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YS/T 509.8-2008Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of calcium oxide and magnesium oxide content. Flame atomic absorption spectrometric 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 509.8-2008 (Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of calcium oxide and magnesium oxide content. Flame atomic absorption spectrometric method) is available as an English-translated PDF.

YS/T 509.8-2008 - This Part specifies the method of determining calcium oxide and magnesium oxide content in spodumene and lepidolite concentrates. This Part is applicable to the determination of calcium oxide and magnesium oxide content in spodumene and lepidolite concentrates. The range of determination is 0.10% ~ 3.00%.

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Document preview — YS/T 509.8-2008

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...7
6 Analytical Procedures...7
7 Calculation of Analysis Result...8
8 Precision...9
9 Quality Assurance and Control...10

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 8.

This Part serves as a replacement of YS/T 509.9-2006 Methods for Chemical Analysis

of Spodumenite and Lepidolite Concentrates - The Atomic Absorption

Spectrophotometric Method for the Determination of Calcium Oxide and Magnesium

Oxide Contents (the former GB/T 3885.9-1983).

In comparison with YS/T 509.9-2006, this Part mainly has the following changes:

---The text formatting is re-edited;

Methods for Chemical Analysis of Spodumene and

Lepidolite Concentrates - Determination of Calcium

Oxide and Magnesium Oxide Content - Flame Atomic

Absorption Spectrometric Method

1 Scope

This Part specifies the method of determining calcium oxide and magnesium oxide

content in spodumene and lepidolite concentrates.

This Part is applicable to the determination of calcium oxide and magnesium oxide

content in spodumene and lepidolite concentrates. The range of determination is 0.10%

~ 3.00%.

2 Method Summary

Use hydrofluoric acid, perchloric acid and hydrochloric acid to decompose the sample.

In the hydrochloric acid medium, add lanthanum and strontium release agents. At

wavelengths of 422.7 nm and 285.2 nm of the atomic absorption spectrometer, use the

air - acetylene (or nitrous oxide - acetylene) enriched flame for the respective

determination of calcium oxide and magnesium oxide.

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 Perchloric acid (rho 1.67 g/mL).

3.2 Hydrofluoric acid (rho 1.15 g/mL).

3.3 Hydrochloric acid (1 + 1).

3.4 Lanthanum solution: weigh-take 40.11 g of lanthanum chloride (LaCl3 - 7H2O);

place it in a 250 mL beaker; use water to dissolve it. When the solution is turbid, add a

few drops of hydrochloric acid (3.3), or heat it up to make it clear. Transfer the solution

into a 500 mL volumetric flask; use water to dilute it to the scale; mix it well. 1 mL of

this solution contains 30 mg of lanthanum.

3.5 Strontium solution: weigh-take 15.2 g of strontium chloride (SrCl2 - 6H2O); place it

---Linear working curve: in accordance with the concentration, divide the working

curve into five equal sections. The ratio of the absorbance difference of the

highest section to the absorbance difference of the lowest section shall be not

less than 0.7.

5 Test Piece

5.1 Spodumene concentrates shall pass through a sieve with a mesh of 0.074 mm;

lepidolite concentrates shall pass through a sieve with a mesh of 0.105 mm.

5.2 Bake the test piece at 105 °C ~ 110 °C for 2 h in advance, then, place it in a

desiccator to cool down to room temperature.

6 Analytical Procedures

6.1 Sample

Weigh-take 0.10 g of the sample, accurate to 0.0001 g.

6.2 Number of Determinations

Conduct parallel determination of two samples; take the average value.

6.3 Blank Test

Conduct a blank test on the accompanying sample.

6.4 Determination

6.4.1 Place the sample (6.1) in a 50 mL platinum dish; use a small amount of water to

moisten it. Add 2 mL of perchloric acid (3.1), 2 mL of hydrochloric acid (3.3) and 10 mL

of hydrofluoric acid (3.2). Place it on a sand bath; heat it up to decompose it. Steam it,

until it emits thick white smoke of perchloric acid. Then, remove it and cool it down.

6.4.2 Use water to rinse the wall of the dish. Place it on a sand bath; continue to heat

it up, until the white smoke of perchloric acid is exhausted, then, remove it and cool it

down.

6.4.3 Add 2.0 mL of hydrochloric acid (3.3) and about 20 mL of water; place it on a

sand bath; heat it up to completely dissolve the salts. Then, remove it and cool it down

to room temperature.

6.4.4 Transfer the solution into a 100 mL volumetric flask. Add 5.0 mL of lanthanum

solution (3.4) and 5.0 mL of strontium solution (3.5); use water to dilute to the scale;

mix it well.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.

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