GB/T 23367.2-2009 English PDF (GBT23367.2-2009)

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GB/T 23367.2-2009: Methods for chemical analysis of lithium cobalt oxide -- Part 2: Determination of lithium, nickel, manganese, magnesium, aluminium, iron, sodium, calcium and copper content -- Inductively coupled plasma atomic emission spectrometry
GB/T 23367.2-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 71
Methods for chemical analysis of lithium cobalt oxide - Part
2: Determination of lithium, nickel, manganese, magnesium,
aluminum, iron, sodium, calcium and copper content -
Inductively coupled plasma atomic emission spectrometry
ISSUED ON: MARCH 19, 2009
IMPLEMENTED ON: JANUARY 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Method summary ... 4 
3 Reagents ... 5 
4 Instruments ... 6 
5 Specimen ... 7 
6 Analytical procedures ... 7 
7 Calculation of analysis results ... 8 
8 Tolerance ... 8 
9 Quality assurance and control ... 9 
Methods for chemical analysis of lithium cobalt oxide - Part
2: Determination of lithium, nickel, manganese, magnesium,
aluminum, iron, sodium, calcium and copper content -
Inductively coupled plasma atomic emission spectrometry
1 Scope
This Part of GB/T 23367 specifies the method for the determination of lithium, nickel,
manganese, magnesium, aluminum, iron, sodium, calcium, copper content, in lithium
cobalt oxide, which is the positive electrode material for lithium ion batteries.
This Part applies to the determination of lithium, nickel, manganese, magnesium,
aluminum, iron, sodium, calcium, copper content in lithium cobalt oxide, which is the
cathode material of lithium ion batteries. The measurement range is as shown in Table
1.
2 Method summary
The sample is dissolved in hydrochloric acid. In the hydrochloric acid medium,
according to the optimized working conditions of the instrument and the recommended
analytical spectrum, the working curve method is used, to determine the content of
lithium, nickel, manganese, magnesium, aluminum, iron, sodium, calcium, copper, by
inductively coupled plasma atomic emission spectrometer. Among them, the lithium is
determined, by using a standard solution matched with a cobalt matrix, which has a
similar composition to the specimen.
3 Reagents
Unless otherwise stated, only reagents, that are confirmed to be superior grade and 18.2
MΩ·cm secondary purified water or water of equivalent purity, are used in the analysis.
3.1 Hydrochloric acid (1 + 1).
3.2 Hydrochloric acid (5 + 95).
3.3 Lithium standard storage solution: 1.00 mg/mL.
3.4 Nickel standard storage solution: 1.00 mg/mL.
3.5 Manganese standard stock solution: 1.00 mg/mL.
3.6 Magnesium standard storage solution: 1.00 mg/mL.
3.7 Aluminum standard storage solution: 1.00 mg/mL.
3.8 Iron standard storage solution: 1.00 mg/mL.
3.9 Sodium standard storage solution: 1.00 mg/mL.
3.10 Calcium standard storage solution: 1.00 mg/mL.
3.11 Copper standard storage solution: 1.00 mg/mL.
3.12 Cobalt matrix solution: Weigh 3.0000 g of metallic cobalt (mass fraction ≥
99.99%), into a 400 mL beaker. Add 50 mL of hydrochloric acid (3.1). Dissolve it at
low temperature. Transfer it into a 1000 mL volumetric flask. Use water to dilute it to
the mark. Mix well. 1 mL of this solution contains 3.0 mg of cobalt.
3.13 Mixed standard solution A: Respectively pipette 10.00 mL of nickel standard
storage solution (3.4), manganese standard storage solution (3.5), magnesium standard
storage solution (3.6), aluminum standard storage solution (3.7), iron standard storage
solution (3.8), sodium standard storage solution (3.9), calcium standard storage solution
(3.10), copper standard storage solution (3.11), in a 100 mL volumetric flask. Use
hydrochloric acid (3.2), to dilute it to the mark. Mix well. 1 mL of this solution contains
100 μg of nickel, manganese, magnesium, aluminum, iron, sodium, calcium, copper.
3.14 Mixed standard solution B: Pipette 10.00 mL of mixed standard solution A (3.13),
put it in a 100 mL volumetric flask. Use hydrochloric acid (3.2), to dilute it to the mark.
Mix well. 1 mL of this solution contains 10 μg of nickel, 10 μg of manganese, 10 μg of
magnesium, 10 μg of aluminum, 10 μg of iron, 10 μg of sodium, 10 μg of calcium, 10
6.4.3 Measurement
6.4.3.1 After the instrument runs stably, according to the optimized working conditions
of the instrument and the recommended analytical spectral line's wavelength (Table 2),
use the standard series solutions (6.4.2.1), to determine the emission light intensity of
nickel, manganese, magnesium, aluminum, iron, sodium, calcium, copper. Use the
standard series solution (6.4.2.2), to measure the emission light intensity of lithium. The
emission light intensity of the analyte element, in the standard series solution, is
measured, from low to high. Take the mass concentration of the measured element as
the abscissa AND the emitted light intensity as the ordinate, to automatically draw the
working curve through computer.
6.4.3.2 Measure the emission light intensity of the tested element, in the sample solution
and the accompanied sample blank solution. The computer automatically calculates the
mass concentration of the tested element, from the working curve.
7 Calculation of analysis results
The content of the element to be tested is calculated by the mass fraction of the element
to be tested, wM; the value is expressed in %, which is calculated according to formula
(1):
Where:
ρM - The mass concentration of the tested element in the test solution, in micrograms
per milliliter (μg/mL);
ρ0 - The mass concentration of the tested element in the blank solution, in
micrograms per milliliter (μg/mL);
V - The total volume of the test solution, in milliliters (mL);
V1 - The volume of the divided test solution, in milliliters (mL);
V2 - The volume of the test solution for determination, in milliliters (mL);
m - The mass of the sample, in grams (g).
8 Tolerance
The difference, between the analysis results between laboratories, shall not be greater
than the allowable difference, which is listed in Table 4 below.