Translated English of Chinese Standard: GB/T33827-2017 www.chinesestandard.net Sales@ChineseStandard.net ICS 71.060.50 G 12 NATIONAL STANDARD OF THE PEOPLE S REPUBLIC OF CHINA GB Determination of magnetic impurities in anode nanomaterials for Li-ion battery 锂电池用纳米负极材料中磁性物质含量的测定方法 How to BUY & immediately GET a full-copy of this standard? 1. www.chinesestandard.net; 2. Search --> Add to Cart --> Checkout (3-steps); 3. No action is required - Full-copy of this standard will be automatically & immediately delivered to your EMAIL address in 0~60 minutes. 4. Support: Sales@ChineseStandard.net. Wayne, Sales manager Issued on: May 31, 2017 Implemented on: December 1, 2017 Issued by: General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration Committee. www.chinesestandard.net Page 1 of 14
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 www.chinesestandard.net Page 2 of 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. www.chinesestandard.net Page 3 of 14
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. www.chinesestandard.net Page 4 of 14
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 water specified in GB/T 6682-2008 are used in the analysis. grade three 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 μg/ml. www.chinesestandard.net Page 5 of 14
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. www.chinesestandard.net Page 8 of 14
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) www.chinesestandard.net Page 12 of 14