HG/T 5918-2021 PDF English
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Cobalt sulfate for battery materials
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HG/T 5918-2021: PDF in English (HGT 5918-2021) HG/T 5918-2021
HG
CHEMICAL INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
CCS G 12
Cobalt sulfate for battery materials
ISSUED ON: DECEMBER 02, 2021
IMPLEMENTED ON: APRIL 01, 2022
Issued by: Ministry of Industry and Information Technology of PRC
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 Categories ... 5
6 Requirements ... 5
7 Test methods ... 6
8 Inspection rules ... 19
9 Signs, labels ... 20
10 Packaging, transportation, storage ... 20
Cobalt sulfate for battery materials
1 Scope
This document specifies the classification, requirements, test methods, inspection rules,
signs, labels, packaging, transportation, storage of cobalt sulfate for batteries.
This document applies to cobalt sulfate for batteries.
2 Normative references
The contents of the following documents constitute essential provisions of this
document through normative references in the text. Among them, for dated reference
documents, only the version corresponding to the date applies to this document; for
undated reference documents, the latest version (including all amendments) applies to
this document.
GB/T 191-2008 Packaging - Pictorial marking for handling of goods
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
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
There are no terms or definitions to be defined in this document.
7 Test methods
Warning: Some of the reagents used in this test method are corrosive, so be careful
when operating! If necessary, perform it in a fume hood. If it splashes on your skin
or eyes, rinse with water immediately. In severe cases, seek medical attention
immediately.
7.1 General provisions
The reagents and water used in this document, unless otherwise specified, refer to
analytically pure reagents and grade-three water specified in Table 1 of GB/T 6682-
2008. The standard titration solutions, impurity standard solutions, preparations,
products used in the test shall be prepared, in accordance with the provisions of HG/T
3696.1, HG/T 3696.2, HG/T 3696.3, unless otherwise specified.
7.2 Appearance inspection
Under natural light, the appearance of the solid cobalt sulfate for batteries is visually
determined, on a watch glass or white porcelain plate with a white substrate. The cobalt
sulfate solution for batteries is placed in a colorimetric tube and visually determined on
a white porcelain plate.
7.3 Determination of cobalt content
7.3.1 Potentiometric titration method (arbitration method)
7.3.1.1 Principle
In an ammoniacal solution, potassium ferricyanide is used to oxidize Co2+ to Co3+; the
excess potassium ferricyanide is titrated with cobalt standard titration solution.
The reaction equation is as follows:
7.3.1.2 Reagents or materials
7.3.1.2.1 Ammonium chloride.
7.3.1.2.2 Ammonia-ammonium citrate mixed solution.
Weigh 50 g of ammonium citrate. Dissolve it in water. A dd 350 mL of ammonia water.
Use water to dilute it to 1000 mL. Mix well.
7.3.1.2.3 Cobalt standard titration solution: ρ (Co) = 3 g/L.
Weigh 3.000 g of metallic cobalt (cobalt mass fraction is not less than 99.98%) (accurate
to 0.0002 g). Place it in a 400 mL beaker. Add a small amount of water to moisten it.
Slowly add 30 mL of nitric acid solution (1 + 1). Heat until it is completely dissolved.
After cooling to room temperature, transfer the entire volume into a 1000 mL
volumetric flask. Use water to dilute it to the mark. Mix well.
7.3.1.2.4 Potassium ferricyanide standard titration solution: c(K3[Fe(CN)6])≈0.05
mol/L.
Follow the following steps for preparation, calibration, test data processing:
a) Preparation: Weigh about 17 g of potassium ferricyanide. Dissolve it in water.
Filter it. Use water to dilute it to 1000 mL. Shake well.
b) Calibration: Use a pipette to transfer 20 mL of potassium ferricyanide solution.
Place it in a 250 mL beaker. Add 5 g of ammonium chloride and 80 mL of
ammonia-ammonium citrate mixed solution. Stir on a magnetic stirrer. On the
adjusted automatic potentiometric titrator, use the platinum electrode as the
indicator electrode and the tungsten electrode as the reference electrode; use
cobalt standard titration solution to make titration, to the sudden jump end point.
c) Test data processing: The concentration of potassium ferricyanide standard
titration solution is measured in c; the value is expressed in moles per liter (mol/L).
Make calculation in accordance with formula (1):
Where:
V1 - The value of the volume of the cobalt standard titration solution, which is
consumed by the titration test solution, in milliliters (mL);
ρ - The exact value of the mass concentration of the cobalt standard titration solution,
in grams per liter (g/L);
V - The value of the volume of the potassium ferricyanide standard titration solution
pipetted, in milliliters (mL);
M - The numerical value of the molar mass of cobalt (Co), in grams per mole (g/mol)
(M = 58.93).
If two people do three parallel measurements at the same time, the ratio -- of the range
of each person's three parallel measurements TO the average -- shall not be greater than
0.2%; the ratio -- of the difference between the average of two people's measurements
TO the average result of two people -- shall not be greater than 0.2%. The result takes
the average value. The concentration value is taken to 4 significant figures.
greater than 0.1%.
7.3.2 EDTA titration method
7.3.2.1 Principle
At around pH 5.5, using hexamethylenetetramine as buffer, xylenol orange and
malachite green as indicators, use disodium ethylenediaminetetraacetate (EDTA)
standard titration solution to make titration, until the solution changes from purple blue
to bright green, which is taken as the end point.
7.3.2.2 Reagents or materials
7.3.2.2.1 p-Nitrophenol.
7.3.2.2.2 Hexamethylenetetramine.
7.3.2.2.3 Hydrochloric acid solution: 1 + 1.
7.3.2.2.4 Ammonia solution: 1 + 1.
7.3.2.2.5 Disodium ethylenediaminetetraacetate (EDTA) standard titration solution: c
(EDTA) ≈ 0.05 mol/L.
7.3.2.2.6 Xylenol orange indicator liquid: 2 g/L.
7.3.2.2.7 Malachite green solution: 2 g/L.
7.3.2.3 Test procedures
Weigh an appropriate amount of specimen (about 3.0 g of solid product, about 7.5 g of
solution product) (accurate to 0.0002 g). Place it in a 150 mL beaker. Add a small
amount of water. Boil the solid sample to dissolve it. After cooling, transfer everything
to a 250 mL volumetric flask. Use water to dilute it to the mark. Shake well.
Use a pipette to transfer 25 mL of the test solution. Place it in a 500 mL conical flask.
Add water to approximately 200 mL. Add 1 ~ 2 drops of p-nitrophenol. Use ammonia
solution to make adjustment, until the solution turns yellow green. Then use
hydrochloric acid solution to make adjustment, until the yellow green color disappears.
Add another 6 drops. Then add 1.0 g ~ 2.0 g of hexamethylenetetramine. Heat until it
is slightly boiling. Add 4 ~ 6 drops of xylenol orange indicator solution and 1 ~ 2 drops
of malachite green solution. Immediately use disodium ethylenediaminetetraacetate
(EDTA) standard titration solution to make titration, until the solution turns from purple
blue to bright green, which is taken as the end point.
At the same time, do the same blank test. Except that no specimen is added to the blank
test solution, the types and amounts of other reagents added (except the standard
titration solution) are the same as the test solution.
7.3.2.4 Test data processing
The cobalt content is calculated as the mass fraction w1 of cobalt (Co), which is
calculated according to formula (3):
Where:
V - The volume of disodium ethylenediaminetetraacetate (EDTA) standard titration
solution, which is consumed by the titration test solution, in milliliters (mL);
V0 - The volume of disodium ethylenediaminetetraacetate (EDTA) standard titration
solution, which is consumed by titrating the blank test solution, in milliliters (mL);
c - The exact value of the concentration of disodium ethylenediaminetetraacetate
(EDTA) standard titration solution, in moles per liter (mol/L);
M - The numerical value of the molar mass of cobalt (Co), in grams per mole (g/mol)
(M = 58.93);
m - The numerical value of the mass of the sample, in grams (g).
Take the arithmetic mean of the parallel measurement results as the measurement result.
The absolute difference between the two parallel measurement results shall not be
greater than 0.1%.
7.4 Determination of water-insoluble matter content
7.4.1 Principle
The specimen is dissolved in water. After filtering and rinsing, it is dried until the mass
is constant. The water-insoluble matter content is determined, based on the amount of
residue after drying.
7.4.2 Instruments and equipment
7.4.2.1 Glass sand crucible: Filter plate pore size is 5 μm ~ 15 μm.
7.4.2.2 Electric constant temperature drying oven: The temperature can be controlled at
105 °C ± 2 °C.
7.4.3 Analytical procedures
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. Boil to dissolve it. After cooling to room temperature,
use a glass sand crucible that has been previously dried at 105 °C ± 2 °C to a constant
7.6.2.3 Water: Grade-II water in compliance with Table 1 of GB/T 6682-2008.
7.6.3 Instruments and equipment
Atomic absorption spectrophotometer: It is equipped with lead hollow cathode lamp.
7.6.4 Test procedures
7.6.4.1 Drawing of standard curve
Use a pipette to transfer 0.00 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.00 mL, 4.00 mL of
lead standard solutions, respectively. Place it in six 100 mL volumetric flasks. Add 25
mL of cobalt matrix solution (see 7.5.2.2) and 2 mL of nitric acid solution to each. Use
water to dilute it to the mark. Shake well.
Adjust the atomic absorption spectrophotometer to the best working conditions. Use
the standard blank solution to zero it. Measure the absorbance of the standard solution,
at a wavelength of 283.3 nm. Draw a standard curve, using the mass of lead (mg) as the
abscissa and the corresponding absorbance as the ordinate.
7.6.4.2 Test
Weigh about 2.5 g of the specimen (accurate to 0.0002 g). Place it in a 100 mL beaker.
Add an appropriate amount of water. Boil the solid sample to dissolve it. After cooling,
add 2 mL of nitric acid solution. Transfer the entire volume to a 100 mL volumetric
flask. Add water to the mark. Shake well.
Measure the absorbance of the lead element in this test solution, on an atomic
absorption spectrophotometer. Find out the corresponding mass of lead from the
standard curve, based on the measured absorbance.
7.6.5 Test data processing
The lead content is measured as the mass fraction w3 of lead (Pb), which is calculated
according to formula (6):
Where:
m1 - The value of the mass of lead in the test solution as found from the standard
curve, in milligrams (mg);
m - The numerical value of the mass of the sample, in grams (g).
Take the arithmetic mean of the parallel measurement results as the measurement result.
The absolute difference between the two parallel measurement results shall not be
greater than 10% of the arithmetic mean.
7.7 Determination of sodium content
7.7.1 Principle
In nitric acid medium, the sodium content is determined by an inductively coupled
plasma optical emission spectrometer, using the standard curve method.
7.7.2 Reagents or materials
7.7.2.1 Nitric acid solution: 1 + 1.
It is prepared with superior grade pure reagents.
7.7.2.2 Sodium standard solution: 1 mL of solution contains 0.01 mg of sodium (Na).
Use a pipette to transfer 1 mL of the sodium standard solution, which is prepared
according to the requirements of HG/T 3696.2. Place it in a 100 mL volumetric flask.
Use water to dilute it to the mark. Shake well. Prepare this solution before use. The
solution shall be stored in polyethylene plastic bottles.
7.7.2.3 Water: Grade-II water compliant with Table 1 of GB/T 6682-2008.
7.7.3 Instruments and equipment
Inductively coupled plasma optical emission spectrometer.
7.7.4 Test procedures
7.7.4.1 Drawing of standard curve
Use a pipette to transfer 0.00 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.00 mL, 4.00 mL of
sodium standard solutions, respectively. Place them into six 100 mL volumetric flasks.
Add an appropriate amount of cobalt matrix solution to each (solid product 2.00 mL,
solution product 0.20 mL) (see 7.5.2.2) and 2 mL of nitric acid solution. Use water to
dilute it to the mark. Shake well.
Adjust the inductively coupled plasma emission spectrometer to the optimal working
conditions. Use a standard blank solution to zero it. Measure the spectral intensity of
the standard solution, at a wavelength of 589.592 nm. Draw a standard curve, using the
mass of sodium (mg) as the abscissa and the corresponding spectral intensity as the
ordinate.
7.7.4.2 Test
Use a pipette to transfer an appropriate amount of test solution (see 7.5.4.2) (20.00 mL
for solid product, 2.00 mL for solution product). Place it in a 100 mL volumetric flask.
standard curve, in milligrams (mg)
m - The numerical value of the mass of the sample, in grams (g).
Take the arithmetic mean of the parallel measurement results as the measurement result.
The absolute difference between the two parallel measurement results shall not be
greater than 10% of the arithmetic mean.
7.9 Determination of oil content
7.9.1 Reagents or materials
7.9.1.1 Tetrachlorethylene.
7.9.1.2 Anhydrous sodium sulfate.
7.9.2 Instruments and equipment
Infrared spectrophotometer.
7.9.3 Test procedures
Weigh about 10 g of specimen (accurate to 0.01 g). Place it in a 200 mL beaker. Add 20
mL of water. Boil the solid sample to dissolve it. After cooling, move everything into a
separatory funnel. Use a pipette to transfer 20 mL of tetrachlorethylene. Extract for 1
minute. Let it stand for stratification. Pour it all into a dehydration column, which has
a thickness of 1 cm ~ 2 cm anhydrous sodium sulfate. Dehydrate it into a 25 mL
colorimetric tube. Cover with lid and set aside.
Adjust the infrared spectroscopic oil meter to the best working conditions. Make
measurement according to the instrument operating procedure. Input the mass of the
specimen and the accurate volume of tetrachlorethylene. Read the oil content in the
specimen directly from the instrument.
Take the arithmetic mean of the parallel measurement results as the measurement result.
The absolute difference between the two parallel measurement results shall not be
greater than 10% of the arithmetic mean.
8 Inspection rules
8.1 All indicator items specified in this document are exit-factory inspection items and
shall be inspected batch by batch.
8.2 Cobalt sulfate for batteries of the same category and model, which is produced by
the manufacturer using the same materials and basically the same production conditions,
in continuous production or by the same shift, forms one 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 to take sample. Mix the sample taken out
uniformly. Use the quartering method to reduce it to not less than 1500 g. Divide it into
two clean dry containers. Seal it. When sampling solution products, insert the sampling
glass tube to 2/3 of the depth of the container to take a sample. Mix the sample collected
uniformly. The total volume is not less than 500 mL. Divide it into two clean dry plastic
bottle. Seal it. Attach a label, to indicate the manufacturer's name, product name,
category, model, batch number, sampling date, sampler's name. One set is for inspection;
the other set is kept for future reference. The storage time is determined according to
the needs of the production enterprise.
8.4 If any index in the inspection results does not meet the requirements of this
document, samples shall be taken from twice the quantity of packaging for re-inspection.
Even if only one index does not meet the requirements of this document in the
reinspection, the entire batch of products will be deemed unqualified.
8.5 Use the rounded value comparison method specified in GB/T 8170, to determine
whether the inspection results comply with this document.
9 Signs, labels
9.1 Cobalt sulfate packaging bags for batteries shall have firm and clear signs, including:
manufacturer name, factory address, product name, category, model, net content, batch
number or production date, this document number, signs of "avoid rain" and "avoid sun
exposure" in Table 1 of GB/T 191-2008.
9.2 Each batch of cobalt sulfate products for batteries leaving the factory shall be
accompanied by a quality certificate, which indicates: manufacturer name, factory
address, product name, category, model, net content, batch number or production date,
this document number.
10 Packaging, transportation, storage
10.1 Cobalt sulfate solid products for batteries are double-packed, wherein the inner
packaging uses polyethylene plastic film bags and the outer packaging uses plastic
woven bags. The inner bag of the package shall be tied with vinyl rope or other ropes
of equivalent quality, OR sealed with other equivalent methods. The outer bag is sewn
using a sewing machine; the stitching is firm without leakage or skipping. The net
content of each bag is 25 kg; it can also be packaged according to the specifications
required by the user. Cobalt sulfate solution products for batteries are packaged in
special tankers or polyethylene barrels. The net content of each barrel is 1000 kg; it can
also be packaged according to the specifications required by the user.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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