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HG/T 5919-2021 (HGT5919-2021)

HG/T 5919-2021_English: PDF (HGT 5919-2021, HGT5919-2021)
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BASIC DATA
Standard ID HG/T 5919-2021 (HG/T5919-2021)
Description (Translated English) (Nickel sulfate for batteries)
Sector / Industry Chemical Industry Industry Standard (Recommended)
Word Count Estimation 15,161
Date of Issue 2021-12-02
Date of Implementation 2022-04-01
Summary This standard specifies the classification, classification, requirements, test methods, inspection rules, signs, labels, packaging, transportation and storage of nickel sulfate for batteries. This standard applies to nickel sulfate for batteries.

Standards related to: HG/T 5919-2021

HG/T 5919-2021
HG
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
CCS G 12
Nickel sulfate for battery materials
ISSUED ON: DECEMBER 02, 2021
IMPLEMENTED ON: APRIL 01, 2022
Issued by: Ministry of Industry and Information Technology of the People's
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Molecular formula and relative molecular mass ... 5
5 Classification ... 5
6 Requirements ... 5
7 Test methods ... 6
8 Inspection rules ... 17
9 Marks, labels ... 18
10 Packaging, transportation, storage ... 18
Nickel sulfate for battery materials
1 Scope
This document specifies the classification, requirements, test methods, inspection rules,
marks, labels, packaging, transportation, storage of nickel sulfate for battery materials.
This document applies to nickel sulfate for battery materials.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 191, Packaging and storage marks
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 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
HG/T 3696.3, Inorganic chemicals for industrial use. Preparations of standard and
reagent solutions for chemical analysis. Part 3: Preparations of reagent solutions
3 Terms and definitions
This document does not have terms and definitions that need to be defined.
4 Molecular formula and relative molecular mass
Molecular formula: NiSO4•6H2O
Relative molecular mass: 262.86 (according to the international relative atomic mass in
2018)
5 Classification
Nickel sulfate for battery materials is divided into two categories: solid type and
solution type.
Solid nickel sulfate for battery materials is divided into Type I and Type II according to
product use:
- Type I is for ternary battery materials;
- Type II is for other battery materials.
6 Requirements
6.1 Appearance: The solid is emerald, green granular crystal. The solution is green
transparent liquid.
6.2 Nickel sulfate for battery materials shall be tested according to the test methods
specified in this document and shall meet the requirements in Table 1.
7.3.1 Weight method (arbitration method)
7.3.1.1 Principle
In the ammonia solution, add tartaric acid to form a soluble complex with impurities
such as iron and aluminum to eliminate interference. Dimethylglyoxalxime nickel
precipitates with red color from dimethylglyoxalxime and nickel. Filter. Wash. Weigh
after drying. Calculate the nickel content.
7.3.1.2 Reagents or materials
7.3.1.2.1 Ethanol solution: 1+4.
7.3.1.2.2 Hydrochloric acid solution: 1+1.
7.3.1.2.3 Ammonia solution: 1+1.
7.3.1.2.4 Ammonium chloride solution: 200 g/L.
7.3.1.2.5 Tartaric acid solution: 200 g/L.
7.3.1.2.6 Ethanol solution of dimethylglyoxalxime: 10 g/L.
7.3.1.3 Instruments and equipment
7.3.1.3.1 Glass sand crucible: filter plate pore size is 5 μm ~ 15 μm.
7.3.1.3.2 Electric constant temperature drying oven: the temperature can be controlled
at 105°C ± 2°C.
7.3.1.4 Test steps
Weigh an appropriate amount of specimen (about 2.0 g for solid product, about 5.0 g
for solution product) (accurate to 0.0002 g). Place in a 250 mL beaker. Add 1 mL of
hydrochloric acid solution and 50 mL of water. The solid specimen is heated until the
sample is dissolved. Cool to room temperature. Transfer completely to a 100 mL
volumetric flask. Use water to dilute to the scale. Shake well.
Use a pipette to pipette 10 mL of the test solution. Place in a 400 mL beaker. Add 150
mL of water, 5 mL of ammonium chloride solution and 5 mL of tartaric acid solution.
Cover with a watch glass. Heat to boiling. When cooling to 70°C~80°C, slowly add 30
mL of dimethylglyoxalxime ethanol solution under continuous stirring. Add dropwise
ammonia solution to adjust the pH of the solution to be 8 ~ 9 (use precision pH test
paper to test). Exceed by 1 mL ~ 2 mL. Incubate at 70°C~80°C for 30 min. Use a glass
sand crucible that has been dried at 105°C ± 2°C to a constant mass to filter. Use ethanol
solution to wash 4~5 times. Dry at 105°C ± 2°C until the mass is constant.
7.3.1.5 Test data processing
0.996 - the coefficient to convert cobalt to nickel.
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between the two parallel determination results is not
more than 0.1%.
7.4 Determination of cobalt, copper, iron, manganese, zinc, calcium, magnesium,
chromium, cadmium and lead content
7.4.1 Principle
In nitric acid medium, use the standard curve method and inductively-coupled plasma
optical emission spectrometer to determine the contents of the analyte elements.
7.4.2 Reagents or materials
7.4.2.1 Nitric acid solution: 1+1.
7.4.2.2 Nickel matrix solution: ρ(Ni)≈20 g/L. The mass fractions of cobalt, copper, iron,
manganese, zinc, calcium, magnesium, chromium, cadmium, lead, and sodium are not
greater than 0.0002%.
Weigh about 20 g of metallic nickel (nickel mass fraction is not less than 99.99%)
(accurate to 0.01 g). Place in a 400 mL beaker. Add a little water to moisten. Slowly
add 150 mL of nitric acid solution. Heat till all is dissolved. Cool to room temperature.
Transfer into a 1000 mL volumetric flask. Use water to dilute to the scale. Shake well.
7.4.2.3 Mixed standard solution: 1 mL contains 0.01 mg each of cobalt, copper, iron,
manganese, zinc, calcium, magnesium, chromium and cadmium, and 0.05 mg of lead.
Respectively pipette 1 mL of cobalt, copper, iron, manganese, zinc, calcium,
magnesium, chromium, cadmium standard solutions prepared according to HG/T
3696.2 and 5 mL of lead standard solution prepared according to HG/T 3696.2. Place
them in the same 100 mL volumetric flask. Use water to dilute to the scale. Shake well.
Prepare this solution when it is needed.
7.4.2.4 Water: grade two water specified in GB/T 6682-2008.
7.4.3 Instruments and equipment
Inductively-coupled plasma optical emission spectrometer.
7.4.4 Test steps
7.4.4.1 Drawing of standard curve
Pipette 0.00 mL, 0.50 mL, 1.00 mL, 2.00 mL, 4.00 mL, 8.00 mL of mixed standard
solutions respectively. Place in six 100 mL volumetric flasks. Add 10 mL of nickel
matrix solution and 2 mL of nitric acid solution respectively. Use water to dilute to the
m - The value of the mass of the test material, in grams (g).
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between two parallel determination results is not more
than 20% of the arithmetic mean.
7.5 Determination of sodium content
7.5.1 Principle
In nitric acid medium, use the standard curve method and inductively-coupled plasma
optical emission spectrometer to determine the sodium content.
7.5.2 Reagents or materials
7.5.2.1 Nitric acid solution: 1+1.
7.5.2.2 Sodium standard solution: 1 mL of solution contains 0.01 mg of sodium (Na).
Use a pipette to pipette 1 mL of sodium standard solution prepared according to HG/T
3696.2. Place in a 100 mL volumetric flask. Use water to dilute to the scale. Shake well.
Prepare this solution when it is needed.
7.5.2.3 Water: grade two water specified in GB/T 6682-2008.
7.5.3 Instruments and equipment
Inductively-coupled plasma optical emission spectrometer.
7.5.4 Test steps
7.5.4.1 Drawing of standard curve
Pipette 0.00 mL, 0.50 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL of sodium
standard solution respectively. Place in seven 100 mL volumetric flasks. Add 10 mL of
nickel matrix solution (see 7.4.2.2) and 2 mL of nitric acid solution respectively. Use
water to dilute to the scale. Shake well.
Tune the inductively-coupled plasma optical emission spectrometer to the optimal
working conditions. Zero with standard blank solution. Determine the spectral intensity
of the standard solution at a wavelength of 589.592 nm. Draw the standard curve with
the mass of sodium (mg) as the abscissa and the corresponding spectral intensity as the
ordinate.
7.5.4.2 Test
Weigh an appropriate amount of specimen (about 1.0 g for solid product, about 2.0 g
for solution product) (accurate to 0.0002 g). Place in a 100 mL beaker. Add appropriate
amount of water. Stir to dissolve all. Add 2 mL of nitric acid solution. Transfer all to a
100 mL volumetric flask. Add water to the scale. Shake well. Use a pipette to pipette
10 mL of the above test solution. Place in a 100 mL volumetric flask. Use water to dilute
to the scale. Shake well.
Determine the spectral intensity of sodium element in the test solution. Find out the
corresponding sodium mass from the standard curve according to the measured spectral
intensity.
7.5.5 Test data processing
Sodium content is calculated as the mass fraction w2 of sodium (Na). Calculate
according to formula (4):
Where,
m1 - the value of the mass of sodium in the test solution detected from the standard
curve, in milligrams (mg);
m - the value of the mass of the test material, in grams (g).
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between two parallel determination results is not more
than 10% of the arithmetic mean.
7.6 Determination of water-insoluble content
7.6.1 Principle
The specimen is dissolved in water. After filtering and washing, dry it to constant mass.
Determine the water-insoluble content based on the amount of residue after drying.
7.6.2 Instruments and equipment
7.6.2.1 Glass sand crucible: filter plate pore size is 5 μm ~ 15 μm.
7.6.2.2 Electric constant temperature drying oven: the temperature can be controlled at
105°C ± 2°C.
7.6.3 Analysis steps
Weigh about 50 g of specimen (accurate to 0.01 g). Place it in a 400 mL beaker. Add
200 mL of water. Heat and stir to dissolve. After cooling to room temperature, use a
glass sand crucible that has been dried at 105°C ± 2°C to a constant mass for suction-
filtration. After fully washing with hot water, place the glass sand crucible in an electric
heating constant temperature drying oven at 105°C ± 2°C. Dry to constant mass.
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between two parallel determination results is not more
than 10% of the arithmetic mean.
7.8 Determination of oil content
7.8.1 Reagents or materials
7.8.1.1 Tetrachlorethylene.
7.8.1.2 Anhydrous sodium sulfate.
7.8.2 Instruments and equipment
Infrared spectrophotometer.
7.8.3 Test steps
Weigh about 10 g of specimen (accurate to 0.01 g). Put it in a 200 mL beaker. Add 20
mL of water. Heat the solid sample to dissolve it completely. After cooling, transfer all
to a separatory funnel. Pipette 20 mL of tetrachlorethylene. Extract for 1 min. Let stand
to layer. Put all the organic phase into the dehydration column that has been added with
1 cm ~ 2 cm thick anhydrous sodium sulfate. After dehydration, transfer to a 25 mL
colorimetric tube. Cover and set aside.
Adjust the infrared spectrophotometer to the best working condition. Determine
according to the instrument operation process. Input the mass of the specimen, the exact
volume of tetrachlorethylene. Read the oil content in the specimen from the instrument.
Take the arithmetic mean of the parallel determination results as the determination
result. The absolute difference between two parallel determination results is not more
than 10% of the arithmetic mean.
8 Inspection rules
8.1 All indicator items specified in this document are exit-factory inspection items.
They shall be inspected batch by batch.
8.2 Nickel sulfate for battery materials of the same type and model produced by the
production enterprise with the same material, basically the same production conditions,
under continuous production or production by the same team are a batch. Each batch of
products shall not exceed 40 t.
8.3 Determine the number of sampling units according to the provisions of GB/T 6678.
When sampling solid products, insert the sampler vertically from the center of the bag
to 3/4 of the depth of the material layer for sampling. Mix the collected samples. Divide
by quartering method to not less than 1500 g. Subpack into two clean, dry containers.
Seal. When sampling the solution product, insert the sampling glass tube to 2/3 of the
depth of the container for sampling. Mix the collected samples. The total amount is not
less than 1500 mL. Subpack into two clean, dry plastic bottles. Seal. Paste the label,
indicating the name of the manufacturer, product name, category, model, batch number,
sampling date and the name of the sampling personnel. One is for inspection. The other
is stored for future reference. The storage time is determined according to the needs of
the manufacturer.
8.4 If any indicators of the inspection results do not meet the requirements of this
document, samples shall be taken from twice the amount of packaging for re-inspection.
Even if only one indicator fails to meet the requirements of this document in the re-
inspection results, the entire batch of products is considered unqualified.
8.5 Use the rounded value comparison method specified in GB/T 8170 to judge whether
the test results conform to this document.
9 Marks, labels
9.1 There shall be a firm and clear mark on the packaging bag of nickel sulfate for
battery materials. The mark shall indicate manufacturer name, factory address, product
name, category, model, net content, batch number or date of production, shelf life,
reference to this document and the marks of "be afraid of rain" and "be afraid of sun"
stipulated in Chapter 2 of GB/T 191-2008.
9.2 Each batch of nickel sulfate for battery materials shall be accompanied by a quality
certificate, indicating manufacturer name, factory address, product name, category,
model, net content, batch number or production date, and reference to this document.
10 Packaging, transportation, storage
10.1 The solid product of nickel sulfate for battery materials is double-packed. Inner
packaging is polyethylene plastic film bag. The outer packaging is a plastic woven bag.
The inner bag of the package is tied with vinylon rope or other ropes of equivalent
quality. Or seal in another equivalent method. Outer pockets are machine-sewn. The
stitching is secure with no leaks or jumpers. The net content of each bag is 25 kg. It can
also be packed according to the specifications required by users. Nickel sulfate solution
products for battery materials are packaged in special tank cars or polyethylene barrels.
The net content of each barrel is 1000 kg. It can also be packed according to the
specifications required by users.
10.2 Nickel sulfate for battery materials shall be protected from rain, heat and moisture
during transportation.
10.3 Nickel sulfate for battery materials shall be stored in a ventilated, cool and dry
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