HG/T 4823-2023 PDF English
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| HG/T 4823-2023 | English | 460 |
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Manganese sulfate for battery materials
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| HG/T 4823-2015 | English | 140 |
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Manganese sulfate for battery materials
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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/HGT4823-2023
HG
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 Contents
Foreword... 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
... 38
1 Scope
This 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 references
The 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 impurity
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Molecular formula and relative molecular mass
Molecular formula of solid product. MnSO4·H2O
Relative molecular mass. 169.01 (according to the 2022 international relative atomic
mass)
5 Classification
Manganese sulfate products for batteries are divided into two categories according to
the form of the product.
6 Requirements
6.1 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 method
Warning. 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 steps
8 Inspection rules
8.1 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 documents
9.1 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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