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GB/T 41704-2022 PDF English

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GB/T 41704-2022: Test methods of cathode materials for lithium ion battery - Determination of magnetic impurities content and residual alkali content
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GB/T 41704-2022230 Add to Cart Auto, 9 seconds. Test methods of cathode materials for lithium ion battery - Determination of magnetic impurities content and residual alkali content Valid

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GB/T 41704-2022: Test methods of cathode materials for lithium ion battery - Determination of magnetic impurities content and residual alkali content


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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.160 CCS H 16 Test Methods of Cathode Materials for Lithium Ion Battery - Determination of Magnetic Impurities Content and Residual Alkali Content Issued on. OCTOBER 12, 2022 Implemented on. FEBRUARY 1, 2023 Issued by. State Administration for Market Regulation; Standardization Administration of the People’s Republic of China.

Table of Contents

Foreword... 3 Introduction... 4 1 Scope... 5 2 Normative References... 5 3 Terms and Definitions... 5 4 Determination of Magnetic Impurities Content... 6 5 Determination of Residual Alkali Content... 13 6 Test Report... 17

1 Scope

This document specifies the determination method for magnetic impurities content and residual alkali content in the cathode materials for lithium ion battery. This document is applicable to the determination of magnetic impurities content and residual alkali content in the cathode materials for lithium ion battery. The determination range of the magnetic impurities content is  1 g/kg; the determination range of residual alkali content (mass fraction) is 0.001% ~ 2.500%.

2 Normative References

The contents of the following documents constitute indispensable clauses of this document through the normative references in this text. In terms of references with a specified date, only versions with a specified date are applicable to this document. In terms of references without a specified date, the latest version (including all the modifications) is applicable to this document. GB/T 601 Chemical Reagent - Preparations of Standard Volumetric Solutions 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

3 Terms and Definitions

The following terms and definitions are applicable to this document. 3.1 Magnetic Impurities Magnetic impurities refer to impurities in the cathode materials for lithium ion battery that can be adsorbed by the magnetic bar with a magnetic induction intensity of not less than 0.5 T (5,000 Gauss). 3.2 Large Particle Magnetic Impurities Large particle magnetic impurities refer to magnetic impurities with a diameter of not less than 10 m under the scanning electron microscope. 3.3 Residual Alkali Residual alkali refers to alkaline substances attached to the surface of the particles of the cathode materials for lithium ion battery.

4 Determination of Magnetic Impurities Content

4.1 Inductively Coupled Plasma Atomic Emission Spectrometry 4.1.1 Principle In a clean environment free of magnetic impurities, use a magnetic bar to adsorb and enrich the magnetic impurities in the cathode material. 4.1.2 Reagents or materials Unless it is otherwise specified, all reagents used in this Method are of guaranteed purity and Grade-1 water specified in GB/T 6682. 4.1.2.1 Nitric acid ( = 1.42 g/mL). 4.1.2.6 Zinc standard stock solution (100 g/mL), prepared from high-purity metals or compounds, or adopt a certified single-element standard stock solution. 4.1.2.7 Lithium standard stock solution (100 g/mL), prepared from high-purity metals or compounds, or adopt a certified single-element standard stock solution. 4.1.2.11 Lithium standard solution B. transfer-take 20.00 mL of lithium standard solution A (4.1.2.10); place it in a 100 mL volumetric flask. Add 3 mL of nitric acid (4.1.2.1); use water to dilute to the scale; mix it well and immediately transfer it to a dry plastic jar. 1 mL of this solution contains 2 g of lithium. 4.1.3 Instruments and equipment 4.1.3.1 Environmental iron removing rod. magnetic induction intensity  0.5 T (5,000 Gauss), wrapped with plastic wrap. 4.1.3.2 Plastic jar. 500 mL. 4.1.4 Sample The particle of the sample shall be not greater than 0.154 mm. 4.1.5 Test procedures 4.1.5.1 Iron removal before test Before the test, use aqua regia (4.1.2.2) to clean the magnetic bar (4.1.3.3); use the environmental iron removing rod (4.1.3.1) to carry out meticulous iron removal treatment on all instruments and supplies used in the test. 4.1.5.4.1 Put the test portion in a 500 mL plastic jar (4.1.3.2), add 300.0 g of water, tighten the lid (to prevent leakage); place it on the ball mill (4.1.3.5), adjust the rotating speed to 60 r/min ~ 100 r/min; after rolling and mixing for 30 min, remove it. 4.1.5.4.3 Transfer the magnetic bar (4.1.3.3) to a clean 200 mL beaker; add water, until the magnetic bar (4.1.3.3) is immersed; prevent the water from directly rushing to the surface of the magnetic bar (4.1.3.3). 4.1.5.4.4 There are two optional modes for dissolution. 4.1.5.4.5 Remove the beaker or colorimetric tube. After cooling, transfer all the solution to a 50 mL volumetric flask. Use a small amount of water to rinse the magnetic bar (4.1.3.3); repeat for 3 times. Then, transfer all the washing solution to a volumetric flask and use water to reach a constant volume; record the volume as V. 4.1.5.5 Preparation of standard series solutions 4.2.5.2 Weigh-take 200.0 g of the sample, accurate to 0.1 g. Place the sample in a 500 mL plastic jar (4.2.3.3); add water to the shoulder of the jar; tighten the lid, then, use the sealing film to seal it. Manually mix the water and the sample, so that there is no precipitation at the bottom of the jar. Put the jar into the magnetic ring sleeve (4.2.3.2); use the heat sealing film to seal it. Place it on the ball mill (4.2.3.4); after mixing it for 30 min, remove it. 4.2.5.3 After removing it, with the magnetic ring sleeve (4.2.3.2), pour out the water and material in the plastic jar (4.2.3.3); use water to repeatedly rinse the wall of the jar for more than 5 times, so as to ensure that there is no precipitation of sample at the bottom of the jar. 4.2.5.4 After assembling the filter film (4.2.2.3) and vacuum filtration device (4.2.3.6), remove the magnetic ring sleeve (4.2.3.2); use water to rinse the wall of the plastic jar (4.2.3.3) for more than 3 times. Pour the washing solution into the vacuum filtration device (4.2.3.6); use water to rinse the wall of the suction and filtration cup for more than 3 times. 4.2.6 Processing of test data Count the number of large particle magnetic impurities. Respectively count the number of iron and stainless steel (iron-chromium-nickel).

5 Determination of Residual Alkali Content

5.1 Principle Use a certain volume of water to dissolve the residual alkali on the surface of the sample with a certain mass. After filtration, take the filtrate; use the standard titration solution of hydrochloric acid to perform titration. 5.2 Reagents or Materials Unless it is otherwise specified, all reagents used in this Method are of guaranteed purity and Grade-1 water specified in GB/T 6682. 5.2.1 Standard titration solution of hydrochloric acid. 0.1 mol/L. Adopt a nationally recognized certified reference material within the validity period, or prepare it in accordance with the stipulations of GB/T 601. 5.2.2 Plastic wrap. 5.3 Instruments and Equipment 5.4 Sample The particle of the sample shall be not greater than 0.154 mm. 5.5 Test Procedures 5.6 Processing of Test Data 5.6.1 The residual lithium carbonate content in the sample, in mass fraction wLi2CO3, shall be calculated in accordance with Formula (4). 5.6.2 The residual lithium hydroxide content in the sample, in mass fraction wLiOH, shall be calculated in accordance with Formula (5). 5.6.3 The residual alkali content in the sample, in mass fraction wra, shall be calculated in accordance with Formula (6). 5.6.4 The residual lithium content in the sample, in mass fraction wrl, shall be calculated in accordance with Formula (7). 5.6.5 The calculation results shall be expressed in three decimal places and rounded off in accordance with the stipulations of GB/T 8170. 5.7 Precision 5.7.1 Repeatability In terms of the measured values of two independent test results obtained under repeatability conditions, within the range of average values provided in Table 2, the absolute difference between the two test results does not exceed the repeatability limit (r), and the circumstance of exceeding the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is obtained through linear interpolation or extrapolation in accordance with the data in Table 2.

6 Test Report

The test report shall include the following aspects. ......

Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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