GB/T 11064.1-2024Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 1: Determination of lithium carbonate content - Titration (English PDF)
碳酸锂、单水氢氧化锂、氯化锂化学分析方法 第 1 部分:碳酸锂含量的测定 滴定法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
September 29, 2024
Implementation date
April 1, 2025
Scope
GB/T 11064.1-2024 is the English-translated version of 碳酸锂、单水氢氧化锂、氯化锂化学分析方法 第 1 部分:碳酸锂含量的测定 滴定法.
This document describes the determination methods of lithium carbonate content in lithium carbonate products, including the acid-alkali titrimetric method (method 1) and the potentiometric method (method 2). It applies to the determination of lithium carbonate content in lithium carbonate products with a determination range (mass fraction) greater than 95.00 %. If other forms of carbonate exist, they are converted into lithium carbonate for deduction.
Document preview — GB/T 11064.1-2024
National Standard of the People's Republic of China
- ICS
- 77.120.99
- Replacing
- GB/T 11064.1-2013
Issued by: State Administration for Market Regulation; Standardization Administration of the People’s Republic of China.
Contents
- Foreword3
- Introduction6
- 1 Scope8
- 2 Normative references8
- 3 Terms and definitions8
- 4 Method 1: acid-alkali titrimetric method9
- 5 Method 2: potentiometric method12
- 6 Test report15
- Annex A (informative) Statistical results of raw data of precision test
Foreword
This document was drafted in accordance with the provisions of GB/T 1.1-2020 “Directives for standardization - Part 1: Rules for the structure and drafting of standardizing documents”.
This document is Part 1 of GB/T 11064 “Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride”. GB/T 11064 has published the following parts:
- Part 1: Determination of lithium carbonate content - Titration;
- Part 2: Determination of lithium hydroxide content - Acid-alkali titrimetric method;
- Part 3: Determination of lithium chloride content - Potentiometric method;
- Part 9: Determination of sulfate content - Barium sulfate turbidity method;
- Part 10: Determination of chloride content - Silver chloride nephelometry method;
- Part 11: Determination of acid-insolubles content - Gravimetric method;
- Part 12: Determination of carbonate content - Acid-alkali titrimetric method;
- Part 15: Determination of fluoride content - Ion selective method;
manganese, cadmium, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry.
This document replaces GB/T 11064.1-2013 “Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 1: Determination of lithium carbonate content - Acid-alkali titrimetric method”. Compared with GB/T 11064.1-2013, in addition to structural adjustments and editorial changes, the main technical changes are as follows:
a) MODIFY the concentration of hydrochloric acid standard titration solution (see b) MODIFY the relevant content of “weighing mass” (see 4.5 of this document, 5.1 c) ADD the relevant content of “blank test” (see 4.5.3 of this document);
d) MODIFY the relevant content of “test data processing” (see 4.6 of this document,
Clause 6 of the 2013 edition);
e) DELETE the relevant content of “allowable difference” (see 7.2 of the 2013 edition);
f) ADD the reproducibility clause (see 4.7.2 of this document);
g) ADD the potentiometric method (see Clause 5 of this document).
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing authority of this document shall not be held responsible for identifying any or all such patent rights.
This document was proposed by China Nonferrous Metals Industry Association.
This document shall be under the jurisdiction of National Technical Committee on Nonferrous Metals of Standardization Administration of China (SAC/TC 243).
and Certification Co., Ltd., Yichun Lithium Battery Industry Research Institute (Jiangxi Lithium Battery Product Quality Supervision and Inspection Center), Jiangxi Jiuling Lithium Industry Co., Ltd., Urumqi Ya’ou Rare Metals Co., Ltd., Ningdu Ganfeng Lithium Co., Ltd., China Nonferrous Metals (Guilin) Geology and Minning Co., Ltd.
Main drafters of this document: Li Qiang, Zhao Wentao, Zhou Jiahong, Wu Jinfang, Xiong Xiaoyan, Liu Binhua, Huang Yanjun, Kang Rujin, Zhang Jun, Zhao Jiang, Liu Shanshan, Chen Yujun, Wang Yongsheng, Xie Tangfeng, Yang Lei, Wen Guangxue, Xu Jianqing, Cai Rongfu, Wu Xuefeng, Peng Wenxiu, Zhang Yuxin, Dai Zehua, Wu Ling, Deng Hongyun, Yang Huilin, Yao Li, Weina, Dai Xiaoyong, Xie Hui, Xu Hua.
This document was first issued in 1989 and revised for the first time in 2013. This is the second revision.
Introduction
Lithium carbonate, lithium hydroxide monohydrate and lithium chloride are widely used in 3C products, electric vehicles, electric bicycles, electric tools, base station energy storage power supplies and other industries. They are also the basic raw materials for products such as nuclear industry and special glass.
GB/T 11064 aims to establish standards for methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride, and consists of 16 parts.
- Part 1: Determination of lithium carbonate content - Titration; the purpose is to establish the determination method of lithium carbonate content.
- Part 2: Determination of lithium hydroxide content - Acid-alkali titrimetric method;
the purpose is to establish the determination method of lithium hydroxide content.
purpose is to establish the determination method of lithium chloride content.
spectrometric method; the purpose is to establish the determination method of potassium and sodium content.
method; the purpose is to establish the determination method of calcium content.
spectrometric method; the purpose is to establish the determination method of magnesium content.
method; the purpose is to establish the determination method of iron content.
method; the purpose is to establish the determination method of silicon content.
purpose is to establish the determination method of sulfate content.
- Part 10: Determination of chloride content - Silver chloride nephelometry method;
the purpose is to establish the determination method of chlorine content.
purpose is to establish the determination method of acid-insolubles content.
purpose is to establish the determination method of lithium carbonate content.
bromide spectrophotometric method; the purpose is to establish the determination method of aluminum content.
method; the purpose is to establish the determination method of arsenic content.
- Part 15: Determination of fluoride content - Ion selective method; the purpose is to establish the determination method of fluorine content.
manganese, cadmium, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry; the purpose is to establish the determination method of multi-element content.
The acid-alkali titrimetric method for determining lithium carbonate content is simple to operate. This revision adds a method for determining lithium carbonate content by potentiometric method, which reflects the latest level of industry development and provides scientific and feasible analysis and test methods for various production and R&D companies, user companies and testing institutions in the upstream and downstream industrial chains.
1 Scope
This document describes the determination methods of lithium carbonate content in lithium carbonate products, including acid-alkali titrimetric method (method 1) and potentiometric method (method 2).
This document applies to the determination of lithium carbonate content in lithium carbonate products, and the determination range (mass fraction): greater than 95.00 %. If other forms of carbonate exist, they will be converted into lithium carbonate for deduction.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values GB/T 12805 Laboratory glassware - Burettes GB/T 17433 Foundation terms for chemical analysis of metallurgical products
3 Terms and definitions
4 Method 1: acid-alkali titrimetric method
4.1 Principle
The test material is dissolved in a certain amount of water, and methyl red-bromocresol green is used as an indicator. The solution is titrated with a standard hydrochloric acid titration solution until the solution changes from green to wine red. The lithium carbonate content is calculated based on the volume of the standard hydrochloric acid titration solution consumed.
4.2 Reagents or materials
Unless otherwise specified, only analytical reagents are used.
4.2.1 Water, GB/T 6682, grade 2, boiled and sealed and cooled to room temperature.
4.2.2 Methyl red-bromocresol green indicator: weigh 0.1 g of bromocresol green, dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution I); weigh 0.2 g of methyl red, dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution II). Take 30 mL of solution I and 10 mL of solution II and mix them well.
4.2.3 Hydrochloric acid standard titration solution (about 0.50 mol/L): pipette 45 mL of hydrochloric acid (ρ = 1.19 g/mL) into a 1000 mL volumetric flask, dilute to the mark with water, and mix well. Calibrate according to the following contents.
a) Weigh three portions of 0.65 g (to the nearest 0.0001 g) of anhydrous sodium carbonate (reference reagent) that has been dried to constant weight at 270 ℃ ~ 300 ℃, place them in 250 mL conical flasks, add 50 mL of water to dissolve, add 10 drops of methyl red-bromocresol green indicator (4.2.2), titrate with hydrochloric acid standard titration solution (4.2.3) until the solution changes from green to wine red, boil for 2 min, and continue titrating until the solution turns wine red again and does not fade for 30 s, which means the end point has been reached. The extreme value of the volume of hydrochloric acid standard titration solution consumed by parallel calibration shall not exceed 0.05 mL, and the average value is taken. The calculation result is retained to four significant figures. A blank test is performed together with the calibration.
4.5 Test procedure
4.5.1 Test material
4.7 Precision
5 Method 2: potentiometric method
5.1 Principle
The test material is dissolved in a certain amount of water and titrated using a potentiometric titrator, with a pH glass composite electrode as the working electrode and a hydrochloric acid standard titration solution as the titrant. The reaction endpoint is determined by the jump point of the indicator electrode potential, and the lithium carbonate content is calculated based on the volume of hydrochloric acid standard titration solution consumed.
5.2 Reagents or materials
Unless otherwise specified, only analytical reagents shall be used. 5.2.1 Water, GB/T 6682, grade 2, boiled and sealed and cooled to room temperature. 5.2.2 Methyl red-bromocresol green indicator: weigh 0.1 g of bromocresol green, dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution I); weigh 0.2 g of methyl red, dissolve in ethanol (95 %), and dilute to 100 mL with ethanol (95 %) (solution II). Take 30 mL of solution I and 10 mL of solution II and mix well. 5.2.3 Hydrochloric acid standard titration solution (about 0.50 mol/L): transfer 45 mL of hydrochloric acid (ρ = 1.19 g/mL) to a 1000 mL volumetric flask, dilute to the mark with water, and mix well. Calibrate according to the following content. […]
5.3 Instrument
5.4 Sample
The sample is pre-dried at 250 ℃ ~ 260 ℃ for 2 h, placed in a desiccator, and cooled to room temperature.
5.5 Test procedure
5.5.2 Parallel test
Perform two tests in parallel and take the average value.
5.5.3 Blank test
Perform a blank test with the test sample.
5.5.4 Determination
Place the test material (5.5.1) in a 150 mL beaker, add 50 mL of water, immerse the pH electrode and the titration head of the burette completely in the solution, start stirring; in the dynamic titration mode, pre-add 20 mL of hydrochloric acid standard titration solution (5.2.3); after stirring for 30 s, titrate with hydrochloric acid standard titration solution (5.2.3) to the obvious jump point, i.e. the end point, and record the volume of hydrochloric acid standard titration solution (5.2.3) consumed.
5.7 Precision
Remaining clauses in the full document
- 6 Test report
- Annex A Statistical results of raw data of precision test
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 16 pages — is available in the English PDF.
Referenced standards
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Related Standards
GB/T 17433-2014 — Foundation terms for chemical analysis of metallurgical products
GB/T 6682-2008 — Water for analytical laboratory use - Specification and test methods
GB/T 8170-2008 — Rules of rounding off for numerical values & expression and judgement of limiting values
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