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

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Issued by

National Development and Reform Commission of China

Level / Type

National · Recommended

Issue date

March 12, 2008

Implementation date

September 1, 2008

Scope

YS/T 509.6-2008 (Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of phosphorus pentoxide content. The molybdenum blue photometric method) is available as an English-translated PDF.

YS/T 509.6-2008 - 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%.

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Document preview — YS/T 509.6-2008

National Standard of the People's Republic of China

ICS: 77.120.99
Classification: H 64

Issued by: National Development and Reform Commission of China

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 (rho 1.84 g/mL).

3.2 Sulfuric acid (1 + 1).

3.3 Sulfuric acid (1 + 3).

3.4 Hydrofluoric acid (rho 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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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 9 pages — is available in the English PDF.

Referenced standards

Cited by

YS/T 261-2011Spodumene concentrate

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