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GB/T 45092-2024: Testing and evaluation of electrodes performance for hydrogen production by water electrolysis Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 45092-2024: Testing and evaluation of electrodes performance for hydrogen production by water electrolysis---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/GBT45092-2024 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 27.010 CCS F 19 Testing and evaluation of electrodes performance for hydrogen production by water electrolysis ISSUED ON: NOVEMBER 28, 2024 IMPLEMENTED ON: MARCH 01, 2025 Issued by: State Administration for Market Regulation; National Standardization Administration. Table of ContentsForeword ... 4 1 Scope ... 5 2 Normative references ... 5 3 Terms and definitions ... 6 4 Test and evaluation indicators ... 6 5 Ultrasonic weight loss test ... 7 5.1 Principle ... 7 5.2 Reagents ... 7 5.3 Equipment ... 7 5.4 Sample ... 8 5.5 Test conditions ... 8 5.6 Test steps ... 8 5.7 Data processing ... 9 6 Overpotential test ... 9 6.1 Principle ... 9 6.2 Reagents ... 10 6.3 Equipment ... 10 6.4 Samples ... 12 6.5 Reference electrode ... 12 6.6 Counter electrode ... 13 6.7 Test conditions ... 13 6.8 Test steps ... 13 6.9 Data processing ... 14 7 Positive and negative polarization stability test ... 14 7.1 Principle ... 14 7.2 Reagents ... 15 7.3 Equipment ... 15 7.4 Sample ... 15 7.5 Reference electrode and counter electrode ... 15 7.6 Test conditions ... 15 7.7 Test steps ... 15 7.8 Data processing ... 16 8 Test of average cell voltage and average cell voltage change rate ... 16 8.1 Principle ... 16 8.2 Reagents ... 17 8.3 Equipment ... 17 8.4 Sample ... 18 8.5 Test conditions ... 18 8.6 Test steps ... 19 8.7 Data processing ... 19 9 Fluctuating current electrolysis test ... 20 9.1 Principle ... 20 9.2 Reagents, equipment, samples, test conditions ... 21 9.3 Test steps ... 21 9.4 Data processing ... 22 10 Test report ... 23 Appendix A (Normative) Electrode potential calibration of reference electrode ... 24 Appendix B (Informative) Potential conversion, current density, potential compensation calculation ... 26 Appendix C (Informative) Single-cell electrolyzer ... 28 References ... 33 Testing and evaluation of electrodes performance for hydrogen production by water electrolysis Warning: This document does not cover all safety issues related to its application. When using this document, the user is responsible for formulating corresponding safety and protection measures, clarifying its limited scope, ensuring compliance with relevant national laws and regulations and mandatory national standards.1 ScopeThis document describes the test and evaluation methods for ultrasonic weight loss, overpotential, positive and negative polarization stability, average cell voltage, average cell voltage change rate, fluctuating current electrolysis of electrodes for hydrogen production by water electrolysis. This document is applicable to the performance test and evaluation of electrodes for hydrogen production by alkaline water electrolysis. The hydrogen evolution electrode and oxygen evolution electrode for hydrogen production by hydroxyl ion exchange membrane water electrolysis shall be implemented with reference to this document.2 Normative referencesThe contents of the following documents constitute essential clauses of this document through normative references in the text. Among them, for dated references, only the version corresponding to that date is applicable to this document; for undated references, the latest version (including all amendments) is applicable to this document. GB/T 678 Chemical reagent - Ethanol GB/T 2306 Chemical reagent - Potassium hydroxide GB/T 2900.98 Electrotechnical terminology - Electrochemistry GB/T 3634.2 Hydrogen - Part 2: Pure hydrogen, high pure hydrogen and ultrapure hydrogen GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 14599 Pure oxygen and high purity oxygen and ultra-pure oxygen GB/T 15724 Laboratory glassware beaker GB/T 21648 Industrial dense woven wire cloth GB/T 28817 Single cell test methods for polymer electrolyte fuel cell (PEFC)3 Terms and definitionsThe terms and definitions defined in GB/T 2900.98, as well as the following terms and definitions, apply to this document. 3.1 Overpotential The absolute value of the difference between the working potential and the theoretical potential, when an electrode reaction occurs on the electrode. Note: The overpotential must indicate the corresponding current density. The working potential and theoretical potential are values relative to the same reference system. 3.2 Average cell voltage The average cell voltage in a certain period of time when electrolysis is carried out at a certain current density. Note: For a single-cell electrolyzer, the average cell voltage is the average electrolyzer voltage in a certain period of time; for a multi-cell electrolyzer, it is the value obtained by dividing the average electrolyzer voltage in a certain period of time by the number of cells in series. 3.3 Reversible hydrogen electrode When hydrogen is introduced into a solution of a certain pH and reaches saturation, the electrode where the redox reaction of hydrogen and hydrogen ions on the platinum electrode reaches equilibrium and which has a balanced electrode potential. Note: The potential of the reversible hydrogen electrode is related to pH. The potential of the reversible hydrogen electrode at 25°C is E=-0.0592pH.4 Test and evaluation indicatorsSee Table 1 for electrode performance test and evaluation requirements. 5.4 Sample 5.4.1 Specifications The test electrode is a 40 mm × 40 mm rectangle. A set of test electrodes has 3 pieces; the 3 pieces shall come from the same batch of electrodes. For electrodes that need to be activated, the activated electrodes shall be used for testing. 5.4.2 Sample preparation The samples shall be cut according to the specifications of the test electrodes, with a size error of less than 2%. After cutting, the electrodes shall be kept flat; the burrs, serrations or sharp protrusions on the edges of the electrodes shall be rounded. 5.5 Test conditions The temperature of the test liquid in the ultrasonic cleaning machine is 30 °C ± 1 °C. 5.6 Test steps The test steps for ultrasonic weight loss of electrodes are as follows. a) Treatment: Rinse the electrodes repeatedly with pure water for at least 3 times; then rinse the electrodes repeatedly with anhydrous ethanol (unless otherwise specified in this document, anhydrous ethanol shall comply with the analytical grade requirements in GB/T 678) for at least 3 times; dry the electrodes in a vacuum oven at 70 °C and a vacuum degree of no more than 200 Pa for more than 2 hours. b) Weighing: Weigh 3 electrodes in turn; record the initial mass mi,0 of the 3 electrodes respectively, with an accuracy of 0.1 mg. c) Ultrasonic treatment: Treat one electrode each time; place the electrode horizontally at the bottom of a 250 mL glass beaker containing 200 mL of test solution (unless otherwise specified in this document, the glass beaker shall comply with the specification of 250 mL nominal capacity in GB/T 15724); place the beaker at the bottom of the ultrasonic cleaning machine and fix it; add water to the ultrasonic cleaning machine until the water level in the inner tank is 50 mm; treat it continuously for 60 min at a temperature of 30 °C ± 1 °C. The sample placement position during ultrasonic weight loss test is shown in Figure 1. d) Take out the test electrode; treat and weigh the post-ultrasonic electrode according to the steps described in a) and b); record the final mass mi of the three electrodes, respectively. electrode with an external salt bridge. Before use, the reference electrode shall be calibrated for potential according to the method described in Appendix A. 6.6 Counter electrode The counter electrode is a pure nickel electrode with a purity of not less than 99.5% and an effective size of 30 mm × 30 mm. 6.7 Test conditions The electrode overpotential test conditions are as follows. a) The test solution temperature is controlled at 25.0 °C ± 0.5 °C. b) When measuring the hydrogen evolution electrode, the test solution is continuously filled with hydrogen to maintain a saturated state; when measuring the oxygen evolution electrode, the test solution is continuously filled with oxygen to maintain a saturated state. Unless otherwise specified in this document, the oxygen used shall comply with the provisions of high purity oxygen in GB/T 14599; the hydrogen shall comply with the provisions of high purity hydrogen in GB/T 3634.2. c) Stir the test solution and keep the magnet speed at 300 r/min. d) Before using the chronopotentiometry to measure the overpotential, it should use the electrochemical impedance spectroscopy (EIS) method to test the resistance to be compensated (internal resistance); the test method shall comply with the provisions of GB/T 28817. 6.8 Test steps The electrode overpotential test steps are as follows. a) Measure the open circuit potential of the working electrode for a duration of not less than 10 minutes. When the potential fluctuation is stable within 5 mV/min, the next step of test can be carried out. b) Turn on the chronopotentiometry measurement function; measure the curve of the potential change of the oxygen evolution electrode over time at current densities of -100 A/m2 and -1000 A/m2, respectively. The sampling frequency shall be not less than 1 Hz; the test time shall be not less than 60 min. Record the potential value of the test electrode; the average value of the potential between 50 min and 60 min should be used as the working potential at the current density. the electrode overpotential is tested in the three-electrode system; the difference in the obtained overpotential is characterized as the positive and negative polarization stability. 7.2 Reagents The test solution shall comply with the provisions of 6.2. During the test, the concentration of KOH solution is maintained at 1.00 mol/L ± 0.05 mol/L by regularly replenishing water and KOH solution; KOH solution can be collected through the sampling port. 7.3 Equipment 7.3.1 The test of positive and negative polarization stability adopts two-electrode test system and three-electrode test system. The test system shall comply with the provisions of 6.3.1, but the two-electrode test system does not contain a reference electrode. 7.3.2 Electrochemical performance tester, electrolytic cell, constant temperature heating pot shall comply with the relevant provisions of 6.3. 7.4 Sample The test electrode shall comply with the provisions of 6.4. 7.5 Reference electrode and counter electrode The reference electrode shall comply with the provisions of 6.5. The counter electrode shall comply with the provisions of 6.6. 7.6 Test conditions The test conditions shall comply with the relevant provisions of 6.7. 7.7 Test steps The steps for the positive and negative polarization stability test are as follows: a) In the three-electrode test system, measure the overpotential ηi,0 of each test electrode before positive and negative polarization according to the provisions of 6.8; Note: The single-cell electrolyzer is a normal pressure electrolyzer. 8.3.4 Alkali circulation pump The flow rate of the alkali circulation pump should be 0.5 L/min. 8.3.5 Rehydration pump The flow rate of the rehydration pump is not less than 20 mL/h. 8.3.6 Gas-liquid separator The material of the gas-liquid separator is polypropylene, polytetrafluoroethylene, carbon steel nickel-plated or 316 L stainless steel. 8.4 Sample The test electrode shall meet the following requirements: a) The electrode shape is rectangular, the size is 50 mm × 40 mm, the length and width size errors are ≤ ±1 mm; the actual size of the electrode is measured with a vernier caliper; b) When the test electrode is a single hydrogen evolution electrode or a single oxygen evolution electrode, a non-coated nickel mesh, which has a basic mesh number (British system) of 46 and a wire diameter of 0.25 mm, is used as the corresponding oxygen evolution anode or hydrogen evolution electrode. The nickel mesh shall comply with the provisions of GB/T 21648; c) After cutting, the test electrode shall be kept flat; the burrs, serrations or sharp protrusions on the electrode edges shall be rounded; d) For electrodes that need to be activated, the activated electrodes shall be used; e) The number of test samples should be no less than 3 pieces. 8.5 Test conditions The test of the average voltage of the cell shall meet the following conditions: a) The test solution temperature is 85 °C ± 1 °C; b) Adjust the cathode and anode outlet valves to maintain the dynamic balance of the two-electrode gas pressure; c) During the test, water shall be added to ensure that the density of the test solution is 1.28 g/cm3 ± 0.03 g/cm3. Note: The density is the corresponding value at 25 °C. 8.6 Test steps The test steps for the average cell voltage and the average cell voltage change rate are as follows. a) Before the test electrode is installed in the electrolytic cell, the test electrode shall be cleaned according to the provisions of 5.6 a); after treatment, the mass of the electrode is weighed as mi,0, with an accuracy of 0.1 mg. b) Start preheating: 10 min before the test, turn on the constant current power supply for preheating. c) In the single-cell electrolytic cell test system, start the constant current electrolysis test, so that the electrolytic cell continues to operate at a constant current density for at least 500 h; the sampling interval shall be 30 s. Note: The current density is usually set to 3000 A/m2, 4000 A/m2, 5000 A/m2, 8000 A/m2 or 10000 A/m2. The set test current density value shall be noted in the report. d) During the test time, record the cell voltage at 70 h ~ 72 h and at (t + 70 h) ~ (t + 72 h), where t ≥ 500 h. The algebraic mean of the cell voltage during the above two periods is taken as the cell average cell voltage. e) After the electrolysis is completed, treat the test electrode after electrolysis according to the provisions of 5.6 a); weigh the mass mi of the electrode with an accuracy of 0.1 mg. 8.7 Data processing 8.7.1 Average cell voltage change rate The average voltage change rate of the cell is calculated according to formula (4): Where: vd - Average cell voltage change rate, in microvolts per hour (μV/h); t - Continued operation time after 72 hours of operation, in hours (h);Appendix A(Normative) Electrode potential calibration of reference electrode A.1 Principle A three-electrode test system is used, with high-purity Pt sheets as test electrodes and counter electrodes; the electrode to be calibrated is used as the reference electrode. During the calibration process, hydrogen is introduced into the test solution to maintain it in a saturated state; then the multi-cycle cyclic voltammetry curve is tested at a rate of 1 mV/s. The value of the electrode to be calibrated is calculated based on the potential value of the zero current in the cyclic voltammetry curve. A.2 Calibration reagents, equipment, electrodes A.2.1 Reagents shall comply with the provisions of 6.2. A.2.2 Equipment shall comply with the provisions of 6.3. A.2.3 The electrodes used in calibration shall meet the following requirements: a) The test electrode is a Pt electrode, which has a purity higher than 99.9%; the effective size of the electrode is 10 mm × 10 mm; b) The reference electrode is the electrode to be calibrated, which is a mercury/mercury oxide electrode or a saturated calomel electrode with an external salt bridge; c) The counter electrode is a Pt electrode, which has a purity higher than 99.9% and an effective size of 20 mm × 20 mm. A.3 Calibration steps The reference electrode calibration steps are as follows: a) Power on and preheat: 10 minutes before starting the test, turn on the power of the electrochemical performance tester for preheating; b) Inflation: Adjust the gas flow rate to 50 mL/min; fill the test solution with hydrogen until saturated. The hydrogen used shall meet the technical requirements of high-purity hydrogen in GB/T 3634.2; c) Constant temperature and stirring: Adjust the constant temperature heating pot; keep the constant test solution temperature at 25 °C ± 0.5 °C; adjust the magnetic rotation speed in the test solution to maintain 300 r/min; ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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