ASTM E878-96
(Test Method)Standard Test Method for Determination of Titanium in Iron Ores and Related Materials by Diantipyrylmethane Untraviolet Spectrometry
Standard Test Method for Determination of Titanium in Iron Ores and Related Materials by Diantipyrylmethane Untraviolet Spectrometry
SCOPE
1.1 This test method covers the determination of titanium in iron ores, concentrates, and agglomerates in the concentration range from 0.01 to 6.0% titanium.
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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Designation: E 878 – 96
Standard Test Method for
Determination of Titanium in Iron Ores and Related
Materials by Diantipyrylmethane Ultraviolet Spectrometry
This standard is issued under the fixed designation E 878; 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 5. Interferences
1.1 This test method covers the determination of titanium in 5.1 None of the elements normally found in iron ores
iron ores, concentrates, and agglomerates in the concentration interfere.
range from 0.01 to 6.0 % titanium.
6. Reagents
1.2 This standard does not purport to address all of the
6.1 Purity of Reagents—Reagent grade chemicals shall be
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on
priate safety and health practices and determine the applica-
Analytical Reagents of the American Chemical Society where
bility of regulatory limitations prior to use.
such specifications are available. Other grades may be used,
2. Referenced Documents
provided it is first ascertained that the reagent is of sufficient
2.1 ASTM Standards: high purity to permit its use without lessening the accuracy of
D 1193 Specification for Reagent Water the determination.
E 877 Practice for Sampling and Sample Preparation of Iron 6.2 Purity of Water—Unless otherwise indicated, references
Ores to water shall be understood to mean reagent water as defined
E 882 Guide for Accountability and Quality Control in the by Type I of Specification D 1193.
Chemical Analysis Laboratory 6.3 Ascorbic Acid Solution (10 g/100 mL) (C H O )—
6 8 6
Dissolve 10 g of ascorbic acid (C H O ) in water and dilute to
6 8 6
3. Summary of Test Method
100 mL. Prepare fresh as needed.
3.1 The sample is decomposed by treatment with hydro-
6.4 Diantipyrylmethane Solution (15 g/L) C H O N ·
23 24 2 4
chloric, nitric, and sulfuric acids, or by sintering with sodium H O—Dissolve 15 g of the reagent in about 300 mL of water
peroxide, or by fusion with sodium tetraborate and sodium
and 30 mL of (H SO ) (1 + 1) (7.10) and dilute to 1 L with
2 4
carbonate. Iron is reduced in an acid medium with ascorbic water. If a residue remains, filter and store the filtrate in a
acid, the color is developed with diantipyrylmethane, and the
brown bottle.
absorbance is measured at approximately 385 nm. 6.5 Ferric Ammonium Sulfate (100 g/L)—Dissolve 100 g of
ferric ammonium sulfate (Fe (SO ) ·(NH ) SO in 800 mL of
2 4 3 4 2 4
4. Significance and Use
water containing 5 mL of H SO (1 + 1) (6.11) and dilute to 1
2 4
4.1 This test method is intended to be used for compliance
L with water.
with compositional specifications for titanium content. It is
6.6 Hydrochloric Acid (1 + 1)—Mix 1 volume of concen-
assumed that all who use these procedures will be trained
trated hydrochloric acid (HCl) with 1 volume of water.
analysts capable of performing common laboratory procedures
6.7 Hydrochloric Acid (1 + 4)—Mix 1 volume HCl with 4
skillfully and safely. It is expected that work will be performed
volumes of water.
in a properly equipped laboratory and that proper waste
6.8 Potassium Pyrosulfate (K S O ).
2 2 7
disposal procedures will be followed. Appropriate quality
6.9 Sodium Tetraborate (Anhydrous) (Na B O )—Dry the
2 4 7
control practices must be followed such as those described in
commercial sodium tetraborate at 60 to 70°C, then at 160°C,
Guide E 882.
and finally calcine at 400°C.
6.10 Sodium Tetraborate/Sodium Carbonate (Na B O /
2 4 7
Na CO ) Fusion Mixture— Mix 1 part of Na B O and 1 part
2 3 2 4 7
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Slags, Refractories, Cement, and
Reagent Chemicals, American Chemical Society Specifications, American
Related Oxide Materials. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved April 10, 1996. Published June 1996. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as E 878 – 82. Last previous edition E 878 – 95. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 11.01. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 03.06. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 878
of Na CO and store in an airtight container.
Amount of
2 3
sulfuric acid
6.11 Sulfuric Acid (1 + 1)—Carefully pour 1 volume of
Weight of test to be added Aliquot,
concentrated sulfuric acid (H SO ) into 1 volume of water.
Ti content, % portion, g in 9.1, mL mL
2 4
6.12 Sulfuric Acid (1 + 9)—Carefully pour 1 volume of
0.01–0.1 1.0 20 20
H SO into 9 volumes of water.
2 4 0.1–0.3 1.0 20 10
0.3–1.0 0.5 10 5
6.13 Sulfuric Acid (2 + 98)—Carefully pour 2 volumes of
1.0–6.0 0.1 10 5
H SO into 98 volumes of water.
2 4
Dry the bottle and contents for1hat105 to 110°C. Cap the
6.14 Standard Titanium Solution:
bottle and cool to room temperature in a desiccator. Momen-
6.14.1 Solution A (1 mL 5 0.1 mg Ti)—Transfer 0.1670 g
tarily release the cap to equalize the pressure and weigh the
of TiO (previously calcined at 900°C) to a platinum crucible,
capped bottle and sample to the nearest 0.1 mg. Repeat the
add3to4gofK S O , cover, and fuse at a temperature of
2 2 7
drying and weighing until there is no further weight loss.
600°C until a clear melt is obtained. Place the cooled crucible
Transfer the test sample to a 250-mL beaker and reweigh the
and cover in a 250-mL beaker, add 50 to 60 mL of H SO
2 4
capped bottle to the nearest 0.1 mg. The difference between the
(1 + 9) (6.12), and heat to dissolve the melt. Wash crucible and
two weights is the weight of the test sample taken for analysis.
cover with H SO (1 + 9) (6.12) and remove, adding the
2 4
8.1.2 Carry a reagent blank through all steps of the proce-
washings to the 250-mL beaker. Transfer the solution of a 1-L
dure, starting with 8.1.3.
volumetric flask, dilute to volume with H SO (1 + 9) (6.12),
2 4
8.1.3 Decomposition of Sample—Moisten the test sample
and mix.
with a few millilitres of water, add 30 mL of hydrochloric acid,
6.14.2 Solution B (1 mL 5 0.02 mg Ti)—Transfer 50.0 mL
cover, and digest below the boiling point until no further attack
of standard titanium Solution A to a 250-mL volumetric flask,
is apparent. Add 5 mL of nitric acid and 10 to 20 mL of sulfuric
dilute to volume with H SO (1 + 9) (6.12), and mix.
2 4
acid (see amounts specified in 8.1.1) evaporate slowly to fumes
of H SO , then heat strongly for 10 min. Allow the solution to
2 4
7. Sampling and Sample Preparation
cool, add slowly 50 mL of water and 20 mL of hydrochloric
7.1 Sampling—The gross sample shall be collected and acid, and warm until soluble salts are in solution.
prepared in accordance with Practice E 877.
8.1.4 Filter on a fine-textured filter paper and collect the
7.2 Sample Preparation—Pulverize the laboratory sample filtrate in a 250-mL beaker. Transfer the residue quantitatively
to the filter paper and wash it two or three times with hot dilute
to pass a No. 100 (150-m) sieve.
sulfuric acid (2+98) (6.13) and two or three times with hot
NOTE 1—To facilitate decomposition, some ores such as specular
water. Reserve the filtrate.
hematite require grinding to pass a No. 200 (75-μm) sieve.
8.1.5 Treatment of Insoluble Matter— Ignite the paper and
residue in a platinum crucible. Cool, moisten with several
8. Procedure
drops of water, add 3 or 4 drops of dilute sulfuric acid (1+1)
NOTE 2—If the procedure is based on acid decomposition, use steps in
(6.11) and 10 mL of hydrofluoric acid. Evaporate slowly to
8.1. If the procedure is based on alkaline sintering, use steps in 8.2. If the
expel silica and excess of sulfuric acid. Cool, add to the residue
procedure is based on alkaline fusion, use steps in 8.3.
about2gof potassium pyrosulfate, cover the crucible, and fuse
8.1 Acid Decomposition:
over a burner (approximately 500°C) until a clear melt is
obtained.
8.1.1 Weigh approximately the amount of the test sample
specified in the table
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