ASTM D3969-01

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.

General Information

• Status: Historical
• Publication Date: 09-Jan-2001
• ICS: 87.060.99 - Other paint ingredients
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.21 - Chemical Analysis of Paints and Paint Materials

Relations

• Replaces: ASTM D3969-85(1994) - Standard Test Method for Zirconium in Paint Driers by EDTA Method
• Effective Date: 10-Jan-2001
• Replaced By: ASTM D3969-01(2006) - Standard Test Method for Zirconium in Paint Driers by EDTA Method
• Effective Date: 01-Jun-2006
• Referred By: ASTM D564-87(2023) - Standard Test Methods for Liquid Paint Driers
• Effective Date: 10-Jan-2001

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3969–01
Standard Test Method for
1
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 3. Summary of Test Method
1.1 This test method covers the titrimetric determination of 3.1 The zirconium drier is digested with concentrated sul-
zirconium in zirconium driers used in the coatings industry and furic acid and 30 % hydrogen peroxide to destroy all organic
utilizes the disodium salt of ethylenediaminetetraacetic acid matter. The diluted solution is boiled with an excess of EDTA,
dihydrate (EDTA). the pH adjusted, and the excess titrated with bismuth nitrate
1.2 This test method is limited to the determination of the using xylenol orange as the indicator.
zirconium content of a liquid zirconium drier that does not
4. Significance and Use
contain other drier elements. The test method is not applicable
4.1 The amount of zirconium drier used in oxidizing-type
to drier blends and does not differentiate hafnium from
zirconium. coatings significantly affects their drying properties. This test
method may be used to confirm the stated content of a pure
1.3 All cations that can be titrated with EDTAin acid media
interfere and must not be present in the sample. liquid zirconium drier manufactured for use by the coatings
industry.
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
5. Apparatus
not suitable for higher or lower zirconium concentrations,
5.1 Centrifuge, capable of developing 1000 to 2000 g.
provided specimen size is adjusted proportionately.
1.5 This standard does not purport to address all of the
6. Reagents
safety concerns, if any, associated with its use. It is the
6.1 Purity of Reagents—Reagent grade chemicals shall be
responsibility of the user of this standard to establish appro-
used in all tests. Unless otherwise indicated, it is intended that
priate safety and health practices and determine the applica-
all reagents shall conform to the specifications of the Commit-
bility of regulatory limitations prior to use.
tee onAnalytical Reagents of theAmerican Chemical Society,
5
2. Referenced Documents
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
2.1 ASTM Standards:
2
sufficiently high purity to permit its use without lessening the
D 600 Specification for Liquid Paint Driers
3
accuracy of the determination.
D 1193 Specification for Reagent Water
6.2 Purity of Water—Unless otherwise indicated, references
E 180 Practice for Determining the Precision of ASTM
to water shall be understood to mean reagent water conforming
Methods for Analysis and Testing of Industrial and Spe-
4
to Type II of Specification D 1193.
cialty Chemicals
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated, am-
E 300 Practice for Sampling Industrial and Specialty
5
monium hydroxide (NH OH).
Chemicals
4
6.4 Bismuth Nitrate, Standard Solution (0.05 M)—Dissolve
24.25 g of bismuth nitrate (Bi(NO )·5H O) in 20 to 30 mL of
3 2
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
concentrated nitric acid (use a magnetic stirrer if possible).
and Related Coatings, Materials, andApplications and is the direct responsibility of
After solution is complete, dilute to 1 L with water.
Subcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.
Current edition approved Jan. 10, 2001. Published April 2001. Originally
NOTE 1—Add the water very slowly to the acid solution, while cooling
published as D 3969 – 80. Last previous edition D 3969 – 85 (1994).
the flask in an ice bath to prevent splattering.
2
Annual Book of ASTM Standards, Vol 06.04.
3
Annual Book of ASTM Standards, Vol 11.01.
6.5 EDTA, Standard Solution (0.05 M)—Dissolve 18.61 g
4
Annual Book of ASTM Standards, Vol 15.05.
of EDTAin 300 to 500 mL of water and dilute to 1 L. Store in
5
Reagent Chemicals, American Chemical Society Specifications, American
a polyethylene or borosilicate glass bottle.
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.
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