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GB/T 11064.16-2023 PDF English

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GB/T 11064.16-2023: 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, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry
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GB/T 11064.16: Evolution and historical versions

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GB/T 11064.16-2023English260 Add to Cart 0-9 seconds. Auto-delivery 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, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry Valid
GB/T 11064.16-2013English90 Add to Cart 0-9 seconds. Auto-delivery 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 atomi Obsolete
GB/T 11064.16-1989English199 Add to Cart 2 days Lithium carbonate--Determination of sodium and potassium contents--Flame atomic emission spectrometric method Obsolete

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GB/T 11064.16-2023: 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, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry



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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.99 CCS H 14 Replacing 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, aluminum, iron and sulfate contents - Inductively coupled plasma atomic emission spectrometry Issued on. AUGUST 06, 2023 Implemented on. MARCH 01, 2024 Issued by. State Administration for Market Regulation; Standardization Administration of the People's Republic of China.

Table of Contents

Foreword... 3 Introduction... 5 1 Scope... 7 2 Normative references... 7 3 Terms and definitions... 8 4 Principle... 8 5 Reagents or materials... 8 6 Instruments and equipment... 10 7 Samples... 10 8 Test steps... 10 9 Test data processing... 12 10 Precision... 12 11 Test report... 15 Annex A (informative) Recommended analytical spectral lines and instrument operating parameters... 16 Annex B (informative) Statistics data derived from laboratory results... 17

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 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 9.Determination of sulfate content - Barium sulfate turbidity method; - Part 10.Determination of chloride content -- Silver chloride nephelometry method; - Part 11.Determination of acid-insoluble content -- Gravimetric method; - Part 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.

1 Scope

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 Terms and definitions

For the purposes of this document, the terms and definitions defined in GB/T 17433 apply.

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 1.0 mg of lead. 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. 5.9 Nickel standard storage solution. Weigh 0.100 g of pure metallic nickel (spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add another 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 1.0 mg of nickel. 5.10 Manganese standard storage solution. Weigh 0.100 g of pure metallic manganese (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. 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 manganese. 5.11 Cadmium standard storage solution. Weigh 0.100 g of pure metal cadmium (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. 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 cadmium. 5.12 Aluminum standard storage solution. Weigh 0.100 g of pure metallic aluminum (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. 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 aluminum. 5.13 Iron standard storage solution. Weigh 0.100 g of pure metal wire (spectrally pure, clean surface oxide before use) into a 200 mL beaker. Add 20.00 mL of nitric acid (5.3). Dissolve in water bath until clear. Cool down. Transfer to a 100 mL volumetric flask. 5.15 Mix standard storage solution. Respectively pipette 5.00 mL of each standard storage solution (5.4~5.14) into a 200 mL volumetric flask. Add 20 mL of nitric acid (5.3). Use water to set the volume constant. Shake well. 1 mL of this solution contains 25 μg of calcium, magnesium, copper, lead, zinc, nickel, manganese, cadmium, aluminum, iron and 75 μg of sulfate. The standard storage solution can also use certified reference materials/standard samples.

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℃~260℃ 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. 8.3 Blank test Weigh 1.331 g of high-purity lithium carbonate (5.2) into a 200 mL beaker. Slowly add 10 mL of nitric acid (5.3). Dissolve until clear. Cool down. Transfer into a 50 mL volumetric flask. Dilute to the scale with water. Shake well. 8.4 Determination 8.5 Drawing of working curve 8.5.1 Weigh 7 portions of 2.661 g of high-purity lithium carbonate (5.2) into a set of 200 mL beakers. Slowly add 20 mL of nitric acid (5.3). Heat over low heat until clear. Cool down. Transfer into seven 100 mL volumetric flasks. 8.5.2 On the inductively coupled plasma atomic emission spectrometer, after the instrument is running stably, at the selected instrument working conditions and the recommended analysis spectral line, zero it with water, and measure a series of standard solutions in order of increasing concentration.

9 Test data processing

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

10 Precision

10.1 Repeatability 10.2 Reproducibility For the measured values of two independent test results obtained under reproducibility conditions, please refer to Annex B for precision test statistics. Within the average range given in Table 6, the absolute difference between the two test results does not exceed the reproducibility limit (R).

11 Test report

The test report shall at least provide the followings. - Test subjects; - Reference to this document; - Analysis results and their expression; - Differences from basic analysis steps; - Details and description of any abnormal phenomena observed during the determination; - Test date. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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