GB/T 11064.16-2023Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - Part 16: Determination of calcium, magnesium, copper, lead, zinc, nickel, manenases, cadmium, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry (English PDF)

Foreword

This document was drafted in accordance with the rules given in GB/T 1.1-2020 "Directives for standardization - Part

1.Rules for the structure and drafting of standardizing documents". This document is Part 16 of GB/T 11064 "Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride". The following parts of GB/T 11064 have been issued. - Part

1.Determination of lithium carbonate content -- Acid-alkali titrimetric method; - Part

2.Determination of lithium hydroxide content -- Acid-alkali titrimetric method; - Part

1 Scope

GB/T 11064.16-2023 is the Chinese national standard on methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride - part 16: determination of calcium, magnesium, copper, lead, zinc, nickel, manenases, cadmium, aluminum, iron and sulfate contents - inductively coupled plasma atomic emission spectrometry, in the field of metallurgy. The /T suffix marks it as a recommended standard: it is not compulsory by itself, but it becomes binding as soon as a contract, a tender or a customer specification calls it up - which in practice is how most foreign buyers meet it. It was issued on 6 August 2023 by the State Administration for Market Regulation; Standardization Administration of China, and has been in force since 1 March 2024. Classification: ICS 77.120.99, CCS H14. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

This document describes methods for the determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, aluminum, iron, and sulfate content in lithium carbonate, lithium hydroxide monohydrate, and lithium chloride. This document is applicable to the determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, aluminum, iron, and sulfate content in lithium carbonate, lithium hydroxide monohydrate, and lithium chloride. The measurement range of each element is shown in Table 1. Table 1 -- Determination range of each element

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 Element Element Determination range/% Determination range/%

GB/T 8170, Rules of rounding off for numerical values and expression and judgement of limiting values

GB/T 17433, Foundation terms for chemical analysis of metallurgical products

3 Determination of lithium chloride content -- Potentiometric method; - Part

4.Determination of potassium and sodium content -- Flame atomic absorption spectrometric method; - Part

5.Determination of calcium content -- Flame atomic absorption spectrometric method; - Part

6.Determination of magnesium content -- Flame atomic absorption spectrometric method; - Part

7.Determination of iron content - 1, 10-Phenanthroline spectrophotometric method; - Part

8.Determination of silicon content -- Molybdenum blue spectrophotometric method; - Part

4 Principle

Lithium carbonate and lithium hydroxide monohydrate are decomposed with nitric acid. Lithium chloride is dissolved in water. In nitric acid medium, the matrix matching standard curve method is used to determine the contents of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, aluminum,

5 Reagents or materials

Unless otherwise stated, only reagents confirmed to be of guaranteed reagents are used in the analysis.

5.1 Water, GB/T 6682, grade 2.

5.2 High purity lithium carbonate (mass fraction is greater than 99.99%, Fe, Cu, Pb, Zn, Ni, Ca, Mg, Mn, Cd, Al, are all less than 0.0001%).

5.3 Nitric acid (1+1).

5.4 Calcium standard storage solution. Weigh 0.2497 g of spectrally pure calcium carbonate into a 200 mL beaker. Then add

20.00 mL of nitric acid (5.3) and dissolve at low temperature until clear. Cool down. Transfer to a 100 mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of this solution contains

1.0 mg of calcium.

5.7 Lead standard storage solution. Weigh 0.1077 g of spectrally pure lead dioxide into a 200 mL beaker. Add

20.00 mL of nitric acid (5.3). Dissolve at low temperature until clear. Cool down. Transfer to a 100 mL volumetric flask. Use water to set the volume constant. Shake well. 1 mL of this solution contains

5.8 Zinc standard storage solution. Weigh 0.1000 g of pure metallic zinc (spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add

20.00 mL of nitric acid (5.3). Dissolve at low temperature until clear.

6 Instruments and equipment

Inductively coupled plasma atomic emission spectrometer, stability and analysis lines of each element are as follows:

7 Samples

7.1 Lithium carbonate and lithium chloride samples shall be baked at 250°C~260°C for 2 h before analysis. Cool to room temperature in a desiccator.

7.2 Lithium hydroxide monohydrate samples shall be packed in plastic containers. Store airtight.

8 Test steps

8.1 Test material Weigh the sample according to Table 2, accurate to 0.0001 g.

8.2 Parallel test Do two tests in parallel. Take the average value.

9 Test data processing

The element content is calculated as the mass fraction wx of each element, calculated according to formula (1).

12 Determination of carbonate content -- Acid-alkali titrimetric method; - Part

13.Determination of aluminum content -- Chrome azurol S-cetylpyridinium bromide spectrophotometric method; - Part

14.Determination of arsenic content -- Molybdenum blue spectrophotometric method; - Part

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

16.Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium and aluminum content -- Inductively coupled plasma atomic emission spectrometry. This document replaces GB/T 11064.16-2013 "Methods for chemical analysis of lithium carbonate, lithium hydroxide monohydrate and lithium chloride -- Part 16. Determination of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium and aluminum content -- Inductively coupled plasma atomic emission spectrometry". Compared with GB/T 11064.16-2013, in addition to the structural adjustments and editorial modifications, the main technical changes in this document are as follows:

a) Add the determination range. Add the determination of iron and sulfate contents (see Chapter 1 of this Edition; Chapter 1 of Edition 2013);

b) Add iron and sulfate standard storage solutions (see 5.13~

5.14 of this Edition);

c) Change the working curve standard solution concentration. Add iron and sulfate standard solutions (see

8.5 of this Edition;

3.16 of Edition 2013);

d) Add the provisions on reproducibility (see

10.2 of this Edition);

e) Delete the allowable difference (see

8.2 of Edition 2013). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing authority 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). The drafting organizations of this document. Tianqi Lithium Industry Co., Ltd., Jiangxi Ganfeng Lithium Industry Co., Ltd., Yichun Silver Lithium New Energy Co., Ltd., Yahua Lithium Industry (Ya'an) Co., Ltd., Xinjiang Nonferrous Metals Research Institute, Guohe General (Qingdao) Test and Evaluation Co., Ltd., Zijin Mining Group Co., Ltd., Zhejiang Huayou Cobalt Co., Ltd., Guangdong Bangpu Recycling Technology Co., Ltd., Jiangxi Jiuling Lithium Co., Ltd. Main drafters of this document. Tu Mingjiang, Yang Yanhui, Liao Shiying, Hu Jun, Cheng Xiaoqin, Huang Yanjun, Yi Liang, Li Changdong, Chen Yanxu, Shang Weiling, Wang Xiangde, Wu Jinrong, Xu Ziyan, Xiong Dayu. This document was first issued in 1989.When it was first revised in 2013, it combined GB/T 11064.17-1989 "Lithium carbonate -- Determination of iron and lead contents-- Coprecipitation-flame atomic absorption spectrometric method" and GB/T 11064.18- 1989 "Lithium carbonate -- Determination of calcium, magnesium, copper, zinc, nickel, manganese and cadmium content -- Ion exchange-flame atomic absorption spectrometric method". This is the second revision.