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HG/T 4823-2015 (HGT 4823-2015)

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BASIC DATA
Standard ID HG/T 4823-2015 (HG/T4823-2015)
Description (Translated English) Manganese sulfate for battery materials
Sector / Industry Chemical Industry Industry Standard (Recommended)
Classification of Chinese Standard G12
Classification of International Standard 71.060.50
Word Count Estimation 11,126
Date of Issue 2015-07-14
Date of Implementation 2016-01-01
Quoted Standard GB/T 191-2008; GB/T 6003.1-2012; GB/T 6678; GB/T 6682-2008; GB/T 8170; GB/T 8946; HG/T 2962-2010; HG/T 3696.1; HG/T 3696.2; HG/T 3696.3
Drafting Organization Guizhou Dalong Huicheng New Material Co., Ltd
Administrative Organization National Chemical Standardization Technical Committee of Inorganic Chemical Sub - Technical Committee
Regulation (derived from) PRC MIIT Announcement (2015 No.49)
Summary This Standard specifies the batteries with manganese sulfate requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage. This Standard applies to batteries with manganese sulfate. This product is mainly used for the preparation of a secondary lithium battery cathode materials (nickel, cobalt and manganese lithium, lithium manganese oxide, lithium-rich manganese-based cathode materials and other products), it can also be used in the manufacture of other manganese salts.


HG/T 4823-2015: PDF in English (HGT 4823-2015)
HG/T 4823-2015
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Registration number: 50865-2015
Manganese sulfate for battery materials
ISSUED ON: JULY 29, 2015
IMPLEMENTED ON: JANUARY 01, 2016
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Molecular formula and relative molecular mass ... 5 
4 Requirements ... 5 
5 Test methods ... 6 
6 Inspection rules ... 15 
7 Markings, labels ... 16 
8 Packaging, transportation and storage ... 16 
Appendix A (Informative) Reference wavelength of analytical spectral line ... 18 
Manganese sulfate for battery materials
1 Scope
This standard specifies the requirements, test methods, inspection rules,
marking, labeling, packaging, transportation and storage of manganese sulfate
for battery materials.
This standard applies to manganese sulfate for battery materials. This product
is mainly used to prepare the positive electrode materials for secondary lithium
battery (nickel-cobalt lithium manganate, lithium manganate, lithium-rich
manganese-based cathode materials, etc.), which can also be used to make
other manganese salts.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 191-2008 Packaging - Pictorial marking for handling of goods
GB/T 6003.1-2012 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 & expression and
judgement of limiting values
GB/T 8946 General technical requirements of plastic woven sack
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
5 Test methods
Warning: Some of the reagents used in this test method are corrosive and
should be handled with care! If it is splashed on the skin or eyes, rinse
immediately with water. In severe cases, seek medical attention
immediately. The high-pressure hydrogen cylinder used in this test
method shall be operated in accordance with the safe operation of high-
pressure steel cylinders. After igniting the plasma, the screen door shall
be opened as little as possible, to prevent high-frequency radiation from
harming the body.
5.1 General provisions
The reagents and water used in this standard, unless otherwise specified, refer
to analytical pure reagents and grade-3 water as specified in GB/T 6682-2008.
The standard titration solution, preparations and products used in the tests are
prepared in accordance with HG/T 3696.1, HG/T 3696.2, HG/T 3696.3, unless
otherwise specified.
5.2 Appearance inspection
In natural light, use the visual observation method to judge the appearance on
a white-backgrounded watch glass or white porcelain.
5.3 Determination of manganese sulfate content
5.3.1 Summary of method
In an ammonia-ammonium chloride buffer solution which has a pH of about 10,
use the chrome black T as an indicator. Use the ethylenediaminetetraacetic acid
disodium (EDTA) standard titration solution to titrate the solution until it changes
from purple-red into pure blue, which is the end point. Based on the
consumption of the titration solution, calculate the manganese sulfate content.
5.3.2 Reagents
5.3.2.1 Ascorbic acid.
5.3.2.2 Ammonia-ammonium chloride buffer solution A: pH ≈ 10.
5.3.2.3 Ethylenediaminetetraacetic acid disodium standard titration solution: c
(EDTA) ≈ 0.05 mol/L.
5.3.2.4 Chrome black T indicator solution: 5 g/L.
5.3.3 Analytical procedures
determination result. When calculated by manganese sulfate (MnSO4 • H2O),
the absolute difference of the results of the two parallel determinations is not
more than 0.5%. When calculated by manganese (Mn), the absolute difference
of the results of the two parallel determinations is not more than 0.2%.
5.4 Determination of iron, zinc, copper, cadmium, potassium, sodium,
calcium, magnesium, nickel, cobalt content
5.4.1 Summary of method
The specimen is dissolved by nitric acid. The inductively coupled plasma optical
emission spectrometry is used to determine the tested elements (iron, zinc,
copper, cadmium, potassium, sodium, calcium, magnesium, nickel, cobalt). The
working curve method is used for quantification.
5.4.2 Reagents
5.4.2.1 Nitric acid solution: 1 + 1.
5.4.2.2 Nitric acid solution: 2 + 98.
5.4.2.3 Mixed standard solution I: 1 mL of solution contains 0.010 mg of cation
(iron, zinc, copper, cadmium, nickel, cobalt).
Respectively, pipette 1.00 mL of iron (Fe), Zinc (Zn), Copper (Cu), Cadmium
(Cd), Nickel (Ni), Cobalt (Co) standard stock solution which are prepared
according to HG/T 3696.2. Place them in 100 mL volumetric flasks. Use the
nitric acid solution (see 5.4.2.2) to dilute it to the mark. Shake it uniformly. It may
also use the solution of the national standard substance with certificate for
accurate dilution. This solution is prepared before use.
5.4.2.4 Mixed standard solution II: 1 mL of solution contains 0.050 mg of cations
(potassium, sodium, calcium, magnesium).
Respectively, pipette 5.00 mL of Potassium (K), Sodium (Na), calcium (Ca),
Magnesium (Mg) standard stock solution which are prepared according to HG/T
3696.2. Place them in 100 mL volumetric flasks. Use the nitric acid solution (see
5.4.2.2) to dilute it to the mark. Shake it uniformly. It may also use the solution
of the national standard substance with certificate for accurate dilution. This
solution is prepared before use.
5.4.2.5 Water: It complies with the specifications of grade-2 water of GB/T 6682-
2008.
5.4.3 Instruments and equipment
Inductively coupled plasma optical emission spectrometer.
5.4.4 Analytical procedures
5.4.4.1 Preparation of test solution
Weigh about 1.0 g of the specimen, accurate to 0.0002 g. Place it into a 100
mL beaker. Use a small amount of water to wet it. Add 2 mL of nitric acid solution
(see 5.4.2.1). Cover the watch glass. On a pressure-regulated electric furnace,
use low-temperature to heat to evaporate it almost dry. After cooling it down,
add a small amount of water to dissolve it. Rinse the solution into a 100 mL
volumetric flask. Use water to dilute it to the mark. Shake it uniformly. According
to the conditions of samples and instruments, dilute it if necessary.
5.4.4.2 Drawing of working curve
Take four 100 mL volumetric flasks. Respectively, add 0.00 mL, 1.00 mL, 2.00
mL, 6.00 mL of mixed standard solution I. Use the nitric acid solution (see
5.4.2.2) to the dilute it to the mark. Shake it uniformly. This solution is used to
determine the content of iron, zinc, copper, cadmium, nickel, cobalt.
Take four 100 mL volumetric flasks. Respectively, add 0.00 mL, 0.50 mL, 2.00
mL, 3.00 mL of mixed standard solution II. Use the nitric acid solution (see
5.4.2.2) to the dilute it to the mark. Shake it uniformly. This solution is used to
determine the content of potassium, sodium, calcium, magnesium.
Under the optimal determination conditions of the inductively coupled plasma
optical emission spectrometry, lead the above series of standard solution into
the inductively coupled plasma optical emission spectrometry. The wavelength
of the analytical spectrum is as shown in Appendix A (or otherwise selected
according to the instrument’s instruction manual). Determine the spectral
intensity of each tested element. Use the mass concentration of the standard
solution (μg/mL) as the abscissa and the corresponding emission intensity as
the ordinate, to draw the working curve.
5.4.4.3 Determination
Under the same conditions as in 5.4.4.2, determine the spectral intensity of
each element to be tested in the test solution. Use the working curve to obtain
the mass concentration of the element to be tested.
5.4.5 Calculation of results
The content of the element to be tested is calculated by the mass fraction w3 of
the element to be tested, which is calculated according to formula (3):
Where:
Use water to dilute it to 100 mL. Use sodium hydroxide solution to adjust the
pH of solution o 1.0 ~ 1.5 (use precision pH test paper to check it). Transfer this
solution into a 250 mL separatory funnel. Use water to dilute it to about 200 mL.
Add 2 mL of Pyrrolidine dithiocarbamate (APDC) solution. Mix it. Use
trichloromethane to extract it for two times. Add 20 mL for each extraction.
Collect the extract (that is, the organic phase) into a 50 mL beak......