GB/T 33827-2017Determination of magnetic impurities in anode nanomaterials for Li-ion battery (English PDF)
锂电池用纳米负极材料中磁性物质含量的测定方法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
May 31, 2017
Implementation date
December 1, 2017
Scope
GB/T 33827-2017 is the English-translated version of 锂电池用纳米负极材料中磁性物质含量的测定方法.
GB/T 33827-2017 is the Chinese national method for measuring the magnetic impurities left in the nanostructured anode materials of lithium ion batteries, by inductively coupled plasma atomic emission spectrometry.
Magnetic material is defined as the metal the magnetic bar picks up under the conditions the standard fixes, and the sum of iron, cobalt, chromium, nickel and zinc is determined over mass fractions from 0.02 x 10^-6 to 20 x 10^-6.
The sample is dispersed in ethanol and rolled against a 6000 GS magnetic bar, which is then heated in nitric and hydrochloric acid so that the particles are eluted and read on the spectrometer.
The standard also fixes the environment, the reagents, the standard solutions, the apparatus and the repeatability obtained in four laboratories. It was issued on 31 May 2017 and has applied since 1 December 2017.
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Document preview — GB/T 33827-2017
National Standard of the People's Republic of China
- ICS
- 71.060.50
- Classification
- G 12
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope4
- 2 Normative references4
- 3 Terms and definitions4
- 4 Determination principle5
- 5 Environmental conditions for determination5
- 6 Reagents and materials5
- 7 Testing instruments and equipment6
- 8 Testing procedures7
- 9 Result calculation and data processing9
- 10 Repeatability9
- 11 Test report10
- Annex A (Informative) Rolling device schematic11
- Annex B (Informative) Removal steps of magnetic bar and precautions12
- Annex C (Informative) Instrument parameter setting14
Foreword
This Standard was drafted in accordance with the rules given in GB/T 1.1-2009.
1 Scope
This Standard specifies the principle, environmental conditions for determination, reagents and instruments, test procedures, analysis and calculation of results, and test report content in determination of magnetic materials in anode nanomaterials for Li-ion battery in inductively coupled plasma atomic emission spectrometry (ICP-OES).
This Standard applies the determination of magnetic materials (the sum of iron, cobalt, chromium, nickel, zinc content) with mass fraction between 0.02 x 10^-6 ~ 20 x 10^-6.
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 4842, Argon
GB/T 6682-2008, Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1 Magnetic materials
the general term for the metal material adsorbed by the magnetic bar under the operation conditions specified in this Standard
4 Determination principle
Disperse the sample in an ethanol medium. Scroll the sample for a certain time using a magnetic bar with a certain magnetic field strength. Heat the adsorbed magnetic particles in an acid solution to elute.
5 Environmental conditions for determination
The determination shall be carried out at room temperature, with a humidity not exceeding 60%RH.
6 Reagents and materials
Warning - Some of the reagents used in this test method are toxic or corrosive and shall be handled with care!
6.1 General requirements
Unless otherwise specified, the analytical reagents and the grade three water specified in GB/T 6682-2008 are used in the analysis.
6.2 Nitric acid
The mass fraction is not less than 65%.
6.3 Hydrochloric acid
The mass fraction is not less than 36%.
6.6 Standard materials
6.6.1 Iron standard solution, with standard number of GSB04-1726-2004, with the concentration of 1000 µg/mL.
6.6.2 Cobalt standard solution, with standard number of GSB04-1722-2004, with the concentration of 1000 µg/mL.
6.7 Preparation of standard solution
6.7.1 Respectively pipet 5.00 mL of iron, cobalt, chromium, nickel, zinc standard solutions (6.6) into a 100.00 mL volumetric flask. Add into 2.00 mL of nitric acid (6.2). Set volume for use. The concentration of iron, cobalt, chromium, nickel, zinc in this standard solution shall be 50.00 µg/mL.
7 Testing instruments and equipment
7.1 Inductively coupled plasma atomic emission spectrometer
(ICP-OES)
7.4 Magnetic bar
magnetic field strength. 6000 GS (allowable deviation of less than 5%); selected diameter. 15mm ~ 20mm, length. 45mm ~ 55mm; appearance.
7.5 Electronic balance
precision of 0.001 g
7.6 Rolling device
rolling diameter. 10cm ~ 12cm; the rotation speed can be set between 60 r/min ~ 100 r/min; refer to Annex A for the rolling method of the rolling machine
7.7 Ultrasonic cleaning instrument
ultrasonic frequency. 28kHz ~ 33kHz
8 Testing procedures
8.1 Magnetic bar cleaning
Place the magnetic bar in a clean conical flask. Add into 2.00 mL of nitric acid, 6.00 mL of hydrochloric acid. Add water till it immerses the magnetic bar. Place onto the heating device to heat.
8.2 Sample weighing
According to the requirements of Table 2, accurately weigh a certain amount of sample into the clean sample can.
8.4 Cleaning
After rolling, take the magnetic bar out and put into the conical flask. See Annex B for removing process. After cleaning with water, add into 50 mL of anhydrous ethanol.
8.5 Digestion of magnetic materials
After cleaning, add into 1.5 mL of nitric acid, 4.5 mL of hydrochloric acid into the conical flask equipped with the magnetic bar. Add into water to make the magnetic bar totally immersed.
8.6 Preparation of blank sample
Carry out the blank test with the sample.
8.7 Determination
Using an inductively coupled plasma emission spectrometer. See Annex C for parameter setting. According to Table 1, select the element wavelength. Test the series of mixed standard solution in sequence.
9 Result calculation and data processing
The content of magnetic material shall be calculated according to equation (1), equation (2).
10 Repeatability
10.1 This method does not have a suitable standard sample available for the determination of the deviation, so the repeatability of the test shall be used to determine its repeatability.
10.2 The same sample shall be tested in four laboratories. The sample mean, standard deviation in the laboratory, inter-laboratories are shown in Table 3.
11 Test report
The test report shall contain but is not limited to the following information. […]
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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