ASTM E1070-00
(Test Method)Standard Test Method for Determination of Phosphorus in Iron Ores by the Phosphometric Method
Standard Test Method for Determination of Phosphorus in Iron Ores by the Phosphometric Method
SCOPE
1.1 This test method covers the determination of phosphorus in iron ores, concentrates, and agglomerates in the concentration range from 0.005 to 1.0% phosphorus.
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:E1070–00
Standard Test Method for
Determination of Phosphorus in Iron Ores by Photometric
Method
This standard is issued under the fixed designation E 1070; 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 solution. The absorbance of the phospho-molybdenum-blue
complex is measured at 725 nm.
1.1 This test method covers the determination of phospho-
rus in iron ores, concentrates, and agglomerates in the concen-
5. Significance and Use
tration range from 0.005 to 1.0 % phosphorus.
5.1 Thistestmethodfortheanalysisofironoreconcentrates
1.2 This standard does not purport to address all of the
and agglomerates is primarily intended as a referee method to
safety concerns, if any, associated with its use. It is the
test for compliance with compositional specifications. It is
responsibility of the user of this standard to establish appro-
assumed that users of this test method will be trained analysts
priate safety and health practices and determine the applica-
capable of performing common laboratory procedures skill-
bility of regulatory limitations prior to use.
fully and safely. It is expected that work will be performed in
2. Referenced Documents a properly-equipped laboratory and that proper waste disposal
procedures will be followed. Appropriate quality control prac-
2.1 ASTM Standards:
ticesshallbefollowed,suchasthosedescribedinGuideE 882.
D 1193 Specification for Reagent Water
5.2 The determination of this element is needed for inter-
E50 Practices for Apparatus, Reagents, and Safety Precau-
national trade and primary iron and steel making.
tions for Chemical Analysis of Metals
E60 Practice for Analysis of Metals, Ores, and Related
6. Interferences
Materials by Molecular Absorption Spectrometery
6.1 Elements normally found in iron ores do not interfere
E 135 Terminology Relating to Analytical Chemistry for
excepting arsenic giving positive interference (0.01 %
Metals, Ores, and Related Materials
As = 0.001 % P).
E 877 PracticeforSamplingandSamplePreparationofIron
Ores and Related Materials
7. Apparatus
E 882 Guide for Accountability and Quality Control in the
4 7.1 Zirconium Crucible, 50 mL capacity.
Chemical Analysis Laboratory
7.2 Spectrophotometer—Visible spectrophotometer capable
3. Terminology of measuring absorbance at the 725 nm wavelength using a
1-cm path length cell in accordance with PracticesE60.
3.1 Definitions—For definitions of terms used in this test
method, refer to Terminolgy E 135.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be
4. Summary of Test Method
used in all tests. Unless otherwise indicated, it is intended that
4.1 Thesampleisfusedinazirconiumcruciblewithsodium
all reagents conform to the specifications of the Committee on
peroxide.The melt is dissolved in water and hydrochloric acid.
Analytical Reagents of theAmerican Chemical Society, where
In a suitable aliquot, the molybdenum blue complex is formed
such specifications are available. Other grades may be used,
by the addition of ammonium molybdate-hydrazine sulfate
provided it is first ascertained that the reagent is of sufficient
high purity to permit its use without lessening the accuracy of
the determination.
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. Reagent Chemicals, American Chemical Society Specifications, American
Current edition approved Nov. 10, 2000. Published January 2001. Originally Chemical Society, Washington, DC. For suggestions on the testing of reagents not
published as E 1070 – 85. Last previous edition E 1070 – 95.
listed by the American Chemical Society, see Analar Standards for Laboratory
Annual Book of ASTM Standards, Vol 11.01. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 03.05. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 03.06. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1070–00
8.2 Purity of Water—Unless otherwise indicated, references 10. Sampling and Sample Preparation
to water shall be understood to mean reagent water as defined
10.1 Collect and prepare gross samples in accordance with
by Type II of Specification D 1193.
Practice E 877.
8.3 Ammonium Molybdate Solution (20 g/L)—To500mLof
10.2 Pulverize the laboratory sample to pass a No. 100
water, add cautiously and slowly 300 mL of H SO and cool.
2 4
(150-µm) sieve.
Add 20 g of ammonium molybdate (NH ) -Mo O ·4H O. Stir
4 6 7 24 2
NOTE 2—To facilitate decomposition, some ores, such as specular
to dissolve and dilute to 1 L with water.
hematite, require grinding to pass a No. 200 (75-µm) sieve.
8.4 Fusion Blank—Dissolve4gofNa O in 40 mL of
2 2
water in a 250-mL beaker.Add 30 mL of HCl. Boil for 2 min.
11. Calibration and Standardization
Cool and dilute to 100 mL with water in a volumetric flask.
11.1 The recommended concentration range is from 0.005
Prepare fresh as needed.
TABLE 1 Statistical Information
Relative Number of
Average Phosphorus Concentration, Number of
A
Sample Standard Deviation Standard Participating
% Replicates
B
Deviation, % Laboratories
C
Japan 830-1 (0.125) 0.1270 0.0035 2.75 8 24
C
NBS 690 (0.011) 0.0085 0.0010 11.76 8 24
C
NBS 692 (0.039) 0.0393 0.0022 5.61 8 24
C
NBS 693 (0.056) 0.0554 0.0020 3.61 8 24
A
Standard deviation.
B
Relative standard deviations in this test method are calculated respectively as follows:
d
s5Œ
~n 2 1!
100 d
v 5
S DŒ
x¯ ~n 2 1!
where:
x¯ = average concentration, %,
d = difference of the determination from the mean, and
n = number of determinations.
C
Certificate value—Phosphorus concentration, %.
8.5 Hydrazine Sulfate (1.5 g/L)—Dissolve 0.15 g of hydra- to 0.10 mg phosphorus in 50 mL of color solution using cell
zine sulfate NH ·NH ·H SO in water and dilute to 100 mL depth of 1 cm.
2 2 2 4
with water. Prepare fresh as needed.
11.2 Into a ser
...
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