GB/T 23367.2-2009Methods 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 (English PDF)
钴酸锂化学分析方法 第2部分:锂、镍、锰、镁、铝、铁、钠、钙和铜量的测定 电感耦合等离子体原子发射光谱法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
March 19, 2009
Implementation date
January 1, 2010
Scope
GB/T 23367.2-2009 is the English-translated version of 钴酸锂化学分析方法 第2部分:锂、镍、锰、镁、铝、铁、钠、钙和铜量的测定 电感耦合等离子体原子发射光谱法.
GB/T 23367.2-2009 is the Chinese standard "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".
Its scope clause reads: 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. Its clauses include method summary; reagents; instruments; specimen; analytical procedures; calculation of analysis results; tolerance; quality assurance and control.
It was issued by the General Administration of Quality Supervision, Inspection and Quarantine on MARCH 19, 2009 and took effect on JANUARY 01, 2010.
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Document preview — GB/T 23367.2-2009
National Standard of the People's Republic of China
- ICS
- 77.120.99
- Classification
- H 71
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope4
- 2 Method summary4
- 3 Reagents5
- 4 Instruments6
- 5 Specimen7
- 6 Analytical procedures7
- 7 Calculation of analysis results8
- 8 Tolerance8
- 9 Quality assurance and control9
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
Mohm·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, w M ; the value is expressed in %, which is calculated according to formula (1):
Where:
rhoM - The mass concentration of the tested element in the test solution, in micrograms per milliliter (µg/mL);
rho 0 - 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);
V 1 - The volume of the divided test solution, in milliliters (mL);
V 2 - 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.
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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