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SJ/T 11795-2022 (SJT11795-2022)

SJ/T 11795-2022_English: PDF (SJT 11795-2022, SJT11795-2022)
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SJ/T 11795-2022English170 Add to Cart 0--9 seconds. Auto-delivery Test method for determining magnetic impurity content of electrode materials in lithium ion batteries Valid SJ/T 11795-2022

BASIC DATA
Standard ID SJ/T 11795-2022 (SJ/T11795-2022)
Description (Translated English) (Test method for magnetic foreign matter content in lithium-ion battery electrode materials)
Sector / Industry Electronics Industry Standard (Recommended)
Word Count Estimation 7,755
Date of Issue 2022-04-08
Date of Implementation 2022-07-01
Summary This standard specifies the test methods for the content of magnetic foreign matter in lithium-ion battery electrode materials, including terms and definitions, test method summary, instruments and utensils, reagents, environmental requirements, pre-treatment, instrument analysis, result calculation, precision and reports. This standard is applicable to the detection of magnetic foreign matter content in lithium-ion battery positive and negative electrode powder materials and their slurries, as well as binders, conductive agents and other auxiliary materials between 10 ��g/kg and 5000 ��g/kg. This standard does not apply to the detection of magnetic foreign matter content in lithium iron phosphate materials.

Standards related to: SJ/T 11795-2022

SJ/T 11795-2022
SJ
ELECTRONICS INDUSTRY STANDARD
OF THE PEOPLE’S 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
μg/kg ~ 5000 μg/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 (%);
ω[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
...