ASTM E878-01(2005)
(Test Method)Standard Test Method for Determination of Titanium in Iron Ores and Related Materials by Diantipyrylmethane Ultraviolet Spectrometry
Standard Test Method for Determination of Titanium in Iron Ores and Related Materials by Diantipyrylmethane Ultraviolet Spectrometry
SIGNIFICANCE AND USE
This test method is intended to be used for compliance with compositional specifications for titanium content. It is assumed that all who use these procedures 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 must be followed such as those described in Guide E 882.
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:E878–01(Reapproved2005)
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 E878; 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 acid, the color is developed with diantipyrylmethane, and the
absorbance is measured at approximately 385 nm.
1.1 This test method covers the determination of titanium in
iron ores, concentrates, and agglomerates in the concentration
5. Significance and Use
range from 0.01 to 6.0 % titanium.
5.1 This test method is intended to be used for compliance
1.2 This standard does not purport to address all of the
with compositional specifications for titanium content. It is
safety concerns, if any, associated with its use. It is the
assumed that all who use these procedures will be trained
responsibility of the user of this standard to establish appro-
analysts capable of performing common laboratory procedures
priate safety and health practices and determine the applica-
skillfully and safely. It is expected that work will be performed
bility of regulatory limitations prior to use.
in a properly equipped laboratory and that proper waste
2. Referenced Documents disposal procedures will be followed. Appropriate quality
control practices must be followed such as those described in
2.1 ASTM Standards:
Guide E882.
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Consid-
6. Interferences
erations for Chemical Analysis of Metals, Ores, and
6.1 None of the elements normally found in iron ores
Related Materials
interfere.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
7. Reagents and Materials
E877 Practice for Sampling and Sample Preparation of Iron
7.1 Purity of Reagents—Reagent grade chemicals shall be
Ores and Related Materials for Determination of Chemical
used in all tests. Unless otherwise indicated, it is intended that
Composition
all reagents conform to the specifications of the Committee on
E882 Guide for Accountability and Quality Control in the
Analytical Reagents of the American Chemical Society where
Chemical Analysis Laboratory
such specifications are available. Other grades may be used,
3. Terminology provided it is first ascertained that the reagent is of sufficient
high purity to permit its use without lessening the accuracy of
3.1 For definitions of terms used in this test method, refer to
the determination.
Terminology E135.
7.2 Purity of Water—Unless otherwise indicated, references
4. Summary of Test Method to water shall be understood to mean reagent water as defined
by Type I of Specification D1193.
4.1 The sample is decomposed by treatment with hydro-
7.3 Ascorbic Acid Solution (10 g/100 mL) (C H O )—
6 8 6
chloric, nitric, and sulfuric acids, or by sintering with sodium
Dissolve 10 g of ascorbic acid (C H O ) in water and dilute to
6 8 6
peroxide, or by fusion with sodium tetraborate and sodium
100 mL. Prepare fresh as needed.
carbonate. Iron is reduced in an acid medium with ascorbic
7.4 Diantipyrylmethane Solution (15 g/L) C H O N ·
23 24 2 4
H O—Dissolve 15 g of the reagent in about 300 mL of water
This test method is under the jurisdiction of ASTM Committee E01 on
and 30 mL of (H SO ) (1 + 1) (7.10) and dilute to 1 L with
2 4
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
water. If a residue remains, filter and store the filtrate in a
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
brown bottle.
lurgical Materials.
Current edition approved May 1, 2005. Published June 2005. Originally
approved in 1982. Last previous edition approved in 2001 as E878 – 01. DOI:
10.1520/E0878-01R05. Reagent Chemicals, American Chemical Society Specifications, American
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM testing of reagents not listed by the American Chemical Society, see the United
Standards volume information, refer to the standard’s Document Summary page on States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
the ASTM website. Inc. (USPC), Rockville, MD, http://www.usp.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E878–01 (2005)
7.5 Ferric Ammonium Sulfate (100 g/L)—Dissolve 100 g of
Amount of
sulfuric acid
ferric ammonium sulfate (Fe (SO ) ·(NH ) SO in 800 mLof
2 4 3 4 2 4
Weight of test to be added Aliquot,
water containing 5 mL of H SO (1+1)(7.11) and dilute to 1
2 4
Ti content, % portion, g in 9.1, mL mL
L with water.
0.01–0.1 1.0 20 20
7.6 Hydrochloric Acid (1 + 1)—Mix 1 volume of concen-
0.1–0.3 1.0 20 10
trated hydrochloric acid (HCl) with 1 volume of water.
0.3–1.0 0.5 10 5
1.0–6.0 0.1 10 5
7.7 Hydrochloric Acid (1 + 4)—Mix 1 volume HCl with 4
volumes of water.
Dry the bottle and contents for1hat105to110°C. Cap the
7.8 Potassium Pyrosulfate (K S O ).
2 2 7 bottle and cool to room temperature in a desiccator. Momen-
7.9 Sodium Tetraborate (Anhydrous) (Na B O )—Dry the
tarily release the cap to equalize the pressure and weigh the
2 4 7
commercial sodium tetraborate at 60 to 70°C, then at 160°C,
capped bottle and sample to the nearest 0.1 mg. Repeat the
and finally calcine at 400°C.
drying and weighing until there is no further weight loss.
7.10 Sodium Tetraborate/Sodium Carbonate (Na B O / Transfer the test sample to a 250-mL beaker and reweigh the
2 4 7
Na CO ) Fusion Mixture— Mix 1 part of Na B O and 1 part
capped bottle to the nearest 0.1 mg.The difference between the
2 3 2 4 7
of Na CO and store in an airtight container. two weights is the weight of the test sample taken for analysis.
2 3
7.11 Sulfuric Acid (1 + 1)—Carefully pour 1 volume of 10.1.2 Carry a reagent blank through all steps of the
procedure, starting with 10.1.3.
concentrated sulfuric acid (H SO ) into 1 volume of water.
2 4
10.1.3 Decomposition of Sample—Moisten the test sample
7.12 Sulfuric Acid (1 + 9)—Carefully pour 1 volume of
with a few milliliters of water, add 30 mLof hydrochloric acid,
H SO into 9 volumes of water.
2 4
cover, and digest below the boiling point until no further attack
7.13 Sulfuric Acid (2 + 98)—Carefully pour 2 volumes of
isapparent.Add5mLofnitricacidand10to20mLofsulfuric
H SO into 98 volumes of water.
2 4
acid (see amounts specified in 10.1.1) evaporate slowly to
7.14 Standard Titanium Solution:
fumes of H SO , then heat strongly for 10 min. Allow the
2 4
7.14.1 Solution A (1 mL = 0.1 mg Ti)—Transfer 0.1670 g of
solution to cool, add slowly 50 mL of water and 20 mL of
TiO (previouslycalcinedat900°C)toaplatinumcrucible,add
hydrochloric acid, and warm until soluble salts are in solution.
3to4gofK S O , cover, and fuse at a temperature of 600°C
2 2 7
10.1.4 Filter on a fine-textured filter paper and collect the
until a clear melt is obtained. Place the cooled crucible and
filtrate in a 250-mL beaker. Transfer the residue quantitatively
cover in a 250-mL beaker, add 50 to 60 mL of H SO (1+9)
2 4
to the filter paper and wash it two or three times with hot dilute
(7.12), and heat to dissolve the melt. Wash crucible and cover
sulfuric acid (2+98) (7.13) and two or three times with hot
with H SO (1+9)(7.12) and remove, adding the washings to
2 4
water. Reserve the filtrate.
the 250-mL beaker. Transfer the solution of a 1-L volumetric
10.1.5 Treatment of Insoluble Matter— Ignite the paper and
flask, dilute to volume with H SO (1+9)(7.12), and mix.
2 4
residue in a platinum crucible. Cool, moisten with several
7.14.2 Solution B (1 mL = 0.02 mg Ti)—Transfer 50.0 mL
drops of water, add 3 or 4 drops of dilute sulfuric acid (1+1)
of standard titanium Solution A to a 250-mL volumetric flask,
(7.11) and 10 mL of hydrofluoric acid. Evaporate slowly to
dilute to volume with H SO (1+9)(7.12), and mix.
2 4
expelsilicaandexcessofsulfuricacid.Cool,addtotheresidue
about2gofpotassiumpyrosulfate,coverthecrucible,andfuse
8. Hazards
over a burner (approximately 500°C) until a clear melt is
8.1 For precautions to be observed in this test method, refer
obtained.
to Practices E50.
10.1.6 Dissolve the cool melt in the reserved filtrate from
10.1.4, remove, and wash the crucible and cover, adding the
9. Sampling and Sample Preparation
washings to the 250-mL beaker. Transfer the solution to a
200-mL volumetric flask, dilute to volume, and mix. Continue
9.1 Sampling—The gross sample shall be collected and
in accordance with 10.4.
prepared in accordance with Practice E877.
10.2 Alkaline Sintering Decompositi
...
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