ASTM D3988-05(2017)
(Test Method)Standard Test Method for Vanadium in Paint Driers by EDTA Method
Standard Test Method for Vanadium in Paint Driers by EDTA Method
SIGNIFICANCE AND USE
4.1 This test method may be used to confirm the stated content of a pure liquid vanadium drier manufactured for use by the coatings industry.
SCOPE
1.1 This test method covers the titrimetric determination of vanadium in liquid vanadium driers and utilizes the disodium salt of ethylenediaminetetraacetic acid dihydrate (EDTA).
1.2 This test method is limited to the determination of the vanadium content of a liquid vanadium drier that does not contain other drier elements. This test method is not applicable to drier blends.
1.3 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample.
1.4 This test method has been tested for concentrations of 3 and 4 % vanadium, but there is no reason to believe that it is not suitable for higher or lower vanadium concentrations provided specimen size is adjusted proportionately.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of 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.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
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Designation: D3988 − 05 (Reapproved 2017)
Standard Test Method for
Vanadium in Paint Driers by EDTA Method
This standard is issued under the fixed designation D3988; 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 D1193 Specification for Reagent Water
E180 Practice for Determining the Precision of ASTM
1.1 This test method covers the titrimetric determination of
Methods for Analysis and Testing of Industrial and Spe-
vanadium in liquid vanadium driers and utilizes the disodium
cialty Chemicals (Withdrawn 2009)
salt of ethylenediaminetetraacetic acid dihydrate (EDTA).
E300 Practice for Sampling Industrial Chemicals
1.2 This test method is limited to the determination of the
vanadium content of a liquid vanadium drier that does not
3. Summary of Test Method
contain other drier elements. This test method is not applicable
3.1 The amount of vanadium drier used in oxidizing-type
to drier blends.
coatings significantly affects their drying properties. The vana-
1.3 All cations that can be titrated with EDTA in alkaline
dium drier is acidified and heated to make the vanadium
media interfere and must not be present in the sample.
available for chelation with EDTA. It is then chelated, the pH
adjusted, and the excess titrated with zinc chloride solution,
1.4 This test method has been tested for concentrations of 3
using Eriochrome Black T as the indicator.
and 4 % vanadium, but there is no reason to believe that it is
not suitable for higher or lower vanadium concentrations
4. Significance and Use
provided specimen size is adjusted proportionately.
4.1 This test method may be used to confirm the stated
1.5 The values stated in SI units are to be regarded as
content of a pure liquid vanadium drier manufactured for use
standard. No other units of measurement are included in this
by the coatings industry.
standard.
1.6 This standard does not purport to address all of the
5. Apparatus
safety concerns, if any, associated with its use. It is the
5.1 Centrifuge, capable of developing 1000 to 2000 g.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 6. Reagents
1.7 This international standard was developed in accor-
6.1 Purity of Reagents—Reagent grade chemicals shall be
dance with internationally recognized principles on standard-
used in all tests. Unless otherwise indicated, it is intended that
ization established in the Decision on Principles for the
all reagents shall conform to the specifications of the Commit-
Development of International Standards, Guides and Recom-
tee on Analytical Reagents of the American Chemical Society,
mendations issued by the World Trade Organization Technical
where such specifications are available. Other grades may be
Barriers to Trade (TBT) Committee.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
2. Referenced Documents
accuracy of the determination.
2.1 ASTM Standards:
6.2 Purity of Water—Unless otherwise indicated, reference
D600 Specification for Liquid Paint Driers
to water shall be understood to mean reagent water conforming
to Type II of Specification D1193.
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. The last approved version of this historical standard is referenced on
Current edition approved July 1, 2017. Published July 2017. Originally approved www.astm.org.
in 1981. Last previous edition approved in 2011 as D3988 – 05 (2011). DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D3988-05R17. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3988 − 05 (2017)
solution to the mixture and titrate again with standard ZnCl solution. Use
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
total volume of each solution for the calculation.
monium hydroxide (NH OH).
8.2.1 Calculate the molarity of the EDTA solution, M , as
6.4 Ascorbic Acid.
follows:
6.5 Buffer Solution—Add 350 mL of concentrated NH OH
M 5 V M /V (2)
2 1 1 2
to 54 g of ammonium chloride and dilute to 1 L with water.
where:
6.6 Eriochrome Black T Indicator—Mix and grind thor-
V = volume of ZnCl solution, mL,
oughly in a mortar a mixture of 0.2 g of Eriochrome Black T
1 2
M = molarity of ZnCl solution, and
and 100 g of sodium chloride. Store the mixture in a tightly
1 2
V = volume of EDTA solution, mL.
stoppered bottle where it is stable indefinitely. 2
6.7 EDTA, Standard Solution (0.01 M)—Weigh about 3.73 g
9. Procedure
of EDTA to the nearest 0.01 g, dissolve in water, and dilute to
9.1 Check the clarity of the drier. If not clear, centrifuge a
approximately 1 L in a glass-stoppered bottle.
portion of the sample until it is clear, keeping the centrifuge
6.8 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
tube stoppered to prevent solvent evaporation.
chloric acid (HCl).
9.2 Place a few grams of the drier in a 50-mL Erlenmeyer
6.9 Isopropyl Alcohol, 99.5 %.
flask fitted with a cork through which passes a dropping tube
and rubber bulb (or eye dropper) and obtain the total weight.
6.10 Zinc Chloride, Standard Solution (ZnCl ) (0.01 M)—
Weigh by difference to 0.5 mg two or three 0.18 to 0.22-g
Weigh about 0.65 g of zinc (Note 1) to 5 mg. Transfer to a 1-L
specimens into 250-mL wide-mouth flasks.
volumetric flask, and add 25 mL of dilute hydrochloric acid
(1 + 3). Warm if necessary on a steam bath to
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D3988 − 05 (Reapproved 2011) D3988 − 05 (Reapproved 2017)
Standard Test Method for
Vanadium in Paint Driers by EDTA Method
This standard is issued under the fixed designation D3988; 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
1.1 This test method covers the titrimetric determination of vanadium in liquid vanadium driers and utilizes the disodium salt
of ethylenediaminetetraacetic acid dihydrate (EDTA).
1.2 This test method is limited to the determination of the vanadium content of a liquid vanadium drier that does not contain
other drier elements. This test method is not applicable to drier blends.
1.3 All cations that can be titrated with EDTA in alkaline media interfere and must not be present in the sample.
1.4 This test method has been tested for concentrations of 3 and 4 % vanadium, but there is no reason to believe that it is not
suitable for higher or lower vanadium concentrations provided specimen size is adjusted proportionately.
1.5 TTheThe values stated in SI units are to be regarded as standard. No other units of measurement are included in this
standard.
1.6 This standard does not purport to address all of 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.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D600 Specification for Liquid Paint Driers
D1193 Specification for Reagent Water
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
(Withdrawn 2009)
E300 Practice for Sampling Industrial Chemicals
3. Summary of Test Method
3.1 The amount of vanadium drier used in oxidizing-type coatings significantly affects their drying properties. The vanadium
drier is acidified and heated to make the vanadium available for chelation with EDTA. It is then chelated, the pH adjusted, and
the excess titrated with zinc chloride solution, using Eriochrome Black T as the indicator.
4. Significance and Use
4.1 This test method may be used to confirm the stated content of a pure liquid vanadium drier manufactured for use by the
coatings industry.
5. Apparatus
5.1 Centrifuge, capable of developing 1000 to 2000 g.
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 June 1, 2011July 1, 2017. Published June 2011July 2017. Originally approved in 1981. Last previous edition approved in 20052011 as D3988 – 05
(2011). . DOI: 10.1520/D3988-05R11.10.1520/D3988-05R17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3988 − 05 (2017)
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 sufficiently high
purity to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, reference to water shall be understood to mean reagent water conforming to
Type II of Specification D1193.
6.3 Ammonium Hydroxide (sp gr 0.90)—Concentrated ammonium hydroxide (NH OH).
6.4 Ascorbic Acid.
6.5 Buffer Solution—Add 350 mL of concentrated NH OH to 54 g of ammonium chloride and dilute to 1 L with water.
6.6 Eriochrome Black T Indicator—Mix and grind thoroughly in a mortar a mixture of 0.2 g of Eriochrome Black T and 100
g of sodium chloride. Store the mixture in a tightly stoppered bottle where it is stable indefinitely.
6.7 EDTA, Standard Solution (0.01 M)—Weigh about 3.73 g of EDTA to the nearest 0.01 g, dissolve in water, and dilute to
approximately 1 L in a glass-stoppered bottle.
6.8 Hydrochloric Acid (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
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
volumetric flask, and add 25 mL of dilute hydrochloric acid (1 + 3). Warm if necessary on a steam bath to dissolve the material
completely. Cool, dilute to the mark with water and mix thoroughly.
NOTE 1—Store the zinc ribbon in a tightly closed container to prevent the surface of the zinc from oxidizing.
7. Sampling
7.1 Take a small sample of liquid drier from bulk using the procedure in Practice E300 appropriate for the size of the container:
section on Bottle Sampling for tanks and tank cars, or section on Tube Sampling for drums and cans.
NOTE 2—Liquid driers are normally homogeneous so that only simple physical tests, such as specific gravity or solids content, on top and bottom
samples from tanks, are required to confirm that separation has not occurred. Agitate the drums in accordance with the section on Tube Sampling of
Practice E300.
7.2 Examine the sample of drier for sediment or suspended matter which, if present, is evidence of noncompliance with
Specification D600.
7.3 If the sample is homogeneous keep it in a stoppered vessel to prevent solvent evaporation prior to analysis.
8. Standardization
8.1 Zinc Chloride, Standard Solution
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