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HG/T 4823-2023: Manganese sulfate for battery materials Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid HG/T 4823: Historical versions
HG/T 4823-2023: Manganese sulfate for battery materials---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/HGT4823-2023HG CHEMICAL INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.060.50 CCS G 12 Replacing HG/T 4823-2015 Manganese sulfate for battery materials Issued on. JULY 28, 2023 Implemented on. FEBRUARY 01, 2024 Issued by. Ministry of Industry and Information Technology of PRC Table of ContentsForeword... 3 1 Scope... 5 2 Normative references... 5 3 Terms and definitions... 6 4 Molecular formula and relative molecular mass... 6 5 Classification... 6 6 Requirements... 6 7 Test method... 8 8 Inspection rules... 35 9 Marking and accompanying documents... 36 10 Packaging, transportation, storage... 36 Appendix A (Informative) Reference wavelength of analytical spectrum... 37 Appendix B (Informative) Recommended operating conditions of ion chromatograph ... 381 ScopeThis document specifies the classification, requirements, test methods, inspection rules, marking and accompanying documents, packaging, transportation, storage of manganese sulfate for batteries. This document is applicable to manganese sulfate for batteries. Note. This product is mainly used to prepare precursors for positive electrode materials of secondary lithium batteries (nickel-cobalt-manganese ternary composite hydroxides, nickel- manganese ternary hydroxides, etc.); it can also be used to manufacture other manganese salts.2 Normative referencesThe contents of the following documents constitute essential clauses of this document through normative references in the text. For dated references, only the version corresponding to that date applies to this document; for undated references, the latest version (including all amendments) applies to this document. GB/T 191-2008 Packaging - Pictorial marking for handling of goods GB/T 6003.1-2022 Test sieves - Technical requirements and testing - Part 1.Test sieves of metal wire cloth GB/T 6678 General principles for sampling chemical products GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods GB/T 8170 Rules of rounding off for numerical values and expression and judgement of limiting values HG/T 2962-2010 Manganous sulphate for industrial use HG/T 3696.1 Inorganic chemicals for industrial use - Preparations of standard and reagent solutions for chemical analysis - Part 1.Preparations of standard volumetric solutions HG/T 3696.2 Inorganic chemicals for industrial use - Preparations of standard and reagent solutions for chemical analysis - Part 2.Preparations of standard solutions for impurity3 Terms and definitionsThere are no terms and definitions that need to be defined in this document.4 Molecular formula and relative molecular massMolecular formula of solid product. MnSO4·H2O Relative molecular mass. 169.01 (according to the 2022 international relative atomic mass)5 ClassificationManganese sulfate products for batteries are divided into two categories according to the form of the product.6 Requirements6.1 Appearance. Category I is light pink white powder; Category II is light red solution. 6.2 Category I manganese sulfate solid for batteries shall comply with the provisions of Table 1, 6.3 Manganese sulfate solution for category II batteries shall comply with the requirements of Table 2, when tested according to the test method specified in this document.7 Test methodWarning. Some reagents used in this test method are corrosive, so be careful when operating! 7.1 General provisions The reagents and water used in this document, unless otherwise specified, refer to analytical reagents and grade 3 water specified in Table 1 of GB/T 6682-2008. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of HG/T 3696.1, HG/T 3696.2, HG/T 3696.3. 7.2 Appearance inspection Under natural light, place the solid product on a white-backed watch glass or white porcelain plate; place the solution product in a beaker; judge the appearance by visual inspection. 7.3 Determination of manganese sulfate content 7.3.1 Principle In an ammonia-ammonium chloride buffer solution with a pH of about 10, use chrome black T as an indicator and use disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution to titrate, until the solution changes from purple-red to pure blue, which is the end point. Calculate the manganese sulfate content based on the consumption of the standard titration solution. 7.3.2 Reagents or materials 7.3.3 Test steps 7.3.4 Test data processing 7.4 Determination of the content of iron, zinc, copper, lead, cadmium, chromium, potassium, sodium, calcium, magnesium, nickel, cobalt, aluminum 7.4.1 Principle The specimen is dissolved in nitric acid; the intensity of the characteristic spectrum of the elements to be measured (iron, zinc, copper, lead, cadmium, chromium, potassium, sodium, calcium, magnesium, nickel, cobalt, aluminum) is determined by inductively coupled plasma emission spectrometer; the working curve method is used for quantification. 7.4.2 Reagents or materials 7.4.2.1 Nitric acid solution. 1+1. Prepared with high-grade pure reagents. 7.4.3 Instruments and equipment Inductively coupled plasma emission spectrometer. 7.4.4 Test steps 7.4.5 Test data processing 7.5.1 Reagents or materials 7.5.2 Instruments and equipment Atomic absorption spectrophotometer. Equipped with a lead hollow cathode lamp. 7.5.3 Test steps 7.5.4 Test data processing 7.5.4.1 Data processing of solid specimen The lead content is calculated as the mass fraction of lead w4 according to formula (6). 7.6 Determination of chloride content 7.6.1 Spectrophotometry (arbitration method) 7.6.2 Ion chromatography 7.6.2.1 Principle The specimen is dissolved in water, separated by anion exchange column using an ion chromatograph, detected by suppressed conductivity method, quantified by external standard method (peak area/peak height). The mass concentration of chlorine is found from the working curve and its content is calculated. 7.6.2.2 Reagents or materials 7.6.2.3 Instruments and equipment 7.6.2.4 Test steps 7.6.2.5 Test data processing 7.7 Determination of water-insoluble matter content 7.7.1 Reagents or materials 7.7.2 Instruments and equipment 7.7.3 Test steps Weigh about 20 g (accurate to 0.01 g) of the specimen. Place it in a 250 mL beaker. Dissolve it in 200 mL hot water without carbon dioxide. Filter it with a glass crucible that has been dried at 105 °C ± 2 °C to a constant mass. Wash it with hot water until there is no sulfate (check with barium chloride solution). Place it in an electric constant temperature drying oven, to dry it at 105 °C ± 2 °C to a constant mass. 7.7.4 Test data processing The water-insoluble content is expressed as mass fraction w7 and is calculated according to formula (12). 7.8 pH determination 7.8.1 Instruments and equipment Acidity meter. The graduation value is 0.1 pH unit; it is equipped with pH electrode and calomel electrode. 7.8.2 Test steps Solid product. Determine according to the method specified in 5.8 of HG/T 2962-2010. Solution product. Take 50 mL of liquid specimen. Place it in a dry beaker. Determine the pH with an acidity meter. 7.9 Determination of fineness 7.9.1 Instruments and equipment Test sieve. φ200×50-0.4/0.25 GB/T 6003.1-2022, equipped with sieve cover and sieve bottom. 7.9.2 Test steps Weigh about 50 g of specimen. Place it in the test sieve. Install the sieve cover and sieve bottom. Perform manual sieving. If there is no residue on the sieve, it means that all the samples have passed. 7.10 Determination of silicon content 7.10.1 Principle The specimen is treated with sulfuric acid. The silicic acid and ammonium molybdate generate silicomolybdic heteropoly acid. Hydrofluoric acid is added to dissolve silicon and eliminate the influence of some impurities. Ammonium ferrous sulfate is used to reduce and generate silicon-molybdenum blue. The absorbance is measured at a wavelength of 810 nm on a spectrophotometer. 7.10.2 Reagents or materials 7.10.3 Instruments and equipment 7.10.4 Test steps 7.10.4.1 Drawing of working curve Pipette 0.00 mL, 1.00 mL, 2.00 mL, 4.00 mL, 8.00 mL, 12.00 mL of silicon standard solution respectively. Place in six 100 mL volumetric flasks. Add 9 mL of sulfuric acid solution respectively. Use water to dilute it to about 40 mL. Place in a 50 °C ± 2 °C constant temperature water bath. After 5 minutes, add 10 mL of ammonium molybdate solution while shaking. Use a small amount of water, to rinse the ammonium molybdate solution attached to the inner wall of the bottle. Keep warm in a 50 °C ± 2 °C constant temperature water bath for 5 minutes. Shake from time to time. Remove and cool to room temperature with running water. Add 15 mL of hydrofluoric acid solution. Mix well. Add 5 mL of ammonium ferrous sulfate solution within 30 seconds. Mix well. Use water to dilute to the mark. Let stand for 15 minutes. Transfer to a set of cuvettes. Use the blank solution as a reference, to measure its absorbance at a wavelength of 810 nm. Draw a working curve with the mass concentration of silicon (mg/L) as the abscissa and the absorbance as the ordinate. 7.10.4.2 Preparation of test solution 7.11 Determination of fluoride content 7.11.1 Fluoride ion selective electrode method (arbitration method) 7.11.1.1 Principle In the presence of a total ionic strength regulator, the fluoride ion content is determined using an ion selective electrode as the indicator electrode and a saturated calomel electrode as the reference electrode. 7.11.1.2 Reagents or materials 7.11.1.3 Instruments and equipment 7.11.1.4 Test steps 7.11.1.5 Test data processing 7.11.2 Ion chromatography 7.12 Determination of magnetic foreign matter content 7.12.1 Principle The magnetic material in the specimen is adsorbed by a magnetic rod and dissolved with aqua regia. The working curve method is used, to determine the nickel, iron, zinc chromium contents with an inductively coupled plasma emission spectrometer; the magnetic foreign matter content is obtained by calculation. 7.12.2 Reagents or materials 7.12.3 Instruments and equipment 7.13 Determination of oil content 7.13.1 Reagents or materials Warning. Perchloroethylene has irritating and anesthetic effects. When using it, it shall strictly follow the safety technical instructions. 7.13.2 Instruments and equipment Infrared spectrophotometer for oil measurement. 7.13.3 Test steps8 Inspection rules8.1 All items specified in the requirements of this document are exit-factory inspection items and shall be inspected batch by batch. 8.2 The same type and grade of manganese sulfate for batteries, which are produced continuously or by the same team using the same material, under basically the same production conditions, is considered a batch. Each batch of products shall not exceed 50 t. 8.3 The number of sampling units shall be determined in accordance with the provisions of GB/T 6678. 8.4 Use the rounded value comparison method specified in GB/T 8170, to determine whether the test results comply with this document. 8.5 If any index of the inspection results does not meet the requirements of this document, samples shall be taken from twice the amount of packaging for reinspection. Even if only one index does not meet the requirements of this document, the entire batch of products shall be unqualified.9 Marking and accompanying documents9.1 The packaging of manganese sulfate for batteries shall have firm and clear markings, including. manufacturer name, factory address, product name, type, grade, net content, batch number or production date, this document number, as well as the "Avoid rain" and "Avoid sun exposure" marks specified in GB/T 191-2008. 9.2 Each batch of manganese sulfate for batteries shall be accompanied by a quality certificate, including. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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