Standard Test Method for Determination of Aluminum in Iron Ores and Related Materials by Complexometric Titration

SIGNIFICANCE AND USE
This test method for the analysis of iron ore concentrates and agglomerates is primarily intended as a referee method to test for compliance with compositional specifications. It is assumed that all who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices shall be followed, such as those described in Guide E 882.
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.
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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30-Sep-2005
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ASTM E738-00(2005) - Standard Test Method for Determination of Aluminum in Iron Ores and Related Materials by Complexometric Titration
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E738–00(Reapproved 2005)
Standard Test Method for
Determination of Aluminum in Iron Ores and Related
Materials by Complexometric Titration
This standard is issued under the fixed designation E738; 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 3. Terminology
1.1 This test method covers the determination of aluminum 3.1 Definitions—For definitions of terms used in this test
in iron ores, concentrates, and agglomerates in the concentra- method, refer to Terminology E135.
tion range from 0.25 to 5 % aluminum.
4. Summary of Test Method
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 4.1 The sample is fused in a zirconium crucible with a
mixed flux of sodium carbonate and sodium peroxide. The
standard.
1.3 This standard does not purport to address all of the fused mass is dissolved in dilute hydrochloric acid. The R O
2 3
hydroxides are precipitated with ammonia and redissolved in
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- hydrochloric acid. Iron, titanium, and so forth, are removed
with cupferron and chloroform. The aqueous phase is treated
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. with nitric and perchloric acids and evaporated to dryness.
After dissolving in dilute hydrochloric acid, the solution is
2. Referenced Documents
filtered, and the filtrate is treated with an excess of ethylene-
2.1 ASTM Standards: diaminetetraacetic acid (EDTA). The excess EDTA is titrated
D1193 Specification for Reagent Water with a standard zinc solution using xylenol orange indicator.
E50 Practices for Apparatus, Reagents, and Safety Consid- Ammonium fluoride is added to release the EDTA bound to
erations for Chemical Analysis of Metals, Ores, and aluminum. This EDTA is then titrated with standard zinc
Related Materials solution, and the percent aluminum is calculated.
E135 Terminology Relating to Analytical Chemistry for
5. Significance and Use
Metals, Ores, and Related Materials
E877 Practice for Sampling and Sample Preparation of Iron 5.1 Thistestmethodfortheanalysisofironoreconcentrates
and agglomerates is primarily intended as a referee method to
Ores and Related Materials for Determination of Chemical
Composition test for compliance with compositional specifications. It is
assumed that all who use this test method will be trained
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory analysts capable of performing common laboratory procedures
skillfully and safely. It is expected that work will be performed
in a properly equipped laboratory and that proper waste
This test method is under the jurisdiction of ASTM Committee E01 on
disposal procedures will be followed. Appropriate quality
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
control practices shall be followed, such as those described in
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Guide E882.
Current edition approved Oct. 1, 2005. Published October 2005. Originally
approved in 1980. Last previous edition approved in 2000 as E738 – 00. DOI:
6. Interferences
10.1520/E0738-00R05.
6.1 None of the elements normally found in iron ores
Bhargava, O. P., “Complexometric Determination of Aluminum in Iron Ore,
Sinter, Concentrates, and Agglomerates,” Talanta, Vol 26, 1979, pp. 146 to 148.
interfere with this test method.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
7. Apparatus
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 7.1 Zirconium Crucible, 50-mL.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E738–00 (2005)
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
Practices E50.
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 Sample the material in accordance with Practice E877.
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
11. Procedure
by Type II of Specification D1193.
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
Aluminum, % Test Sample Weight, g Weight, mg
8.4 Ammonium Fluoride Solution—Dissolve 10 g of ammo-
nium fluoride (NH F) in 100 mL of water in a polyethylene
4 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
previously dried at about 105°C. Dry the bottle and contents
8.6 Cupferron Solution (60 g/L)—Dissolve6gof cupferron
for 1 h at 105 to 110°C. Cap the bottle and cool to room
in 80 mL of cold water, dilute to 100 mL, and filter. Prepare
temperature in a desiccator. Momentarily release the cap to
fresh as needed.
equalize the pressure and weigh the capped bottle and sample
8.7 Ethylenediaminetetraacetic Acid (EDTA) Solution
to the nearest 0.1 mg. Repeat the drying and weighing until
(0.01 mol/L).
thereisnofurtherweightloss.Transferthetestsampletoadry,
8.8 Sodium Acetate Buffer Solution—Dissolve 136 g of
zirconium crucible containing 0.5 g of sodium carbonate and
sodium acetate trihydrate (CH COONa·3H O) in about 600
3 2
reweigh the capped bottle to the nearest 0.1 mg.The difference
mLof water.Add 7 mLof glacial acetic acid and dilute to 1 L.
between the two weights is the weight of the test sample taken
Store in a polyethylene bottle.
for analysis. Add 2 g of sodium peroxide to the crucible and
8.9 Sodium Carbonate.
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 sodiu
...

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