ASTM E738-00
(Test Method)Standard Test Method for Determination of Aluminum in Iron Ores and Related Materials by Complexometric Titration
Standard Test Method for Determination of Aluminum in Iron Ores and Related Materials by Complexometric Titration
SCOPE
1.1 This test method covers the determination of aluminum in iron ores, concentrates, and agglomerates in the concentration range from 0.25 to 5% aluminum.
1.2 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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An American National Standard
Designation:E738–00
Standard Test Method for
Determination of Aluminum in Iron Ores and Related
Materials by Complexometric Titration
This standard is issued under the fixed designation E 738; 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 4. Summary of Test Method
1.1 This test method covers the determination of aluminum 4.1 The sample is fused in a zirconium crucible with a
in iron ores, concentrates, and agglomerates in the concentra- mixed flux of sodium carbonate and sodium peroxide. The
tion range from 0.25 to 5 % aluminum. fused mass is dissolved in dilute hydrochloric acid. The R O
2 3
1.2 This standard does not purport to address all of the hydroxides are precipitated with ammonia and redissolved in
safety concerns, if any, associated with its use. It is the hydrochloric acid. Iron, titanium, and so forth, are removed
responsibility of the user of this standard to establish appro- with cupferron and chloroform. The aqueous phase is treated
priate safety and health practices and determine the applica- with nitric and perchloric acids and evaporated to dryness.
bility of regulatory limitations prior to use. After dissolving in dilute hydrochloric acid, the solution is
filtered, and the filtrate is treated with an excess of ethylene-
2. Referenced Documents
diaminetetraacetic acid (EDTA). The excess EDTA is titrated
2.1 ASTM Standards: with a standard zinc solution using xylenol orange indicator.
D 1193 Specification for Reagent Water
Ammonium fluoride is added to release the EDTA bound to
E 50 Practices for Apparatus, Reagents, and Safety Precau- aluminum. This EDTA is then titrated with standard zinc
tions for Chemical Analysis of Metals
solution, and the percent aluminum is calculated.
E 135 Terminology Relating to Analytical Chemistry for
5. Significance and Use
Metals, Ores, and Related Materials
E 877 PracticeforSamplingandSamplePreparationofIron 5.1 Thistestmethodfortheanalysisofironoreconcentrates
Ores and Related Materials and agglomerates is primarily intended as a referee method to
E 882 Guide for Accountability and Quality Control in the test for compliance with compositional specifications. It is
Chemical Analysis Laboratory assumed that all who use this test method will be trained
analysts capable of performing common laboratory procedures
3. Terminology
skillfully and safely. It is expected that work will be performed
3.1 Definitions—For definitions of terms used in this test in a properly equipped laboratory and that proper waste
method, refer to Terminology E 135.
disposal procedures will be followed. Appropriate quality
control practices shall be followed, such as those described in
Guide E 882.
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
6. Interferences
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. 6.1 None of the elements normally found in iron ores
Current edition approved Nov. 10, 2000. Published January 2001. Originally
interfere with this test method.
published as E 738 – 80. Last previous edition E 738 – 95a.
Bhargava, O. P., “Complexometric Determination of Aluminum in Iron Ore,
7. Apparatus
Sinter, Concentrates, and Agglomerates,” Talanta, Vol 26, 1979, pp. 146 to 148.
Annual Book of ASTM Standards, Vol 11.01. 7.1 Zirconium Crucible, 50-mL.
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E738–00
8. Reagents and Materials 9. Hazards
9.1 For precautions to be observed in this method, refer to
8.1 Purity of Reagents—Reagent grade chemicals shall be
Practice E 50.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
10. Sampling and Sample Preparation
Analytical Reagents of the American Chemical Society where
such specifications are available. Other grades may be used,
10.1 SamplethematerialinaccordancewithPracticeE 877.
provided it is first ascertained that the reagent is of sufficient
10.2 Pulverize the laboratory sample to pass a No. 100
high purity to permit its use without lessening the accuracy of
(150-µm sieve).
the determination.
NOTE 1—To facilitate decomposition, some ores, such as specular
8.2 Purity of Water—Unless otherwise indicated, references
hematite, require grinding to pass a No. 200 (75-µm) sieve.
to water shall be understood to mean reagent water as defined
by Type II of Specification D 1193. 11. Procedure
8.3 Ammonium Chloride Solution (10 g/L)—Dissolve 10 g
11.1 Select and weigh a test sample in accordance with the
of ammonium chloride in water and dilute to 1 L.Add 2 drops
following:
(0.1 mL) of ammonium hydroxide per 100 mL of solution.
Tolerance in Test Sample
8.4 Ammonium Fluoride Solution—Dissolve 10 g of ammo- Aluminum, % Test Sample Weight, g Weight, mg
nium fluoride (NH F) in 100 mL of water in a polyethylene
0.25 to 1 0.3 5
beaker. Prepare fresh each day.
1to2 0.2 5
2to5 0.1 5
8.5 Ammonium Hydroxide (1 + 1)—Mix 1 volume of am-
monium hydroxide (NH OH) with 1 volume of water.
Transfer the prepared sample to a small weighing bottle
8.6 Cupferron Solution (60 g/L)—Dissolve6gof cupferron
previously dried at about 105°C. Dry the bottle and contents
in 80 mL of cold water, dilute to 100 mL, and filter. Prepare
for 1 h at 105 to 110°C. Cap the bottle and cool to room
fresh as needed.
temperature in a desiccator. Momentarily release the cap to
8.7 Ethylenediaminetetraacetic Acid (EDTA) Solution
equalize the pressure and weigh the capped bottle and sample
(0.01 mol/L).
to the nearest 0.1 mg. Repeat the drying and weighing until
8.8 Sodium Acetate Buffer Solution— Dissolve 136 g of
thereisnofurtherweightloss.Transferthetestsampletoadry,
sodium acetate trihydrate (CH COONa·3H O) in about 600
zirconium crucible containing 0.5 g of sodium carbonate and
3 2
mLof water.Add 7 mLof glacial acetic acid and dilute to 1 L.
reweigh the capped bottle to the nearest 0.1 mg.The difference
Store in a polyethylene bottle.
between the two weights is the weight of the test sample taken
8.9 Sodium Carbonate.
for analysis. Add 2 g of sodium peroxide to the crucible and
mix with a dry, stainless steel spatula.
8.10 Sodium Hydroxide Solution (10 %).
11.2 Fuse over a burner, swirling the crucible until the melt
8.10.1 Dissolve 100 g of sodium hydroxide (NaOH) in
is cherry red and clear. Remove from the heat and swirl until
about 100 mL of wat
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