CN1243245A - Method for detection of micro water-content in non-water electrolyte, and infrared absorbing pool - Google Patents
Method for detection of micro water-content in non-water electrolyte, and infrared absorbing pool Download PDFInfo
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- CN1243245A CN1243245A CN 99109463 CN99109463A CN1243245A CN 1243245 A CN1243245 A CN 1243245A CN 99109463 CN99109463 CN 99109463 CN 99109463 A CN99109463 A CN 99109463A CN 1243245 A CN1243245 A CN 1243245A
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- electrolytic solution
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- absorption cell
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Abstract
The present invention relates to a method for determining micro water content in LiAlCl4-SOCl2 non-aqueous electrolytic solution and its infrared absorption cell. Said method includes the following steps: firstly, making working curve of absorbance and water content, then measuring the water content in the sample, andthe described infrared quartz absorption cell can be sealed, and is formed from quartz absorption cell body whose upper portion possesses a ground mouth in which a teflon plug can be closely fitted with the ground mouth. The use of said method can monitor the micro water content in the LiAlCl4-SOCl2 electrolytic solution.
Description
The invention belongs to a kind of water content method for measuring and apparatus field, be specifically related to a kind of LiAlCl
4-SOCl
2Trace water assay method and cell for infrared absorption thereof in the nonaqueous electrolytic solution.
In lithium battery, meet water fierce reaction can take place, discharge the gas harmful, not only consume lithium, and worsen battery performance battery as the lithium metal of negative pole.So must adopt nonaqueous electrolytic solution.At Li-SOCl
2In the series battery, electrolytic solution is with inorganic salts LiAlCl
4Be dissolved in SOCl with finite concentration
2In, prepare inorganic electrolyte liquid LiAlCl
4-SOCl
2Water can not exist with free state in this electrolytic solution, it can and SOCl
2Reaction generates SO rapidly
2And HCl, with LiAlCl
4Reaction generates LiAl (OH) Cl
3And HCl.Reaction product HCl and LiAl (OH) Cl
3The Cl that in electrolytic solution, forms
-, OH
-React together with lithium metal.Therefore, LiAlCl
4-SOCl
2Moisture content in the nonaqueous electrolytic solution electrolytic solution must strict control.Because moisture content is at LiAlCl
4-SOCl
2Can not exist with free state in the electrolytic solution, then Chang Gui moisture content part analysis method all can not be used as Ka Erfeixiufa, vapor-phase chromatography etc.In the prior art, all unmatchful both at home and abroad LiAlCl
4-SOCl
2Electrolytic solution carries out the bibliographical information of moisture content control part analysis method.
The object of the present invention is to provide trace water assay method and cell for infrared absorption thereof in a kind of nonaqueous electrolytic solution.To realize monitoring to trace water in this electrolytic solution, improve the performance of lithium battery, prolong it and receive the order.
The object of the present invention is achieved like this: trace water assay method in a kind of nonaqueous electrolytic solution may further comprise the steps successively:
A. room temperature, relative humidity less than 2% condition under, quantitative minor amount of water is injected SOCl
2Or LiAlCl
4-SOCl
2In the electrolytic solution sample;
B. under condition same as described above, extract quantitative sample, inject dry infrared quartz absorption cell from the above-mentioned electrolytic solution that has injected quantitative minor amount of water, and the stopper of rapid jam-pack cell for infrared absorption;
C. the infrared absorption spectrum of the sample of gained among the determination step b calculates this electrolytic solution sample at 2780cm
-1And 3379cm
-1The absorbance part at place Wei A
1And A
2
D. change to inject the consumption of electrolytic solution sample minor amount of water, repeat the operation of above a to c, draw the working curve of the content C of minor amount of water in electrolytic solution absorbance A-electrolytic solution sample according to the gained data, the intercept part that draws two working curves Wei a
1, a
2, slope part of two working curves Wei K
1, K
2
E. be sample with the electrolytic solution in the actual production, press the infrared absorption spectrum of this sample of time-and-motion study of above-mentioned a to c, calculate the content of moisture content in this sample as follows:
Described infrared quartz absorption cell seals, and is made up of quartzy absorption cell body, and a ground is arranged at the top of quartzy absorption cell, have in the ground one can with the teflon stopper of ground driving fit.A kind of microinjection apparatus that is used for this method comprises syringe, is connected with dry polyethylene pipe on the syringe needle of syringe, and the other end of polyethylene pipe is connected with glass capillary.
Good effect of the present invention is: can monitor LiAlCl
4-SOCl
2Water content in the electrolytic solution makes the production of a hermetically sealed lithium-thionyl chloride battery be able to normally carry out by quality control requirement, is being one of indispensable means aspect the storage life that guarantees lithium-thionyl chloride battery electrical property and sealing and length.
Below in conjunction with drawings and Examples the present invention is further described:
Accompanying drawing 1 is the working curve of the content C of minor amount of water in electrolytic solution absorbance A-electrolytic solution sample;
Embodiment:
Trace water assay method in a kind of nonaqueous electrolytic solution may further comprise the steps successively:
A. room temperature, relative humidity less than 2% condition under, the glass capillary that quantitative minor amount of water will be housed with dry polyethylene pipe connects with the syringe needle of 5 μ l micro syringes, and quantitative minor amount of water is injected SOCl
2Or LiAlCl
4-SOCl
2In the electrolytic solution sample;
B. under condition same as described above, 10ml glass syringe with dry zone tygon tubule, extract victory 10ml sample from the above-mentioned electrolytic solution that has injected quantitative minor amount of water, inject dry infrared quartz absorption cell, and the stopper of rapid jam-pack cell for infrared absorption;
C. the infrared absorption spectrum of the sample of gained among the determination step b calculates this electrolytic solution sample at 2780cm
-1And 3379cm
-1The absorbance part at place Wei A
1And A
2
D. change the consumption that injects electrolytic solution sample minor amount of water, repeat the operation of above a to c, the working curve of drawing the content C of minor amount of water in electrolytic solution absorbance A-electrolytic solution sample according to the gained data as shown in Figure 1, the intercept part that draws two working curves Wei a
1=0, a
2Article=0.005, two, slope part of working curve Wei K
1=0.0076, K
2=0.0040;
E. be sample with the electrolytic solution in the actual production, press the infrared absorption spectrum of this sample of time-and-motion study of above-mentioned a to c, obtain A
1=0.0378, A
2=0.1761, calculate the content of moisture content in this sample as follows:
=47.523 (μ g/g) so, the water content in this batch sample is 47.523 μ g/g.
As shown in Figure 2, used infrared quartz absorption cell can seal, and it is made up of quartzy absorption cell body 3, and a ground 2 is arranged on the top of quartzy absorption cell body 3, have in the ground 2 one can with the teflon stopper 1 of ground driving fit.
Claims (3)
1. trace water assay method in the nonaqueous electrolytic solution may further comprise the steps successively: a. room temperature, relative humidity less than 2% condition under, quantitative minor amount of water is injected SOCl
2Or LiAlCl
4-SOCl
2In the electrolytic solution sample; B. under condition same as described above, extract quantitative sample, inject dry infrared quartz absorption cell from the above-mentioned electrolytic solution that has injected quantitative minor amount of water, and the stopper of rapid jam-pack cell for infrared absorption; C. the infrared absorption spectrum of the sample of gained among the determination step b calculates this electrolytic solution sample at 2780cm
-1And 3379cm
-1The absorbance part at place Wei A
1And A
2D. change to inject the consumption of electrolytic solution sample minor amount of water, repeat the operation of above a to c, draw the working curve of the content C of minor amount of water in electrolytic solution absorbance A-electrolytic solution sample according to the gained data, the intercept part that draws two working curves Wei a
1, a
2, slope part of two working curves Wei K
1, K
2E. be sample with the electrolytic solution in the actual production, press the infrared absorption spectrum of this sample of time-and-motion study of above-mentioned b to c, calculate the content of moisture content in this sample as follows:
2. one kind is used for the infrared quartz absorption cell of method according to claim 1, form by quartzy absorption cell body (3), it is characterized in that: a ground (2) is arranged at the top of quartzy absorption cell body (3), have in the ground one can with the teflon stopper (1) of ground driving fit.
3. one kind is used for the microinjection apparatus of method according to claim 1, comprises syringe, it is characterized in that: be connected with dry polyethylene pipe on the syringe needle of syringe, the other end of polyethylene pipe is connected with glass capillary.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99109463 CN1110697C (en) | 1999-07-07 | 1999-07-07 | Method for detection of micro water-content in non-water electrolyte, and infrared absorbing pool |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99109463 CN1110697C (en) | 1999-07-07 | 1999-07-07 | Method for detection of micro water-content in non-water electrolyte, and infrared absorbing pool |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1243245A true CN1243245A (en) | 2000-02-02 |
| CN1110697C CN1110697C (en) | 2003-06-04 |
Family
ID=5273934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99109463 Expired - Fee Related CN1110697C (en) | 1999-07-07 | 1999-07-07 | Method for detection of micro water-content in non-water electrolyte, and infrared absorbing pool |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1110697C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113686801A (en) * | 2021-09-03 | 2021-11-23 | 武汉昊诚锂电科技股份有限公司 | Method for measuring water absorption capacity of lithium-ion battery electrolyte based on infrared spectroscopy |
-
1999
- 1999-07-07 CN CN 99109463 patent/CN1110697C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113686801A (en) * | 2021-09-03 | 2021-11-23 | 武汉昊诚锂电科技股份有限公司 | Method for measuring water absorption capacity of lithium-ion battery electrolyte based on infrared spectroscopy |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1110697C (en) | 2003-06-04 |
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| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20030604 Termination date: 20130707 |