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GB/T 11064.3-2013Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 3: Determination of lithium chloride content - Potentiometric method (English PDF)

碳酸锂、单水氢氧化锂、氯化锂 化学分析方法 第 3 部分:氯化锂量的测定 电位滴定法

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Issued by

SAC; GAQSIQ

Level / Type

National · Recommended

Issue date

September 6, 2013

Implementation date

May 1, 2014

Scope

GB/T 11064.3-2013 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 3 部分:氯化锂量的测定 电位滴定法.

The determination method for lithium chloride content in lithium chloride. This Part applies to the determination of lithium chloride content in lithium chloride. The determination range: more than 95.00%.

Document preview — GB/T 11064.3-2013

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 64
Replacing
GB/T 11064.3-1989

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.

Contents

  • Foreword3
  • 1 Scope5
  • 2 Method summary5
  • 3 Reagents5
  • 4 Instruments7
  • 5 Samples7
  • 6 Analysis steps7
  • 7 Calculation of analysis results8
  • 8 Precision9
  • 9 Test report9
  • Annex A Example of test record format

Foreword

GB/T 11064 “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 method;

- 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 nephelometry method;

- Part 10: Determination of chloride content - Silver chloride nephelometry method;

- Part 11: Determination of Acid-insolubles Content - Gravimetric method;

- Part 15: Determination of fluoride content - Ion selective method;

manganese, cadmium and aluminum content - Inductively coupled plasma atomic emission spectrometry.

This Part is drafted in accordance with the rules given in GB/T 1.1-2009.

This Part replaces GB/T 11064.3-1989 “Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 3: Determination of lithium chloride content - Potentiometric method”.

Compared with GB/T 11064.3-1989, the main changes of this Part are following:

- 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: Sichuan Tianqi Lithium Co., Ltd., Jiangxi Ganfeng Lithium Co., Ltd., Xinjiang Institute of Nonferrous Metals, and Beijing General Research Institute of Mining and Metallurgy.

Main drafters of this Part: Tu Mingjiang, Luo Yuping, Gou Haixia, Yi Qingyun, Zeng Xianqin, Zhang Shaohui, and Jiang Qiutao.

The historical version replaced by this Part is as follows:

1 Scope

This Part of GB/T 11064 specifies the determination method for lithium chloride content in lithium chloride.

This Part applies to the determination of lithium chloride content in lithium chloride. The determination range: more than 95.00%.

2 Method summary

The sample is dissolved in water. In acidic solution, use silver (or silver-silver sulfide) electrode as measuring electrode; use calomel electrode as reference electrode; and use silver nitrate standard solution to titrate chloride. Use secondary derivative to determine the reaction end; use the consumed amount of silver nitrate standard titration solution to calculate the content of lithium chloride.

3 Reagents

Unless otherwise indicated, all reagents used in this Part are analytical reagent, the water used is deionized water.

3.1 Nitrate (1+1), guarantee reagent.

3.2 Bromophenol blue ethanol solution (1g/L).

3.3 Sodium chloride standard solution [c(NaCl) = 0.1000mol/L]: Weigh 5.8443g of sodium chloride (reference reagent) which has been burned in advance at 450°C ~ 500°C for 1.5h, and placed in the dryer to cool to room temperature. Place them in a 250mL beaker; add 50mL of water to dissolve; transfer to a 1000mL volumetric flask; dilute with water to scale; mix well. 3.4 Silver nitrate standard titration solution [c(AgNO3) = 0.1000mol/L]. 3.4.1 Preparation: Weigh 17.0g of silver nitrate; place them in a 250mL beaker; add 50mL of water to dissolve; transfer to a 1000mL brown volumetric flask; dilute with water to scale; mix well. 3.4.2 Calibration: Calibration shall be done with sample determination in parallel. Weigh three-portions 25.00mL of sodium chloride standard solution (3.3); place them in 250mL beakers respectively; add water to 150mL; add a drop of bromophenol blue ethanol solution (3.2); add 1 drop ~ 2 drops of nitrate (3.1) until the solution turns to yellow; place electromagnetic stirring bars; place the beakers on an electromagnetic stirrer; start the electromagnetic stirrer; […]

4 Instruments

4.1 Potentiometer: the accuracy is 2mV.

4.2 Measuring electrode: silver electrode or silver-silver sulfide electrode.

4.3 Reference electrode: double-liquid-junction-type saturated calomel electrode; the outer casing is filled with nitrate titration solution (0.1mol/L) during titration.

5 Samples

Samples shall be baked in advance at 250°C ~ 260°C for 2h, and placed in the dryer to cool to room temperature.

6 Analysis steps

6.1 Samples

Weigh 4g ~ 5g of samples; place them in a weighting flask, which has been weighed to constant weight and baked in advance at 250°C ~ 260°C for 2h; […]

6.2 Number of determination

Independently carry out two measurements; take the mean value.

6.3 Blank test

Conduct blank test along with the sample.

7 Calculation of analysis results

Content of lithium chloride is calculated in mass fraction wLiCl of lithium chloride, expressed in %, according to equation (3).

the sample solution, in milliliters (mL);

the blank solution, in milliliters (mL);

V0 - The total volume of the sample solution, in milliliters (mL);

V7 - The volume of the separately weighed sample solution, in milliliters (mL);

m0 - The mass of the sample, in grams (g);

42.39 - The molar mass based on (LiCl) as the basic unit, in grams per mole (g/mol);

The result shall be expressed to two decimal places.

8 Precision

8.1 Repeatability

For the two independent test results obtained under repeatability conditions, within the average-value range as given below, the absolute difference of these two test results does not exceed the repeatability limit (r), and the situation exceeding repeatability limit (r) is not more than 5%. Repeatability limit (r), according to Table 1, adopts linear interpolation to obtain.

8.2 Allowable difference

The difference of analysis results among laboratories shall not be more than the allowable difference in Table 2.

9 Test report

The test report shall contain the following content:

- Analysis result and its expression;

- Difference with the basic analysis step;

- Anomalies observed in the determination;

Annex A Example of test record format

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.

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