YS/T 1006.2-2014 English PDF
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YS/T 1006.2-2014: Methods for Chemical Analysis of Lithium Nickel Cobalt Manganese Oxide - Part 2: Determination of Lithium, Nickel, Cobalt, Manganese, Sodium, Magnesium, Aluminum, Potassium, Copper, Calcium, Iron, Zinc and Silicon Content - Inductively Coupled Plasma Atomic Emission Spectrometry
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YS NON-FERROUS METAL INDUSTRY STANDARD ICS 77.120.99 H 14 Methods for Chemical Analysis of Lithium Nickel Cobalt Manganese Oxide - Part 2.Determination of Lithium, Nickel, Cobalt, Manganese, Sodium, Magnesium, Aluminum, Potassium, Copper, Calcium, Iron, Zinc and Silicon Content - Inductively Coupled Plasma Atomic Emission Spectrometry Issued on. OCTOBER 14, 2014 Implemented on. APRIL 1, 2015 Issued by. Ministry of Industry and Information Technology of the People’s Republic of China
Table of Contents
Foreword... 3 1 Scope... 4 2 Method Summary... 5 3 Reagents... 5 4 Instrument... 8 5 Specimen... 9 6 Analytical Procedures... 9 7 Calculation of Analysis Result... 10 8 Precision... 11 9 Test Report... 12Foreword
YS/T 1006-2014 Methods for Chemical Analysis of Lithium Nickel Cobalt Manganese Oxide is divided into 2 parts. ---Part 1.Determination the Total of Nickel Cobalt Manganese Content - EDTA Disodium Salt Titration; ---Part 2.Determination of Lithium, Nickel, Cobalt, Manganese, Sodium, Magnesium, Aluminum, Potassium, Copper, Calcium, Iron, Zinc and Silicon Content - Inductively Coupled Plasma Atomic Emission Spectrometry. This is Part 2 of YS/T 1006. This Part shall be under the jurisdiction of National Technical Committee on Non- ferrous Metals of Standardization Administration of China (SAC/TC 243). The drafting organizations of this Part. CITIC GUOAN MGL Power Science & Technology Co., Ltd.; Guangdong BRUNP Recycling Technology Co., Ltd.; Jining Wujie Science & Technology Co., Ltd.; Shenzhen Tianjiao Technology Development Co., Ltd. The main drafters of this Part. Peng Fuying, Zhu Xiaopei, Han Lijuan, Zhang Xi, Li Changdong, Yu Haijun, Xie Yinghao, Jiang Yongle, Jiang Yongshan, Zhou Yijing, Sun Pingfang. Methods for Chemical Analysis of Lithium Nickel Cobalt Manganese Oxide - Part 2.Determination of Lithium, Nickel, Cobalt, Manganese, Sodium, Magnesium, Aluminum, Potassium, Copper, Calcium, Iron, Zinc and Silicon Content - Inductively Coupled Plasma Atomic Emission Spectrometry1 Scope
This Part of YS/T 1006 specifies the method for the determination of lithium, nickel, cobalt, manganese, sodium, magnesium, aluminum, potassium, copper, calcium, iron, zinc and silicon content in lithium nickel cobalt manganese oxide, which is the cathode material for lithium ion batteries. This Part is applicable to the determination of lithium, nickel, cobalt, manganese, sodium, magnesium, aluminum, potassium, copper, calcium, iron, zinc and silicon content in lithium nickel cobalt manganese oxide, which is the cathode material for lithium ion batteries. The range of determination is shown in Table 1.2 Method Summary
Use hydrochloric acid to dissolve the specimen. In the hydrochloric acid medium, in accordance with the optimized operating conditions of the instrument and the recommended analytical spectrums, adopt the working curve method and an inductively coupled plasma atomic emission spectrometer to determine the lithium, nickel, cobalt, manganese, sodium, magnesium, aluminum, potassium, copper, calcium, iron, zinc and silicon content, in which, the determination of the lithium, nickel, cobalt and manganese content is conducted by adding yttrium standard solution as an internal standard.3 Reagents
Unless it is otherwise specified, only reagents of top-grade purity and Grade-2 (and above) water are used in the analysis. 3.5 Internal standard solution. weigh-take 2.5400 g of yttrium trioxide [w(Y2O3) ≥ 99.99%] in a beaker; add 30 mL of hydrochloric acid (3.3). Heat it up to dissolve it, then, remove it and cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 2 mg of yttrium. 3.8 Cobalt standard stock solution. weigh-take 1.0000 g of pure cobalt [w(Co) ≥ 99.99%] in a beaker; add 50 mL of hydrochloric acid (3.3). Heat it up to dissolve it, then, remove it and cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 500 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 2.0 mg of cobalt. 3.9 Manganese standard stock solution. weigh-take 1.0000 g of pure manganese [w(Mn) ≥ 99.99%] in a beaker; add 50 mL of hydrochloric acid (3.3). Heat it up to dissolve it, then, remove it and cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 500 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 2.0 mg of manganese. 3.10 Sodium standard stock solution. weigh-take 2.5420 g of dried reference sodium chloride [w(NaCl) ≥ 99.99%] in a beaker; slowly add 100 mL of water and cover the watch glass. Conduct low-temperature dissolution, then, cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 1.0 mg of sodium. 3.11 Magnesium standard stock solution. weigh-take 1.6580 g of dried magnesium oxide [w(MgO) ≥ 99.99%] in a beaker; slowly add 50 mL of hydrochloric acid (3.3) and cover the watch glass. Conduct low-temperature dissolution, then, cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 1.0 mg of magnesium. 3.13 Potassium standard stock solution. weigh-take 1.9068 g of dried reference potassium chloride [w(KCl) ≥ 99.99%] in a beaker; slowly add 100 mL of water and cover the watch glass. Conduct low-temperature dissolution, then, cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 1.0 mg of potassium. 3.16 Iron standard stock solution. weigh-take 1.0000 g of pure iron [w(Fe) ≥ 99.99%] in a beaker; slowly add 50 mL of hydrochloric acid (3.3) and cover the watch glass. Conduct low-temperature dissolution, then, remove it and cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 1.0 mg of iron. 3.17 Zinc standard stock solution. weigh-take 1.0000 g of pure zinc [w(Zn) ≥ 99.99%] in a 400 mL beaker; slowly add 50 mL of nitric acid (3.4) and cover the watch glass. Conduct low-temperature dissolution to drive off nitrogen oxides, then, remove it and cool it down. Use water to wash the watch glass and the wall of the beaker; transfer it into a 1,000 mL volumetric flask. Use water to dilute it to the scale, then, mix it up. 1 mL of this solution contains 1.0 mg of zinc. 3.18 Silicon standard stock solution. weigh-take 2.1395 g of pure silicon oxide [w(SiO2) ≥ 99.99%] in a platinum crucible; add 15 g of anhydrous sodium carbonate; mix it up and cover it. Then, transfer it into a 400 °C muffle furnace; raise the temperature to 900 °C and melt it for 1 h; take it out and cool it down. Use water to wash the inner wall of the crucible; place it in a PTFE plastic beaker. Add 100 mL of hot water; conduct low-temperature dissolution, then, cool it down. Transfer it into a 1,000 mL volumetric flask. Use water to dilute to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 1.0 mg of silicon. 3.19 Mixed standard solution A. respectively transfer-take 10.00 mL of sodium standard stock solution (3.10), magnesium standard stock solution (3.11), aluminum standard stock solution (3.12), potassium standard stock solution (3.13), copper standard stock solution (3.14), calcium standard stock solution (3.15), iron standard stock solution (3.16) and zinc standard stock solution (3.17); place it in a 100 mL volumetric flask. Use hydrochloric acid (5 + 95) to dilute it to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 100 μg of sodium, magnesium, aluminum, potassium, copper, calcium, iron and zinc. 3.20 Mixed standard solution B. transfer-take 10.00 mL of mixed standard solution A (3.19); place it in a 100 mL volumetric flask. Use hydrochloric acid (5 + 95) to dilute it to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 1 mL of this solution contains 10 μg of sodium, magnesium, aluminum, potassium, copper, calcium, iron and zinc.4 Instrument
4.1 Inductively Coupled Plasma Atomic Emission Spectrometer 4.2 Analytical Spectrums Table 2 lists out the recommended analytical spectrums. 4.4 Linearity of Working Curve In terms of the linearity of the working curve, the correlation coefficient shall be greater than 0.999.5 Specimen
5.1 The specimen shall pass through a 50 μm sieve. 5.2 Before analysis, the specimen shall be dried at 110 °C ± 5°C for 2 h and placed in a desiccator to cool down to room temperature.6 Analytical Procedures
6.1 Specimen Weigh-take 0.20 g of specimen, accurate to 0.0001 g. 6.2 Number of Determinations Independently conduct two determinations; take the average value. 6.3 Blank Test Conduct a blank test on the accompanying specimen. 6.4 Determination 6.4.1 Processing of specimen 6.4.2 Preparation of a series of standard solutions 6.4.2.1 Respectively transfer-take 0 mL, 0.60 mL, 2.00 mL, 5.00 mL, 10.00 mL, 20.00 mL, 30.00 mL and 40.00 mL of standard solution (3.20); place it in a 200 mL volumetric flask. Use water to dilute to the scale, then, mix it up; immediately transfer it to a dry plastic bottle. 6.4.3 Measurement After the instrument stably operates, in accordance with the optimized operating conditions of the instrument and the recommended analytical spectrum wavelengths (see Table 2), use the series of standard solutions (6.4.2.1) to determine the light emission intensity of sodium, magnesium, aluminum, potassium, copper, calcium, iron and zinc; use the standard series of solution (6.4.2.2) to determine the light emission intensity of silicon; use the standard series of solution (6.4.2.3) to determine the light emission intensity of lithium, nickel, cobalt and manganese. From low to high, determine the light emission intensity of the measured element in the standard series of solution.7 Calculation of Analysis Result
The content of the measured element shall be counted as mass fraction (wM), expressed in (%) and calculated in accordance with Formula (1).8 Precision
8.1 Repeatability In terms of the measured value of two independent test results obtained under repeatability conditions, the absolute difference between the two test results shall not exceed the repeatability limit (r), and the circumstance of exceeding the repeatability limit (r) shall not exceed 5%. The value of the repeatability limit (r) shall comply with the data in Table 3. 8.2 Allowable Difference The difference of the inter-laboratory analysis results shall be not greater than the values shown in Table 4.9 Test Report
The test report shall include the following contents. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
