ASTM D3969-85(1994)
(Test Method)Standard Test Method for Zirconium in Paint Driers by EDTA Method
Standard Test Method for Zirconium in Paint Driers by EDTA Method
SCOPE
1.1 This test method covers the titrimetric determination of zirconium in zirconium driers used in the coatings industry and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA).
1.2 This test method is limited to the determination of the zirconium content of a liquid zirconium drier that does not contain other drier elements. The test method is not applicable to drier blends and does not differentiate hafnium from zirconium.
1.3 All cations that can be titrated with EDTA in acid media interfere and must not be present in the sample.
1.4 This test method has been tested for concentrations of 6 and 12% zirconium, but there is no reason to believe that it is not suitable for higher or lower zirconium concentrations provided specimen size is adjusted proportionately.
1.5 This standard does not purport to address the safety problems 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.
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Designation: D 3969 – 85 (Reapproved 1994)
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
Zirconium in Paint Driers by EDTA Method
This standard is issued under the fixed designation D 3969; 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 matter. The diluted solution is boiled with an excess of EDTA,
the pH adjusted, and the excess titrated with bismuth nitrate
1.1 This test method covers the titrimetric determination of
using xylenol orange as the indicator.
zirconium in zirconium driers used in the coatings industry and
utilizes the disodium salt of ethylenediaminetetraacetic acid
4. Significance and Use
dihydrate (EDTA).
4.1 The amount of zirconium drier used in oxidizing-type
1.2 This test method is limited to the determination of the
coatings significantly affects their drying properties. This test
zirconium content of a liquid zirconium drier that does not
method may be used to confirm the stated content of a pure
contain other drier elements. The test method is not applicable
liquid zirconium drier manufactured for use by the coatings
to drier blends and does not differentiate hafnium from
industry.
zirconium.
1.3 All cations that can be titrated with EDTA in acid media
5. Apparatus
interfere and must not be present in the sample.
5.1 Centrifuge, capable of developing 1000 to 2000 g.
1.4 This test method has been tested for concentrations of 6
and 12 % zirconium, but there is no reason to believe that it is
6. Reagents
not suitable for higher or lower zirconium concentrations
6.1 Purity of Reagents—Reagent grade chemicals shall be
provided specimen size is adjusted proportionately.
used in all tests. Unless otherwise indicated, it is intended that
1.5 This standard does not purport to address all of the
all reagents shall conform to the specifications of the Commit-
safety concerns, if any, associated with its use. It is the
tee on Analytical Reagents of the American Chemical Society,
responsibility of the user of this standard to establish appro-
where such specifications are available. Other grades may be
priate safety and health practices and determine the applica-
used, provided it is first ascertained that the reagent is of
bility of regulatory limitations prior to use.
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
2. Referenced Documents
6.2 Purity of Water—Unless otherwise indicated, references
2.1 ASTM Standards:
2 to water shall be understood to mean reagent water conforming
D 600 Specification for Liquid Paint Driers
to Type II of Specification D 1193.
D 1193 Specification for Reagent Water
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated, am-
E 180 Practice for Determining the Precision of ASTM
monium hydroxide (NH OH).
Methods for Analysis and Testing of Industrial Chemicals
5 6.4 Bismuth Nitrate, Standard Solution (0.05 M)—Dissolve
E 300 Practice for Sampling Industrial Chemicals
24.25 g of bismuth nitrate (Bi(NO )·5H O) in 20 to 30 mL of
3 2
3. Summary of Test Method concentrated nitric acid (use a magnetic stirrer if possible).
After solution is complete, dilute to 1 L with water.
3.1 The zirconium drier is digested with concentrated sul-
furic acid and 30 % hydrogen peroxide to destroy all organic
NOTE 1—Add the water very slowly to the acid solution, while cooling
the flask in an ice bath to prevent splattering.
6.5 EDTA, Standard Solution (0.05 M)—Dissolve 18.61 g
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 of EDTA in 300 to 500 mL of water and dilute to 1 L. Store in
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
a polyethylene or borosilicate glass bottle.
Current edition approved Oct. 25, 1985. Published December 1985. Originally
6.6 Eriochrome Black-T Indicator—Triturate 0.100 g of
published as D 3969 – 80. Last previous edition D 3969 – 80.
powdered Eriochrome Black-T with 100 g of sodium chloride
Annual Book of ASTM Standards, Vol 06.04.
Annual Book of ASTM Standards, Vol 11.01.
(NaCl), and store the mixture in a tightly stoppered bottle. This
Annual Book of ASTM Standards, Vol 15.05.
mixture remains stable for several years.
Reagent Chemicals, American Chemical Society Specifications, American
6.7 Formic Acid (sp gr 1.22, 90 %) HCOOH.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory 6.8 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
chloric acid (HCl).
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
6.9 Hydrogen Peroxide (30 %).
MD.
D 3969
6.10 Isopropyl Alcohol (99.5 %).
V 5 volume of EDTA solution, mL.
6.11 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
8.3 Bismuth Nitrate, Standard Solution (0.05 M)—Pipet 24
(HNO ).
3 mL of 0.05 M EDTA into a 250-mL Erlenmeyer flask, add 75
6.12 Phenolphthalein Indicator (1.0 %)—Dissolve 1.0 g of
mL of distilled water, neutralize with concentrated NH OH to
phenolphthalein indicator in 100 mL of methanol, ethanol, or
a pink end point with phenolphthalein, and then add 15 mL of
isopropanol.
concentrated formic acid. After cooling to room temperature,
6.13 Sodium Sulfite (Na SO ).
2 3 titrate with 0.05 M bismuth nitrate solution and xylenol orange
6.14 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
from a yellow to a pink end point.
(H SO ).
2 4 8.3.1 Calculate the molarity, M , of the Bi(NO ) solution as
3 3 3
6.15 Xylenol Orange (0.2 %)—Dissolve 0.2 g in 100 mL of
follows:
water. Prepare fresh each day used.
V M
3 2
6.16 Zinc Chloride, Standard Solution (0.100 M)— Dis- M 5 (3)
V
solve 6.538 g of zinc ribbon (Note 2) in concentrated HCl,
keeping the excess of acid as small as possible. After the zinc where:
has dissolved, cool to room t
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