GB/T Translated English of Chinese Standard: GB/T

Transcription

1 Translated English of Chinese Standard: GB/T GB NATIONAL STANDARD OF THE PEOPLE S REPUBLIC OF CHINA ICS H 64 GB/T Replacing GB/T Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 5: Determination of calcium content - Flame atomic absorption spectrometric method 碳酸锂 单水氢氧化锂 氯化锂化学分析法第 5 部分 : 钙量的测定火焰原子吸收光谱法 Issued on: November 27, 2013 Implemented on: August 01, 2014 Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People s Republic of China; Standardization Administration of the People s Republic of China. Page 1 of 9

2 Table of Contents Foreword Scope Method summary Reagents Apparatus Samples Analysis steps Calculation of analysis results Precision Test report Page 2 of 9

3 Foreword GB/T Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride is divided into 16 parts: - Part 1: Determination of lithium carbonate content - Acid-alkali titrimetric - Part 2: Determination of lithium hydroxide content - Acid-alkali titrimetric - Part 3: Determination of lithium chloride content - Potentiometric - Part 4: Determination of potassium and sodium content - Flame atomic absorption spectrometric - Part 5: Determination of calcium content - Flame atomic absorption spectrometric - Part 6: Determination of magnesium content - Flame atomic absorption spectrometric - Part 7: Determination of iron content - 1,10-phenanthroline spectrophotometric - Part 8: Determination of silicon content - Molybdenum blue spectrophotometric - Part 9: Determination of sulfate content - Barium sulfate nephelometry - Part 10: Determination of chloride content - Silver chloride nephelometry - Part 11: Determination of Acid-insolubles Content - Gravimetric - Part 12: Determination of carbonate content - Determination of lithium chloride content - Potentiometric - Part 13: Determination of aluminum content - Chromazurol S-cetylpyridine bromide spectrophotometric - Part 14: Determination of arsenic content - Molybdenum blue spectrophotometric - Part 15: Determination of fluoride content - Ion selective - Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium and aluminum content - Inductively coupled plasma atomic emission spectrometry. This Part is part 5 of GB/T Page 3 of 9

4 This Part is drafted in accordance with rules given in GB/T The Part replaces GB/T "Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 5: Determination of calcium content - Flame atomic absorption spectrometric method". Compared with GB/T , the main changes of this Part are as follows: - REVISE the determination range %~0.350% to be %~0.35% ; - REVISE add 5mL of citric acid solution to be add 1mL of citric acid solution ; - ADD the repeatability terms; - RE-EDIT the text format; ADD the test report. This Part shall be under the jurisdiction of National Standardization Technical Committee of Nonferrous Metals (SAC/TC 243). Drafting organizations of this Part: Xinjiang Wuxin Lithium Salt Development Co., Ltd., Ganzhou Nonferrous Metallurgy Research Institute, and Haimen Ronghui General Lithium Industry Co., Ltd. The main drafters of this Part: Guan Yuzhen, Zhao Fanglan, Lai Jian, Liu Hong, Deng Hongyun, Chen Xian an, and Liu Yan. The historical version replaced by this Part is as follows: - GB/T Page 4 of 9

5 Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 5: Determination of calcium content - Flame atomic absorption spectrometric method 1 Scope This Part of GB/T specifies the determination method of calcium in lithium carbonate, in lithium hydroxide monohydrate, and in lithium chloride. This Part applies to the determination of calcium in lithium carbonate, in lithium hydroxide monohydrate, and in lithium chloride. The determination range: %~0.35%. 2 Method summary The lithium carbonate and lithium hydroxide samples are dissolved in hydrochloric acid; lithium chloride sample is dissolved in water. In the dilute hydrochloric acid medium, at wavelength of 422.7nm on atomic absorption spectrometer, use lanthanum salt and citric acid as release agent, use air - acetylene flame and standard addition method to determine it. 3 Reagents Unless otherwise indicated, all reagents used in this Part are guaranteed reagent, the water used is deionized water. 3.1 Hydrochloric acid (1+1). 3.2 Lanthanum salt solution: weigh 5.864g of lanthanum oxide [ w ( La O ) % ]; 2 place them in a 100mL beaker; add hydrochloric acid to dissolve and make it clear (heat it if necessary); transfer them in 500mL flask; use water to dilute to scale; shake well. 1mL of this solution contains 10mg of lanthanum. 3.3 Citric acid solution (100g/L): weigh 50g of citric acid; place in a 500mL beaker; add 500mL of water to dissolve; use hydrogen-type cation exchange resin to purify. 3.4 Calcium standard stock solution: weigh g of calcium carbonate Page 5 of 9

6 The difference of analysis results among laboratories shall not be more than the allowable difference in Table 3. Mass fraction of calcium/% Table 3 Allowable difference/% ~ >0.0060~ >0.010~ >0.050~ >0.10~ Test report The test report shall contain the following content: - Sample; - The number of this Part national standard; - Analysis result and its expression; - Difference with the basic analysis step; - Anomalies observed in the determination; - Determination date. END Page 9 of 9