CN101101279A - Quantitative analysis method for battery electrolyte organic components - Google Patents
Quantitative analysis method for battery electrolyte organic components Download PDFInfo
- Publication number
- CN101101279A CN101101279A CNA2006100213588A CN200610021358A CN101101279A CN 101101279 A CN101101279 A CN 101101279A CN A2006100213588 A CNA2006100213588 A CN A2006100213588A CN 200610021358 A CN200610021358 A CN 200610021358A CN 101101279 A CN101101279 A CN 101101279A
- Authority
- CN
- China
- Prior art keywords
- quantitative analysis
- analysis method
- battery electrolyte
- sample
- thing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000003792 electrolyte Substances 0.000 title claims abstract description 31
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 42
- 238000001819 mass spectrum Methods 0.000 claims abstract description 5
- 239000008151 electrolyte solution Substances 0.000 claims description 35
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 19
- 230000005477 standard model Effects 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000004440 column chromatography Methods 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000004817 gas chromatography Methods 0.000 claims description 2
- 238000004451 qualitative analysis Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 4
- 230000007547 defect Effects 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 19
- 229910001416 lithium ion Inorganic materials 0.000 description 19
- 150000002500 ions Chemical class 0.000 description 17
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 6
- 238000012113 quantitative test Methods 0.000 description 6
- 239000005486 organic electrolyte Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 206010011469 Crying Diseases 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 125000005910 alkyl carbonate group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- NPAXBRSUVYCZGM-UHFFFAOYSA-N carbonic acid;propane-1,2-diol Chemical compound OC(O)=O.CC(O)CO NPAXBRSUVYCZGM-UHFFFAOYSA-N 0.000 description 1
- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses the quantitative analysis method of organic constituent of battery solution, firstly qualitative analysis the kinds of organic constituent by using gas chromatograph hyphen mass spectrum for the waiting select electrolyte of unknown component, and then quantitative analysis the content of the kinds of organic constituent, lead in standard curve and contrastion in the process of quantitative analysis, the method of the invention skillfully conquers defects of knowing preliminarily the content of part component in existence technology, and can test the content of kinds of organic constituent of electrolyte precisely.
Description
Technical field
The present invention relates to a kind of battery electrolyte analytical approach, particularly relate to a kind of quantitative analysis method that detects organic component content in the battery electrolyte.
Background technology
Lithium-ion battery electrolytes is very responsive to performances such as the energy density of electrode and battery, cycle life, securities.Conductivity, the battery that Chen Dejun has summarized lithium ion battery organic electrolyte commonly used at 1999 the 4th (4) phase 149-153 pages or leaves of " battery industry " periodical learned the general requirement to electrolytic solution of performance such as stability and battery.Wear the Quannan and rolled up the latest developments that the 6-12 page or leaf has been reported lithium-ion battery electrolytes at 1996 the 11st at " the 22nd physical power source nd Annual Meeting collection of China ".For lithium ion battery, selecting suitable organic electrolyte is one of crux problem that obtains high-energy-density, long circulation life and cell safety.The initial charge/discharge capacity of battery has sizable difference owing to the combination of material with carbon element and electrolytic solution is different, so lay special stress on electrolytic solution will adapt with carbon anode when the design battery.In the commodity lithium ion battery, the most frequently used lithium salts of electrolytic solution is LiPF
6, solvent is that cyclic carbonate Arrcostab (EC, PC etc.) and chain alkyl carbonate (DEC, DMC, DME and EMC) mix, and is binary, ternary or multicomponent system that main body is formed with EC.Organic electrolyte plays a part to carry lithium ion between the both positive and negative polarity of lithium ion battery, although can form electrolytic solution by a variety of organic solvents and lithium salts, but that really can use in lithium ion battery is few in number, because separate liquid and must satisfy some specific performance properties requirements should having access to electricity.
The organic component of lithium-ion battery electrolytes mainly contains:
Dimethyl carbonate ((CH
3O)
2CO) Dimethyl Carbonate, DMC
Diethyl carbonate (C
2H
5O)
2CO Diethyl Carbonate, DEC
Ethylene carbonate ester C
3H
4O
3Ethylene Carbonate, EC
Propylene glycol carbonate C
4H
6O
3Propylene Carbonate, PC
Methyl ethyl carbonate (C
2H
5O) CO (OCH
3) Ethyl Methyl carbonate, EMC
Bradley A.Johnson and Ralph E.white were at J.of Power Sour periodical in 1998, the 70th volume 48-54 page or leaf proposes to utilize GC/MS to analyze the lithium ion battery organic electrolyte, and they have collected Sony, Sanyo Electric, Matsushita Electric Industrial, MoliEnergy and A﹠amp; 85 lithium ion batteries of T Battery five companies are analyzed.Article utilizes gas chromatograph-mass spectrometer (GCMS) (GC/MS) only each component of lithium ion battery organic electrolyte to be carried out qualitative analysis, quantitative test is not done in this experiment, but confirmed substantially except the Sony electrolyte system be principal ingredient (its negative material is coke Coke) with PC, the electrolyte system of other company is principal ingredient (its negative material is graphite GraPhite) with EC.
Because the performances such as specific inductive capacity of different solvents are different, therefore by the variety classes solvent, and the performances such as conductivity of the lithium-ion battery electrolytes of different proportion solvent composition different fully, thereby different solvent compositions can directly have influence on the performance index of lithium-ion battery electrolytes, is directly connected to the quality of product.Therefore, select suitable lithium-ion battery electrolytes component Determination on content method for use, to the monitoring in the electrolytic solution production run, guarantee that prescription is correct and the analysis of known electrolytes solvent component etc. all had crucial effect.
The Chinese patent application CN200410027764.6 of domestic Biyadi Co Ltd (publication number: CN1712956A) provide a kind of gas chromatograph-mass spectrometer (GCMS) that utilizes to adopt the method for selecting ion method that lithium-ion battery electrolytes organic solvent component is carried out quantitative test.When this method is carried out quantitative test to electrolytic solution, require at first the mass ratio of each organic component in the testing sample to be estimated, with the reference of this mass ratio as the mass ratio of each organic component in the preparation standard sample, this requirement is infeasible for analyzing all unknown electrolytic solution of a kind of component and content.Another Chinese patent application CN200410066175.9 adopts area to proofread and correct normalization method solvent is measured, because the method requires the peak of all components all will to measure and proofread and correct, carrying out quantitatively so this method can only be used for the mixed solvent of electrolytic solution before adding salt, quantitatively also is inaccurate for electrolytic solution.
Summary of the invention
The objective of the invention is at the problems of the prior art, a kind of quantitative analysis method that can accurately detect organic component content in the battery electrolyte is provided.
For achieving the above object, the present invention has adopted following technical scheme:
The invention discloses a kind of quantitative analysis method of battery electrolyte organic components, may further comprise the steps:
The kind of organic component in a, the qualitative detection electrolytic solution to be measured;
B, at least two parts of standard models of configuration, every part of standard model contains the above-mentioned organic component of specified rate and contrasts thing;
C, configuration testing sample contain the electrolytic solution to be measured of specified rate and contrast thing in the testing sample;
D, usefulness gas chromatograph-mass spectrometer (GCMS) (GC/MS) examination criteria sample, according to the gas chromatography-mass spectrum testing result each organic component is generated a typical curve respectively, described typical curve horizontal ordinate is this organic component content and the ratio of contrasting thing content, and ordinate is the response of this organic component in gas chromatography-mass spectrometry analysis and the ratio of contrasting the thing response;
E, detect testing sample, calculate the content of each organic component in electrolytic solution to be measured by the specified rate according to thing and electrolytic solution to be measured in typical curve and the testing sample with gas chromatograph-mass spectrometer (GCMS).
When detecting testing sample with gas chromatograph-mass spectrometer (GCMS) (GC/MS), the response of each organic component is this organic component content and the ratio of contrasting thing content in the testing sample with ratio pairing horizontal ordinate on the respective standard curve of contrasting the thing response in the testing result, thereby, again according to just calculating the content of this organic component in electrolytic solution to be measured according to the content of thing and the content of electrolytic solution to be measured in the testing sample.
Among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, the scanning of the mass spectrum process adopts the mode of selecting ion scan.
In standard model and testing sample, identical according to the content of thing, get the unit content of being convenient to calculate usually.
Among the present invention, the condition that should satisfy according to thing comprises: 1, do not exist in testing sample; 2, chemical property is similar to the organic component in the electrolytic solution to be measured, thereby makes retention time approach organic component in the electrolytic solution to be measured; 3, do not react with testing sample; 4, chromatogram stable in properties; 5, can be when GC/MS analyzes in interested component, flow out near the organic component promptly to be measured.
Among described step b and the step c, when configuration standard sample or testing sample, adopt same organic solvent, described organic solvent comprises acetone, isopropyl alcohol, ethanol, methylene chloride, preferred acetone.
Among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, setting solvent time delay is 0.5～2min, sample size is 0.2～2.0 μ L, the injection port split ratio is 20～100: 1, and sample size hour influences measuring accuracy very much, and can influence the degree of separation at peak when too big.
Gas chromatography adopts capillary column chromatography, and used capillary column is a quartz capillary column, model: HP-5MS, and specification is 0.25mm*30m*0.25 μ m.
Column temperature is temperature programme: 50 ℃ of initial temperatures, and constant temperature 1～3min is warming up to 250 ℃ with 20～30 ℃/min speed, constant temperature 2～5min then; 250～300 ℃ of injector temperatures; Injection port pressure is 82Kpa, and carrier gas is high-purity He, flow rate of carrier gas 1.0mL/min.
The mass spectroscopy condition is: EI ion gun, electron energy 70ev, 220～240 ℃ of ion source temperatures, 140～160 ℃ of quadrupole rod temperature, 270～290 ℃ of interface temperature, electron-multiplier voltage 1800V, the full spectrum scanning in ion detection mass-to-charge ratio m/z=10～450.
Because adopted above scheme, the beneficial effect that the present invention is possessed is:
The present invention utilizes gas chromatography-mass spectrography the electrolytic solution to be measured of component the unknown to be adopted the kind of first qualitative analysis organic component, the method of each organic component content of quantitative test again, in the quantitative test process, also adopt according to thing by introducing typical curve, overcome dexterously and must understand the defective of part component concentration in the prior art in advance, thereby can determine the content of each organic component in the electrolytic solution comparatively exactly; Adopt according to thing to reduce experimental error between each standard model, guaranteed the accuracy that typical curve is drawn; When utilizing method of the present invention to detect electrolytic solution to be measured, whether electrolytic solution detected before or after adding salt does not have particular requirement, has enlarged the range of application of the inventive method.
Description of drawings
Fig. 1 is the GC/MS image of standard model 1.
Fig. 2 carries out GC/MS to standard model to analyze the DMC canonical plotting of being done.
Fig. 3 carries out GC/MS to standard model to analyze the EMC canonical plotting of being done.
Fig. 4 carries out GC/MS to standard model to analyze the EC canonical plotting of being done.
Fig. 5 is the GC/MS image of testing sample.
Embodiment
Also the present invention is described in further detail in conjunction with the accompanying drawings below by specific embodiment.
With present widely used lithium-ion battery electrolytes EC/EMC/DMC system is example.
1, instrument and material
Use instrument: Agilent 6890N gas chromatograph, Agilent 5973 mass detector organic solvents are acetone reagent: Fujian Province's three spherings are learned reagent company limited and are produced, chromatographically pure.
Standard organic component: EC, EMC, DMC, DEC
2, testing process
1) thing is contrasted in organic component in the qualitative analysis testing sample and selection:
When the lithium-ion battery electrolytes sample to composition the unknown detects, at first adopt Bradley A.Johnson and Ralph E.white at J.of Power Sour periodical in 1998, method described in the 70th volume 48-54 page or leaf, utilize gas chromatograph-mass spectrometer (GCMS) (GC/MS) that each organic component of electrolytic solution is carried out qualitative analysis, detect the kind of organic component contained in the unknown electrolytic solution.Select according to thing according to testing result.Selected must be the composition that does not comprise in the electrolytic solution to be measured according to thing, the organic component similar performance in chemical property and the electrolytic solution to be measured, and do not react with electrolytic solution to be measured.Selected also must satisfy the chromatogram stable in properties according to thing, can be when GC/MS analyzes in interested component, flow out near the organic component promptly to be measured.
In the present embodiment, for ease of the accuracy of assessment the inventive method, adopt the kind and all known electrolytic solution sample of content of organic component to detect.Used electrolytic solution sample is present widely used lithium-ion battery electrolytes EC/EMC/DMC system, and the organic component that is comprised is EC, EMC, DMC, and selects for use DEC as contrasting thing.
2) preparation of standard model:
According to the kind of organic component in the electrolytic solution sample to be measured and selected according to thing, respectively from the organic component of each standard and according to the thing by below the accurate weighing of listed numerical value in the table 1, and be mixed with standard model 1～5 in the form.
Table 1
| |
|
|
|
|
|
| DEC (according to thing)/g | 1.0000 | 1.0000 | 1.0000 | 1.0000 | 1.0000 |
| EMC/g | 1.0000 | 2.0000 | 3.0000 | 4.0000 | 5.0000 |
| EC/g | 1.0000 | 2.0000 | 3.0000 | 4.0000 | 5.0000 |
| DMC/g | 1.0000 | 2.0000 | 3.0000 | 4.0000 | 5.0000 |
More than 5 standard specimens in the volumetric flask of 500ml, prepare respectively, prepared the back be settled to scale with acetone.Get five standard specimens respectively with the injection sampler more afterwards and in sample bottle, wait for upward sample in right amount.
3) preparation of testing sample
Accurately take by weighing 3g electrolytic solution to be measured in the 500ml volumetric flask, and add 1g, be settled to scale with acetone again according to thing DEC.Get testing sample with the injection sampler afterwards and in sample bottle, wait for upward sample in right amount.
4) utilize GC/MS that standard model is carried out scanning analysis and sets up typical curve
Setting solvent time delay: 1min, sample size: 0.2 μ L, injection port split ratio: 20: 1
The condition determination of capillary column chromatography: quartz capillary column, model: HP-5MS, 0.25mm*30m*0.25 μ m
Column temperature is temperature programme: 50 ℃ of initial temperatures, and constant temperature 1min is warming up to 250 ℃ with 25 ℃/min speed, constant temperature 3min;
280 ℃ of injector temperatures; Carrier gas is high-purity He, and pressure is 82Kpa, flow rate of carrier gas 1.0mL/min, total flow 12.4mL/min
Mass spectroscopy condition: EI ion gun, electron energy 70ev, 230 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature, 280 ℃ of interface temperature, electron-multiplier voltage 1800V, the full spectrum scanning in ion detection mass-to-charge ratio m/z=20～300.
The retention time scope that records each component is as follows:
Table 2
| Component | Retention time scope (min) | |
| DMC | t0～t1 | 1.6～2.0 |
| EMC | t1～t2 | 2.0～2.4 |
| DEC (according to thing) | t2～t3 | 2.4～4.0 |
| EC | t3～t4 | 4.0～10 |
Figure is as shown in Figure 1 as a result for the GC/MS of standard model 1.
The mass spectrometer scanning process adopts the mode of selecting ion scan, characteristic ion and qualification ion (as shown in table 3 below) by each selected component carry out scanning analysis to standard model 1～5, and according to scanning result each organic component is set up a typical curve respectively, as Fig. 2 to shown in Figure 4.In the typical curve, horizontal ordinate be in the sample each component concentration with according to the ratio of thing content, ordinate be the response (GC/MS is the integral area of chromatographic peak among the figure as a result) and the ratio of contrasting the thing response of each component.The so-called mode of selecting ion scan is meant from total quasi-molecular ions of fractions tested selects several ionic strengths and mass-to-charge ratio (m/z) big and can represent the quasi-molecular ions of this component, carry out test scan, wherein can represent the ion of this component is characteristic ion, and crying of other limits ion.
Table 3
| Component | Characteristic ion (m/z) | Limit ion (m/z) | ||
| DEC (according to thing) | 91.0 | 63.0 | 45.0 | 29.0 |
| DMC | 59.0 | 45.0 | 31.0 | 29.0 |
| EMC | 77.0 | 59.0 | 45.0 | 29.0 |
| EC | 88.0 | 43.0 | 44.0 | 29.0 |
5) utilize GC/MS that testing sample is scanned, calculate each component concentration according to typical curve
Adopt condition and the method identical that testing sample is carried out the GC/MS test analysis with standard model.Figure is as shown in Figure 5 as a result for the GC/MS of testing sample.With the response of each component in the testing sample with according to the ratio of thing response as ordinate, and on the typical curve of respective components, obtain corresponding horizontal ordinate, this horizontal ordinate is this component concentration and the ratio of contrasting thing content, thereby tries to achieve this component concentration in the testing sample.
Resulting result is as shown in the table:
Table 4
| Component | DMC | EMC | EC | DMC∶EMC∶EC |
| Actual value | 33.33％ | 33.33％ | 33.34％ | 1.00∶1.00∶1.00 |
| Measured value | 30.68％ | 31.14％ | 30.71％ | 1.00∶1.01∶1.00 |
The result of last table 4 shows, when adopting method of the present invention that the battery electrolyte of composition the unknown is carried out the quantitative test of organic component, measured value can react truth more exactly, method accuracy height of the present invention, reliable results.
Claims (9)
1, a kind of quantitative analysis method of battery electrolyte organic components may further comprise the steps:
The kind of organic component in a, the qualitative detection electrolytic solution to be measured;
B, at least two parts of standard models of configuration, every part of standard model contains the above-mentioned organic component according to thing and specified rate of specified rate;
C, configuration testing sample contain the electrolytic solution to be measured of specified rate and contrast thing in the testing sample;
D, usefulness gas chromatograph-mass spectrometer (GCMS) (GC/MS) examination criteria sample, according to the gas chromatography-mass spectrum testing result each organic component is generated a typical curve respectively, described typical curve horizontal ordinate is this organic component content and the ratio of contrasting thing content, and ordinate is the response of this organic component in gas chromatography-mass spectrometry analysis and the ratio of contrasting the thing response;
E, detect testing sample, calculate the content of each organic component in electrolytic solution to be measured by the specified rate according to thing and electrolytic solution to be measured in typical curve and the testing sample with gas chromatograph-mass spectrometer (GCMS).
2, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 is characterized in that: among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, the scanning of the mass spectrum process adopts the mode of selecting ion scan.
3, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2 is characterized in that: in described standard model and the testing sample, all identical according to the content of thing.
4, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2, it is characterized in that: among described step b and the step c, when configuration standard sample or testing sample, adopt same organic solvent, described organic solvent comprises acetone, isopropyl alcohol, ethanol, methylene chloride.
5, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 4 is characterized in that: described organic solvent is an acetone.
6, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2, it is characterized in that: among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, setting solvent time delay is 0.5～2min, sample size is 0.2～2.0 μ L, and the injection port split ratio is 20～100: 1.
7, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2, it is characterized in that: among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, gas chromatography adopts capillary column chromatography, and used capillary column is a quartz capillary column.
8, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2, it is characterized in that: among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, column temperature is temperature programme: 50 ℃ of initial temperatures, constant temperature 1～3min, be warming up to 250 ℃ with 20～30 ℃/min speed then, constant temperature 2～5min; 250～300 ℃ of injector temperatures; Injection port pressure is 82Kpa, and carrier gas is high-purity He, flow rate of carrier gas 1.0mL/min.
9, the quantitative analysis method of a kind of battery electrolyte organic components according to claim 1 and 2, it is characterized in that: among described steps d and the step e, during with the gas chromatograph-mass spectrometer (GCMS) test sample, the mass spectroscopy condition is: EI ion gun, electron energy 70ev, 220～240 ℃ of ion source temperatures, 140～160 ℃ of quadrupole rod temperature, 270～290 ℃ of interface temperature, electron-multiplier voltage 1800V, the full spectrum scanning in ion detection mass-to-charge ratio m/z=10～450.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100213588A CN101101279A (en) | 2006-07-04 | 2006-07-04 | Quantitative analysis method for battery electrolyte organic components |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100213588A CN101101279A (en) | 2006-07-04 | 2006-07-04 | Quantitative analysis method for battery electrolyte organic components |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101101279A true CN101101279A (en) | 2008-01-09 |
Family
ID=39035660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100213588A Pending CN101101279A (en) | 2006-07-04 | 2006-07-04 | Quantitative analysis method for battery electrolyte organic components |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101101279A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236561A (en) * | 2013-03-29 | 2013-08-07 | 东莞市杉杉电池材料有限公司 | Method for detecting alkylsilazane compounds in lithium hexafluorophosphate electrolyte |
| CN104792901A (en) * | 2015-05-06 | 2015-07-22 | 哈尔滨工业大学 | Quantitative measuring method of lithium ion battery electrolyte solvent |
| CN105242211A (en) * | 2015-09-02 | 2016-01-13 | 国网电力科学研究院武汉南瑞有限责任公司 | All-vanadium redox flow battery fault rapid detection and location method |
| CN105467058A (en) * | 2016-01-25 | 2016-04-06 | 惠州市豪鹏科技有限公司 | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte |
| CN106124675A (en) * | 2016-06-13 | 2016-11-16 | 合肥国轩高科动力能源有限公司 | Method for pretreatment of lithium battery electrolyte chromatographic test |
| CN106841465A (en) * | 2017-02-17 | 2017-06-13 | 南通新宙邦电子材料有限公司 | A kind of lithium battery electrolytes detection method |
| CN108027352A (en) * | 2015-10-06 | 2018-05-11 | 株式会社Lg化学 | Use the high-speed gas analyzing device and its method of gas chromatography |
| CN117849247A (en) * | 2024-03-05 | 2024-04-09 | 上海瑞浦青创新能源有限公司 | Electrolyte detection method |
-
2006
- 2006-07-04 CN CNA2006100213588A patent/CN101101279A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236561A (en) * | 2013-03-29 | 2013-08-07 | 东莞市杉杉电池材料有限公司 | Method for detecting alkylsilazane compounds in lithium hexafluorophosphate electrolyte |
| CN103236561B (en) * | 2013-03-29 | 2015-04-15 | 东莞市杉杉电池材料有限公司 | Method for detecting alkylsilazane compounds in lithium hexafluorophosphate electrolyte |
| CN104792901A (en) * | 2015-05-06 | 2015-07-22 | 哈尔滨工业大学 | Quantitative measuring method of lithium ion battery electrolyte solvent |
| CN105242211B (en) * | 2015-09-02 | 2019-03-26 | 国网电力科学研究院武汉南瑞有限责任公司 | A kind of all-vanadium flow battery failure quickly detects localization method |
| CN105242211A (en) * | 2015-09-02 | 2016-01-13 | 国网电力科学研究院武汉南瑞有限责任公司 | All-vanadium redox flow battery fault rapid detection and location method |
| CN108027352A (en) * | 2015-10-06 | 2018-05-11 | 株式会社Lg化学 | Use the high-speed gas analyzing device and its method of gas chromatography |
| CN105467058A (en) * | 2016-01-25 | 2016-04-06 | 惠州市豪鹏科技有限公司 | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte |
| CN105467058B (en) * | 2016-01-25 | 2017-05-17 | 惠州市豪鹏科技有限公司 | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte |
| CN106124675A (en) * | 2016-06-13 | 2016-11-16 | 合肥国轩高科动力能源有限公司 | Method for pretreatment of lithium battery electrolyte chromatographic test |
| CN106124675B (en) * | 2016-06-13 | 2019-07-19 | 合肥国轩高科动力能源有限公司 | Method for pretreatment of lithium battery electrolyte chromatographic test |
| CN106841465A (en) * | 2017-02-17 | 2017-06-13 | 南通新宙邦电子材料有限公司 | A kind of lithium battery electrolytes detection method |
| CN106841465B (en) * | 2017-02-17 | 2019-09-10 | 南通新宙邦电子材料有限公司 | A kind of lithium battery electrolytes detection method |
| CN117849247A (en) * | 2024-03-05 | 2024-04-09 | 上海瑞浦青创新能源有限公司 | Electrolyte detection method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101101279A (en) | Quantitative analysis method for battery electrolyte organic components | |
| CN104792901B (en) | A kind of method for quantitative measuring of lithium-ion battery electrolytes solvent | |
| CN110412102B (en) | Method for determining additive content in lithium ion battery electrolyte | |
| Terborg et al. | Development of gas chromatographic methods for the analyses of organic carbonate-based electrolytes | |
| CN105467058B (en) | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte | |
| US10804562B2 (en) | Method and system for determining concentration of electrolyte components for lithium-ion cells | |
| CN110808203A (en) | Device and method for quickly and accurately detecting impurities in high-purity hydrogen for hydrogen fuel cell | |
| Tao et al. | Protocol for quantifying inactive lithium in anode-free lithium batteries by mass spectrometry titration | |
| CN102788856B (en) | The analytical approach of elementary sulfur quantitative and qualitative analysis in liquefied petroleum gas (LPG) | |
| CN109212112B (en) | Method for detecting inorganic salt in lithium ion electrolyte | |
| CN100348975C (en) | Quantitative analysis for electrolytic liquor organic component of lithium ion battery | |
| CN102445364A (en) | Gathering device of gas produced in lithium ion battery | |
| CN209247678U (en) | Battery electrolyte condition checkout gear | |
| CN110726785A (en) | SF analysis based on GC-Q-ToF-MS6Method for medium trace permanent gas | |
| CN111060608A (en) | Method for detecting alkyl silicon compounds in lithium ion battery electrolyte | |
| CN205581220U (en) | Lithium ion battery electrode material electrical performance test device | |
| CN110220887A (en) | A method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal | |
| US20220011281A1 (en) | Ion-exchange chromatography system for analyzing electrolyte solution, method of quantitative analysis of lithium salts in electrolyte solution, and preparation method for electrolyte solution using same | |
| CN100405055C (en) | Method for detecting oxidation preventive content in jet fuel | |
| CN1314960C (en) | Method for measurement of solvent in lithium ion battery electrolyte | |
| CN114965344A (en) | Quantitative analysis method for SEI (solid electrolyte interphase) film of lithium ion battery cathode | |
| CN115808474A (en) | Method for detecting lithium analysis content of lithium ion battery | |
| CN103940888A (en) | Method used for detecting anti-oxidant content of transformer oil via linear sweep voltammetry | |
| CN111141725A (en) | Quantitative detection method for lithium hexafluorophosphate in lithium ion battery electrolyte | |
| KR101372010B1 (en) | A method for analyzing the components in an electrolytic solution of lithium-ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20080109 |