009) 5.1.2 Gas-pressure regulator and metering devices for ni-
E288 Specification for Laboratory Glass Volumetric Flasks trous oxide and acetylene,
5.1.3 Titanium hollow cathode lamp with regulated
3. Summary of Test Method
constant-current supply,
5.1.4 Monochromator and associated optics,
3.1 The specimen is prepared for analysis by ashing at
5.1.5 Photosensitive detector connected to an electronic
450°Cfollowedbydigestionwithsulfuricacidandammonium
amplifier,
sulfate as in Test Methods D1394. The titanium content is
5.1.6 Readout device.
5.2 Muffle Furnace, capable of maintaining 450 6 25°C.
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
5.3 Circulating Oven, maintained at 105 6 2°C.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
5.4 Porcelain Dishes, 90-mm diameter.
Current edition approved Feb. 1, 2008. Published February 2008. Originally
approved in 1986. Last previous edition approved in 2002 as D4563 - 02. DOI:
5.5 Plastic Disposable Syringe, 10-mL capacity.
10.1520/D4563-02R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.6 Agate Mortar and Pestle, 95-mm outside diameter.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 5.7 Wide-Mouth Erlenmeyer Flask, 500-mL capacity.
the ASTM website.
5.8 Hot Plate, with variable surface temperature control
The last approved version of this historical standard is referenced on
www.astm.org. from 10°C above ambient to 370°C accurate to within 65°C.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4563 − 02 (2008)
5.9 Burner. 8. Calibration and Standardization
5.10 Volumetric Flask, 1000 mL, plastic (see Specification 8.1 Operational instructions for atomic absorption spectro-
E288). photometers vary with different models. Consult the manufac-
turer’s literature for establishing optimum conditions for the
5.11 Paint Shaker.
specific instrument used.
5.12 Weighing Bottles, wide-mouth, with an external-fitting
8.2 Turn the instrument on and set the wavelength to the
cap, and no larger than necessary for required amount of
365.3-nm titanium line.Apply the recommended current to the
sample.
titanium hollow cathode lamp. Allow the instrument to warm
5.13 Desiccator.
upforabout15minandsettheproperslitwidth.Adjustthegas
pressures and ignite the burner in accordance with instructions
6. Reagents
for using nitrous oxide and acetylene.
6.1 Purity of Reagents—Reagent grade chemicals shall be
8.3 Aspirate the water to rinse the atomizer chamber from
used in all tests. Unless otherwise indicated, it is intended that
10 to 15 min until the burner head achieves temperature
all reagents shall conform to the specifications of the Commit-
equilibrium. Set the instrument reading to zero while doing
tee onAnalytical Reagents of theAmerican Chemical Society,
4 this. While aspirating the working standard from 6.7.2 set the
where such specifications are available. Other grades may be
instrument to the percent TiO (determined in 6.7.1). Reaspi-
used, provided it is first ascertained that the reagent is of
rate the water and reset the instrument to ZERO. Repeat this
sufficient high purity to permit its use without reducing the
procedure until the readings become stable.
accuracy of the determination.
8.3.1 Expanding the scale of a spectrophotometer increases
6.2 Purity of Water—Unless otherwise indicated, references
the noise level of the readout system. Therefore, if expanding
towatershallbeunderstoodtomeanreagentwaterconforming
the scale to make the readout indicate 60 % TiO has this
to Type II of Specification D1193.
effect, do not use any expansion. For instance, it is not
necessary to make the instrument read 60 for 60 % TiO
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
standard. It may read 30. If 60 % equals 30, a pigment giving
monium hydroxide (NH OH).
a reading of 25 would have a TiO content of 50 %.
6.4 Ammonium Sulfate (NH ) SO ).
4 2 4
PIGMENT CONTENT
6.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl).
9. Procedure
6.6 Hydrofluoric Acid (HF)—Approximately 49 %.
9.1 Mix the samples until homogenous, preferably on a
6.7 Standard Pigment Solution.
mechanical shaker. If air bubbles become entrapped in the
6.7.1 Following the procedure in Section 9 recover the
sample, stir by hand.
pigment from a paint that is similar to the unknown specimen.
9.2 Draw approximately5gofthe paint under test into a
Analyze the extracted pigment for TiO content in accordance
with theAluminum Reduction Method inTest Methods D1394 10-mL syringe and weigh to 1 mg. Transfer, by dropwise
addition, between 2.0 and 4.0 g of the specimen to a tared
and record the percent TiO found in the pigment.
6.7.2 Following the procedure in 12.1-12.5 take a specimen porcelaindishcontainingeither2mLofwater(forwater-borne
paint) or 2 mL of toluene (for solvent-borne paint). Reweigh
of the pigment extracted in 6.7.1 into solution. Store this
solution for no more than 3 months in a plastic bottle marked the syringe to 1 mg. Swirl the dish during the addition of the
paint and continue to swirl until the specimen is completely
with the percent TiO as determined in 6.7.1.
dispersed. If a water-borne paint tends to agglomerate or form
6.8 Sulfuric Acid (sp gr 1.84), concentrated sulfuric acid
lumps that cannot be dispersed, a drop or two of concentrated
(H SO ).
2 4
NH OH may help the dispersement. If the lumps persist,
6.9 Toluene.
discard the specimen, and prepare a new one. Prepare a
duplicate specimen in the same manner.
7. Hazards
9.3 Dry the specimens at 110°C for 30 min and then drive
7.1 Concentrated Hydrofluoric Acid—Make certain to ob-
off the remaining solvent or water at the lowest temperature
serve manufacturer’s recommended precautions for handling.
possibleusingaMekerburner(underahood).Donotleavethe
7.2 Warning—Nitrous oxide and acetylene can cause ex-
dishes on the burners after the flames have subsided.
plosions, if not used properly. See the supplier’s manual of
9.4
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D4563–86 (Reapproved 1996) Designation:D4563–02(Reapproved2008)
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
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
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 1394 Test Methods for Chemical Analysis of White Titanium Pigments
E 180 Practice for Determining the Precision Data of ASTM Methods for Analysis and Testing of Industrial and Specialty
Chemicals
E 288Specification for Volumetric Flasks Specification for Laboratory Glass Volumetric Flasks
3. Summary of Test Method
3.1 The specimen is prepared for analysis by ashing at 450°C followed by digestion with sulfuric acid and ammonium sulfate
as inTest Methods D 1394.The titanium content is determined by atomic absorption spectroscopy using a specimen similar to that
previously analyzed by the Aluminum Reduction Method in Test Methods D 1394.
3.2 By utilizing the pigment analyzed in Test Methods D 1394 as an atomic absorption standard, several hundred TiO
determinations can be made. The AA technique is much faster than the technique in Test Methods D 1394 for multiple
determinations and uses only acids. This keeps reagents and time to a minimum.
4. Significance and Use
4.1 This test method may be used in quality control laboratories when the repeated analysis of titanium dioxide in similar paints
may be required. Reagents and time are kept to a minimum when this test method is used in place of wet chemical analysis such
as in Test Methods D 1394. However, reproducibility and repeatability are not as good as in Test Methods D 1394.
5. Apparatus
5.1 Atomic Absorption Spectrophotometer , consisting of
5.1.1 Atomizer and nitrous oxide burner,
5.1.2 Gas-pressure regulator and metering devices for nitrous oxide and acetylene,
5.1.3 Titanium hollow cathode lamp with regulated constant-current supply,
5.1.4 Monochromator and associated optics,
This test method is under the jurisdiction of ASTM Committee D-1 on Paint and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Jan. 31, 1986. Published March 1986.
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 D01.21 on Chemical Analysis of Paints and Paint Materials .
Current edition approved Feb. 1, 2008. Published February 2008. Originally approved in 1986. Last previous edition approved in 2002 as D 4563 - 02.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4563–02 (2008)
5.1.5 Photosensitive detector connected to an electronic amplifier,
5.1.6 Readout device.
5.2 Muffle Furnace, capable of maintaining 450 6 25°C.
5.3 Circulating Oven, maintained at 105 6 2°C.
5.4 Porcelain Dishes, 90-mm diameter.
5.5 Plastic Disposable Syringe , 10-mL capacity.
5.6 Agate Mortar and Pestle, 95-mm outside diameter.
5.7 Wide-Mouth Erlenmeyer Flask , 500-mL capacity.
5.8 Hot Plate, with variable surface temperature control from 10°C above ambient to 370°C accurate to within 65°C.
5.9 Burner.
5.10 Volumetric Flask, 1000 mL, plastic (see Specification E 288).
5.11 Paint Shaker.
5.12 Weighing Bottles, wide-mouth, with an external-fitting cap, and no larger than necessary for required amount of sample.
5.13 Desiccator.
6. Reagents
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient high
purity to permit its use without reducing the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Type II of Specification D 1193.
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated ammonium hydroxide (NH OH).
6.4 Ammonium Sulfate (NH ) SO ).
4 2 4
6.5 Hydrochloric Acid (sp gr 1.19) —Concentrated hydrochloric acid (HCl).
6.6 Hydrofluoric Acid (HF)—Approximately 49 %.
6.7 Standard Pigment Solution .
6.7.1 Following the procedure in Section 9 recover the pigment from a paint that is similar to the unknown specimen.Analyze
the extracted pigment for TiO content in accordance with theAluminum Reduction Method in Test Methods D 1394 and record
the percent TiO found in the pigment.
6.7.2 Following the procedure in 12.1-12.5 take a specimen of the pigment extracted in 6.7.1 into solution. Store this solution
for no more than 3 months in a plastic bottle marked with the percent TiO as determined in 6.7.1.
6.8 Sulfuric Acid (sp gr 1.84), concentrated sulfuric acid (H SO ).
2 4
6.9 Toluene.
7. Hazards
7.1 Concentrated Hydrofluoric Acid— Make certain to observe manufacturer’s recommended precautions for handling.
7.2 Warning—Nitrousoxideandacetylenecancauseexplosions,ifnotusedproperly.Seethesupplier’smanualofinstructions
for the atomic absorption instrument for proper operation with these gases.
8. Calibration and Standardization
8.1 Operational instructions for atomic absorption spectrophotometers vary with different models. Consult the manufacturer’s
literature for establishing optimum conditions for the specific instrument used.
8.2 Turntheinstrumentonandsetthewavelengthtothe365.3-nmtitaniumline.Applytherecommendedcurrenttothetitanium
hollow cathode lamp. Allow the instrument to warm up for about 15 min and set the proper slit width. Adjust the gas pressures
and ignite the burner in accordance with instructions for using nitrous oxide and acetylene.
8.3 Aspirate the water to rinse the atomizer chamber from 10 to 15 min until the burner head achieves temperature equilibrium.
Set the instrument reading to zero while doing this. While aspirating the working standard from 6.7.2 set the instrument to the
percentTiO (determinedin6.7.1).ReaspiratethewaterandresettheinstrumenttoZERO.Repeatthisprocedureuntilthereadings
become stable.
8.3.1 Expanding the scale of a spectrophotometer increases the noise level of the readout system. Therefore, if expanding the
scale to make the readout indicate 60 % TiO has this effect, do not use any expansion. For instance, it is not necessary to make
the instrument read 60 for 60 % TiO standard. It may read 30. If 60 % equals 30, a pigment giving a reading of 25 would have
aTiO content of 50 %.
Annual Book of ASTM Standards, Vol 06.01.Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D4563–02 (2008)
PIGMENT CONTENT
9. Procedure
9.1 Mix the samples until homogenous, preferably on a mechanical shaker. If air bubbles become entrapped in the sample, stir
by hand.
9.2 Draw approximately5gofthe paint under test into a 10-mL syringe and weigh to 1 mg. Trans
...
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