ASTM D521-02(2007)
(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)
SIGNIFICANCE AND USE
These test methods compile procedures which can be used to check the composition of purity of metallic zinc powder. This information is useful to both the formulator and users.
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:
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D521 − 02 (Reapproved 2007)
StandardTest Methods for
Chemical Analysis of Zinc Dust (Metallic Zinc Powder)
This standard is issued under the fixed designation D521; 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 E40 Method for Chemical Analysis of Slab Zinc (Spelter)
(Withdrawn 1993)
1.1 These test methods cover procedures for the chemical
E68 Method for Polarographic Determination of Lead and
analysis of metallic zinc powder in the form commercially
Cadmium in Zinc (Withdrawn 1980)
known as zinc dust for use as a pigment in paints.
3. Significance and Use
1.2 The analytical procedures appear in the following order:
Sections
3.1 These test methods compile procedures which can be
Moisture and Other Volatile Matter 7
used to check the composition of purity of metallic zinc
Coarse Particles 8
powder. This information is useful to both the formulator and
Matter Soluble in Hexane 9 and 10
Total Zinc 11 and 12
users.
Metallic Zinc 13 and 14
Zinc Oxide 15
4. Treatment of Sample
Calcium 16 and 17
Lead 18 4.1 Store the laboratory sample in a tightly stoppered bottle
Iron 19
to protect it from oxidation. Mix the whole sample thoroughly
Cadmium 20
before taking portions for analysis.
Chlorine 21 and 22
Sulfur 23 and 24
5. Purity of Reagents
1.3 The values stated in SI units are to be regarded as
5.1 Purity of Reagents—Unless otherwise indicated, it is
standard. No other units of measurement are included in this
intended that all reagents shall conform to the specifications of
standard.
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
1.4 This standard does not purport to address all of the
cal Society, where such specifications are available. Other
safety concerns, if any, associated with its use. It is the
grades may be used, provided it is first ascertained that the
responsibility of the user of this standard to establish appro-
reagent is of sufficiently high purity to permit its use without
priate safety and health practices and determine the applica-
lessening the accuracy of the determination.
bility of regulatory limitations prior to use.
5.2 Purity of Water—Unless otherwise indicated, references
2. Referenced Documents
to water shall be understood to mean reagent water conforming
to Type II of Specification D1193.
2.1 ASTM Standards:
B214 Test Method for Sieve Analysis of Metal Powders
6. Precision
D185 Test Methods for Coarse Particles in Pigments
6.1 Precision statements have not been established.
D280 Test Methods for Hygroscopic Moisture (and Other
Matter Volatile Under the Test Conditions) in Pigments
MOISTURE AND OTHER VOLATILE MATTER
D1193 Specification for Reagent Water
D6580 Test Method for The Determination of Metallic Zinc
7. Procedure
Content in Both Zinc Dust Pigment and in Cured Films of
7.1 Determine moisture and other volatile matter in accor-
Zinc-Rich Coatings
dance with Method A of Test Methods D280, except heat the
sample for only 1 h.
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.31 on Pigment Specifications. The last approved version of this historical standard is referenced on
Current edition approved June 1, 2007. Published June 2007. Originally www.astm.org.
approved in 1939. Last previous edition approved in 2002 as D521 – 02. DOI: Reagent Chemicals, American Chemical Society Specifications, American
10.1520/D0521-02R07. 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
D521 − 02 (Reapproved 2007)
COARSE PARTICLES 11.2 Uranyl Nitrate Indicator Solution— Dissolve5gof
uranyl nitrate (UO (NO ) ·6H O) in 100 mL of water.
2 3 2 2
8. Procedure
12. Procedure
8.1 Determine the percent of coarse particles in the pigment
12.1 Transfer 0.25 g of the sample to a 400-mL beaker,
in accordance with Test Methods D185 or B214.
moisten with alcohol, and dissolve in 10 mL of HCl (sp gr
MATTER SOLUBLE IN HEXANE
1.19) and 20 mL of water.
12.2 Continue with the procedure used in standardizing the
9. Reagent
K Fe(CN) solution as described in 10.1, beginning with the
4 6
9.1 Hexane—Pure hexane or commercial hexane or petro-
addition of the litmus paper and the adjustment of the acidity
leum ether of boiling point not higher than 75°C. Redistill
with NH OH and HCl.
before using.
12.3 Calculation—Calculate the percent of total zinc, T,as
follows:
10. Procedure
T 5 @ V 2 B Z/S # 3100 (2)
~ !
2 2 1
10.1 Place 100 g of the pigment in an extraction thimble in
where:
a Soxhlet extraction apparatus. Record the tare weight of the
receiving flask. Charge the flask with a suitable volume of V =K Fe(CN) solution required for titration of the
2 4 6
hexane and extract the sample for 4 h, subjecting the specimen
specimen, mL,
to not less than 20 extractions in this time. Make a blank B =K Fe(CN) solution required for titration of the
2 4 6
determination at the same time. blank, mL,
Z = zinc equivalent of the K Fe(CN) solution, g/mL, and
4 6
10.2 Remove the receiving flask, evaporate or distill off the
S = 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
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
NOTE 2—Metallic zinc may also be determined in accordance withTest
Method D6580.
11. Reagents
13. Reagents
11.1 Potassium Ferrocyanide, Standard Solution—Dissolve
22 g of potassium ferrocyanide (K Fe(CN) ·3H O) in water
4 6 2 13.1 Ferric Chloride Solution—Prepare a solution contain-
and dilute to 1 L.To standardize, transfer 0.2 g of metallic zinc
ing 20 g of ferric chloride (FeCl ·6H O) and 20 mL of 20 %
3 2
or freshly ignited zinc oxide (ZnO) to a 400-mL beaker.
sodium acetate (NaC H O ) solution per 100 mL. It is
2 3 2
Dissolve in 10 mL of hydrochloric acid (HCl), sp gr 1.19 and
advisable to make up only one day’s supply at a time (50 mL
20 mL of water. Drop in a small piece of litmus paper, add
are required for each determination).
ammonium hydroxide (NH OH) until slightly alkaline, then
13.2 Potassium Permanganate, Standard Solution (0.1 N,1
add HCl until just acid, and then 3 mL more of HCl. Dilute to
mL = 0.008 g TiO )—Dissolve 3.16 g of KMnO in water and
2 4
about 250 mLwith hot water and heat nearly to boiling. Run in
dilute to 1 L. Let stand 8 to 14 days, siphon off the clear
the K Fe(CN) solution slowly from a buret, while stirring
4 6
solution (or filter through a medium porosity fritted disk), and
constantly, until a drop tested on a white porcelain plate with a
standardize against the National Institute of Standards and
drop of the uranyl indicator solution shows a brown tinge after
Technology (NIST) standard chemical No. 40 of sodium
standing 1 min. Do not allow the temperature of the solution to
oxalate (Na C O ) as follows: In a 400-mL beaker dissolve
2 2 4
fall below 70°C during the titration. Run a blank using the
0.2500 to 0.3000 g of the NIST sodium oxalate in 250 mL of
same amounts of reagents and water as in the standardization.
hot water (80 to 90°C) and add 15 mLof H SO (1+1). Titrate
2 4
The standardization must be made under the same conditions
at once with the KMnO solution, stirring the liquid vigorously
of temperature, volume, and acidity as obtained when the
and continuously. The KMnO must not be added more rapidly
sample is titrated. Calculate the strength of the K Fe(CN)
4 6
than 10 to 15 mL/min, and the last 0.5 to 1 mL must be added
solution in terms of grams of zinc as follows:
dropwise with particular care to allow each drop to be fully
Z 5 W/~V 2 B! (1)
decolorized before the next is introduced. The solution shall
not be below 60°C by the time the end point has been reached.
where:
(More rapid cooling may be prevented by allowing the beaker
Z = zinc equivalent of the K Fe(CN) solution, g/mL,
4 6
to stand on a small hot plate during the titration. The use of a
W = zinc used (or equivalen
...
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