Designation: D 521 – 02

Standard Test Methods for

Chemical Analysis of Zinc Dust (Metallic Zinc Powder)1
This standard is issued under the fixed designation D 521; 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 E 40 Test Method for Chemical Analysis of Slab Zinc

1.1 These test methods cover procedures for the chemical (Spelter)6
analysis of metallic zinc powder in the form commercially E 68 Method for Polarographic Determination of Lead and
known as zinc dust for use as a pigment in paints. Cadmium in Zinc7
1.2 The analytical procedures appear in the following order: 3. Significance and Use
Sections
Moisture and Other Volatile Matter 7 3.1 These test methods compile procedures which can be
Coarse Particles 8 used to check the composition of purity of metallic zinc
Matter Soluble in Hexane 9 and 10
Total Zinc 11 and 12
powder. This information is useful to both the formulator and
Metallic Zinc 13 and 14 users.
Zinc Oxide 15
Calcium 16 and 17 4. Treatment of Sample
Lead 18
Iron 19 4.1 Store the laboratory sample in a tightly stoppered bottle
Cadmium 20 to protect it from oxidation. Mix the whole sample thoroughly
Chlorine 21 and 22
Sulfur 23 and 24
before taking portions for analysis.

1.3 This standard does not purport to address all of the 5. Purity of Reagents
safety concerns, if any, associated with its use. It is the 5.1 Purity of Reagents—Unless otherwise indicated, it is
responsibility of the user of this standard to establish appro- intended that all reagents shall conform to the specifications of
priate safety and health practices and determine the applica- the Committee on Analytical Reagents of the American Chemi-
bility of regulatory limitations prior to use. cal Society, where such specifications are available.8 Other
grades may be used, provided it is first ascertained that the
2. Referenced Documents
reagent is of sufficiently high purity to permit its use without
2.1 ASTM Standards: lessening the accuracy of the determination.
B 214 Test Method for Sieve Analysis of Metal Powders2 5.2 Purity of Water—Unless otherwise indicated, references
D 185 Test Methods for Coarse Particles in Pigments, to water shall be understood to mean reagent water conforming
Pastes, and Paints3 to Type II of Specification D 1193.
D 280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments3 6. Precision
D 1193 Specification for Reagent Water4 6.1 Precision statements have not been established.
D 6580 Test Method for The Determination of Metallic
Zinc Content in Both Zinc Dust Pigment and in Cured
Films of Zinc-Rich Coatings5

1
These test methods are under the jurisdiction of ASTM Committee D01 on
6
Paint and Related Coatings, Materials, and Applications and are the direct Discontinued—See 1993 Annual Book of ASTM Standards, Vol 03.05.
7
responsibility of Subcommittee D01.31 on Pigment Specifications. Discontinued—See 1979 Annual Book of ASTM Standards, Part 12.
8
Current edition approved Jan. 10, 2002. Published March 2002. Originally Reagent Chemicals, American Chemical Society Specifications, American
published as D 521 – 39 T. Last previous edition D 521 – 90(1999). Chemical Society, Washington, DC. For suggestions on the testing of reagents not
2
Annual Book of ASTM Standards, Vol 02.05. listed by the American Chemical Society, see Analar Standards for Laboratory
3
Annual Book of ASTM Standards, Vol 06.03. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
4
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
5
Annual Book of ASTM Standards, Vol 06.01. MD.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 521
MOISTURE AND OTHER VOLATILE MATTER W = zinc used (or equivalent to the ZnO used), g,
V1 = K4Fe(CN) 6 solution required for titration of the
7. Procedure standard, mL, and
7.1 Determine moisture and other volatile matter in accor- B = K4Fe(CN)6 solution required for titration of the
dance with Method A of Test Methods D 280, except heat the blank, mL.
sample for only 1 h. 11.2 Uranyl Nitrate Indicator Solution— Dissolve 5 g of
uranyl nitrate (UO2(NO3)2·6H 2O) in 100 mL of water.
COARSE PARTICLES
12. Procedure
8. Procedure
12.1 Transfer 0.25 g of the sample to a 400-mL beaker,
8.1 Determine the percent of coarse particles in the pigment moisten with alcohol, and dissolve in 10 mL of HCl (sp gr
in accordance with Test Methods D 185 or B 214. 1.19) and 20 mL of water.
12.2 Continue with the procedure used in standardizing the
MATTER SOLUBLE IN HEXANE
K4Fe(CN)6 solution as described in 10.1, beginning with the
9. Reagent addition of the litmus paper and the adjustment of the acidity
with NH4OH and HCl.
9.1 Hexane—Pure hexane or commercial hexane or petro- 12.3 Calculation—Calculate the percent of total zinc, T, as
leum ether of boiling point not higher than 75°C. Redistill follows:
before using.
T 5 @~V2 2 B2!Z/S1# 3 100 (2)
10. Procedure
where:
10.1 Place 100 g of the pigment in an extraction thimble in V 2 = K4Fe(CN)6 solution required for titration of the
a Soxhlet extraction apparatus. Record the tare weight of the specimen, mL,
receiving flask. Charge the flask with a suitable volume of B2 = K4Fe(CN) 6 solution required for titration of the
hexane and extract the sample for 4 h, subjecting the specimen blank, mL,
to not less than 20 extractions in this time. Make a blank Z = zinc equivalent of the K4Fe(CN)6 solution, g/mL,
determination at the same time. and
10.2 Remove the receiving flask, evaporate or distill off the S1 = sample used, g.
hexane on a steam bath, and dry the flask at 105 6 2°C for 1
h. Cool and weigh. METALLIC ZINC
10.3 Calculate the percent of matter soluble in hexane, NOTE 1—Sections 12 and 13 cover a rapid method for determining
allowing for any material found in the blank. metallic zinc, intended for routine analysis. The results are inclined to be
somewhat low, and for highest accuracy and particularly for referee tests,
TOTAL ZINC the hydrogen evolution method should be used.9
NOTE 2—Metallic zinc may also be determined in accordance with Test
11. Reagents Method D 6580.
11.1 Potassium Ferrocyanide, Standard Solution—Dissolve 13. Reagents
22 g of potassium ferrocyanide (K4Fe(CN)6·3H 2O) in water
and dilute to 1 L. To standardize, transfer 0.2 g of metallic zinc 13.1 Ferric Chloride Solution—Prepare a solution contain-
or freshly ignited zinc oxide (ZnO) to a 400-mL beaker. ing 20 g of ferric chloride (FeCl3·6H 2O) and 20 mL of 20 %
Dissolve in 10 mL of hydrochloric acid (HCl), sp gr 1.19 and sodium acetate (NaC2H3O2) solution per 100 mL. It is advis-
20 mL of water. Drop in a small piece of litmus paper, add able to make up only one day’s supply at a time (50 mL are
ammonium hydroxide (NH4OH) until slightly alkaline, then required for each determination).
add HCl until just acid, and then 3 mL more of HCl. Dilute to 13.2 Potassium Permanganate, Standard Solution (0.1 N, 1
about 250 mL with hot water and heat nearly to boiling. Run in mL = 0.008 g TiO2)—Dissolve 3.16 g of KMnO4 in water and
the K 4Fe(CN)6 solution slowly from a buret, while stirring dilute to 1 L. Let stand 8 to 14 days, siphon off the clear
constantly, until a drop tested on a white porcelain plate with a solution (or filter through a medium porosity fritted disk), and
drop of the uranyl indicator solution shows a brown tinge after standardize against the National Institute of Standards and
standing 1 min. Do not allow the temperature of the solution to Technology (NIST) standard chemical No. 40 of sodium
fall below 70°C during the titration. Run a blank using the oxalate (Na2C2O4) as follows: In a 400-mL beaker dissolve
same amounts of reagents and water as in the standardization. 0.2500 to 0.3000 g of the NIST sodium oxalate in 250 mL of
The standardization must be made under the same conditions hot water (80 to 90°C) and add 15 mL of H2SO4 (1+1). Titrate
of temperature, volume, and acidity as obtained when the at once with the KMnO4 solution, stirring the liquid vigorously
sample is titrated. Calculate the strength of the K 4Fe(CN)6 and continuously. The KMnO4 must not be added more rapidly
solution in terms of grams of zinc as follows: than 10 to 15 mL/min, and the last 0.5 to 1 mL must be added
dropwise with particular care to allow each drop to be fully
Z 5 W/~V1 2 B! (1)

where: 9
Wilson, L. A., “The Evaluation of Zinc Dust: A Proposed Method of Analysis,”
Z = zinc equivalent of the K4Fe(CN)6 solution, g/mL, Proceedings, ASTEA, Am. Soc. Testing and Mats., Vol 18, Part II, 1918, p. 220.

2
 D 521
decolorized before the next is introduced. The solution shall CALCIUM
not be below 60°C by the time the end point has been reached. 16. Reagents
(More rapid cooling may be prevented by allowing the beaker
to stand on a small hot plate during the titration. The use of a 16.1 Ammonium Oxalate, Saturated Solution—Mix 50 g of
small nonmercury type thermometer as a stirring rod is most ammonium oxalate and 1 L of water.
convenient.) Keep the KMnO4 solution in a glass-stoppered 16.2 Ammonium Oxalate Solution (10 g/L)—Dissolve 10 g
bottle painted black to keep out light, or in a brown glass bottle of ammonium oxalate in water and dilute to 1 L.
stored in a dark place. 16.3 Potassium Permanganate, Standard Solution (0.1
13.3 Sodium Acetate Solution (200 g/L)—Dissolve 200 g of N)—See 13.2.
sodium acetate (NaC2H 3O2) or 332 g of NaC2H3O2·3H 2O, in 17. Procedure
water and dilute to 1 L. 17.1 Transfer 10 g of the sample, weighed to 0.1 g, to a
13.4 Zimmerman-Reinhardt Solution—Prepare a solution 400-mL beaker. Dissolve in 30 mL of HCl (1 + 1), keeping the
containing 67 g of manganese sulfate (MnSO4·4H 2O) 130 mL beaker covered. Dilute to 200 mL. The solution at this point
of H2SO4 (sp gr 1.84), and 138 mL of phosphoric acid (H3PO4) should be clear and transparent. Neutralize with NH4OH.
(85 %) per L. (Some zinc, because of its high concentration, will precipitate
14. Procedure out as hydroxide at this point.) Add NH4OH (sp gr 0.90)
dropwise, stirring until the solution becomes clear. Heat nearly
14.1 Weigh 0.2 g of the sample, transfer immediately to a to boiling and add 75 mL of saturated ammonium oxalate
dry, 600-mL heavy-wall Erlenmeyer flask, and add 50 mL of solution. Boil until the precipitate assumes a dense crystalline
the FeCl 3 solution. Tightly stopper the flask and agitate appearance. Allow to settle on a steam bath for 20 min and then
constantly for approximately 15 min. As soon as the zinc dust cool. Filter on close-grained paper and wash five times with a
is all dissolved, add 50 mL of the Zimmerman-Reinhardt cold ammonium oxalate solution (10 g/L).
solution and 250 mL of water. Titrate with 0.1 N KMnO4 17.2 Carefully dissolve the precipitate from the filter paper,
solution. using alternately hot HCl (1+3) and hot water. Catch in a clean
NOTE 3—If preferred, the reduced iron may be titrated with 0.1 N 400-mL beaker, dilute (if necessary) to a volume of about 250
potassium dichromate (K2Cr2O7) solution, using sodium diphenylamine mL, and add 25 mL of saturated ammonium oxalate solution.
sulfonate in the presence of phosphoric acid (H 3PO4) as an internal Bring to a boil, and add NH4OH in slight excess. Boil until the
indicator.10 precipitate becomes crystalline and dense. Let stand 1 h on a
14.2 Blank—Make a blank determination, following the steam bath. Allow to cool. Filter and wash with small amounts
same procedure and using the same amounts of all reagents of hot water until all ammonium oxalate is removed.
prior to the titration. (The blank is usually 0.1 to 0.2 mL of 0.1 17.3 Remove the paper from the funnel and spread it out on
N KMnO4 solution.) the inside of a 600-mL beaker above 300 mL of warm water to
14.3 Calculation—Calculate the percent of metallic zinc, which has been added 20 mL of H2SO4 (1+1). Rinse the
M, as follows: precipitate off the paper with water from a wash bottle and
M 5 @~V3 2 B 3!~N 3 0.0327!/S2# 3 100 (3) warm the solution to 80°C. Titrate at this temperature with
KMnO4 solution. As soon as a persistent pink end point is
where: obtained, drop the paper into the liquid, rinse the side of the
V3 = KMnO4 solution required for titration of the beaker, and quickly complete the titration.
specimen, mL, 17.4 Calculation—Calculate the percent of calcium, C, as
B3 = KMnO4 solution required for titration of the CaO, as follows:
blank, mL,
C 5 @~V4N 3 0.02804!/S 3# 3 100 (5)
N = normality of the KMnO4 solution,
S2 = sample used, g, and where:
0.327 = milliequivalent weight of Zn. V 4 = KMnO4 solution required for titration of the sample,
mL,
ZINC OXIDE N = normality of the KMnO4 solution, and
S 3 = specimen used, g.
15. Calculation
15.1 Calculate the percent of zinc oxide (ZnO), Z, as LEAD
follows: 18. Procedure
Z 5 ~A 2 C! 3 1.2447 (4) 18.1 Determine the lead content in accordance with Section
6 of Test Method E 40.
where:
A = total zinc, % (Section 10), and NOTE 4—Lead may also be determined in accordance with Test Method
C = metallic zinc, % (Section 12). E 68.

IRON
10
19. Procedure
Kolthoff, I. M., and Sandell, E. B., Textbook of Quantitative Inorganic
Analysis, 1945, p. 608. 19.1 Determine the iron content in accordance with Section

3
 D 521
22 of Test Method E 40. of barium chloride (BaCl2·2H 2O) in water and dilute to 1 L.
23.2 Bromine Water (saturated).
CADMIUM
20. Procedure 24. Procedure
20.1 Determine the cadmium content in accordance with 24.1 Transfer 20 g of the specimen, weighed to the nearest
18.1 and 18.3 of Test Method E 40. 0.1 g, to a 600-mL beaker. Cover the sample with 50 mL of
NOTE 5—Cadmium may also be determined in accordance with Test saturated bromine water and then cautiously add HNO3(sp gr
Method E 68. 1.42) until solution is complete.
24.2 Add 1 g of anhydrous sodium carbonate (Na 2CO3) and
CHLORINE
boil down until salts just begin to separate, then add 75 mL of
21. Reagents HCl (sp gr 1.19) and again boil down until salts begin to
21.1 Silver Nitrate Solution (3.5 g/L)—Dissolve 3.5 g of separate. Repeat this operation and, finally, dilute to 100 mL,
silver nitrate (AgNO3) in water and dilute to 1 L. heat until solution is complete, and filter into a 400-mL beaker
21.2 Sodium Chloride, Standard Solution (0.01 N)— through close-texture paper.
Dissolve 0.5850 g of pure sodium chloride (NaCl) in water and 24.3 Wash the paper with hot water, make the filtrate
dilute to 1 L. alkaline with NH4OH, and then just acid with HCl. Heat to
boiling and hold at boiling temperature at least 5 to 10 min to
22. Procedure drive out CO 2 then slowly add with stirring 5 mL of BaCl2
22.1 Transfer 1.000 g of the sample to a 200-mL electrolytic solution. Allow to stand at least 5 h (preferably overnight).
beaker. Add 20 mL of water and then cautiously add 5 mL of 24.4 Filter on a weighed Gooch crucible, wash free from
nitric acid (HNO 3) (sp gr 1.42). Cover with a watch glass and
chlorides with hot water, dry, and ignite carefully at 900°C.
heat on a steam bath with frequent stirring for 5 min, or until
Cool and weigh. The difference between the original and final
a clear solution results. Add 70 mL of water and cool to room
weight is BaSO 4.
temperature.
22.2 To the specimen and to a blank (prepared in similar 24.5 Blank—Make a blank determination, following the
fashion) add 5.0 mL of AgNO3 solution (3.5 g/L) and stir. To same procedure and using the same amounts of all reagents.
the blank, add dropwise from a 10-mL buret, with thorough 24.6 Calculation—Calculate the percent of sulfur, S, as
mixing, enough NaCl solution to develop a turbidity matching follows:
that of the sample. Keep the contents of both beakers well S 5 @~~W1 2 B 4! 3 0.1374!/S4# 3 100 (7)
stirred and view against a black background in equal illumi-
nation. where:
22.3 Calculation—Calculate the percent of chlorine, C, as W1 = BaSO4, g,
follows: B4 = correction for blank, g,
C 5 0.035 V5 (6)
S4 = sample used, g, and
0.1374 = S/BaSO4 = 32.06/233.42.
where V5 = 0.01 N NaCl solution added to the blank, mL.
SULFUR 25. Keywords
23. Reagents 25.1 calcium; chlorine; potassium ferrocyanide; zinc dust;
23.1 Barium Chloride Solution (100 g/L)—Dissolve 117 g zinc powder

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