CN106841465A - A kind of lithium battery electrolytes detection method - Google Patents
A kind of lithium battery electrolytes detection method Download PDFInfo
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- CN106841465A CN106841465A CN201710086295.2A CN201710086295A CN106841465A CN 106841465 A CN106841465 A CN 106841465A CN 201710086295 A CN201710086295 A CN 201710086295A CN 106841465 A CN106841465 A CN 106841465A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
To overcome the detection method of lithium battery electrolytes in the prior art to containing 1, the electrolyte accuracy of detection of 2~bis- (cyanoethoxyl) ethane (DENE) is low, damage big problem to chromatographic column, the invention provides a kind of lithium battery electrolytes detection method, including the electrolyte to be measured containing DENE is mixed with acetonitrile by dilution ratio, mixed liquor to be measured is obtained, gas chromatographic analysis then is carried out to the mixed liquor to be measured.The method that the present invention is provided is applied to the electrolyte containing DENE, and the method high precision, reproducible, efficiency high, easy to operate, while effectively reducing the corrosion to chromatographic post, extends the service life of chromatographic column.
Description
Technical field
The present invention provides a kind of lithium battery electrolytes detection method, especially analyzes each group distribution ratio in lithium battery electrolytes
Detection method.
Background technology
Lithium battery electrolytes are the critical materials of lithium ion battery, equivalent to " blood " of lithium battery, to the performance of battery
Such as cycle life, high temperature performance, large current density performance have very direct influence.The performance of electrolyte depends on group again
Into composition and its proportioning.The actual proportioning of electrolyte product composition whether be accurately product quality important embodiment, and electrolyte
Constituent analysis quality management and control of the accuracy to electrolyte it is particularly significant, the analysis method that accuracy is good, reappearance is strong is matter
The basis of buret control.
In general, lithium battery electrolytes include three class main components：Lithium salts, solvent and additive.Wherein lithium salts is usual
It is lithium hexafluoro phosphate, in addition to heat is decomposed, lithium hexafluoro phosphate is not responded in gas spectrum.Current gas chromatographic analysis is
Can adapt to the electrolye analysis containing lithium salts, method comparative maturity, simply its analyte corrosivity is larger, the life-span of chromatographic column
It is shorter.In electrolyte, the main component of solvent is usually carbonic ester or carboxylic acid esters, such as dimethyl carbonate (DMC), methyl ethyl carbonate
Ester (EMC), diethyl carbonate (DEC), ethylene carbonate (EC), propene carbonate (PC), ethyl acetate (EA), propyl acetate
(PA), ethyl propionate (EP), propyl propionate (PP) etc., above-mentioned solvent boiling point is relatively low, easily detection, and analysis method also compares into
It is ripe.And for additive, its species is various, it is related to solid, the liquid even various forms such as gas, the species of its compound is also each
There is difference, there is aromatic hydrocarbons such as biphenyl (BP), cyclohexylbenzene (CHB), dimethylbenzene (XYL), toluene (TOL) etc.；Also there are carbonates
Such as vinylene carbonate (VC), fluorinated ethylene carbonate (FEC), vinyl ethylene carbonate (VEC)；Sulfonic acid esters such as 1,3~
Propane sultone (PS), 1,4~butyl sultone (BS), methane-disulfonic acid methylene ester (MMDS) etc.；Nitrile such as succinonitrile (SN),
Dintrile (ADN)；Ethers such as fluorine-containing ether HFE458 etc..Typically, the difficult point of the detection and analysis of lithium battery electrolytes generally exists
In the analysis of additive, more particularly there is the additive of special physico-chemical property.Involved in the present invention is that one kind contains
The analysis method of special ether 1,2~bis- (cyanoethoxyl) ethane (DENE).
In the prior art, the detection method to lithium battery electrolytes is gas chromatography, generally using direct injected detection.
For the lithium battery electrolytes of most of formulas, direct injected gas spectrum detection method is ripe, and reappearance preferably, disclosure satisfy that
The requirement of analysis, thus be widely used.However, (logical as additive DE NE containing special nature in electrolyte
Chang Hanliang is 1~5% or so), actually detected discovery, containing DENE/LiPF6The direct gas spectrum detection of lithium electrolyte of system, DENE
Content reappearance is poor, and peak area percent is unstable.This may exist with decomposition of the DENE in gas-chromatography, and catabolite
Residual is relevant in chromatogram.Even same bottle standard specimen, different time is analyzed, still suffer from that front and rear content deviation is larger to ask
Topic.Therefore, existing direct gas spectrum sample detection technology is unable to Accurate Determining and goes out containing DENE/LiPF6The lithium electrolyte of system
Proportioning, it is impossible to obtain accurate and stabilization test result, the qualitative control to this kind of electrolyte brings bigger difficulty.
The content of the invention
The technical problems to be solved by the invention are directed to the detection method of lithium battery electrolytes in the prior art to containing
The electrolyte accuracy of detection of DENE is low, damage big problem to chromatographic column, and through great efforts, the present inventor have found a kind of effective
Solution.
The technical scheme that present invention solution above-mentioned technical problem is used is as follows：
A kind of detection method of lithium battery electrolytes, including：Electrolyte to be measured is mixed with acetonitrile by dilution ratio, is obtained
Mixed liquor to be measured, then carries out gas chromatographic analysis to the mixed liquor to be measured；Contain 1,2~bis- in the electrolyte to be measured
(cyanoethoxyl) ethane.
In the present invention, electrolyte is diluted using acetonitrile, the lithium salts in electrolyte can be effectively reduced to chromatographic column
Damage, extend the service life of chromatographic column, reduce the operation cost of gas chromatograph.Meanwhile, it was found by the inventors of the present invention that
Use acetonitrile of the invention unique is diluted to sample, can be prevented effectively from be diluted using such as acetone, methyl alcohol, ethanol and
The problem that the peak area percent of generation is unstable, poor repeatability, precision are low.
Although this principle it is not immediately clear, the cyano group knot that inventor speculates may be had with acetonitrile and DENE is similar
Structure, according to " similar to mix " principle, acetonitrile can preferably dissolve catabolites of the DENE in chromatographic column and be taken away, from
And it is relevant to reduce harmful effect of the catabolite to chromatographic column.
It is easy to use in addition, acetonitrile is volatile, the intersolubility of easy measure and electrolyte is good, low cost, easily obtain；And
The composition of the non-lithium battery electrolytes of acetonitrile, is easy to deduct in test result, does not interfere with measurement result.
Importantly, the method that the present invention is provided is particularly suitable for the electrolyte containing special additives such as such as DENE, effectively
Overcome the problem that cannot carry out accurate detection to the electrolyte containing special additives such as DENE in the prior art.
Specific embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention, is not intended to limit the present invention.
It is well known that electrolyte is mixture, aborning, generally according to the Ju Ti Pei Fang (institute of fixed electrolyte
The various materials and the content of each material for containing) prepared, but due to the influence of various objective factors, the electrolysis prepared
The final composition of liquid product it is more or less there is deviation with the concrete composition of formula, it is therefore desirable to the electrolyte to preparing production
Product is detected.
In the present invention, the formula of electrolyte is defined as " the theory composition " of electrolyte.
The detection method of the electrolyte that the present invention is provided includes：Electrolyte to be measured is mixed with acetonitrile by dilution ratio, is obtained
To mixed liquor to be measured, gas chromatographic analysis then is carried out to the mixed liquor to be measured；Contain 1,2~bis- in the electrolyte to be measured
(cyanoethoxyl) ethane.
The composition of electrolyte is analyzed using gas-chromatography be method commonly used in the prior art, its concrete operations
Process is known in the art, and it is dilute that innovative point of the invention is that creative use acetonitrile is carried out to electrolyte to be measured
Release, damage of the lithium salts in electrolyte to chromatographic column can be effectively reduced, extend the service life of chromatographic column, reduce gas-chromatography
The operation cost of instrument.Meanwhile, it was found by the inventors of the present invention that the unique use acetonitrile of the present invention is diluted to sample, can have
Effect avoids using the unstable peak area percent that such as acetone, methyl alcohol, ethanol are diluted and produce, poor repeatability, precision
Low problem.
It is that detection method of the invention is completely illustrated in the present invention, now the citing of detection method process is described in detail such as
Under：
S1, electrolyte to be measured include lithium salts and the component to be detected including additive and solvent, obtain component to be detected
In each composition correction factor F；The correction factor F is calculated by such as method of following formula 1：
Formula 1：FiThe percentage composition M ' of component i in=standard sampleiThe area percentage S ' of component i in/standard samplei；
Wherein, the composition of the standard sample is identical with the theory composition of the component to be detected；
The percentage composition M ' of component i in the standard sampleiFor：In the standard sample, the weight percent of component i
Than；
The area percentage S ' of component i in the standard sampleiFor：Standard sample is mixed with acetonitrile by dilution ratio,
Standard specimen mixed liquor is obtained, gas chromatographic analysis then is carried out to the standard specimen mixed liquor, the area of component i in measurement standard sample
Percentage S 'i；
S2, electrolyte to be measured is mixed with acetonitrile by the dilution ratio, mixed liquor to be measured is obtained, then to described to be measured
Mixed liquor carries out gas chromatographic analysis, measures the area percentage S of each composition in the component to be detected；
S3, the content by each composition in the component to be detected as described in the calculating of the method for following formula 2：
Formula 2：The content M of component i in component to be detectediThe correction factor F of=component iiThe area percentage S of × component ii。
As known to those skilled in the art, generally, electrolyte includes lithium salts, solvent and additive.In the present invention,
For ease of description, electrolyte is divided into lithium salts and component to be detected including additive and solvent.
According to the present invention, before being detected, the correction of each composition in component to be detected in the electrolyte to be measured need to be first obtained
The factor.It should be understood that for the electrolyte of same composition, the correction factor of each composition can only first in its component to be detected
Measured during secondary detection, when subsequently the electrolyte to same composition is measured, can directly using the correction factor known
.
For correction factor, according to the present invention, can be measured by the following manner and be calculated：
For a certain electrolyte that well-known theory is constituted, first according to its theory composition, standard sample is prepared.Normal conditions
Under, due to carrying out during gas chromatographic detection, lithium salts (such as LiPF6) do not responded in gas-chromatography.It is that may be present to reduce
Lithium salts decomposes and corrosion is produced to chromatographic column, when standard sample is prepared, without lithium salts, and only adds the addition in addition to lithium salts
Agent and solvent, i.e., foregoing component to be detected.
In the present invention, the composition of the standard sample is identical with the theory composition of the component to be detected, i.e. standard sample
Containing with identical composition in electrolyte component to be detected, and in standard sample the percentage by weight of each composition with to be detected group
Percentage by weight (non-each composition original weight amount hundred in the electrolytic solution on the basis of component weight to be detected of each composition in point
Point than) it is identical.
After obtaining standard sample, standard sample is mixed with acetonitrile, standard sample is diluted, obtain standard specimen mixing
Liquid.
When being mixed, the purity of above-mentioned acetonitrile is chromatographically pure.Moisture in acetonitrile is less than 500PPM, preferably shorter than
50ppm, more preferably less than 10PPM.
Mixed proportion when standard sample mixes with acetonitrile is dilution ratio.In the present invention, during mixing, the standard sample
The weight of product：Weight=1 of acetonitrile：1~20, preferably 1：1~5, i.e. dilution ratio are 1：1~20, preferably 1：1~5.
After standard sample and acetonitrile are mixed to get into standard specimen mixed liquor, by standard specimen mixed liquor, constant temperature is preserved at 20~25 DEG C
10~30min is to ensure the well mixed of standard specimen mixed liquor, and temperature is consistent with standard sample.
It is first micro- using standard specimen mixed liquor rinse before carrying out chromatography to standard specimen mixed liquor under preferable case in the present invention
Amount injector 5~8 times.
Standard sample is diluted after obtaining standard specimen mixed liquor, gas chromatographic analysis is carried out to standard specimen mixed liquor, measured
The area percentage S ' of each composition in standard sample, accordingly, the area percentage of component i in the standard sample that detection is obtained
Than being designated as S 'i。
In the present invention, above-mentioned chromatography of gases analysis can be carried out using existing various conventional equipments and method, for example, can adopted
Detected with the gas chromatograph of model Agilent 7890B, the chromatographic column for using can be KB~200, injector is certainly
Dynamic injector G4513A.Testing conditions and method can be：Column temperature：2min is kept at 100 DEG C, then with the liter of 10 DEG C/min
Warm speed is warming up to 160 DEG C, and constant temperature keeps 10min, then is warming up to 260 DEG C with the heating rate of 30 DEG C/min, and constant temperature is protected
Hold 5min.Column flow is 1.5mL/min, and split ratio is 50：1.
The area percentage S ' of each composition in standard sample can be obtained by the above method.For component i, by formula 1
Its correction factor F can be calculatedi：
Formula 1：FiThe percentage composition M ' of component i in=standard sampleiThe area percentage S ' of component i in/standard samplei。
For each composition in standard sample, the F of each composition can be calculated as stated above.
In the present invention, for the electrolyte of same composition, the above-mentioned correction factor F for detecting can repeat to make
With.But it is noted that when the condition for changing gas chromatographic detection and during hardware (such as chromatographic column), need to retest correction because
Sub- F.
After obtaining the correction factor F of above-mentioned each composition, can start to detect electrolyte to be measured.If it should be understood that
The correction factor directly known using early stage, directly can be detected to electrolyte to be measured.
Specifically, electrolyte to be measured is mixed with acetonitrile by the dilution ratio, mixed liquor to be measured is obtained.
It is identical with the acetonitrile used when preparing standard specimen mixed liquor now to mix used acetonitrile, is similarly chromatographically pure level.
Moisture in acetonitrile is less than 500PPM, more preferably less than preferably shorter than 50ppm, 10PPM.
Dilution ratio when standard sample mixes with acetonitrile when above-mentioned dilution ratio is preparation standard specimen mixed liquor.
After electrolyte to be measured and acetonitrile are mixed to get into mixed liquor to be measured, by mixed liquor to be measured, constant temperature is protected at 20~25 DEG C
10~30min is deposited, chromatography is then carried out.The temperature and time that now constant temperature is preserved is preserved with the standard specimen mixed liquor constant temperature
Temperature and time it is identical.
In the present invention, before carrying out chromatography to mixed liquor to be measured, first using mixed liquor rinse microsyringe 5 to be measured~
8 times.Method and number of times when the method and number of times of now rinse are with using standard specimen mixed liquor rinse is identical.
Then, gas chromatographic analysis is carried out to the mixed liquor to be measured, the face of each composition in the component to be detected is measured
Product percentage S.Accordingly, the area percentage of component i is designated as S in the electrolyte described to be measured that detection is obtainedi.May be appreciated
It is that the component i in above-mentioned electrolyte to be measured is same substance with the component i in standard sample.
Finally, then by the content of each composition in the component to be detected as described in the calculating of the method for following formula 2：
Formula 2：The content M of component i in component to be detectediThe correction factor F of=component iiThe area percentage S of × component ii。
The content of each composition in the component to be detected of electrolyte to be measured can be obtained by the above method, i.e. know and treat
Survey the actual proportioning of electrolyte.
The method that the present invention is provided is applied widely, may not only be applied to the electrolyte detection containing conventional additives and solvent,
Particularly with the electrolyte containing special additives such as such as 1,2~bis- (cyanoethoxyl) ethane (DENE), its effect is more notable, has
Effect overcomes the problem that cannot carry out accurate detection to the electrolyte containing special additives such as DENE in the prior art.
For the electrolyte for containing 1,2~bis- (cyanoethoxyl) ethane, under preferable case, wherein, 1,2~bis- (cyanogen ethoxies
Base) ethane theoretical content be 0.5~10%.
The present invention is further detailed by the following examples.
In the present invention, illustrated by taking the electrolyte of following theoretical composition (formula) as an example：
PP：54%, VC：3%, EC：20%, SN：3%, PC：5%, DENE：3%, LiPF6：12%.
Embodiment 1
The present embodiment is used to illustrate the detection method of lithium battery electrolytes disclosed by the invention.
Standard sample (the PP of composition same with the component to be detected of electrolyte to be measured is prepared first：VC：EC：SN：PC：
DENE=54:3:20:3:5:3) 1 is pressed with acetonitrile (chromatographically pure, moisture is less than 100PPM)：3 weight is marked than dilution
Sample mixed liquor, then constant temperature preserves 20min at 20 DEG C.
According to following each parameter of instrumentation condition setting instrument：Using the gas chromatograph of model Agilent 7890B
Detected, the chromatographic column for using can be KB~200, injector is automatic sampler G4513A.
After after instrument stabilizer, with standard specimen mixed liquor repeatedly 10 μ l microsyringes of rinse 8 times after, draw 0.2 μ l standards and mix
Close liquid injection gas chromatograph.
Then detected as follows：Column temperature：2min is kept at 100 DEG C, then with the intensification speed of 10 DEG C/min
Rate is warming up to 160 DEG C, and constant temperature keeps 10min, then is warming up to 260 DEG C with the heating rate of 30 DEG C/min, and constant temperature keeps
5min.Column flow is 1.5mL/min, and split ratio is 50：1.Detect the area percentage S ' of each composition, then calculate correction because
Sub- F.
Electrolyte to be measured and acetonitrile (chromatographically pure, moisture is less than 100PPM) are pressed 1：3 weight is treated than dilution
After surveying mixed liquor, constant temperature preserves 20min at 20 DEG C.After after instrument stabilizer, with mixed liquor to be measured repeatedly the μ l of rinse 10 it is micro enter
After sample device 8 times, 0.2 μ l mixed liquor injection gas chromatographs to be measured are drawn.
Then detected as follows：Column temperature：2min is kept at 100 DEG C, then with the intensification speed of 10 DEG C/min
Rate is warming up to 160 DEG C, and constant temperature keeps 10min, then is warming up to 260 DEG C with the heating rate of 30 DEG C/min, and constant temperature keeps
5min.Column flow is 1.5mL/min, and split ratio is 50：1.Detect the area percentage S of each composition, then calculate it is each into
The content M for dividing.
Repeat said process 10 times, the RSD of each component content of 10 acquisitions and 10 measurements is inserted into table 1.
Embodiment 2
The present embodiment is used to illustrate the detection method of lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that dilution ratio is 1：1.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Embodiment 3
The present embodiment is used to illustrate the detection method of lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that dilution ratio is 1：5.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Embodiment 4
The present embodiment is used to illustrate the detection method of lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that dilution ratio is 1：20.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Comparative example 1
This comparative example is used for the detection method of comparative illustration lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is, undiluted, is directly tested using electrolyte to be measured.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Comparative example 2
This comparative example is used for the detection method of comparative illustration lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that replacing acetonitrile using acetone is diluted.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Comparative example 3
This comparative example is used for the detection method of comparative illustration lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that replacing acetonitrile using methyl alcohol is diluted.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Comparative example 4
This comparative example is used for the detection method of comparative illustration lithium battery electrolytes disclosed by the invention.
Detected using the method for embodiment 1.Difference is that replacing acetonitrile using ethanol is diluted.
Repeat said process 3 times, the RSD of each component content of 3 acquisitions and 3 measurements is inserted into table 1.
Table 1
Be can be seen that from the test result of above-mentioned DENE
1st, containing DENE/LiPF6The lithium electrolyte finished product of system, direct injected detection DENE is not diluted, and testing result is unstable
It is fixed；
2nd, containing DENE/LiPF6The lithium electrolyte finished product of system, sample introduction after being diluted with acetone or methyl alcohol or ethanol, test knot
The repeatability of fruit is also undesirable；
3rd, containing DENE/LiPF6The lithium electrolyte finished product of system, after sample introduction after dilution in acetonitrile, the reappearance of test result
Well.
Therefore, it is diluted with acetonitrile, in addition to the reappearance of DENE test results is good, also significantly reduces electrolysis
Injury of the liquid to gas chromatographic column, is conducive to being lifted the service life of chromatographic column, reduces the use cost of chromatographic column, many at one stroke
.Therefore the program has stronger practicality and economic worth.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (5)
1. a kind of lithium battery electrolytes detection method, it is characterised in that including：Electrolyte to be measured and acetonitrile are mixed by dilution ratio
Close, obtain mixed liquor to be measured, gas chromatographic analysis then is carried out to the mixed liquor to be measured；Contain 1 in the electrolyte to be measured,
2~bis- (cyanoethoxyl) ethane.
2. lithium battery electrolytes detection method according to claim 1, it is characterised in that the dilution ratio is：It is described
The weight of electrolyte to be measured：Weight=1 of acetonitrile：1~20.
3. lithium battery electrolytes detection method according to claim 1, it is characterised in that the purity of the acetonitrile is chromatogram
It is pure.
4. lithium battery electrolytes detection method according to claim 1, it is characterised in that in the acetonitrile, moisture
Less than 500PPM.
5. the lithium battery electrolytes detection method according to any one in Claims 1 to 4, it is characterised in that the electricity
In solution liquid, the content of 1,2~bis- (cyanoethoxyl) ethane is 0.5~10%.
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| CN108362781A (en) * | 2018-01-29 | 2018-08-03 | 江苏理文化工有限公司 | A kind of analysis method of lithium battery electrolytes |
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| CN111487346A (en) * | 2020-04-29 | 2020-08-04 | 江苏天鹏电源有限公司 | Quantitative method for detecting small amount of organic additives in electrolyte by GC-MS (gas chromatography-Mass spectrometer) combination |
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| CN115389641A (en) * | 2021-05-25 | 2022-11-25 | 南通新宙邦电子材料有限公司 | Detection method of lithium battery electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108362781A (en) * | 2018-01-29 | 2018-08-03 | 江苏理文化工有限公司 | A kind of analysis method of lithium battery electrolytes |
| CN111024866A (en) * | 2020-01-21 | 2020-04-17 | 大同新成新材料股份有限公司 | Lithium battery electrolyte chromatographic test method |
| CN111487346A (en) * | 2020-04-29 | 2020-08-04 | 江苏天鹏电源有限公司 | Quantitative method for detecting small amount of organic additives in electrolyte by GC-MS (gas chromatography-Mass spectrometer) combination |
| CN114624346A (en) * | 2020-12-11 | 2022-06-14 | 诺莱特电池材料(苏州)有限公司 | Method for detecting content of methylene methanedisulfonate in lithium ion battery electrolyte |
| CN114624346B (en) * | 2020-12-11 | 2024-03-29 | 诺莱特电池材料(苏州)有限公司 | Method for detecting content of methane disulfonic acid methylene ester in lithium ion battery electrolyte |
| CN115389641A (en) * | 2021-05-25 | 2022-11-25 | 南通新宙邦电子材料有限公司 | Detection method of lithium battery electrolyte |
| CN115389641B (en) * | 2021-05-25 | 2024-02-09 | 南通新宙邦电子材料有限公司 | Detection method of lithium battery electrolyte |
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