CN113376304A - Method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS (gas chromatography-mass spectrometry) - Google Patents
Method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS (gas chromatography-mass spectrometry) Download PDFInfo
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Abstract
The invention relates to the technical field of lithium ion battery electrolyte, and discloses a method for detecting carbonate organic matters and additives in the lithium ion battery electrolyte by GC-MS (gas chromatography-mass spectrometry). by pretreating the electrolyte, solid particles and hydrofluoric acid in the electrolyte are effectively prevented from causing the loss and corrosion of a supporter in a chromatographic column, the replacement frequency of the chromatographic column and a sample injection needle is reduced, and the maintenance cost of equipment is reduced; by adopting the mode full-spectrum scanning combining SCAN and SIM, the carbonate organic solvent with high concentration in the electrolyte can be detected, and a small amount of functional additive can be detected without omission; the linearity and the reproducibility of the components of the electrolyte are quantitatively analyzed by an external standard method, and the measurement accuracy is high.
Description
Technical Field
The invention relates to the technical field of lithium ion battery electrolyte, in particular to a method for detecting carbonate organic matters and additives in the lithium ion battery electrolyte by GC-MS.
Background
The electrolyte of the lithium ion battery consists of an organic solvent, a functional additive and electrolyte lithium salt, the performance of the electrolyte is closely related to the performance of the organic solvent, and the organic solvent widely used at the present stage comprises carbonates, ethers and carboxylates. Carbonates mainly include cyclic carbonates (e.g., ethylene carbonate EC and propylene carbonate PC) and chain carbonates (e.g., dimethyl carbonate DMC, diethyl carbonate DEC, ethyl methyl carbonate EMC). The functional additive can obviously improve certain performances of the lithium battery, such as SEI film performance improvement, lithium ion conductivity improvement, electrolyte thermal stability improvement, battery safety performance improvement and electrolyte stability improvement.
When a gas chromatography-mass spectrometer is used for testing and analyzing the lithium ion battery electrolyte, electrolyte lithium salt is easy to form solid particles in a chromatographic column, and lithium salt is also easy to react with water to generate hydrofluoric acid (HF), such as: LiPF6+H2O→POF3+2HF + LiF, corrode the syringe needle, cause supporter loss, corruption in the chromatographic column, have great destruction effect to the packing stability of gas chromatographic column, lead to the test procedure center pillar to run off seriously, the accuracy and the stability of test result reduce, influence the precision of instrument, on the other hand causes the life-span of chromatographic column to shorten, and the syringe needle is changed frequently, has increased the fault rate of equipment, has improved the maintenance cost that detects maintenance equipment.
The method for detecting the carboxylic ester compounds in the lithium ion battery electrolyte is disclosed in a Chinese patent with an authorization number of CN105467058B and a publication date of 2017, 5 and 17, and is characterized in that a gas chromatography-mass spectrometer is used for carrying out qualitative and quantitative analysis on the carboxylic ester compounds by adopting an external standard method; impurities in the sample have no influence on the analysis result, and the method has good reproducibility and high accuracy; according to the invention, before a sample is analyzed, the sample to be detected is diluted to obtain a detection solution, and then the detection solution is detected and analyzed, so that the column loss is reduced, the corrosion of the sample to be detected on a chromatographic column is effectively prevented, and the maintenance cost of detection equipment is reduced; meanwhile, the influence of other impurities in the sample to be detected on the analysis result can be avoided.
In the patent, the sample to be detected is diluted, so that the corrosion of electrolyte to a chromatographic column cannot be effectively prevented, the diluted sample has low peak intensity due to too small concentration and is difficult to detect, and a full-spectrum scanning mode is adopted during operation, so that characteristic peaks of a target substance are easy to omit.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS. And (3) qualitatively analyzing the detection solution by combining an SCAN mode and an SIM mode in a full-spectrum scanning mode of a gas chromatography-mass spectrometer, determining the types of the carbonate organic solvent and a small amount of additives, and then quantifying by adopting an external standard method. The invention relates to pretreatment of electrolyte, selection of chromatographic column, a temperature-raising program and an external standard quantitative method.
The specific technical scheme of the invention is as follows: a GC-MS method for detecting carbonate organic matters and additives in lithium ion battery electrolyte comprises the following steps:
s1: adding an inorganic solution into the electrolyte, shaking up, centrifuging, and filtering to obtain a to-be-detected electrolyte;
s2: preparing a detection solution, measuring the detection solution in an SCAN and SIM mode, and determining characteristic qualitative ion peaks of each component in the detection solution;
s3: adding a solvent into the electrolyte to be detected in S1 to prepare a liquid to be detected, detecting the liquid to be detected according to the same method of S2, and performing qualitative determination on each component to be detected in the liquid to be detected;
s4: weighing at least three groups of pure substances of the components to be detected as S3, wherein the concentrations of the components to be detected in each group are different, the mass percentages of the components to be detected are consistent, and adding a solvent to obtain at least three groups of mixed standard solutions with different concentrations;
s5: detecting each standard solution by using an ion monitoring mode of a gas chromatography-mass spectrometer, recording the peak area corresponding to each standard solution, and drawing a standard curve according to the content and the peak area of each component to be detected in each standard solution to obtain a standard curve linear equation;
s6: and detecting the solution to be detected according to the same method of S5, recording peak areas, and calculating according to the standard curve linear equation to obtain the concentration of each component to be detected in the lithium ion battery electrolyte.
Preferably, the chromatographic determination conditions in S3 and S3 are as follows: the chromatographic column is Rxi-5Sil MS30m multiplied by 0.25mm multiplied by 0.25um, the carrier gas is helium, the column flow is 1-1.5mL/min, the split ratio is (20: 1) - (50: 1), the injection port temperature is 240-: keeping the temperature at 35-45 ℃ for 3-8min, heating to 80-120 ℃ at the heating rate of 5-8 ℃/min, heating to 260 ℃ at the heating rate of 15-25 ℃/min, keeping the temperature for 1-3min, and finally heating to 300 ℃ at the heating rate of 270 ℃ to 300 ℃ at the heating rate of 10-50 ℃/min, and keeping the temperature for 1-3 min.
Determining the temperature of a sample inlet according to each component in the electrolyte, wherein the temperature of the sample inlet is greater than the highest boiling point of each component in the liquid to be detected, and the temperature cannot be too high, so that the decomposition and denaturation of the electrolyte are avoided, and the temperature of the sample inlet and the temperature rise rate ensure that each component can be well separated; the sample feeding amount and the split flow ratio are adjusted, so that the phenomenon that the chromatographic column is overloaded, excessive samples enter the chromatographic column and are overloaded, the separation efficiency is reduced, the peak is deformed and trailing, the corresponding component content cannot be detected due to the saturation of a detector, and the service life of the chromatographic column is influenced; the chromatographic column is thin, a sample to be detected cannot enter the chromatographic column instantly after being vaporized to generate gas expansion, a certain time is needed, and the time is too long to cause the spectral bandwidth, so that a part of the sample needs to be shunted in time.
Preferably, the solvent is one of acetone, methanol, ethanol or isopropanol.
Preferably, the inorganic solution in S1 is a saturated sodium carbonate solution.
Preferably, the centrifugation rate in S1 is 3000-5000 r/min.
Into the electrolyteAdding saturated sodium carbonate solution, centrifuging, collecting supernatant, and filtering to remove electrolyte lithium salt LiPF6And the lithium salt reacts with water in the storage process to generate hydrofluoric acid, so that the corrosion of the liquid to be detected on the sample injection needle is effectively prevented, the loss and the corrosion of a supporter in the chromatographic column are avoided, the maintenance cost of detection and maintenance equipment is reduced, and the qualitative and quantitative errors in the test caused by less additive content are reduced.
Preferably, the concentration of the detection solution in S2 and the concentration of the test solution in S3 are 1500-.
Preferably, the chromatographic column is a weakly polar column or a nonpolar column.
Preferably, the column temperature program sets the SIM mode fine scanning at 10.5-10.8min and 11.2-11.6min, and SCANs in SCAN mode at other times.
And the SCAN mode and the SIM mode in the full-spectrum scanning mode are mutually combined to carry out qualitative analysis on the detection liquid, so that each component to be detected in the detection liquid can be detected more comprehensively and accurately.
Compared with the prior art, the invention has the beneficial effects that:
(1) the electrolyte is pretreated, so that the carrier in the chromatographic column is effectively prevented from being lost and corroded due to solid particles and hydrofluoric acid, the replacement frequency of the chromatographic column and a sample injection needle is reduced, and the maintenance cost of equipment is reduced;
(2) by adopting the full-spectrum scanning and qualitative mode combining SCAN and SIM, the method can ensure that the carbonate organic solvent with high concentration in the electrolyte can be detected, and a small amount of functional additives can be detected without omission;
(3) the components of the electrolyte are quantitatively analyzed by adopting an external standard method, the linearity and the reproducibility are good, and the measurement accuracy is high.
Drawings
FIG. 1 is a GC-MS chromatogram of example 1 of the present invention;
FIG. 2 is a GC-MS chromatogram of example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous technical effects of the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and the detailed description. The devices, connections, and methods referred to in this disclosure are those known in the art, unless otherwise indicated.
Example 1
Knowing each organic matter component in the electrolyte sample, respectively weighing 9 compounds of Ethylene Carbonate (EC), Propylene Carbonate (PC), diethyl carbonate (DEC), dimethyl carbonate (DMC) and Ethyl Methyl Carbonate (EMC) with the same mass, Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), Phenylsulfone (PS) and Adiponitrile (ADN), and preparing a solution with the concentration of 2000ppm by taking acetone as a solvent to serve as a detection solution.
Adopting a GCMS-QP2010SE model gas chromatography-mass spectrometer, wherein the chromatographic conditions are as follows: the chromatographic column is Rxi-5Sil MS30m × 0.25mm × 0.25um (RESTEK chromatography), the carrier gas is helium, the column flow is 1.2mL/min, the split ratio is 50: 1, the injection port temperature is 240 ℃, the injection amount is 1uL, purging is 3mL/min, and the column temperature program: keeping the temperature at 40 deg.C for 5min, heating to 100 deg.C at a heating rate of 6 deg.C/min, heating to 260 deg.C at a heating rate of 20 deg.C/min, keeping the temperature for 2min, and heating to 280 deg.C at a heating rate of 40 deg.C/min, and keeping the temperature for 2 min.
The gas chromatography-mass spectrometer is used for carrying out full spectrum scanning qualitative analysis on the detection liquid, SIM mode fine scanning is set at 10.5-10.8min and 11.2-11.6min, scanning is carried out in a SCAN mode at other time, the test result is shown in figure 1 (the ordinate in the figure is ion intensity, the unit of the ion intensity is not significant and is not marked), EC, PC, DEC, DMC, EMC, VC, FEC, PS and ADN are respectively detected, the peak intensities of 9 components are different, are not overlapped and are well separated, and the peak intensities of 3 components of VC, EC and PS are weaker.
Example 2
Putting 2g of electrolyte into a glass test tube, dropwise adding 0.2g of saturated sodium carbonate solution, shaking uniformly, putting the glass test tube into a tubular centrifuge, performing centrifugal separation at 3500r/min, and removing electrolyte lithium salt LiPF6And hydrofluoric acid generated by the reaction of the lithium salt with water during storage; taking supernatant in a glass test tube, filtering to obtain a sample to be detected, taking acetone as a solvent, and preparing a solution with the concentration of 1500ppmAs the solution to be tested.
Adopting a GCMS-QP2010SE model gas chromatography-mass spectrometer, wherein the chromatographic conditions are as follows: the chromatographic column is Rxi-5Sil MS30m × 0.25mm × 0.25um (RESTEK chromatography), the carrier gas is helium, the column flow is 1.5mL/min, the split ratio is 50: 1, the sample injection amount is 1uL, the purging is 3mL/min, and the column temperature program: keeping the temperature at 40 deg.C for 5min, heating to 100 deg.C at a heating rate of 6 deg.C/min, heating to 280 deg.C at a heating rate of 30 deg.C/min, keeping the temperature for 2min, and heating to 300 deg.C at a heating rate of 50 deg.C/min, and keeping the temperature for 2 min.
AND carrying out full spectrum scanning qualitative analysis on the liquid to be detected by a gas chromatography-mass spectrometer, setting SIM mode fine scanning at 10.5-10.8min AND 11.2-11.6min, scanning in an SCAN mode at other time, AND detecting EC, EMC, DEC, PC, PS AND AND in the electrolyte respectively as shown in figure 2 (the ordinate in the figure is ion strength, AND the unit does not have significance AND is not marked) of the test result.
Weighing chromatographically pure chemicals of components to be detected according to the components of the carbonate organic solvent and the functional additive determined by qualitative analysis, and preparing three groups of mixed standard solutions with different concentrations by taking acetone as a solvent, wherein the mass percentages of all organic matter components in an electrolyte sample are EC: EMC: DEC: PC: PS: AND: LiPF625: 40: 15: 4.5: 2.5: 0.5: 12.5, the component concentrations of the three sets of mixed standard solutions with different concentrations are shown in table 1:
table 13 sets of mixed standard solutions of different concentrations
| Components | Standard solution A/ppm | Standard solution B/ppm | Standard solution C/ppm |
| EC | 20 | 100 | 1000 |
| EMC | 20 | 100 | 1000 |
| DEC | 3.75 | 75 | 750 |
| PC | 6 | 30 | 300 |
| | 5 | 25 | 250 |
| AND | 1.5 | 7.5 | 75 |
Example 3
Example 3 differs from example 2 in that: in the process of pretreating the electrolyte by using a saturated sodium carbonate solution, the reaction temperature is kept at 4 ℃, and then the solution to be tested is tested. The remaining test procedures and parameters were the same as in example 2.
Detecting the standard solution B by using an ion monitoring mode of a gas chromatography-mass spectrometer, recording peak areas corresponding to all components, drawing a standard curve corresponding to the concentration and the peak areas, wherein 6 components in the electrolyte have good linearity in the standard solution B, and the correlation coefficient is 0.9999. The sample introduction of the standard solution B is repeated for 5 times, the peak area reproducibility results of the components are shown in Table 2, the peak area relative standard deviation is less than 1%, and the reproducibility is good.
TABLE 2 reproducibility of peak area for each component in Standard solution B
| EC | EMC | DEC | PC | PS | ADN | |
| 1 | 2907 | 553 | 412 | 273 | 326 | 259 |
| 2 | 2900 | 552 | 410 | 272 | 329 | 257 |
| 3 | 2903 | 549 | 412 | 275 | 324 | 258 |
| 4 | 2899 | 548 | 415 | 276 | 327 | 255 |
| 5 | 2915 | 554 | 413 | 278 | 326 | 256 |
| Average | 2905 | 551 | 412 | 275 | 326 | 257 |
| RSD％ | 0.22 | 0.47 | 0.44 | 0.85 | 0.56 | 0.62 |
Example 3 compared to example 2, the measured contents of the components in the electrolyte were more accurate, because the low temperature environment of the reaction reduced the volatilization of the electrolyte during the pretreatment of the electrolyte with the saturated sodium carbonate solution, making the contents of the components more accurate.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (8)
1. A GC-MS method for detecting carbonate organic matters and additives in lithium ion battery electrolyte is characterized by comprising the following steps:
s1: adding an inorganic solution into the electrolyte, shaking up, centrifuging, and filtering to obtain a to-be-detected electrolyte;
s2: preparing a detection solution, measuring the detection solution in an SCAN and SIM mode, and determining characteristic qualitative ion peaks of each component in the detection solution;
s3: adding a solvent into the electrolyte to be detected in S1 to prepare a liquid to be detected, detecting the liquid to be detected according to the same method of S2, and performing qualitative determination on each component to be detected in the liquid to be detected;
s4: weighing at least three groups of pure substances of the components to be detected as S3, wherein the concentrations of the components to be detected in each group are different, the mass percentages of the components to be detected are consistent, and adding a solvent to obtain at least three groups of mixed standard solutions with different concentrations;
s5: detecting each standard solution by using an ion monitoring mode of a gas chromatography-mass spectrometer, recording the peak area corresponding to each standard solution, and drawing a standard curve according to the content and the peak area of each component to be detected in each standard solution to obtain a standard curve linear equation;
s6: and detecting the solution to be detected according to the same method of S5, recording peak areas, and calculating according to the standard curve linear equation to obtain the concentration of each component to be detected in the lithium ion battery electrolyte.
2. The method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS as claimed in claim 1, wherein the chromatographic determination conditions in S3 and S3 are as follows: the chromatographic column is Rxi-5Sil MS30m multiplied by 0.25mm multiplied by 0.25um, the carrier gas is helium, the column flow is 1-1.5mL/min, the split ratio is 20: 1-50: 1, the injection port temperature is 240-: keeping the temperature at 35-45 ℃ for 3-8min, heating to 80-120 ℃ at the heating rate of 5-8 ℃/min, heating to 260 ℃ at the heating rate of 15-25 ℃/min, keeping the temperature for 1-3min, and finally heating to 300 ℃ at the heating rate of 270 ℃ to 300 ℃ at the heating rate of 10-50 ℃/min, and keeping the temperature for 1-3 min.
3. The method for detecting carbonate organic compounds and additives in the lithium ion battery electrolyte by GC-MS according to claim 1, wherein the solvent is one of acetone, methanol, ethanol or isopropanol.
4. The method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS as claimed in claim 1, wherein said inorganic solution in S1 is saturated sodium carbonate solution.
5. The method for detecting carbonate organic matters and additives in the lithium ion battery electrolyte by GC-MS as claimed in claim 1, wherein the centrifugation rate in S1 is 3000-5000 r/min.
6. The method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS as claimed in claim 1, wherein the concentration of the detection solution in S2 and the detection solution in S3 is 1500-.
7. The method for detecting carbonate organic matters and additives in lithium ion battery electrolyte by GC-MS as claimed in claim 2, wherein the chromatographic column is a weakly polar column or a non-polar column.
8. The method for detecting carbonate organic compounds and additives in lithium ion battery electrolyte by GC-MS as claimed in claim 2, wherein said column temperature program sets SIM mode fine SCAN at 10.5-10.8min and 11.2-11.6min, and SCANs in SCAN mode at other times.
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