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HG/T 5919-2021 English PDF (HGT5919-2021)

HG/T 5919-2021 English PDF (HGT5919-2021)

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HG/T 5919-2021: Nickel sulfate for battery materials

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.
HG/T 5919-2021
HG
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE 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 ??m ~ 15 ??m.
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: ??(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 ??m ~ 15 ??m.
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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