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Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of phosphorus pentoxide content. The molybdenum blue photometric method
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| YS/T 509.6-2006 | English | 199 |
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Methods for chemical analysis of sqodumenite and lepidolite concentrates The o-phenanthroline photometric method for the determination of ferric oxide content
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YS/T 509.6-2008: PDF in English (YST 509.6-2008) YS/T 509.6-2008
YS
NON-FERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing YS/T 509.7-2006
Methods for Chemical Analysis of Spodumene and
Lepidolite Concentrates - Determination of
Phosphorus Pentoxide Content - The Molybdenum
Blue Photometric Method
ISSUED ON: MARCH 12, 2008
IMPLEMENTED ON: SEPTEMBER 1, 2008
Issued by: National Development and Reform Commission of China
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method Summary ... 5
3 Reagents ... 5
4 Instrument ... 6
5 Test Piece ... 6
6 Analytical Procedures ... 6
7 Calculation of Analysis Result ... 7
8 Precision ... 8
9 Quality Assurance and Control ... 9
Foreword
YS/T 509 Methods for Chemical Analysis of Spodumene and Lepidolite Concentrates
is divided into 11 parts:
---Part 1: Determination of Lithium Oxide Sodium Oxide and Potassium Oxide
Contents - Flame Atomic Absorption Spectrometric Method;
---Part 2: Determination of Rubidium Oxide and Caesium Oxide Contents - Flame
Atomic Absorption Spectrometric Method;
---Part 3: Determination of Silicon Dioxide Content - Gravimetric - Molybdenum
Blue Photometric Method;
---Part 4: Determination of Aluminum Oxide Content - EDTA Compleximetric
Method;
---Part 5: Determination of Ferric Oxide Content - O-phenanthroline Photometric
Method and EDTA Compleximetric Method;
---Part 6: Determination of Phosphorus Pentoxide Content - The Molybdenum
Blue Photometric Method;
---Part 7: Determination of Beryllium Oxide Content - Chromazurol S and
Cetyltrimethyl Ammonium Bromide Spectrophotometric Method;
---Part 8: Determination of Calcium Oxide and Magnesium Oxide Content - Flame
Atomic Absorption Spectrometric Method;
---Part 9: Determination of Calcium Oxide and Magnesium Oxide Content - Flame
Atomic Absorption Spectrometric Method;
---Part 10: Determination of Manganous Oxide Content - Persulfate Oxidation
Photometric Method;
---Part 11: Determination of Loss on Ignition - Gravimetric Method.
This Part is Part 6.
This Part serves as a replacement of YS/T 509.7-2006 Methods for Chemical Analysis
of Spodumenite and Lepidolite Concentrates - The Molybdenum Blue Photometric
Method for the Determination of Phosphorus Pentoxide Content (the former GB/T
3885.7-1983).
In comparison with YS/T 509.7-2006, this Part mainly has the following changes:
---“place it in a beaker” in 3.7 is modified into “place it in a 250 mL beaker”;
Methods for Chemical Analysis of Spodumene and
Lepidolite Concentrates - Determination of
Phosphorus Pentoxide Content - The Molybdenum
Blue Photometric Method
1 Scope
This Part specifies the method of determining phosphorus pentoxide content in
spodumene and lepidolite concentrates.
This Part is applicable to the determination of phosphorus pentoxide content in
spodumene and lepidolite concentrates. The range of determination is 0.01% ~ 1.00%.
2 Method Summary
Use hydrofluoric acid and sulfuric acid to decompose the test piece; sulfuric acid emits
smoke, which drives off silicon and fluorine, and is leached with water. Add ammonium
molybdate to 0.5 mol/L ~ 0.65 mol/L H2SO4 medium to make phosphorus generate
phosphomolybdenum heteropoly acid. Use ascorbic acid as a reducing agent; heat up
in boiling water to reduce phosphomolybdenum heteropoly acid to phosphorus
molybdenum blue. At a wavelength of 700 nm of the spectrophotometer, measure its
absorbance.
3 Reagents
Unless it is otherwise specified, only reagents that are confirmed to be analytically pure,
and distilled water or water of equivalent purity are used in the analysis.
3.1 Sulfuric acid ( 1.84 g/mL).
3.2 Sulfuric acid (1 + 1).
3.3 Sulfuric acid (1 + 3).
3.4 Hydrofluoric acid ( 1.15 g/mL).
3.5 Ammonium molybdate solution (40 g/L).
3.6 Ascorbic acid solution (50 g/L): prepare it right before use.
3.7 Phosphorus pentoxide standard stock solution: weigh-take 1.9175 g of potassium
Conduct a blank test on the accompanying sample.
6.4 Determination
6.4.1 Place the sample (6.1) in a platinum dish; add 10 mL of hydrofluoric acid (3.4)
and 5 mL of sulfuric acid (3.2). Place it on a sand bath and heat it up to decompose it;
steam it, until it emits white smoke of sulfur trioxide for 3 min ~ 5 min. Make the
remaining volume of the solution about 2 mL, then, remove it and cool it down.
6.4.2 Use water to wash the wall of the dish. Add 20 mL of water; heat it up on a sand
bath. When all salts are dissolved, remove it; cool it down to room temperature. Then,
transfer it into a 100 mL volumetric flask; use water to dilute it to the scale; mix it well.
6.4.3 Transfer-take 25.00 mL of solution (6.4.2); place it in a 50 mL volumetric flask.
Add 5 mL of sulfuric acid (3.3) and 5 mL of ascorbic acid solution (3.6). Under constant
shaking, add 4 mL of ammonium molybdate solution (3.5); mix it up. Use water to rinse
the neck of the volumetric flask. Add water to make the volume of the color-developing
solution about 45 mL; mix it well.
6.4.4 Place the volumetric flask in a boiling water bath to heat it up for 5 min. Then,
take it out. Use running water to cool it down to room temperature. Use water to dilute
to the scale; mix it well.
6.4.5 Transfer part of the solution (6.4.4) into a 1 cm cuvette; take the blank of the
accompanying sample as a reference. At a wavelength of 700 nm of the
spectrophotometer, measure its absorbance. Through the working curve, find out the
corresponding phosphorus pentoxide content.
6.5 Drawing of Working Curve
6.5.1 Transfer-take 0 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL and 5.00 mL of
phosphorus pentoxide standard solution (3.8). Respectively place them in a group of
50 mL volumetric flasks. Add 7 mL of sulfuric acid (3.3), 25 mL of water and 5 mL of
ascorbic acid solution (3.6). Under constant shaking, add 4 mL of ammonium
molybdate solution (3.5); mix it well. Use water to rinse the neck of the volumetric flask.
Add water to make the volume of the color-developing solution about 45 mL; proceed
in accordance with the steps in 6.4.4.
6.5.2 Transfer part of the solution (6.5.1) into a 1 cm cuvette; take the reagent blank
as a reference. At a wavelength of 700 nm of the spectrophotometer, measure its
absorbance. Use phosphorus pentoxide content as the x-coordinate; take its
absorbance as the y-coordinate; draw a working curve.
7 Calculation of Analysis Result
The mass fraction w of phosphorus pentoxide, expressed in (%), shall be calculated in
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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