ASTM E1070-00(2005)

Standard Test Method for Determination of Phosphorus in Iron Ores by the Phosphometric Method

SIGNIFICANCE AND USE
This test method for the analysis of iron ore concentrates and agglomerates is primarily intended as a referee method to test for compliance with compositional specifications. It is assumed that users of this test method 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 shall be followed, such as those described in Guide E 882.
The determination of this element is needed for international trade and primary iron and steel making.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2005
• ICS: 73.060.10 - Iron ores
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.02 - Ores, Concentrates, and Related Metallurgical Materials

Relations

• Replaces: ASTM E1070-00 - Standard Test Method for Determination of Phosphorus in Iron Ores by the Phosphometric Method
• Effective Date: 01-Oct-2005
• Replaced By: ASTM E1070-11 - Standard Test Method for Determination of Phosphorus in Iron Ores by Phospho-Molybdenum-Blue Spectrophotometry
• Effective Date: 01-Sep-2011

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E1070–00(Reapproved2005)
Standard Test Method for
Determination of Phosphorus in Iron Ores by Photometric
Method
This standard is issued under the fixed designation E1070; 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 4. Summary of Test Method
1.1 This test method covers the determination of phospho- 4.1 Thesampleisfusedinazirconiumcruciblewithsodium
rus in iron ores, concentrates, and agglomerates in the concen- peroxide.The melt is dissolved in water and hydrochloric acid.
tration range from 0.005 to 1.0 % phosphorus. In a suitable aliquot, the molybdenum blue complex is formed
1.2 The values stated in SI units are to be regarded as by the addition of ammonium molybdate-hydrazine sulfate
standard. No other units of measurement are included in this solution. The absorbance of the phospho-molybdenum-blue
standard. complex is measured at 725 nm.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 5.1 Thistestmethodfortheanalysisofironoreconcentrates
and agglomerates is primarily intended as a referee method to
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. test for compliance with compositional specifications. It is
assumed that users of this test method will be trained analysts
2. Referenced Documents
capable of performing common laboratory procedures skill-
2.1 ASTM Standards: fully and safely. It is expected that work will be performed in
D1193 Specification for Reagent Water a properly-equipped laboratory and that proper waste disposal
E50 Practices for Apparatus, Reagents, and Safety Consid- procedures will be followed. Appropriate quality control prac-
erations for Chemical Analysis of Metals, Ores, and tices shall be followed, such as those described in Guide E882.
Related Materials 5.2 The determination of this element is needed for inter-
E60 Practice for Analysis of Metals, Ores, and Related national trade and primary iron and steel making.
Materials by Molecular Absorption Spectrometry
6. Interferences
E135 Terminology Relating to Analytical Chemistry for
6.1 Elements normally found in iron ores do not interfere
Metals, Ores, and Related Materials
E877 Practice for Sampling and Sample Preparation of Iron excepting arsenic giving positive interference (0.01 %
As = 0.001 % P).
Ores and Related Materials for Determination of Chemical
Composition
7. Apparatus
E882 Guide for Accountability and Quality Control in the
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
3.1 Definitions—For definitions of terms used in this test 1-cm path length cell in accordance with Practice E60.
method, refer to Terminology E135.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be
This test method is under the jurisdiction of ASTM Committee E01 on
used in all tests. Unless otherwise indicated, it is intended that
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
all reagents conform to the specifications of the Committee on
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials. Analytical Reagents of theAmerican Chemical Society, where
Current edition approved Oct. 1, 2005. Published October 2005. Originally
approved in 1985. Last previous edition approved in 2000 as E1070 – 00. DOI:
10.1520/E1070-00R05.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1070–00 (2005)
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
s5
Œ
~n 2 1!
100 d
v 5 Œ
S D
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, %.
such specifications are available. Other grades may be used, ofsolutionAintoa50-mLvolumetricflask,dilutetomarkwith
provided it is first ascertained that the reagent is of sufficient water, and mix. This solution, B, provides the standard
high purity to permit its use without lessening the accuracy of phosphorus solution for calibration 1 mL = 10 µg P.
the determination.
8.2 Purity of Water—Unless otherwise indicated, references 9. Hazards
to water shall be understood to mean reagent water as defined
9.1 For precautions to be observed in this method, refer to
by Type II of Specification D1193.
Practices E50.
8.3 Ammonium Molybdate Solution (20 g/L)—To500mLof
water, add cautiously and slowly 300 mL of H SO and cool.
2 4
10. Sampling and Sample Preparation
Add 20 g of ammonium molybdate (NH ) -Mo O ·4H O. Stir
4 6 7 24 2
10.1 Collect and prepare gross samples in accordance with
to dissolve and dilute to 1 L with water.
Practice E877.
8.4 Fusion Blank—Dissolve4gofNa O in40mLofwater
2 2
10.2 Pulverize the laboratory sample to pass a No. 100
in a 250-mL beaker. Add 30 mL of HCl. Boil for 2 min. Cool
(150-µm) sieve.
and dilute to 100 mL with water in a volumetric flask. Prepare
fresh as needed.
NOTE 2—To facilitate decomposition, some ores, such as specular
8.5 Hydrazine Sulfate (1.5 g/L)—Dissolve 0.15 g of hydra-
hematite, require grinding to pass a No. 200 (75-µm) sieve.
zine sulfate NH ·NH ·H SO in water and dilute to 100 mL
2 2 2 4
11. Calibration and Standardization
with water. Prepare fresh as needed.
8.6 Molybdate (5 g/L) Hydrazine Sulfate (0.15 g/L)
11.1 The recommended concentration range is from 0.005
Solution—Add 50 mL of ammonium molybdate solution (20
to 0.10
...