GB/T 17413.1-2010 English PDF (GBT17413.1-2010)

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GB/T 17413.1-2010: Methods for chemical analysis of lithium, rubidium and cesium ores -- Part 1: Determination of lithium content
GB/T 17413.1-2010
GB
NATIONAL STANDARD OF THE
PEOPLE'S REPUBLIC OF CHINA
ICS 73.060
D 43
Replacing GB 17413.1-1998
Methods for chemical analysis of lithium, rubidium and
cesium ores - Part 1: Determination of lithium content
ISSUED ON: NOVEMBER 10, 2010
IMPLEMENTED ON: FEBRUARY 1, 2011
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Principle ... 5
4 Reagents ... 6
5 Apparatus ... 6
6 Sample ... 6
7 Analysis steps ... 7
8 Result calculation ... 8
9 Precision ... 9
Appendix A (Informative) Atomic absorption spectrophotometer reference working
conditions ... 10
Methods for chemical analysis of lithium, rubidium and
cesium ores - Part 1: Determination of lithium content
WARNING -- The personnel using this part shall have practical experience in
formal laboratory work. This part does not indicate all possible safety issues. Users
are responsible for taking appropriate safety and health measures and ensuring
compliance with the conditions stipulated by relevant national laws and
regulations.
1 Scope
This part of GB/T17413 specifies the methods for determining the amount of lithium
oxide in lithium ores, rubidium ores, and cesium ores.
This part applies to lithium ores, rubidium ores, and cesium ores, and also applies to
the determination of lithium oxide content in tantalum, niobium ores, and rare earth
ores.
Measuring range: 10 μg/g~4×104 μg/g lithium oxide.
2 Normative references
The provisions in the following documents become the provisions of this part through
reference in this part of GB/T 17413. For the dated references, the subsequent
amendments (excluding corrections) or revisions do not apply to this standard, however,
parties who reach an agreement based on this standard are encouraged to study if the
latest versions of these documents are applicable. For undated references, the latest
editions of the referenced documents apply to this standard.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Principle
The sample is decomposed by hydrofluoric acid and sulfuric acid, in 1% sulfuric acid
medium, on an atomic absorption spectrophotometer at a wavelength of 670.8 nm, with
an air-acetylene flame, measured for the absorbance or emission intensity of lithium
oxide, and then the amount of lithium oxide is calculated.
4 Reagents
Unless otherwise stated, analytical grade reagents and analytical laboratory water
complying with GB/T 6682 are used in the analysis.
4.1 Hydrofluoric acid (ρ1.13 g/mL). WARNING: Hydrofluoric acid is toxic and
corrosive. Wear gloves when operating to prevent contact with the skin!
4.2 Hydrochloric acid (ρ1.19 g/mL).
4.3 Sulfuric acid (1+1). WARNING: Improper operation during dilution may cause
burns!
4.4 Lithium oxide standard solution:
a) Lithium oxide standard stock solution: Weigh 1.2364 g of spectrally pure
lithium carbonate (dry at 105 °C~110 °C for 2 hours and place in a desiccator
to cool to room temperature), place it in a 400 mL beaker, add 200 mL of water,
and cover with a watch glass; slowly add a small amount of hydrochloric acid
(4.2) to completely dissolve it, heat the solution to boil to drive out the carbon
dioxide, remove the solution, and cool it; wash the watch glass with water,
transfer the solution to a 500 mL volumetric flask, dilute it with water to the
mark, and shake well. The mass concentration of lithium oxide in this solution
is 1.0 mg/mL;
b) Lithium oxide standard solution: Pipette 25.00 mL of lithium oxide standard
stock solution [4.4a)], place it in a 500 mL volumetric flask, dilute to the mark
with water, and shake well. The mass concentration of lithium oxide in this
solution is 50.00 μg/mL.
5 Apparatus
5.1 Atomic absorption spectrophotometer (with emission function). A lithium hollow
cathode lamp is attached.
5.2 Analytical balance: Level 3, and the sensitivity is 0.1 mg.
6 Sample
6.1 The particle size of the sample shall be less than 74 μm.
6.2 The sample is dried in an oven at 105 °C for 2 h~4 h, and placed in a desiccator to
cool to room temperature for later use.
7.5 Preparation of calibration solution series
Take 0.00 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, and 10.00 mL lithium
oxide standard solution [4.4b)] into a series of 50 mL volumetric flasks, add 1 mL of
sulfuric acid (4.3), dilute with water to the mark, and shake well. The mass
concentrations of lithium oxide in this series of solutions are 0.00 μg/mL, 1.00 μg/mL,
2.00 μg/mL, 4.00 μg/mL, 6.00 μg/mL, 8.00 μg/mL, and 10.00 μg/mL.
7.6 Determination
WARNING: The air-acetylene flame shall be ignited or extinguished according to
the usage regulations of the atomic absorption spectrophotometer to avoid possible
explosion hazards!
Use a flame atomic absorption spectrophotometer to measure the absorbance or
emission intensity of lithium oxide in the calibration solution series, blank solution and
sample solution (7.4.1 and 7.4.2) at a wavelength of 670.8 nm according to the
instrument working conditions (see Appendix A).
7.7 Drawing of the calibration curve
Taking the amount of lithium oxide as the abscissa and the absorbance or emission
intensity as the ordinate, draw a calibration curve, and obtain the corresponding amount
of lithium oxide from the calibration curve.
8 Result calculation
The amount of lithium oxide is expressed as mass fraction w (Li2O), and the value is
expressed in μg/g (micrograms per gram), calculated according to formula (1):
where:
m1 -- the amount of lithium oxide in the sample solution obtained from the
calibration curve, in micrograms (μg);
m0 -- the amount of lithium oxide in the blank test (6.2) obtained from the
calibration curve, in micrograms (μg);
V -- the total volume of the sample solution, in milliliters (mL);
m -- the weighed mass of the specimen, in grams (g);
V1 -- the volume of the sample solution taken, in milliliters (mL).