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YS/T 509.4-2008Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of aluminium oxide content. EDTA compleximetric 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 509.4-2008 (Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of aluminium oxide content. EDTA compleximetric method) is available as an English-translated PDF.

YS/T 509.4-2008 — This Part specifies the determination methods for aluminum oxide content in spodumene, lepidolite concentrates. This Part is applicable to the determination of aluminum oxide content in spodumene, lepidolite concentrates. Determination range: 10.00%~30.00%.

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Document preview — YS/T 509.4-2008

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

Contents

  • Foreword...3
  • 1 Scope...5
  • 2 Method summary...5
  • 3 Reagents...5
  • 4 Specimen...7
  • 5 Analysis steps...7
  • 6 Calculation of analysis result...8
  • 7 Precision...9
  • 8 Quality assurance and control...9

Foreword

YS/T 509 "Methods for chemical analysis of spodumene and lepidolite

concentrates" consists of the following 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 met;

- Part 8: Determination of calcium oxide and magnesium oxide content -

Flame atomic absorption spectrometric method;

- Part 9: Determination of fluorine content - lon selective electrode 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 4.

This Part replaces YS/T 509.4-2006 "Methods for chemical analysis of

spodumenite and lepidolite concentrates The EDTA volumetric method for the

determination of aluminum oxide content" (previous edition is GB/T 3885.4-

1983).

Compared with YS/T 509.4-2006, the main changes in this Part are as follows:

- modified the titer (T) of lead standard solution and aluminum oxide to the

concentration of the substance;

Methods for chemical analysis of spodumene and

lepidolite concentrates - Determination of aluminum

oxide content - EDTA compleximetric method

1 Scope

This Part specifies the determination methods for aluminum oxide content in

spodumene, lepidolite concentrates.

This Part is applicable to the determination of aluminum oxide content in

spodumene, lepidolite concentrates. Determination range: 10.00%~30.00%.

2 Method summary

The test material is melted with potassium hydroxide. Use water to leach.

Pipette part of the solution. Add excessive EDTA. Boil complexed aluminum at

pH5~pH6. Excessive EDTA uses xylenol orange as indicator. Use lead standard

solution to back drip. Add fluoride. Use lead standard solution to titrate the

released EDTA. Calculate the amount of aluminum oxide from the volume of

lead standard solution consumed.

3 Reagents

Unless otherwise stated, only the confirmed analytically-pure reagents and

distilled water or water of comparable purity are used in the analysis.

3.1 Potassium hydroxide.

3.2 Ammonium fluoride.

3.3 Absolute ethanol.

3.4 Hydrochloric acid (rho1.19g/mL).

3.5 Ammonium hydroxide (1+1).

3.6 Ammonium hydroxide (1+19).

3.7 Buffer solution (pH5.5): Dissolve 120.5g of anhydrous sodium acetate in

water. Add 10mL of glacial acetic acid. Transfer to a 1000mL volumetric flask.

V1 - Volume of lead standard solution (3.10) consumed to titrate aluminum oxide,

in milliliters (mL);

V0 - Volume of lead standard solution (3.10) consumed to titrate blank solution,

in milliliters (mL);

0.05098 - Amount of aluminum oxide equivalent to 1.00mL of lead standard

solution [c(Pb)=1.0000mol/L], in grams per mole (g/mol).

Conduct parallel calibration in triplicate. The extreme deviation value of the

consumed lead standard solution (3.10) shall not exceed 0.05mL. Take the

average value. Otherwise, recalibrate.

3.11 Bromophenol blue solution (1g/L).

3.12 Xylenol orange ethanol (1+1) solution (5g/L): Prepare when used.

4 Specimen

4.1 Spodumene concentrate shall pass through a sieve with an aperture of

0.074mm. Lepidolite concentrate shall pass through a sieve with an aperture of

0.105mm.

4.2 The specimen is pre-baked at 105°C~110°C for 2h. Place in a desiccator to

cool to room temperature.

5 Analysis steps

5.1 Test material

Weigh 0.25g of specimen, to the nearest of 0.0001g.

5.2 Number of determinations

Make parallel determinations of two test materials. Take the average value.

5.3 Blank test

Conduct blank test with test material.

5.4 Determination

5.4.1 Place the test material (5.1) in a 30mL silver crucible. Add 5 drops of

absolute ethanol (3.3) to moisten. Add 4g of potassium hydroxide (3.1). Put the

lid on the crucible and leave a little gap. Remove moisture on an electric stove.

Place in 600°C~650°C high temperature furnace to melt for 10min~15min. Take

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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.

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