ASTM D521-02(2019)
(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
3.1 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:
Sections
Moisture and Other Volatile Matter
7
Coarse Particles
8
Matter Soluble in Hexane
9 and 10
Total Zinc
11 and 12
Metallic Zinc
13 and 14
Zinc Oxide
15
Calcium
16 and 17
Lead
18
Iron
19
Cadmium
20
Chlorine
21 and 22
Sulfur
23 and 24
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 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
Relations
Standards Content (Sample)
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.
Designation: D521 − 02 (Reapproved 2019)
Standard Test 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 D185 Test Methods for Coarse Particles in Pigments
D280 Test Methods for Hygroscopic Moisture (and Other
1.1 These test methods cover procedures for the chemical
Matter Volatile Under the Test Conditions) in Pigments
analysis of metallic zinc powder in the form commercially
D1193 Specification for Reagent Water
known as zinc dust for use as a pigment in paints.
D6580 Test Method for The Determination of Metallic Zinc
1.2 The analytical procedures appear in the following order:
Content in Both Zinc Dust Pigment and in Cured Films of
Sections
Zinc-Rich Coatings
Moisture and Other Volatile Matter 7
E40 Method for Chemical Analysis of Slab Zinc (Spelter)
Coarse Particles 8
(Withdrawn 1993)
Matter Soluble in Hexane 9 and 10
Total Zinc 11 and 12
E68 Method for Polarographic Determination of Lead and
Metallic Zinc 13 and 14
Cadmium in Zinc (Withdrawn 1980)
Zinc Oxide 15
Calcium 16 and 17
Lead 18
3. Significance and Use
Iron 19
Cadmium 20 3.1 These test methods compile procedures which can be
Chlorine 21 and 22
used to check the composition of purity of metallic zinc
Sulfur 23 and 24
powder. This information is useful to both the formulator and
1.3 The values stated in SI units are to be regarded as
users.
standard. No other units of measurement are included in this
standard.
4. Treatment of Sample
1.4 This standard does not purport to address all of the
4.1 Store the laboratory sample in a tightly stoppered bottle
safety concerns, if any, associated with its use. It is the
to protect it from oxidation. Mix the whole sample thoroughly
responsibility of the user of this standard to establish appro-
before taking portions for analysis.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
5. Purity of Reagents
1.5 This international standard was developed in accor-
5.1 Purity of Reagents—Unless otherwise indicated, it is
dance with internationally recognized principles on standard-
intended that all reagents shall conform to the specifications of
ization established in the Decision on Principles for the
theCommitteeonAnalyticalReagentsoftheAmericanChemi-
Development of International Standards, Guides and Recom-
cal Society, where such specifications are available. Other
mendations issued by the World Trade Organization Technical
grades may be used, provided it is first ascertained that the
Barriers to Trade (TBT) Committee.
reagent is of sufficiently high purity to permit its use without
2. Referenced Documents lessening the accuracy of the determination.
2.1 ASTM Standards: 5.2 Purity of Water—Unless otherwise indicated, references
B214 Test Method for Sieve Analysis of Metal Powders to water shall be understood to mean reagent water conforming
to Type II of Specification D1193.
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, 2019. Published June 2019. Originally www.astm.org.
approved in 1939. Last previous edition approved in 2012 as D521 – 02 (2012). Reagent Chemicals, American Chemical Society Specifications, American
DOI: 10.1520/D0521-02R19. 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 (2019)
6. Precision Z 5 W/ V 2 B (1)
~ !
6.1 Precision statements have not been established.
where:
Z = zinc equivalent of the K Fe(CN) solution, g/mL,
4 6
MOISTURE AND OTHER VOLATILE MATTER
W = zinc used (or equivalent to the ZnO used), g,
V =K Fe(CN) solution required for titration of the
1 4 6
7. Procedure
standard, mL, and
7.1 Determine moisture and other volatile matter in accor-
B =K Fe(CN) solution required for titration of the blank,
4 6
dance with Method A of Test Methods D280, except heat the
mL.
sample for only 1 h.
11.2 Uranyl Nitrate Indicator Solution—Dissolve5gof
uranyl nitrate (UO (NO ) ·6H O) in 100 mL of water.
COARSE PARTICLES
2 3 2 2
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 D185 or B214.
1.19) and 20 mL of water.
MATTER SOLUBLE IN HEXANE
12.2 Continue with the procedure used in standardizing the
K Fe(CN) solution as described in 10.1, beginning with the
4 6
9. Reagent
addition of the litmus paper and the adjustment of the acidity
9.1 Hexane—Pure hexane or commercial hexane or petro-
with NH OH and HCl.
leum ether of boiling point not higher than 75°C. Redistill
12.3 Calculation—Calculate the percent of total zinc, T,as
before using.
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
V =K Fe(CN) solution required for titration of the
2 4 6
receiving flask. Charge the flask with a suitable volume of
specimen, mL,
hexane and extract the sample for 4 h, subjecting the specimen
B =K Fe(CN) solution required for titration of the blank,
2 4 6
to not less than 20 extractions in this time. Make a blank
mL,
determination at the same time.
Z = zinc equivalent of the K Fe(CN) solution, g/mL, and
4 6
S = sample used, g.
10.2 Remove the receiving flask, evaporate or distill off the 1
hexane on a steam bath, and dry the flask at 105 6 2°C for 1
METALLIC ZINC
h. Cool and weigh.
NOTE 1—Sections 12 and 13 cover a rapid method for determining
metallic zinc, intended for routine analysis. The results are inclined to be
10.3 Calculate the percent of matter soluble in hexane,
somewhat low, and for highest accuracy and particularly for referee tests,
allowing for any material found in the blank.
the hydrogen evolution method should be used.
NOTE 2—Metallic zinc may also be determined in accordance withTest
TOTAL ZINC
Method D6580.
11. Reagents
13. Reagents
11.1 Potassium Ferrocyanide, Standard Solution—Dissolve
13.1 Ferric Chloride Solution—Prepare a solution contain-
22 g of potassium ferrocyanide (K Fe(CN) ·3H O) in water
4 6 2
ing 20 g of ferric chloride (FeCl ·6H O) and 20 mL of 20 %
3 2
and dilute to 1 L.To standardize, transfer 0.2 g of metallic zinc
sodium acetate (NaC H O ) solution per 100 mL. It is advis-
2 3 2
or freshly ignited zinc oxide (ZnO) to a 400-mL beaker.
able to make up only one day’s supply at a time (50 mL are
Dissolve in 10 mL of hydrochloric acid (HCl), sp gr 1.19 and
required for each determination).
20 mL of water. Drop in a small piece of litmus paper, add
13.2 Potassium Permanganate, Standard Solution (0.1 N,1
ammonium hydroxide (NH OH) until slightly alkaline, then
mL = 0.008 g TiO )—Dissolve 3.16 g of KMnO in water and
2 4
add HCl until just acid, and then 3 mL more of HCl. Dilute to
dilute to 1 L. Let stand 8 to 14 days, siphon off the clear
about 250 mLwith hot water and heat nearly to boiling. Run in
solution (or filter through a medium porosity fritted disk), and
the K Fe(CN) solution slowly from a buret, while stirring
4 6
standardize against the National Institute of Standards and
constantly, until a drop tested on a white porcelain plate with a
Technology (NIST) standard chemical No. 40 of sodium
drop of the uranyl indicator solution shows a brown tinge after
oxalate (Na C O ) as follows: In a 400-mL beaker dissolve
standing 1 min. Do not allow the temperature of the solution to 2 2 4
0.2500 to 0.3000 g of the NIST sodium oxalate in 250 mL of
fall below 70°C during the titration. Run a blank using the
hot water (80 to 90°C) and add 15 mLof H SO (1+1). Titrate
same amounts of reagents and water as in the standardization. 2 4
at once with the KMnO solution, stirring the liquid vigorously
The standardization must be made under the same conditions
of temperature, volume, and acidity as obtained when the
sample is titrated. Calculate the strength of the K Fe(CN)
4 6 Wilson, L.A., “The Evaluation of Zinc Dust:AProposed Method ofAnalysis,”
solution
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