ASTM E278-96E1
(Test Method)Standard Test Method for the Determiniation of Phosphorus in Iron Ores by Phosphomolybdate Coprecipitation and Nitric Acid Titrimetry
Standard Test Method for the Determiniation of Phosphorus in Iron Ores by Phosphomolybdate Coprecipitation and Nitric Acid Titrimetry
SCOPE
1.1 This test method covers the determination of phosphorus in iron ores, concentrates, and agglomerates.
1.2 This test method covers the determination of phosphorus in the concentration range from 0.01 to 1.00%.
1.3 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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Designation: E 278 – 96
Standard Test Method for
Phosphorus in Iron Ores (Titrimetric)
This standard is issued under the fixed designation E 278; 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.
e NOTE—Editorial changes were made throughout in June 1997.
1. Scope with compositional specifications for phosphorus content. It is
assumed that all who use these procedures will be trained
1.1 This test method covers the determination of phospho-
analysts capable of performing common laboratory procedures
rus in iron ores, concentrates, and agglomerates.
skillfully and safely. It is expected that work will be performed
1.2 This test method covers the determination of phospho-
in a properly equipped laboratory and that proper waste
rus in the concentration range from 0.01 to 1.00 %.
disposal procedures will be followed. Appropriate quality
1.3 This standard does not purport to address all of the
control practices shall be followed, such as those described in
safety concerns, if any, associated with its use. It is the
Guide E 882.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Interferences
bility of regulatory limitations prior to use.
5.1 Vanadium and arsenic, elements commonly found in
2. Referenced Documents iron ores, coprecipitate with the phosphorus. Provisions for
their removal or elimination of their interference are included
2.1 ASTM Standards:
in this test method.
D 1193 Specification for Reagent Water
5.2 Titanium tends to form an insoluble compound with
E 691 Practice for Conducting an Interlaboratory Study to
phosphorus and thus may cause low values for phosphorus.
Determine the Precision of a Test Method
Provision for its removal is included in this test method.
E 877 Practice for Sampling and Sample Preparation of Iron
Ores
6. Reagents
E 882 Guide for Accountability and Quality Control in the
4 6.1 Purity of Reagents—Reagent grade chemicals shall be
Chemical Analysis Laboratory
used in all tests. Unless otherwise indicated, it is intended that
3. Summary of Test Method all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
3.1 The sample is dissolved in hydrochloric and nitric acids.
such specifications are available. Other grades may be used,
After the addition of perchloric acid, the solution is evaporated
provided it is first ascertained that the reagent is of sufficient
to strong fumes to dehydrate the silica. The insoluble residue is
high purity to permit its use without lessening the accuracy of
filtered off, ignited, and treated for the recovery of any
the determination.
contained phosphorus. Ammonium molybdate is added to
6.2 Purity of Water—Unless otherwise indicated, references
precipitate phosphomolybdate. The precipitate is filtered off
to water shall be understood to mean reagent water as defined
and washed free from acid. It is then dissolved in an excess of
by Type I of Specification D 1193.
standard sodium hydroxide solution. The excess sodium hy-
6.3 Ammonium Molybdate Solution (Acidic)—Reagent No.
droxide is titrated with a standard solution of nitric acid using
102.
phenolphthalein as an indicator.
6.4 Ammonium Nitrate (NH NO ).
4 3
4. Significance and Use
6.5 Ferric Chloride Solution—Dissolve 0.3 g of pure iron
wire in 25 mL of HCl (1 + 1). Oxidize by adding HNO
4.1 This test method is intended to be used for compliance 3
dropwise to the hot solution. Cool, add 25 mL of HCl, dilute to
1 L and mix.
This test method is under the jurisdiction of ASTM Committee E-1 on
6.6 Ferrous Sulfate Solution—Dissolve 100 g of ferrous
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
sulfate (FeSO ·7H O) in 1 L of sulfuric acid (H SO , 5 + 95).
4 2 2 4
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
Current edition approved April 10, 1996. Published June 1996. Originally
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published as E 278 – 65 T. Last previous edition E 278 – 86 (1991) . “Reagent Chemicals, American Chemical Society Specifications,” Am. Chem.
Annual Book of ASTM Standards, Vol 11.01. Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
Annual Book of ASTM Standards, Vol 14.02. American Chemical Society, see “Reagent Chemicals and Standards,” by Joseph
Annual Book of ASTM Standards, Vol 03.06. Rosin, D. Nostrand Co., Inc., New York, NY, and the “United States Pharmacopeia.”
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 278
6.7 Hydrobromic Acid (1 + 4)—Mix 20 mL of concentrated h, cap the bottle, and cool to room temperature in a desiccator.
hydrobromic acid (HBr, sp gr 1.49) with 80 mL of water. Momentarily release the cap to equalize pressure and weigh the
6.8 Hydrochloric Acid (1 + 1)—Mix equal volumes of con-
capped bottle to the nearest 0.1 mg. Repeat the drying and
centrated hydrochloric acid (HCl, sp gr 1.19) and water. weighing until there is no further weight loss. Transfer the test
6.9 Hydrofluoric Acid (sp gr 1.15)—Concentrated hydrof-
sample to a 400-mL beaker and reweigh the capped bottle to
luoric acid (HF).
the nearest 0.1 mg. The difference between the two weights is
6.10 Nitric Acid, Standard (0.15 N)—Transfer 10 mL of
the weight of the test sample.
clear and water white concentrated nitric acid (HNO ,spgr
8.2 Moisten the test sample with a few millilitres of water
1.42) to a 1-L flask, dilute to the mark, and mix. Standardize
and add 25 mL of HCl for each gram of test sample. Cover and
this solution against the standard NaOH solution using phe-
digest below the boiling point until all soluble minerals are in
nolphthalein as indicator. If desired, this solution may be made
solution. Add 5 mL of HNO and 20 mL of HClO and
3 4
equivalent to the standard sodium hydroxide solution by
evaporate to strong fumes to dehydrate the silica. Cool, add 50
dilution with water.
mL of water, and warm until soluble salts are in solution. Filter
6.11 Nitric Acid, Wash Solution (1 + 99)—Mix 10 mL of
and collect the filtrate in a 300-mL Erlenmeyer flask. Wash the
concentrated HNO , (sp gr 1.42) with 990 mL of water.
residue with HNO (1 + 99), and finally with hot water until
6.12 Perchloric Acid (70 %) (HClO ).
free from perchlorates. Evaporate the filtrate using a low heat.
6.13 Phenolphthalein Indicator Solution—Dissolve 0.2 g of
8.3 Ignite the paper and residue in a platinum crucible.
phenolphthalein in 100 mL of ethanol.
Cool, moisten with several drops of water and add 2 mL of
6.14 Potassium Nitrate, Wash Solution (10 g/L)—Dissolve
HClO and 5 mL of HF, and evaporate to complete dryness.
10 g of potassium nitrate (KNO ) in water, dilute to 1 L, and
Fuse the residue with3gofNa CO . Place the crucible in a
2 3
mix.
250-mL beaker and add 100 mL of water. Heat to disintegrate
6.15 Potassium Permanganate Solution (25 g/L)—Dissolve
the melt and to dissolve all soluble salts. Remove, wash, and
25 g of potassium permanganate (KMnO ) in water and dilute
police the crucible. Filter the alkaline solution through a
to1L.
medium-texture paper and collect the filtrate in the 400-mL
6.16 Sodium Carbonate (Na CO ).
2 3
beaker. Wash the residue with hot water and discard. Acidify
6.17 Sodium Hydroxide, Stock Solution—Dissolve 300 g of
the filtrate with HCl, add 5 mL of the FeCl solution, and
sodium hydroxide (NaOH) in 1 L of water. Add a slight excess
render the solution alkaline to litmus with NH OH
...
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