ASTM D3988-85(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D3988–85(Reapproved 1999)
Standard Test Method for
Vanadium in Paint Driers by EDTA Method
This standard is issued under the fixed designation D 3988; 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 titrimetric determination of 4.1 This test method may be used to confirm the stated
vanadium in liquid vanadium driers and utilizes the disodium content of a pure liquid vanadium drier manufactured for use
salt of ethylenediaminetetraacetic acid dihydrate (EDTA). by the coatings industry.
1.2 This test method is limited to the determination of the
5. Apparatus
vanadium content of a liquid vanadium drier that does not
5.1 Centrifuge, capable of developing 1000 to 2000 g.
contain other drier elements. This test method is not applicable
to drier blends.
6. Reagents
1.3 All cations that can be titrated with EDTA in alkaline
6.1 Purity of Reagents—Reagent grade chemicals shall be
media interfere and must not be present in the sample.
used in all tests. Unless otherwise indicated, it is intended that
1.4 This test method has been tested for concentrations of 3
all reagents shall conform to the specifications of the Commit-
and 4 % vanadium, but there is no reason to believe that it is
tee onAnalytical Reagents of theAmerican Chemical Society,
not suitable for higher or lower vanadium concentrations
where such specifications are available. Other grades may be
provided specimen size is adjusted proportionately.
used, provided it is first ascertained that the reagent is of
1.5 This standard does not purport to address all of the
sufficiently high purity to permit its use without lessening the
safety concerns, if any, associated with its use. It is the
accuracy of the determination.
responsibility of the user of this standard to establish appro-
6.2 Purity of Water—Unless otherwise indicated, reference
priate safety and health practices and determine the applica-
to water shall be understood to mean reagent water conforming
bility of regulatory limitations prior to use.
to Type II of Specification D 1193.
2. Referenced Documents
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
2.1 ASTM Standards: monium hydroxide (NH OH).
6.4 Ascorbic Acid.
D 600 Specification for Liquid Paint Driers
D 1193 Specification for Reagent Water 6.5 Buffer Solution—Add 350 mL of concentrated NH OH
to 54 g of ammonium chloride and dilute to 1 L with water.
E 180 Practice for Determining the Precision of ASTM
Methods forAnalysis and Testing of Industrial Chemicals 6.6 Eriochrome Black T Indicator—Mix and grind thor-
oughly in a mortar a mixture of 0.2 g of Eriochrome Black T
E 300 Practice for Sampling Industrial Chemicals
and 100 g of sodium chloride. Store the mixture in a tightly
3. Summary of Test Method
stoppered bottle where it is stable indefinitely.
3.1 The amount of vanadium drier used in oxidizing-type 6.7 EDTA, Standard Solution (0.01 M)—Weigh about 3.73
coatings significantly affects their drying properties. The vana- g of EDTA to the nearest 0.01 g, dissolve in water, and dilute
dium drier is acidified and heated to make the vanadium to approximately 1 L in a glass-stoppered bottle.
available for chelation with EDTA. It is then chelated, the pH 6.8 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
adjusted, and the excess titrated with zinc chloride solution, chloric acid (HCl).
using Eriochrome Black T as the indicator. 6.9 Isopropyl Alcohol, 99.5 %.
6.10 Zinc Chloride, Standard Solution (ZnCl ) (0.01 M)—
Weigh about 0.65 g of zinc (Note 1) to 5 mg. Transfer to a 1-L
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, andApplications and is the direct responsibility of
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Oct. 25, 1985. Published December 1985. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as D 3988 – 81. Last previous edition D 3988 – 81a.
listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 06.04. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.05. MD.
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D3988
NOTE 4—This is the correct specimen weight range for a vanadium
volumetric flask, and add 25 mL of dilute hydrochloric acid
drier containing 3 to 6 % of vanadium (16 to 24 mL of standard 0.01 M
(1 + 3). Warm if necessary on a steam bath to dissolve the
ZnCl solution is required for the titration).
material completely. Cool, dilute to the mark with water and
9.3 Add to each flask, 15 mL of isopropyl alcohol and 1.0
mix thoroughly.
mL of concentrated HCl. Boil the solutions (use a steam bath
NOTE 1—Store the zinc ribbon in a tightly closed container to prevent
if possible, and boiling aids) gently for 5 min, then cool for 5
the surface of the zinc from oxidizing.
to 10 min in a cold water bath (Note 5). Add 35 mL more of
7. Sampling isopropyl alcohol to each flask.
7.1 Take a small sample of liquid drier from bulk using the
NOTE 5—Boiling with HCl converts, bi-
...