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Similar standardsSJ/T 11723-2018: Electrolyte solution used for lithium ion battery---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/SJT11723-2018SJ ELECTRONIC INDUSTRY STANDARD ICS 31-030 L 90 Record number. Electrolyte solution used for lithium ion battery Issued on: JULY 04, 2018 Implemented on: OCTOBER 01, 2018 Issued by. Ministry of Industry and Information Technology of the People's Republic of China Table of ContentsForeword... 3 1 Scope... 4 2 Normative references... 4 3 Requirements... 4 4 Test methods... 5 5 Inspection rules... 14 6 Marking, packaging, transportation and storage... 17 Appendix A (Normative) Determination of sulfate ion (SO42-)... 19 Appendix B (Normative) Determination of K, Na, Fe, Ca, Pb, Cu, Zn, Ni, Cr by inductively coupled plasma optical emission spectrometry... 21 Electrolyte solution used for lithium ion battery1 ScopeThis Standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation and storage of electrolyte solution used for lithium ion battery. This Standard applies to the electrolyte solution used for lithium ion battery which is composed of electrolyte lithium salts, solvents, etc.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the dated version applies to this document. For undated references, the latest edition (including all amendments) applies to this document. GB/T 3143, Color determination method of liquid chemicals (Hazen unit; Platinum-cobalt scale) GB/T 6682-2008, Water for analytical laboratory use - Specification and test methods GB 13690, General rule for classification and hazard communication of chemicals GB 15258, General rules for preparation of precautionary label for chemicals GB/T 26125, Electrical and electronic products - Determination of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls, polybrominated diphenyl ethers) GB/T 26572, Requirements of concentration limits for certain restricted substances in electrical and electronic products3 Requirements3.1 Appearance The electrolyte solution used for lithium ion battery shall be a solution without precipitation, suspended matter or stratification. 3.2 Technical requirements 4.4.3.3 Weigh (3 ~ 5) g of sample (accurate reading to 0.001 g) using the reduction method on an electronic balance and use a syringe to draw the sample. 4.4.3.4 Inject the extracted sample into the titration cell from the injection port; stir thoroughly for 10 seconds and then start titration. 4.4.3.5 After the titration is completed, input the sample mass and record the water content determination results in the sample. 4.4.3.6 Two parallel tests shall be performed for each test, and the absolute difference between the parallel test values shall be ≤2 mg/kg. 4.4.4 Result processing Take the arithmetic mean of the values measured in two parallel tests as the test result. 4.5 Determination of free acid 4.5.1 Potentiometric titration 4.5.1.1 Principle Immerse the indicator electrode and the reference electrode in the same solution to be measured. During the titration process, the potential of the reference electrode remains constant, and the potential of the indicator electrode changes with the concentration of the substance to be measured. Before and after the stoichiometric point, the change in the concentration of the substance to be measured in the solution will cause a sharp change in the potential of the indicator electrode. The sudden jump point of the indicator electrode potential is the titration end point. 4.5.1.2 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Potentiometric titrator. sensitivity 0.1 mV. b) pH electrode. c) Electronic balance. minimum graduation value 1 mg. 4.5.1.3 Reagents Sodium methoxide standard titration solution (concentration 0.02 mol/L). a) Preparation. Weigh 1.08 g of sodium methoxide; dissolve it in 1 000 mL of methanol; shake well. b) Calibration. Weigh 0.396 g of the standard reagent potassium hydrogen phthalate dried to constant weight in an oven at (110 ~ 120) °C and dissolve it in 1 000 4.5.2 Ice water chemical titration 4.5.2.1 Method summary Use ice-water mixture as solvent and bromothymol blue solution as indicator; use sodium hydroxide standard titration solution to titrate the total free acid in the sample; calculate based on hydrofluoric acid. 4.5.2.2 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Electronic balance. minimum graduation value 1 mg; b) Alkali burette. 10 mL, minimum graduation value 0.01 mL; c) Syringe. 10 mL; d) Erlenmeyer flask. 250 mL. 4.5.2.3 Reagents and Materials The required reagents and materials are as follows. a) Sodium hydroxide standard titration solution. 0.002 mol/L. b) Ice cubes. Freeze water in an ice cube tray to obtain cubes with a length, width and height of approximately 1 cm. c) Bromothymol blue indicator solution (1 g/L). Weigh 0.1 g of bromothymol blue; dissolve it in 50 mL of ethanol (95%); then, use ethanol (95%) to dilute to 100 mL. 4.5.2.4 Test steps Measure 50 mL of water frozen to (0 ~ 4) ℃ in a 250 mL conical flask; add (3 ~ 4) ice cubes; then, add (2 ~ 3) drops of bromothymol blue indicator solution. Use a syringe to take a sample; weigh about 10 g of the sample (accurate to 0.001 g) by the reduction method; add it to the conical flask; shake it thoroughly. Use the calibrated 0.002 mol/L sodium hydroxide standard solution; shake the conical flask while titrating, until the solution suddenly changes from yellow to blue, which is the end point; record the volume of sodium hydroxide standard titration solution consumed in the titration. Do a blank test at the same time. 4.5.2.5 Result processing The free acid content is based on HF according to Formula (2). Before testing, first draw water at about 25 °C to calibrate the instrument. After calibration, draw the sample to be tested to rinse the U-shaped tube of the density meter (3 ~ 4) times; then, draw the sample to be tested; record the density value of the sample at 25.0 °C in the U-shaped tube. After the test is completed, discharge the sample; first wash the U-shaped tube with anhydrous ethanol (3 ~ 4) times, and then wash it with water. Perform two parallel tests for each test. 4.6.2.5 Result processing Take the arithmetic mean of the values measured in two parallel tests as the test result. 4.6.3 During arbitration, density shall be determined using the density bottle method. 4.7 Determination of electrical conductivity 4.7.1 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Conductivity meter. measuring range (0 ~ 100) mS/cm; b) Conductivity electrode. the electrode constant matches the measurement range; c) Thermometer. minimum graduation value 0.1 ℃. 4.7.2 Reagents Potassium chloride (KCl) conductivity standard solution. 0.1 mol/L, the conductivity value is 12.852 mS/cm at 25 °C. 4.7.3 Test steps 4.7.3.1 Turn on the conductivity meter and preheat for 0.5 h. 4.7.3.2 Use 0.1 mol/L potassium chloride (KCl) conductivity standard solution to calibrate the instrument. 4.7.3.3 Add about 20 mL of electrolyte solution to a 100 mL clean plastic cup; control the temperature at (25 ± 3) °C; insert the electrodes and thermometer into the electrolyte solution; adjust the instrument temperature so that the instrument compensation temperature is consistent with the electrolyte temperature to be measured. When the reading stabilizes, it is the conductivity of the electrolyte solution at 25 °C. 4.7.3.4 Two parallel tests shall be performed for each test, and the absolute difference between the parallel test values shall be ≤0.2 mS/cm. 4.7.4 Result processing Take the arithmetic mean of the values measured in two parallel tests as the test result. 4.8 Determination of chloride ion (Cl-) content 4.8.1 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Potentiometric titrator, sensitivity 0.1 mV; b) Silver ion selective electrode; c) Electronic balance. minimum graduation value 1 mg. 4.8.2 Reagents Silver nitrate standard titration solution (concentration 0.001 mol/L). a) Preparation. Weigh 0.175 g of silver nitrate; dissolve in 1 000 mL of ethanol; shake well. Store the solution in a brown bottle. b) Calibration. Weigh 0.050 g of the reference reagent, sodium chloride, which is burned to constant weight in a high-temperature furnace at (500 ~ 600) ℃; dissolve it in 2 000 mL of water; shake well. Measure 50 mL of the above sodium chloride solution and titrate it with silver nitrate standard titration solution on a potentiometric titrator to calibrate the concentration of the silver nitrate standard titration solution. 4.8.3 Test steps 4.8.3.1 Automatically calibrate the potentiometric titrator. 4.8.3.2 Weigh (40 ~ 60) g of sample (accurate reading to 0.001 g) and place in a 100 mL clean plastic cup. 4.8.3.3 Immerse the electrode in the solution to be tested and stir the solution thoroughly. 4.8.3.4 Input the concentration value of the silver nitrate standard titration solution into the potentiometric titrator and start titration. When the titration endpoint is reached, record the volume of the silver nitrate standard titration solution consumed. 4.8.3.5 Two parallel tests shall be performed for each test, and the absolute difference between the parallel test values shall be ≤0.5 mg/kg. 4.8.4 Result processing Calculate the content of chloride ion (Cl-) according to Formula (4). 5.3 Quality consistency inspection 5.3.1 Batch inspection 5.3.1.1 Batching An inspection batch consists of electrolyte solution used for lithium ion battery that is continuously produced using the same raw materials, under the same production conditions, using the same process, and submitted for inspection at the same time. 5.3.1.2 Sampling When the number of packaging units in each batch is less than 3 barrels, all barrels are drawn; when the number of packaging units in each batch is greater than or equal to 3 barrels, 3 barrels are drawn. In principle, the first barrel, the middle barrel (odd barrel n+1/2, even barrel n/2), and the last barrel of each batch are drawn. Before sampling, use high-purity nitrogen or argon to purge the sampling pipe for 2 minutes; then, connect it to the liquid outlet of the packaging barrel of the product to be tested with a quick connector; open the valve; release (150 ~ 200) mL of the product to be tested (to clean the pipe); then, use the product to be tested to rinse the sampling bottle (2 ~ 3) times before starting sampling. When the number of sampling barrels is 3, the sampling volume per barrel is (150 ~ 200) mL; when the number of sampling barrels is 2, the sampling volume per barrel is (200 ~ 250) mL; when the number of sampling barrels is 1, the sampling volume per barrel is (400 ~ 500) mL. After sampling, tighten the bottle cap immediately. Mix the samples in equal amounts to form a batch sample. Divide the batch sample into two parts; mark them with the product brand, batch number, sampling date and name of the sampler, one for testing and the other for storage in a sealed container. The above operations must be carried out in an environment with a moisture content of ≤1 mg/kg. 5.3.1.3 Inspection items The batch inspection items include appearance, chroma, density, moisture, conductivity and free acid content, as shown in Table 2. 5.3.1.4 Judgment of conformity When all batch inspection items are qualified, the batch of products is qualified; if any batch inspection item is unqualified, the batch of products is unqualified. 5.3.2 Periodic inspection 5.3.2.1 Sampling Randomly draw (400 ~ 500) mL of the sample, which can be drawn from the product packaging unit or in an online closed sampling. 5.3.2.2 Inspection items The periodic inspection items include chloride ion content, sulfate ion content and metal impurity content, as shown in Table 2.The inspection cycle is 1 week. 5.3.2.3 Judgment of conformity When the test results of all periodic inspection items are qualified, the periodic inspection is qualified; if any periodic inspection item is unqualified, the periodic inspection is unqualified. 5.3.2.4 Non-conforming treatment If the periodic inspection fails, the supplier shall immediately stop the delivery of the products produced in the period and find out the reasons for the failure of the periodic inspection items. According to the reasons for the failure, take appropriate measures to rectify the products produced in the period and resubmit for inspection. The products can be delivered only after they pass the inspection. For products that have been delivered, the supplier shall notify the buyer of any unqualified items in periodic inspection, and the two parties shall resolve the issue through negotiation.6 Marking, packaging, transportation and storage6.1 Marking The product packaging shall have firm and clear markings, indicating the manufacturer's name, address, product name, designation, net weight, batch number, precautions, etc., and shall comply with the requirements of GB 15258. Each batch of products shall be accompanied by a certificate of conformity or a certificate of quality, which shall include. manufacturer name, product name, designation, net weight, batch number, production date, shelf life, etc. 6.2 Packaging The electrolyte solution used for lithium ion battery shall be packaged in stainless steel barrels (with quick connectors) and filled with (0.015 ~ 0.025) MPa high-purity nitrogen or argon as protection. 6.3 TransportationAppendix A(Normative) Determination of sulfate ion (SO42-) A.1 Scope This Appendix specifies the method for determining the sulfate ion (SO42-) content in the electrolyte solution used for lithium ion battery. This Appendix applies to the determination of sulfate ion (SO42-) content in electrolyte solution used for lithium ion battery. A.2 Method summary In the hydrochloric acid medium, barium ions and sulfate ions generate insoluble barium sulfate. When the sulfate ion content is low, the barium sulfate is suspended for a certain period of time, making the solution turbid. Determine the turbidity of the solution and the standard comparison solution by visual method to obtain the measurement result. A.3 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Colorimetric tube. 50 mL; b) Electronic balance. minimum graduation value 1 mg. A.4 Reagents The required reagents are as follows. a) Ethanol-water solution. methanol. mwater = 1.2; b) Barium chloride aqueous solution. 0.5 mol/L, (pH=1, hydrochloric acid system); c) Concentrated hydrochloric acid; d) Sulfate ion standard solution. C(SO42-) = 100 μg/g. A.5 Analysis steps A.5.1 Prepare a reference solution containing 50 μg of SO42-. Accurately weigh 0.5 g of sulfate ion standard solution; add ethanol water solution to 25 mL; mix well; add 5Appendix B(Normative) Determination of K, Na, Fe, Ca, Pb, Cu, Zn, Ni, Cr by inductively coupled plasma optical emission spectrometry B.1 Scope This Appendix specifies the method for determining the contents of K, Na, Fe, Ca, Pb, Cu, Zn, Ni and Cr in electrolyte solution used for lithium ion battery by inductively coupled plasma optical emission spectrometry. This Appendix is applicable to the determination of K, Na, Fe, Ca, Pb, Cu, Zn, Ni and Cr contents in electrolyte solution used for lithium ion battery. The recommended concentration range of the determined elements is 0.01 mg/kg ~ 10 mg/kg. B.2 Method summary After the sample is introduced into the nebulization system by the carrier gas (argon) for atomization, it enters the plasma in the form of aerosol. In the high temperature and inert gas atmosphere, the excited atoms and ions release strong characteristic electromagnetic radiation. The quantification is carried out according to the different radiation spectra of different elements and the proportional relationship between the strength of the radiation spectra and the element concentration. B.3 Instruments and apparatuses The required instruments and apparatuses are as follows. a) Inductively coupled plasma optical emission spectrometer (ICP-OES). equipped with a complete set of hydrofluoric acid resistant injection system; b) Electronic balance. minimum graduation value 0.1 mg; c) Plastic bottle for experiments. the material is resistant to corrosion by hydrofluoric acid. B.4 Reagents The required reagents are as follows. a) Water; b) Gas. liquid argon, purity not less than 99.999%; gas required for purifying compressed air or other instruments; c) Multi-element mixed standard solution. The concentration of K, Na, Fe, Ca, Pb, Cu, Zn, Ni, and Cr is 100 mg/kg. Standard solutions of other concentrations can also be used; d) Ethanol. guaranteed reagent; e) Nitric acid. guaranteed reagent; f) Ethanol/water solution. Vethanol. Vwater = 1.2.Add guaranteed nitric acid to adjust the pH value of the ethanol/water solution to 1. B.5 Analysis steps B.5.1 Sample preparation Take an appropriate amount of the sample to be tested into a clean plastic bottle and dilute it 20 times with ethanol/water solution. The ethanol/water solution is the blank solution. Note. The dilution factor of the sample can be adjusted appropriately according to the content of the element to be tested in the sample. B.5.2 Preparation of standard solutions for working curve series The concentrations of the working curve series standard solutions are 0 mg/kg, 0.1 mg/kg, 0.15 mg/kg, 0.2 mg/kg and 0.25 mg/kg. Accurately weigh appropriate amounts of multi-element mixed standard solutions and add them to 5 clean plastic bottles; use ethanol/water solution to dilute to the above concentrations; mix evenly. Note. The concentration range of the working curve series standard solution and the number of points for drawing the working curve can be adjusted appropriately according to the conditions of each instrument and the content of the element to be measured in the sample. The number of points for drawing the working curve is usually (3 ~ 5). B.5.3 Instrumental analysis B.5.3.1 According to the instrument requirements, select the characteristic spectral line wavelength of the element to be measured (see Table B.1) and choose the standard addition method. B.5.3.2 Under normal working conditions of the instrument, test the working curve series of standard solutions in sequence, and draw the standard working curve with the characteristic spectral line intensity as the ordinate and the concentration as the abscissa (the linear correlation coefficient is not less than 0.995). B.5.3.3 Test the sample solution and blank solution under the same conditions. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of English version of SJ/T 11723-2018 be delivered?Answer: The full copy PDF of English version of SJ/T 11723-2018 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice.Question 2: Can I share the purchased PDF of SJ/T 11723-2018_English with my colleagues?Answer: Yes. 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