Standard Test Method for Determination of Copper in Iron Ores and Related Materials by Atomic Absorption Spectroscopy

SCOPE
1.1 This test method covers the determination of copper in iron ores, concentrates, agglomerates, and related materials in the concentration range from 0.003 to 1%.  
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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Publication Date
09-Nov-1999
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ASTM E841-99 - Standard Test Method for Determination of Copper in Iron Ores and Related Materials by Atomic Absorption Spectroscopy
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E 841 – 99
Standard Test Method for
Determination of Copper in Iron Ores and Related Materials
by Atomic Absorption Spectrometry
This standard is issued under the fixed designation E 841; 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. Significance and Use
1.1 This test method covers the determination of copper in 4.1 In the making of iron and steel during the reduction of
iron ores, concentrates, agglomerates, and related materials in iron ores, copper forms alloy with iron and steel hence the
the concentration range from 0.003 to 1 %. necessity of determining the copper concentration for metal-
1.2 This standard does not purport to address all of the lurgical consideration.
safety concerns, if any, associated with its use. It is the 4.2 This test method is intended to be used for compliance
responsibility of the user of this standard to establish appro- with compositional specifications for copper content. It is
priate safety and health practices and determine the applica- assumed that all who use these procedures will be trained
bility of regulatory limitations prior to use. analysts capable of performing common laboratory procedures
skillfully and safely. It is expected that work will be performed
2. Referenced Documents
in a properly equipped laboratory and that proper waste
2.1 ASTM Standards: disposal procedures will be followed. Appropriate quality
E 50 Practices for Apparatus, Reagents, and Safety Precau-
control practices must be followed, such as those described in
tions for Chemical Analysis of Metals Guide E 882.
E 173 Practice for Conducting Interlaboratory Studies of
5. Interferences
Methods for Chemical Analysis of Metals
E 276 Test Method for Particle Size or Screen Analysis at 5.1 None of the elements normally found in iron ores
No. 4 (4.75-mm) Sieve and Finer for Metal-Bearing Ores interfere with this test method.
and Related Materials
3 6. Apparatus
E 663 Practice for Flame Atomic Absorption Analysis
6.1 Atomic Absorption Spectrometer, meeting the following
E 877 Practice for Sampling and Sample Preparation of Iron
Ores and Related Materials criteria:
6.1.1 Minimum Sensitivity—The absorbance of the highest
E 882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory calibration solution (see 7.5) must be at least 0.3.
6.1.2 Curve—Linearity—The difference between the read-
3. Summary of Test Method
ings of the two highest calibration solutions must be more than
3.1 The sample is dissolved in hydrochloric acid with the 1.4 times the difference between the readings for the zero
addition of a small amount of nitric and hydrofluoric acids. solution and the lowest calibration solution (see 7.5).
After evaporation to fumes with perchloric acid, the solution is 6.1.3 Minimum Stability—The coefficient of variation of a
diluted with water and filtered. A portion of the solution is number of measurements of the highest calibration solution
examined by atomic absorption spectroscopy using standards and of the zero calibration solution must be less than 1.5 and
containing approximately the same amount of iron as the test 0.5 % respectively, relative to the measurement of the highest
sample. calibration solution.
NOTE 1—A strip chart recorder or digital readout device, or both is
advisable to measure the criteria in 6.1 and for all subsequent measure-
This test method is under the jurisdiction of ASTM Committee E-1 on
ments.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
NOTE 2—A background corrector equipped with a hydrogen or a
responsibility of Subcommittee E01.02 on Ores, Concentrates and Related Metal-
deuterium hollow cathode lamp is advisable for the concentration range
lurgical Materials.
Current edition approved Nov. 10, 1999. Published January 2000. Originally from 0.003 to 0.010 % Cu.
published as E 841 – 81. Last previous edition E 841 – 94.
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.
E841–99
NOTE 3—Instrument parameters will vary with each instrument. The
to room temperature in a desiccator. Momentarily release the
following parameters were successfully used in several laboratories and
cap to equalize the pressure and weigh the capped bottle and
they can be used as guidelines. Solutions were aspirated into an air-
sample to the nearest 0.1 mg. Repeat drying and weighing until
– acetylene flame of a premix burner.
there is no further weight loss. Transfer the sample to a 250-mL
Hollow cathode lamp, mA 3
beaker and reweigh the capped bottle to the nearest 0.1 mg.
Wavelength, nm 324.7
Air flow-rate, L/min 10
The difference between the two weights is the weight of the
Acetylene flow-rate, L/min 2.5
sample taken for analysis.
9.2 Carry a reagent blank through all steps of the procedure
7. Reagents and Materials
starting with 9.3.
7.1 Purity and Concentration of Reagents—The purity and
9.3 Decomposition of Sample—Moisten the sample with a
concentration of the common chemical reagents used shall
few millilitres of water, add 25 mL of HCl, cover, and digest
conform to Practice E 50. Special apparatus and reagents
below the boiling point until no further attack is apparent. Add
required are located in separate section preceding the proce-
5mLofHNO and heat for 10 min. Remove cover, add 3 mL
dure.
of hydrofluoric acid, and heat for 10 min. Rinse wall of the
7.2 Copper Standard Solution A (1 mL = 1.0 mg Cu)—
beaker with water, add 5 mL of HClO , and evaporate slowly
Dissolve 1.000 g of copper metal (minimum 99.5 %) in 30 mL
to dense white fumes of HClO . Fume for 2 to 3 min and allow
of nitric acid (1 + 1) and dilute to 1 L.
the solution to cool. Add 50 mL of water and warm until the
7.3 Copper Standard Solution B (1 mL = 0.10 mg Cu)—
soluble salts are in solution. Filter the solution through a fine
Transfer 100 mL of Standard Solution A to a 1-L volumetric
texture paper, wash the residue with warm water, receiving the
flask, dilute to volume, and mix.
filtrate and washings in a 100-mL volumetric flask. Ignite the
7.4 Copper Standard Solution C (1 mL = 0.01 mg Cu)—
filter paper containing the insoluble residue in a platinum
Transfer 100 mL of Standard Solution B to a 1-L volumetric
crucible, moisten the residue with a few drops of water, add
flask, dilute to volume, and mix.
7.5 Copper Standard Calibration Solution—Depending on about 3 mL of hydrofluoric acid and 2 drops of sulfuric acid.
Add a few drops of nitric acid. Mix and evap
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