YS/T 509.1-2008 English PDF (YST509.1-2008)

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YS/T 509.1-2008: Methods for chemical analysis of spodumene and lepidolite concentrates. Determination of lithium oxide, sodium oxide, and potassium oxide contents. Flame atomic absorption spectrometric method
YS/T 509.1-2008
YS
NONFERROUS METALS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 64
Replacing YS/T 509.1-2006
Methods for chemical analysis of spodumene and
lepidolite concentrates - Determination of lithium
oxide, sodium oxide and potassium oxide contents -
Flame atomic absorption spectrometric 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 Instruments ... 6 
5 Specimen ... 7 
6 Analysis steps ... 7 
7 Calculation of analysis results ... 9 
8 Precision... 9 
9 Quality assurance and control ... 10 
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 complexometric
method;
- Part 5. Determination of ferric oxide content-0-phenanthroline
photometric method and EDTA complexometric 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 1.
This Part replaces YS/T 509.1-2006 "Methods for chemical analysis of
spodumene and lepidolite concentrates The atomic absorption
spectrophotometric method for determination of lithium oxide sodium oxide and
potassium oxide contents" (previous edition is GB/T 3885.1-1983).
Compared with YS/T 509.1-2006, the main changes in this Part are as follows.
- re-edited the text format;
- added the provisions on quality assurance and control, added repetitive
Methods for chemical analysis of spodumene and
lepidolite concentrates - Determination of lithium
oxide, sodium oxide and potassium oxide contents -
Flame atomic absorption spectrometric method
1 Scope
This Part specifies the determination methods for lithium oxide, sodium oxide
and potassium oxide contents in spodumene, lepidolite concentrates.
This Part is applicable to the determinations of lithium oxide, sodium oxide and
potassium oxide contents in spodumene, lepidolite concentrates.
Determination range. 3.00% ~ 8.00% for lithium oxide; 0.10% ~ 10.00% for
sodium oxide, potassium oxide.
2 Method summary
The test material is decomposed with hydrofluoric acid-sulfuric acid. In a sulfuric
acid medium, determine the lithium oxide, sodium oxide, and potassium oxide
by using an air-acetylene gas lean burn flame at wavelengths of 670.8 nm,
589.0 nm, and 766.5 nm, respectively, in an atomic absorption spectrometer.
3 Reagents
Unless otherwise stated, only the reagents identified as analytically pure and
distilled water or water of comparable purity are used in the analysis.
3.1 Hydrofluoric acid (ρ1.15 g/mL).
3.2 Sulfuric acid (1+1).
3.3 Lithium standard stock solution. weigh 2.4729 g of lithium carbonate (99.9%
or more) that has been previously dried at 105°C ~ 110°C for 2h and left to cool
in a desiccator to room temperature. Place in a 250mL beaker. Add 80mL of
water. Cover a wide-mouth bottle. Slowly add 10mL of sulfuric acid from the
mouth (3.2). Heat to dissolve all lithium carbonate. Boil off carbon dioxide and
cool to room temperature. Blow and wash the wide-mouth bottle with water.
Transfer solution to a 1000mL volumetric flask. Dilute with water to the scale,
concentration standard solution of which its standard deviation does not
exceed 1.5% of the average absorbance. Measure the absorbance 10
times with the minimum concentration standard solution (not "zero"
concentration standard solution) of which its standard deviation does not
exceed 0.5% of the average absorbance.
- Linearity of the working curve. divide the working curve into five segments
according to concentration, the ratio of the difference between the
absorbance of the highest segment and the absorbance of the lowest
segment is not greater than 0.7.
5 Specimen
5.1 Spodumene concentrate shall pass through 0.074mm mesh screen.
Lithium mica concentrate Shall pass 0.105mm sieve.
5.2 The specimen is pre-baked at 105°C-110°C for 2h and placed in a
desiccator to cool to room temperature.
6 Analysis steps
6.1 Test material
Weigh 0.10 g of specimen, to the nearest of 0.001 g.
6.2 Measurement quantity
Perform the parallel determination of two test materials. Take the average value.
6.3 Blank test
Perform the blank test accompanying with test material.
6.4 Determination
6.4.1 Place the test material (6.1) in a 50 mL platinum dish. Wet it with water.
Add 3mL of sulfuric acid (3.2), 15mL of hydrofluoric acid (3.1). Put it on a sand
bath and decompose it by heating. Steam to white sulfur trioxide, remove, cool
down.
6.4.2 Add 25mL of water and put it on a sand bath to completely dissolve the
salts. Remove, cool to room temperature.
6.4.3 Transfer the solution to a 100 mL volumetric flask, dilute to the scale
with water, and mix well.
6.4.4 Pipette the solution (6.4.3) according to Table 1, add sulfuric acid (3.2)