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YS/T 509.6-2008 English PDF (YST509.6-2008)

YS/T 509.6-2008 English PDF (YST509.6-2008)

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YS/T 509.6-2008: Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of phosphorus pentoxide content. The molybdenum blue photometric method
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%.
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
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