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SJ/T 11723-2018: Electrolyte solution used for lithium ion battery
SJ/T 11723-2018
SJ
ELECTRONIC INDUSTRY STANDARD
ICS 31-030
L 90
Record number.
Electrolyte solution used for lithium ion battery
ISSUED ON. JULY 04, 2018
IMPLEMENTED ON. OCTOBER 01, 2018
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 Requirements... 4
4 Test methods... 5
5 Inspection rules... 14
6 Marking, packaging, transportation and storage... 17
Appendix A (Normative) Determination of sulfate ion (SO42-)... 19
Appendix B (Normative) Determination of K, Na, Fe, Ca, Pb, Cu, Zn, Ni, Cr by
inductively coupled plasma optical emission spectrometry... 21
Electrolyte solution used for lithium ion battery
1 Scope
This Standard specifies the requirements, test methods, inspection rules, marking,
packaging, transportation and storage of electrolyte solution used for lithium ion battery.
This Standard applies to the electrolyte solution used for lithium ion battery which is
composed of electrolyte lithium salts, solvents, etc.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
GB/T 3143, Color determination method of liquid chemicals (Hazen unit;
Platinum-cobalt scale)
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods
GB 13690, General rule for classification and hazard communication of chemicals
GB 15258, General rules for preparation of precautionary label for chemicals
GB/T 26125, Electrical and electronic products - Determination of six regulated
substances (lead, mercury, cadmium, hexavalent chromium, polybrominated
biphenyls, polybrominated diphenyl ethers)
GB/T 26572, Requirements of concentration limits for certain restricted substances
in electrical and electronic products
3 Requirements
3.1 Appearance
The electrolyte solution used for lithium ion battery shall be a solution without
precipitation, suspended matter or stratification.
3.2 Technical requirements
4.4.3.3 Weigh (3 ~ 5) g of sample (accurate reading to 0.001 g) using the reduction
method on an electronic balance and use a syringe to draw the sample.
4.4.3.4 Inject the extracted sample into the titration cell from the injection port; stir
thoroughly for 10 seconds and then start titration.
4.4.3.5 After the titration is completed, input the sample mass and record the water
content determination results in the sample.
4.4.3.6 Two parallel tests shall be performed for each test, and the absolute difference
between the parallel test values shall be ≤2 mg/kg.
4.4.4 Result processing
Take the arithmetic mean of the values measured in two parallel tests as the test result.
4.5 Determination of free acid
4.5.1 Potentiometric titration
4.5.1.1 Principle
Immerse the indicator electrode and the reference electrode in the same solution to be
measured. During the titration process, the potential of the reference electrode remains
constant, and the potential of the indicator electrode changes with the concentration of
the substance to be measured. Before and after the stoichiometric point, the change in
the concentration of the substance to be measured in the solution will cause a sharp
change in the potential of the indicator electrode. The sudden jump point of the indicator
electrode potential is the titration end point.
4.5.1.2 Instruments and apparatuses
The required instruments and apparatuses are as follows.
a) Potentiometric titrator. sensitivity 0.1 mV.
b) pH electrode.
c) Electronic balance. minimum graduation value 1 mg.
4.5.1.3 Reagents
Sodium methoxide standard titration solution (concentration 0.02 mol/L).
a) Preparation. Weigh 1.08 g of sodium methoxide; dissolve it in 1 000 mL of
methanol; shake well.
b) Calibration. Weigh 0.396 g of the standard reagent potassium hydrogen phthalate
dried to constant weight in an oven at (110 ~ 120) °C and dissolve it in 1 000
4.5.2 Ice water chemical titration
4.5.2.1 Method summary
Use ice-water mixture as solvent and bromothymol blue solution as indicator; use
sodium hydroxide standard titration solution to titrate the total free acid in the sample;
calculate based on hydrofluoric acid.
4.5.2.2 Instruments and apparatuses
The required instruments and apparatuses are as follows.
a) Electronic balance. minimum graduation value 1 mg;
b) Alkali burette. 10 mL, minimum graduation value 0.01 mL;
c) Syringe. 10 mL;
d) Erlenmeyer flask. 250 mL.
4.5.2.3 Reagents and Materials
The required reagents and materials are as follows.
a) Sodium hydroxide standard titration solution. 0.002 mol/L.
b) Ice cubes. Freeze water in an ice cube tray to obtain cubes with a length, width
and height of approximately 1 cm.
c) Bromothymol blue indicator solution (1 g/L). Weigh 0.1 g of bromothymol blue;
dissolve it in 50 mL of ethanol (95%); then, use ethanol (95%) to dilute to 100
mL.
4.5.2.4 Test steps
Measure 50 mL of water frozen to (0 ~ 4) ℃ in a 250 mL conical flask; add (3 ~ 4) ice
cubes; then, add (2 ~ 3) drops of bromothymol blue indicator solution. Use a syringe to
take a sample; weigh about 10 g of the sample (accurate to 0.001 g) by the reduction
method; add it to the conical flask; shake it thoroughly. Use the calibrated 0.002 mol/L
sodium hydroxide standard solution; shake the conical flask while titrating, until the
solution suddenly changes from yellow to blue, which is the end point; record the
volume of sodium hydroxide standard titration solution consumed in the titration. Do a
blank test at the same time.
4.5.2.5 Result processing
The free acid content is based on HF according to Formula (2).
Before testing, first draw water at about 25 °C to calibrate the instrument. After
calibration, draw the sample to be tested to rinse the U-shaped tube of the density meter
(3 ~ 4) times; then, draw the sample to be tested; record the density value of the sample
at 25.0 °C in the U-shaped tube. After the test is completed, discharge the sample; first
wash the U-shaped tube with anhydrous ethanol (3 ~ 4) times, and then wash it with
water. Perform two parallel tests for each test.
4.6.2.5 Result processing
Take the arithmetic mean of the values measured in two parallel tests as the test result.
4.6.3 During arbitration, density shall be determined using the density bottle method.
4.7 Determination of electrical conductivity
4.7.1 Instruments and apparatuses
The required instruments and apparatuses are as follows.
a) Conductivity meter. measuring range (0 ~ 100) mS/cm;
b) Conductivity electrode. the electrode constant matches the measurement range;
c) Thermometer. minimum graduation value 0.1 ℃.
4.7.2 Reagents
Potassium chloride (KCl) conductivity standard solution. 0.1 mol/L, the conductivity
value is 12.852 mS/cm at 25 °C.
4.7.3 Test steps
4.7.3.1 Turn on the conductivity meter and preheat for 0.5 h.
4.7.3.2 Use 0.1 mol/L potassium chloride (KCl) conductivity standard solution to
calibrate the instrument.
4.7.3.3 Add about 20 mL of electrolyte solution to a 100 mL clean plastic cup; control
the temperature at (25 ± 3) °C; insert the electrodes and thermometer into the electrolyte
solution; adjust the instrument temperature so that the instrument compensation
temperature is consistent with the electrolyte temperature to be measured. When the
reading stabilizes, it is the conductivity of the electrolyte solution at 25 °C.
4.7.3.4 Two parallel tests shall be performed for each test, and the absolute difference
between the parallel test values shall be ≤0.2 mS/cm.
4.7.4 Result processing
Take the arithmetic mean of the values measured in two parallel tests as the test result.
4.8 Determination of chloride ion (Cl-) content
4.8.1 Instruments and apparatuses
The required instruments and apparatuses are as follows.
a) Potentiometric titrator, sensitivity 0.1 mV;
b) Silver ion selective electrode;
c) Electronic balance. minimum graduation value 1 mg.
4.8.2 Reagents
Silver nitrate standard titration solution (concentration 0.001 mol/L).
a) Preparation. Weigh 0.175 g of silver nitrate; dissolve in 1 000 mL of ethanol;
shake well. Store the solution in a brown bottle.
b) Calibration. Weigh 0.050 g of the reference reagent, sodium chloride, which is
burned to constant weight in a high-temperature furnace at (500 ~ 600) ℃;
dissolve it in 2 000 mL of water; shake well. Measure 50 mL of the above
sodium chloride solution and titrate it with silver nitrate standard titration
solution on a potentiometric titrator to calibrate the concentration of the silver
nitrate standard titration solution.
4.8.3 Test steps
4.8.3.1 Automatically calibrate the potentiometric titrator.
4.8.3.2 Weigh (40 ~ 60) g of sample (accurate reading to 0.001 g) and place in a 100
mL clean plastic cup.
4.8.3.3 Immerse the electrode in the solution to be tested and stir the solution thoroughly.
4.8.3.4 Input the concentration value of the silver nitrate standard titration solution into
the potentiometric titrator and start titration. When the titration endpoint is reached,
record the volume of the silver nitrate standard titration solution consumed.
4.8.3.5 Two parallel tests shall be performed for each test, and the absolute difference
between the parallel test values shall be ≤0.5 mg/kg.
4.8.4 Result processing
Calculate the content of chloride ion (Cl-) according to Formula (4).
5.3 Quality consistency inspection
5.3.1 Batch inspection
5.3.1.1 Batching
An inspection batch consists of electrolyte solution used for lithium ion battery that is
continuously produced using the same raw materials, under the same production
conditions, using the same process, and submitted for inspection at the same time.
5.3.1.2 Sampling
When the number of packaging units in each batch is less than 3 barrels, all barrels are
drawn; when the number of packaging units in each batch is greater than or equal to 3
barrels, 3 barrels are drawn. In principle, the first barrel, the middle barrel (odd barrel
n+1/2, even barrel n/2), and the last barrel of each batch are drawn.
Before sampling, use high-purity nitrogen or argon to purge the sampling pipe for 2
minutes; then, connect it to the liquid outlet of the packaging barrel of the product to be
tested with a quick connector; open the valve; release (150 ~ 200) mL of the product to
be tested (to clean the pipe); then, use the product to be tested to rinse the sampling
bottle (2 ~ 3) times before starting sampling. When the number of sampling barrels is
3, the sampling volume per barrel is (150 ~ 200) mL; when the number of sampling
barrels is 2, the sampling volume per barrel is (200 ~ 250) mL; when the number of
sampling barrels is 1, the sampling volume per barrel is (400 ~ 500) mL.
After sampling, tighten the bottle cap immediately. Mix the samples in equal amounts
to form a batch sample. Divide the batch sample into two parts; mark them with the
product brand, batch number, sampling date and name of the sampler, one for testing
and the other for storage in a sealed container.
The above operations must be carried out in an environment with a moisture content of
≤1 mg/kg.
5.3.1.3 Inspection items
The batch inspection items include appearance, chroma, density, moisture, conductivity
and free acid content, as shown in Table 2.
5.3.1.4 Judgment of conformity
When all batch inspection items are qualified, the batch of products is qualified; if any
batch inspection item is unqualified, the batch of products is unqualified.
5.3.2 Periodic inspection
5.3.2.1 Sampling
Randomly draw (400 ~ 500) mL of the sample, which can be drawn from the product
packaging unit or in an online closed sampling.
5.3.2.2 Inspection items
The periodic inspection items include chloride ion content, sulfate ion content and metal
impurity content, as shown in Table 2.The inspection cycle is 1 week.
5.3.2.3 Judgment of conformity
When the test results of all periodic inspection items are qualified, the periodic
inspection is qualified; if any periodic inspection item is unqualified, the periodic
inspection is unqualified.
5.3.2.4 Non-conforming treatment
If the periodic inspection fails, the supplier shall immediately stop the delivery of the
products produced in the period and find out the reasons for the failure of the periodic
inspection items. According to the reasons for the failure, take appropriate measures to
rectify the products produced in the period and resubmit for inspection. The products
can be delivered only after they pass the inspection.
For products that have been delivered, the supplier shall notify the buyer of any
unqualified items in periodic inspection, and the two parties shall resolve the issue
through negotiation.
6 Marking, packaging, transportation and storage
6.1 Marking
The product packaging shall have firm and clear markings, indicating the
manufacturer's name, address, product name, designation, net weight, batch number,
precautions, etc., and shall comply with the requirements of GB 15258.
Each batch of products shall be accompanied by a certificate of conformity or a
certificate of quality, which shall include. manufacturer name, product name,
designation, net weight, batch number, production date, shelf life, etc.
6.2 Packaging
The electrolyte solution used for lithium ion battery shall be packaged in stainless steel
barrels (with quick connectors) and filled with (0.015 ~ 0.025) MPa high-purity
nitrogen or argon as protection.
6.3 Transportation
Appendix A
(Normative)
Determination of sulfate ion (SO42-)
A.1 Scope
This Appendix specifies the method for determining the sulfate ion (SO42-) content in
the electrolyte solution used for lithium ion battery.
This Appendix applies to the determination of ...