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GB/T 33827-2017 English PDF (GBT33827-2017)

GB/T 33827-2017 English PDF (GBT33827-2017)

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GB/T 33827-2017: Determination of magnetic impurities in anode nanomaterials for Li-ion battery

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).
GB/T 33827-2017
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.060.50
G 12
Determination of magnetic impurities in
anode nanomaterials for Li-ion battery
ISSUED ON. MAY 31, 2017
IMPLEMENTED ON. DECEMBER 1, 2017
Issued by. General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration Committee.
3. No action is required - Full-copy of this standard will be automatically and immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Determination principle ... 5
5 Environmental conditions for determination ... 5
6 Reagents and materials ... 5
7 Testing instruments and equipment ... 6
8 Testing procedures ... 7
9 Result calculation and data processing ... 9
10 Repeatability ... 9
11 Test report ... 10
Annex A (Informative) Rolling device schematic ... 11
Annex B (Informative) Removal steps of magnetic bar and precautions ... 12 Annex C (Informative) Instrument parameter setting ... 14
Foreword
This Standard was drafted in accordance with the rules given in GB/T
1.1-2009.
This Standard was proposed by Chinese Academy of Sciences.
This Standard shall be under the jurisdiction of Subcommittee on
Nanomaterials, National Technical Committee on Nanotechnology of
Standardization Administration of China (SAC/TC 279 / SC 1).
The drafting organizations of this Standard. Shenzhen Beitui New Energy Materials Co., Ltd., Hefei Guoxuan Hi-Tech Power Energy Co., Ltd., Henan Cologne New Energy Co., Ltd., Metallurgical Industry Information Standards Institute, Shenzhen BRT Nanotechnology Limited, Tianjin BRT New Energy
Technology Co., Ltd.
Main drafters of this Standard. Yue Min, Mao Aiping, Ge Daobin, Cheng Di, Dai Shifeng, Zha Xiufang, Chen Nanmin, Yang Xulai, Xu Yunjun, Huang
Youyuan, Liu Xiuming.
Determination of magnetic impurities in
anode nanomaterials for Li-ion battery
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??10-6 ~ 20??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
NOTE. The particles sucked out by the magnetic bar in anode nanomaterials for Li-ion battery usually contain elemental or compound of iron, cobalt, chromium, nickel, zinc. 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. Determine the contents of iron, cobalt, chromium, nickel and zinc by inductively coupled plasma atomic emission spectrometer. And calculate the sum of the contents of the five elements.
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%.
6.4 Anhydrous ethanol
The mass fraction is not less than 99.7%.
6.5 Argon
The argon shall meet general requirements of GB/T 4842. The volume
fraction is not less than 99.999%.
6.6 Standard materials
6.6.1 Iron standard solution, with standard number of GSB04-1726-2004,
with the concentration of 1000 ??g/mL.
0.5 ~ 1.0 100??1.00
>1.0 200??5.00
8.3 Adsorption of magnetic materials
Add 300 mL of anhydrous ethanol into the sample can containing sample.
Add into the clean magnetic bar. Cover the lid. After well shaking, place the sample can on the rolling device. And set the rolling speed at 60 r/min ~ 80 r/min. Rolling 30 min and shake it not less than 3 times during the rolling process.
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. Ultrasound on the ultrasonic cleaning instrument 1 min. Repeat three times. Then clean the magnetic bar and the conical flask three times. After cleaning, it needs to use another magnetic bar at the bottom outside the flask to absorb the magnetic bar inside the flask to prevent the solution from falling out of the magnetic bar.
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. Place onto the heating device to heat. Heat it and make sure it slightly boiling 30 min. Shake it not less than 3 times during the heating process. During shaking, try to make the acid solution cover the surface of the magnetic bar. After heating, remove it and naturally cool it to room temperature. Move the cooled solution into a 100 mL volumetric flask. Use a small amount of water to wash the conical flask and the magnetic bar 3~4 times. Incorporate the washing liquid into the volumetric flask. Set volume and well shake it.
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. Draw the working curve. Then determine the sample blank and testing sample in the same method.
Use the deducted blank for result correction.
Annex B
(Informative)
Removal steps of magnetic bar and precautions
B.1 Steps
The steps are as follows.
a) place the well-rolled sample can on the test bench;
b) use another magnetic bar to absorb the magnetic bar in the sample can; c) hold the can body, uncover the inner and outer lids and place on the test bench;
d) select the clean conical flask of corresponding number; the mouth of the conical flask faces down, close to the sample can mouth; use another
hand to hold the conical flask and the sample can;
e) use another hand to hold the magnetic bar outside the sample bar which absorbs the magnetic bar in the can; slowly lift it to make the magnetic bar in the sample can into the conical flask;
f) remove the magnetic bar outside the conical flask and it shall
successfully take the magnetic bar in the sample can out.
B.2 Precautions
The precautions are as follows.
a) the removal process shall prevent the magnetic bars inside and outside the sample can contact with each other;
b) the removal process shall prevent the magnetic stick crumpled the
conical flask and cut the skin;
c) the waste and anhydrous ethanol used for magnetic materials shall be properly treated (consider recycling).
B.3 Removal of the magnetic bar (see Figure B.1)

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