ASTM D521-90(1999)
(Test Method)Standard Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)
Standard Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)
SCOPE
1.1 These test methods cover procedures for the chemical analysis of metallic zinc powder in the form commercially known as zinc dust for use as a pigment in paints.
1.2 The analytical procedures appear in the following order: SectionsMoisture and Other Volatile Matter7Coarse Particles8Matter Soluble in Hexane9 and 10Total Zinc11 and 12Metallic Zinc13 and 14Zinc Oxide15Calcium16 and 17Lead18Iron19Cadmium20Chlorine21 and 22Sulfur23 and 24
1.3 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.
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Designation: D 521 – 90 (Reapproved 1999)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods for
Chemical Analysis of Zinc Dust (Metallic Zinc Powder)
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 3. Significance and Use
1.1 These test methods cover procedures for the chemical 3.1 These test methods compile procedures which can be
analysis of metallic zinc powder in the form commercially used to check the composition of purity of metallic zinc
known as zinc dust for use as a pigment in paints. powder. This information is useful to both the formulator and
1.2 The analytical procedures appear in the following order: users.
Sections
4. Treatment of Sample
Moisture and Other Volatile Matter 7
Coarse Particles 8
4.1 Store the laboratory sample in a tightly stoppered bottle
Matter Soluble in Hexane 9 and 10
to protect it from oxidation. Mix the whole sample thoroughly
Total Zinc 11 and 12
Metallic Zinc 13 and 14
before taking portions for analysis.
Zinc Oxide 15
Calcium 16 and 17
5. Purity of Reagents
Lead 18
Iron 19
5.1 Purity of Reagents—Unless otherwise indicated, it is
Cadmium 20
intended that all reagents shall conform to the specifications of
Chlorine 21 and 22
the Committee on Analytical Reagents of the American Chemi-
Sulfur 23 and 24
cal Society, where such spedcifications are available. Other
1.3 This standard does not purport to address all of the
grades may be used, provided it is first ascertained that the
safety concerns, if any, associated with its use. It is the
reagent is of sufficiently high purity to permit its use without
responsibility of the user of this standard to establish appro-
lessening the accuracy of the determination.
priate safety and health practices and determine the applica-
5.2 Purity of Water—Unless otherwise indicated, references
bility of regulatory limitations prior to use.
to water shall be understood to mean reagent water conforming
to Type II of Specification D 1193.
2. Referenced Documents
2.1 ASTM Standards:
6. Precision
B 214 Test Method for Sieve Analysis of Metal Powders
6.1 Precision statements have not been established.
D 185 Test Methods for Coarse Particles in Pigments,
Pastes, and Paints
MOISTURE AND OTHER VOLATILE MATTER
D 280 Test Methods for Hygroscopic Moisture (and Other
7. Procedure
Matter Volatile Under the Test Conditions) in Pigments
D 1193 Specification for Reagent Water
7.1 Determine moisture and other volatile matter in accor-
E 40 Test Methods for Chemical Analysis of Slab Zinc
dance with Method A of Test Methods D 280, except heat the
(Spelter)
sample for only 1 h.
E 68 Method for Polarographic Determination of Lead and
COARSE PARTICLES
Cadmium in Zinc
8. Procedure
1 8.1 Determine the percent of coarse particles in the pigment
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
in accordance with Test Methods D 185 or B 214.
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D01.31 on Pigment Specifications.
Current edition approved May 25, 1990. Published July 1990. Originally
published as D 521 – 39 T. Last previous edition D 521 – 81. Reagent Chemicals, American Chemical Society Specifications, American
Annual Book of ASTM Standards, Vol 02.05. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 06.03. listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Discontinued—See 1979 Annual Book of ASTM Standards, Part 12. MD.
D 521
MATTER SOLUBLE IN HEXANE addition of the litmus paper and the adjustment of the acidity
with NH OH and HCl.
9. Reagent
12.3 Calculation—Calculate the percent of total zinc, T,as
9.1 Hexane—Pure hexane or commercial hexane or petro-
follows:
leum ether of boiling point not higher than 75°C. Redistill
T 5 @~V 2 B !Z/S # 3 100 (2)
2 2 1
before using.
where:
10. Procedure
V 5 K Fe(CN) solution required for titration of the
2 4 6
10.1 Place 100 g of the pigment in an extraction thimble in
specimen, mL,
a Soxhlet extraction apparatus. Record the tare weight of the
B 5 K Fe(CN) solution required for titration of the
2 4 6
receiving flask. Charge the flask with a suitable volume of blank, mL,
hexane and extract the sample for 4 h, subjecting the specimen Z 5 zinc equivalent of the K Fe(CN) solution, g/mL,
4 6
and
to not less than 20 extractions in this time. Make a blank
S 5 sample used, g.
determination at the same time.
10.2 Remove the receiving flask, evaporate or distill off the
METALLIC ZINC
hexane on a steam bath, and dry the flask at 105 6 2°C for 1
h. Cool and weigh.
NOTE 1—Sections 12 and 13 cover a rapid method for determining
10.3 Calculate the percent of matter soluble in hexane,
metallic zinc, intended for routine analysis. The results are inclined to be
allowing for any material found in the blank.
somewhat low, and for highest accuracy and particularly for referee tests,
the hydrogen evolution method should be used.
TOTAL ZINC
13. Reagents
11. Reagents
13.1 Ferric Chloride Solution—Prepare a solution contain-
11.1 Potassium Ferrocyanide, Standard Solution—Dissolve
ing 20 g of ferric chloride (FeCl ·6H O) and 20 mL of 20 %
3 2
22 g of potassium ferrocyanide (K Fe(CN) ·3H O) in water
4 6 2
sodium acetate (NaC H O ) solution per 100 mL. It is advis-
2 3 2
and dilute to 1 L. To standardize, transfer 0.2 g of metallic zinc
able to make up only one day’s supply at a time (50 mL are
or freshly ignited zinc oxide (ZnO) to a 400-mL beaker.
required for each determination).
Dissolve in 10 mL of hydrochloric acid (HCl), sp gr 1.19 and
13.2 Potassium Permanganate, Standard Solution (0.1 N,1
20 mL of water. Drop in a small piece of litmus paper, add
mL 5 0.008 g TiO )—Dissolve 3.16 g of KMnO in water and
2 4
ammonium hydroxide (NH OH) until slightly alkaline, then
dilute to 1 L. Let stand 8 to 14 days, siphon off the clear
add HCl until just acid, and then 3 mL more of HCl. Dilute to
solution (or filter through a medium porosity fritted disk), and
about 250 mL with hot water and heat nearly to boiling. Run in
standardize against the National Institute of Standards and
the K Fe(CN) solution slowly from a buret, while stirring
4 6
Technology (NIST) standard chemical No. 40 of sodium
constantly, until a drop tested on a white porcelain plate with a
oxalate (Na C O ) as follows: In a 400-mL beaker dissolve
2 2 4
drop of the uranyl indicator solution shows a brown tinge after
0.2500 to 0.3000 g of the NIST sodium oxalate in 250 mL of
standing 1 min. Do not allow the temperature of the solution to
hot water (80 to 90°C) and add 15 mL of H SO (1+1). Titrate
2 4
fall below 70°C during the titration. Run a blank using the
at once with the KMnO solution, stirring the liquid vigorously
same amounts of reagents and water as in the standardization.
and continuously. The KMnO must not be added more rapidly
The standardization must be made under the same conditions
than 10 to 15 mL/min, and the last 0.5 to 1 mL must be added
of temperature, volume, and acidity as obtained when the
dropwise with particular care to allow each drop to be fully
sample is titrated. Calculate the strength of the K Fe(CN)
4 6
decolorized before the next is introduced. The solution shall
solution in terms of grams of zinc as follows:
not be below 60°C by the time the end point has been reached.
Z 5 W/~V 2 B! (1)
(More rapid cooling may be prevented by allowing the beaker
to stand on a small hot plate during the titration. The use of a
where:
small nonmercury type thermometer as a stirring rod is most
Z 5 zinc equivalent of the K Fe(CN) solution, g/mL,
4 6
convenient.) Keep the KMnO solution in a glass-stoppered
W 5 zinc used (or equivalent to the ZnO used), g,
bottle painted black to keep out light, or in a brown glass bottle
V 5 K Fe(CN) solution required for titration of the
1 4 6
stored in a dark place.
standard, mL, and
13.3 Sodium Acetate Solution (200 g/L)—Dissolve 200 g of
B 5 K Fe(CN) solution requ
...
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