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SJ/T 11795-2022 English PDF (SJT11795-2022)

SJ/T 11795-2022 English PDF (SJT11795-2022)

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SJ/T 11795-2022: Test method for determining magnetic impurity content of electrode materials in lithium ion batteries

This document specifies the test method for magnetic impurity content in electrode materials of lithium-ion battery, including terms and definitions, test method summary, instruments and appliances, reagents, environmental requirements, pre-treatment, instrument analysis, result calculation, precision, reporting. This document is applicable to the testing of magnetic impurity content between 10 ????g/kg ~ 5000 ????g/kg, in positive and negative electrode powder materials of lithium-ion battery, their slurries, as well as binders, conductive agents and other auxiliary materials. This standard is not applicable to the detection of magnetic impurity content in lithium iron phosphate materials.
SJ/T 11795-2022
SJ
ELECTRONICS INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS 31.030
CCS L 90
Test method for determining magnetic impurity content of
electrode materials in lithium ion batteries
ISSUED ON: APRIL 24, 2022
IMPLEMENTED ON: JULY 01, 2022
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 5
4 Summary of test methods ... 5
5 Instruments and appliances ... 5
6 Reagents ... 6
7 Environmental requirements ... 6
8 Pre-treatment ... 6
9 Instrumental analysis ... 8
10 Result calculation ... 9
11 Precision ... 10
12 Reports ... 10
Test method for determining magnetic impurity content of
electrode materials in lithium ion batteries
1 Scope
This document specifies the test method for magnetic impurity content in electrode materials of lithium-ion battery, including terms and definitions, test method summary, instruments and appliances, reagents, environmental requirements, pre-treatment, instrument analysis, result calculation, precision, reporting.
This document is applicable to the testing of magnetic impurity content between 10 ??g/kg ~ 5000 ??g/kg, in positive and negative electrode powder materials of lithium-ion battery, their slurries, as well as binders, conductive agents and other auxiliary materials. This standard is not applicable to the detection of magnetic impurity content in lithium iron phosphate materials.
2 Normative references
The contents of the following documents constitute essential provisions of this document through normative references in the text. Among them, for dated reference documents, only the version corresponding to the date applies to this document; for undated reference documents, the latest version (including all amendments) applies to this document.
GB/T 6379.1-2004 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions
GB/T 6379.2-2004 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods
JY/T 015-1996 General rules for inductivity coupled plasma-atomic emission spectrometry
3 Terms and definitions
The terms and definitions, which are defined in GB/T 6379.1-2004, as well as the following terms and definitions, apply to this document.
3.1
Magnetic impurity
Magnetic impurities presented in lithium-ion battery materials that can be attracted by magnets.
Note: Harmful magnetic impurity in lithium-ion battery materials mainly includes iron (Fe), chromium (Cr), nickel (Ni), zinc (Zn).
4 Summary of test methods
The sample is divided into a suitable liquid at a suitable concentration. After mixing and adsorption, an acidic solution is added to dissolve the adsorbed magnetic impurity. An inductively coupled plasma emission spectrometer is used to detect the content of iron (Fe), chromium (Cr), nickel (Ni), zinc (Zn), etc., in the test solution. 5 Instruments and appliances
5.1 Inductively coupled plasma optical emission spectrometer (ICP-OES): Instrument performance shall comply with the requirements of JY/T 015-1996.
5.2 Two-dimensional mixer: Horizontal rolling, recommended speed adjustment range (0 ~ 270) r/min;
5.3 Magnetic rod: PTFE-coated cylindrical magnetic rod, 52 mm long, 17 mm in diameter, with the strongest magnetic strength (5500 ~ 7500) GS.
5.4 Constant temperature water bath or heating device with equivalent performance: The temperature can reach 100 ??C.
5.5 Electronic balance: Sensitivity is 0.01 g.
5.6 Ultrasonic cleaning machine.
5.7 Sample jar: Wide-mouth plastic bottle, 500 mL, diameter (80 ~ 90) mm. 5.8 Other appliances: Plastic stoppered colorimetric tube (50 mL, inner diameter 3 cm), beaker (500 mL), plastic or wooden clamps, auxiliary magnets (1000 GS ~ 3000 GS). Note: The instruments (magnetic rods, sample jars, beakers, test tubes, etc.) used for testing different materials need to be separated and dedicated; use non-metallic tools and containers during the operation, to avoid the introduction of external impurities. 6 Reagents
6.1 The water used in this document shall comply with the requirements of grade II water in GB/T 6682-2008.
6.2 Concentrated nitric acid: Mass fraction is not less than 65%, superior grade pure or higher.
6.3 Concentrated hydrochloric acid: Mass fraction is not less than 36%, superior grade pure or higher.
6.4 Anhydrous ethanol: Mass fraction is not less than 99.7%, analytically pure. 6.5 N-methylpyrrolidone, analytically pure.
6.6 Argon gas: Purity not less than 99.999%.
6.7 Fe, Cr, Ni, Zn standard solutions: Single element or mixed standard solutions with certificates, OR prepared using certified reference materials within the validity period. 6.8 Aqua regia solution (1:1): Prepared according to the volume ratio of concentrated hydrochloric acid: concentrated nitric acid: water = 3:1:4.
7 Environmental requirements
7.1 Ambient temperature: The instrument analysis ambient temperature (20 ~ 25) ??C. 7.2 Environmental humidity: The relative humidity of the instrument analysis environment shall not be greater than 60%.
8 Pre-treatment
8.1 Weighing samples
Weigh 200 g of specimen, accurate to 0.01 g.
8.2 Mixing
Place the specimen in the sample jar. Add a clean magnetic rod. Add 300 mL of dispersion solvent (pure water or absolute ethanol or NMP). Seal it. Shake the sample jar for about 30 seconds, to mix the sample and dispersion solvent evenly. The solvent 8.7 Fixation of volume
Take out the colorimetric tube. Cool to room temperature. Transfer the digestion test solution to a 50 mL volumetric flask (if the test solution contains insoluble matter, it needs to be filtered). Use an appropriate amount of water, to rinse the colorimetric tube 3 times. Transfer the cleaning solution into a volumetric flask. Make the volume reach to the mark. Shake well, to obtain the one-time adsorbed test solution. 8.8 Multiple adsorption
8.8.1 Add a clean magnetic rod to the sample jar after the first adsorption. Perform the i-th (i = 2, 3..., n) adsorption, at a rotation speed of 90 r/min for 10 minutes. After each adsorption, immediately use an auxiliary magnet to attach the magnetic rod to the side or top cover of the sample jar. Take out the magnetic rod. Then put in a clean magnetic rod and continue mixing and adsorption.
8.8.2 Repeat steps 8.4 ~ 8.7, to obtain the test liquid adsorbed n times. 8.8.3 The number of adsorptions shall satisfy the adsorption rate An-1 > 80%. The adsorption rate An-1 is the ratio -- of the total adsorption amount of (n-1) times to the total adsorption content of n times, which is calculated according to formula (1): Where:
An-1 - Adsorption rate, in percentage (%);
??[Total(i)] - The content of magnetic impurity adsorbed for the i-th time, i = 1, 2?€?n. 8.9 Blank test
Except that no specimen to be tested is added, a blank test shall be performed along with the specimen under the same conditions for each operation, to obtain a blank test solution.
9 Instrumental analysis
9.1 Select a reasonable dilution factor, to prepare the standard solution. It can use step- by-step dilution. Use 2% nitric acid solution to dilute it to the mark. Shake well. The concentration of standard solutions and recommended spectral lines are as shown in Table 2.
9.2 Under the selected optimal working conditions, introduce the reagent blank and a series of standard solutions into the inductively coupled plasma optical emission spectrometer (ICP-OES) in sequence. Draw a standard curve. Then introduce the blank

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