YS/T 509.4-2008 English PDF (YST509.4-2008)

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YS/T 509.4-2008: Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of aluminium oxide content. EDTA compleximetric method
YS/T 509.4-2008
YS
NONFERROUS METALS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing YS/T 509.4-2006
Methods for chemical analysis of spodumene and
lepidolite concentrates - Determination of aluminum
oxide content - EDTA compleximetric 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 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 (ρ1.19g/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