D2374 PDF
D2374 PDF
D2374 PDF
1. Scope 5. Apparatus
1.1 This test method covers a titrimetric determination of 5.1 Centrifuge, capable of developing 1000 to 2000 g.
lead in liquid paint driers that can be dissolved in glacial acetic
acid and utilizes the disodium salt of ethylenediaminetetraace- 6. Reagents
tic acid dihydrate (EDTA). 6.1 Purity of Reagents—Reagent grade chemicals shall be
1.2 This test method is not applicable to drier blends. If used in all tests. Unless otherwise indicated, it is intended that
driers other than cobalt are present, they may interfere by all reagents shall conform to the specifications of the Commit-
reacting with EDTA under the conditions used for analysis. tee on Analytical Reagents of the American Chemical Society,
1.3 All cations that can be titrated with EDTA in alkaline where such specifications are available.5 Other grades may be
media interfere and must not be present in the sample. used, provided it is first ascertained that the reagent is of
1.4 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, references
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.
6.3 Ammonium Chloride (NH4Cl).
2. Referenced Documents 6.4 Ammonium Hydroxide (sp gr 0.90)—Concentrated am-
2.1 ASTM Standards: monium hydroxide (NH4OH).
D 600 Specification for Liquid Paint Driers2 6.5 Buffer Solution (pH 10.0)—Dissolve 67.5 g of NH4Cl in
D 1193 Specification for Reagent Water3 water, add 570 mL of concentrated NH4OH (sp gr 0.90), and
E 180 Practice for Determining the Precision of ASTM dilute to 1 L.
Methods for Analysis and Testing of Industrial Chemicals4 6.6 Cupric Sulfate, Standard Solution (0.05 M)—Dissolve
E 300 Practice for Sampling Industrial Chemicals4 12.5 g of cupric sulfate pentahydrate (CuSO4·5H2O) in water
and dilute to 1 L.
3. Summary of Test Method 6.7 Eriochrome Black-T Indicator—Triturate 0.20 g of the
3.1 The liquid drier is dissolved in glacial acetic acid, concentrated dye with 100 g of NaCl and store in a tightly
diluted with isopropyl alcohol and water, and treated with an stoppered jar. This mixture remains stable for several years.
excess of standard EDTA solution. The excess is titrated with 6.8 EDTA, Standard Solution (0.05 M)—Dissolve 18.62 g
standard cupric sulfate solution using PAN as the metal of EDTA in water and dilute to 1 L. Store in a polyethylene or
indicator. borosilicate glass bottle.
6.9 Glacial Acetic Acid (sp gr 1.06).
4. Significance and Use 6.10 Isopropyl Alcohol (99.5 %).
4.1 The amount of lead drier used in oxidizing-type coatings 6.11 Methyl Red Indicator—Dissolve 0.2 g of methyl red in
significantly affects their drying properties. This test method 100 mL of methanol, ethanol, or isopropanol.
may be used to confirm the stated lead content of pure liquid 6.12 PAN Indicator (1(2-Pyridylazo)-2-Naphthol)—Prepare
lead drier soluble in glacial acetic acid and manufactured for a dilute solution of the indicator by dissolving 0.10 g in 100 mL
use by the coatings industry. of ethanol or isopropanol.
6.13 Sodium Acetate Solution—Prepare a saturated aqueous
solution of sodium acetate (NaC2H3O2) in water.
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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
5
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 2374 – 65 T. Last previous edition D 2374 – 79. listed by the American Chemical Society, see Analar Standards for Laboratory
2
Annual Book of ASTM Standards, Vol 06.04. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
3
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
4
Annual Book of ASTM Standards, Vol 15.05. MD.
1
D 2374
6.14 Sodium Chloride (NaCl). M1 5 molarity of EDTA solution,
6.15 Sodium Hydroxide Solution (80 g/L)—Dissolve 80 g of V2 5 EDTA solution, mL, and
sodium hydroxide (NaOH) in water and dilute to 1 L. V3 5 CuSO4 solution, mL.
6.16 Sulfuric Acid (5+1)—Carefully mix 8 volumes of
concentrated sulfuric acid (H2SO4, sp gr 1.84) with 1 volume 9. Procedure
of water. 9.1 Check the clarity of the drier. If not clear, centrifuge a
6.17 Zinc Oxide (ZnO). portion of the sample until it is clear. Keep the centrifuge tube
stoppered so that solvent will not evaporate.
7. Sampling 9.2 Weigh the following specimen amounts into a 500-mL
7.1 Take a small sample of liquid drier from bulk using the Erlenmeyer flask and add 5 mL of glacial acetic acid: (1) for
procedures in Practice E 300 appropriate for the size of the 24 % lead, 1.0 to 1.5 g, (2) for 30 and 32 % lead, 0.7 to 0.9 g
container: section on Bottle Sampling for tanks and tank cars, and (3) for more or less lead use proportionate specimen sizes.
or section on Tube Sampling for drums and cans. Warm on a hot plate at low heat, swirling the flask until the
specimen is completely dissolved.
NOTE 1—Liquid driers are normally homogeneous so that only simple
9.3 In a second flask (blank) put the same amount of glacial
physical tests, such as specific gravity or solids content, on top and bottom
samples from tanks are required to confirm that separation has not acetic acid but no specimen. Add 200 mL of isopropyl alcohol,
occurred. Agitate drums in accordance with the section on Tube Sampling 100 mL of water, 6 mL of concentrated NH4OH, 10 mL of
of Practice E 300. Na2C2H3O2, and 50 mL of EDTA solution to each flask. Swirl
to ensure complete mixing and warm both flasks at steam bath
7.2 Examine the sample of drier for sediment or suspended
temperature for 5 min.
matter which if present is evidence of noncompliance with
9.4 To each of the flasks add 2 mL of PAN indicator and
Specification D 600.
titrate with the standard CuSO4 solution to a blue end point.
7.3 If the sample is homogeneous keep it in a stoppered
vessel to prevent solvent evaporation prior to analysis. NOTE 2—Because of the color of metal indicators (and some of their
complexes) being affected by pH changes, the pH must be kept constant
8. Standardization during titration by the recommended buffer during titration.
8.1 Weigh to the nearest 0.1 mg approximately 1.5 g of ZnO 10. Calculation
into a 100-mL beaker and add 10 mL of H2SO4(8 + 1). Transfer 10.1 Calculate the percent of lead, A, present as follows:
the solution to a 500-mL volumetric flask and dilute to the
mark with water. Pipet a 50-mL aliquot into a 500-mL
Erlenmeyer flask, add 100 mL of distilled water, 2 or 3 drops
A 5 F ~ B 2 V 4 ! 3 M2 3 F
S G 3 100 (3)
of methyl red solution, and neutralize with NaOH solution (80 where:
g/L). Add 5 mL of buffer solution, 0.2 g of Eriochrome Black-T B 5 CuSO4 solution required for titration of the blank,
indicator, and titrate with EDTA until the color changes from mL,
red to blue, where the last red shade just disappears. V4 5 CuSO4 solution required for the specimen, mL,
8.1.1 Calculate the molarity, M1, of the EDTA solution as M2 5 molarity of CuSO4 solution,
follows: F 5 millimolecular weight of the metal in the sample
W 5 0.2072 for lead, and
M1 5
~V1 3 0.0814!
(1) S 5 specimen used, g.
2
D 2374
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