CN116008459A - Quantitative detection method for purity of sodium bisoxalato borate - Google Patents
Quantitative detection method for purity of sodium bisoxalato borate Download PDFInfo
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Abstract
The invention provides a quantitative detection method for purity of sodium bisoxalato borate, belongs to the field of purity analysis, and can solve the technical problems that the traditional method for detecting content of sodium bisoxalato borate is complex in operation process, large in error and incapable of truly reflecting the content of sodium bisoxalato borate. The detection method comprises the following steps: firstly, dissolving sodium bisoxalato borate in an organic solvent to prepare a solution to be detected, then establishing a standard curve by using bisoxalato borate ion standard solutions with different concentrations, finally measuring the peak area of the solution to be detected by adopting an ion chromatography, and calculating the content of the sodium bisoxalato borate in the solution to be detected according to the standard curve; wherein, the blocking liquid is used for blocking when the solution to be detected is sampled. The quantitative detection method for the purity of the sodium bisoxalato borate provided by the invention has the characteristics of simplicity and convenience in operation, high accuracy, short time consumption and high efficiency, and can be applied to the aspect of quantitative detection of the sodium bisoxalato borate.
Description
Technical Field
The invention belongs to the field of purity analysis, and particularly relates to a quantitative detection method for purity of sodium bisoxalato borate.
Background
The sodium bisoxalato borate is an important sodium ion battery additive, has the advantages of high ionic conductivity, wide electrochemical stability window, good thermal stability, good cycling stability and the like, can improve the stability of a negative electrode SEI film, improves the electrochemical performance of a battery, has high-temperature cycling performance, has high safety performance and has very broad market prospect. The composition of the electrolyte is one of the key factors influencing the performance of sodium batteries, and the development of high-performance electrolyte salts and additives is the key to the development of the batteries. Important indexes such as the storage capacity, electrochemical performance, safety performance and the like of the sodium ion battery are closely related to the purity and impurities of electrolyte salt and additives. It can be seen that the quantitative determination of battery additives and the like is a key to the evaluation/prediction of the above-mentioned important indicators of sodium ion batteries.
At present, the traditional method for detecting the content of the sodium bisoxalato borate generally adopts a method for respectively measuring the content of sodium, the content of boron and the content of oxalic acid radical in the product. For example, titration is used for sodium content, titration is used for boron content, and titration is used for oxalate content. However, the detection methods are complicated in pretreatment process steps, the content of the sodium bisoxalato borate is indirectly inferred, the content of the sodium bisoxalato borate cannot be directly and truly reflected, and errors of various detection methods are superimposed and larger.
Therefore, a direct quantitative detection method for the purity of the sodium bisoxalato borate, which has the advantages of high accuracy, short time consumption, convenient test and high efficiency, is urgently needed.
Disclosure of Invention
Aiming at the technical problems that the traditional method for detecting the content of the sodium bisoxalato borate is complex in operation process, large in error and incapable of truly reflecting the content of the sodium bisoxalato borate, the invention provides the quantitative detection method for the purity of the sodium bisoxalato borate, and the quantitative detection method has the characteristics of simplicity and convenience in operation, high accuracy, short time consumption and high efficiency.
In order to achieve the above purpose, the invention adopts the following technical scheme:
firstly, dissolving sodium bisoxalato borate in an organic solvent to prepare a solution to be detected, then establishing a standard curve by using bisoxalato borate ion standard solutions with different concentrations, finally measuring the peak area of the solution to be detected by adopting an ion chromatography, and calculating the content of the sodium bisoxalato borate in the solution to be detected according to the standard curve; wherein, the blocking liquid is used for blocking when the solution to be detected is sampled.
In one embodiment, the mass ratio of the sodium bisoxalato borate to the organic solvent is 1: (500-1500).
In one embodiment, the organic solvent is selected from any one of methanol, ethylene glycol dimethyl ether, ethylene carbonate, or propylene carbonate.
In one embodiment, the barrier fluid is selected from acetonitrile or dimethyl carbonate, the acetonitrile being chromatographic grade, the content being > 99.9%.
In one embodiment, the ion chromatography conditions are:
a detector: a conductivity detector;
chromatographic column: metrosep A support 7;
column temperature: 35-40 ℃;
flow rate: 0.7mL/min;
quantitative ring: 50. Mu.L.
In one embodiment, the quantitative determination method for purity of sodium bisoxalato borate specifically comprises the following steps:
preparing a solution to be tested: dissolving the weighed sodium bisoxalato borate in an organic solvent to prepare a solution to be measured;
standard curve establishment: according to the content of the sodium bisoxalato borate in the solution to be detected, diluting the bisoxalato borate ion standard solution into bisoxalato borate ion standard solutions with different concentration gradients, measuring peak areas by adopting an ion chromatography, and establishing a standard curve by taking the concentration as an abscissa and the corresponding peak area as an ordinate;
quantitative determination of sodium bisoxalato borate: and measuring the solution to be measured by adopting an ion chromatography, blocking by using a blocking liquid after the solution to be measured is injected, measuring the peak area of the solution to be measured under the action of a high-concentration organic phase mobile phase, and calculating the content of sodium bisoxalato borate in the solution to be measured according to the standard curve.
In one embodiment, the high concentration organic phase mobile phase is (20.0-30.0) mmol/L sodium carbonate in water, 40% acetonitrile.
In one embodiment, the high concentration organic phase mobile phase is 30.0mmol/L sodium carbonate in water, 40% acetonitrile.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the invention provides a quantitative detection method for purity of sodium bisoxalato borate, which is a detection method for directly reflecting content of sodium bisoxalato borate, quantitatively detects the sodium bisoxalato borate by an ion chromatography, and simultaneously, as the solubility of the sodium bisoxalato borate in an organic solvent system commonly used by the ion chromatography is smaller, the sodium bisoxalato borate (methanol, ethylene glycol dimethyl ether, ethylene carbonate or propylene carbonate) is dissolved by a proper organic solvent, so that the sodium bisoxalato borate can be fully dissolved, and the decomposition of the bisoxalato borate can not be caused; after the sample injection of the solution to be detected, the blocking liquid is used for blocking so as to prevent the decomposition of the bisoxalato borate, and finally, the accurate detection of the purity of the bisoxalato borate is realized, so that the technical problems that the traditional method for quantitatively detecting the bisoxalato borate is complex in operation process, large in error and incapable of truly reflecting the content of the bisoxalato borate are solved;
2. the quantitative detection method for the purity of the sodium bisoxalato borate provided by the invention has the characteristics of simplicity and convenience in operation, high accuracy, short time consumption and high efficiency.
Drawings
FIG. 1 is a standard curve of a standard solution of bisoxalato borate ions provided in an embodiment of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The embodiment of the invention provides a quantitative detection method for purity of sodium bisoxalato borate, which comprises the steps of firstly dissolving sodium bisoxalato borate in an organic solvent to prepare a solution to be detected, then establishing a standard curve by using bisoxalato borate ion standard solutions with different concentrations, finally measuring the peak area of the solution to be detected by adopting an ion chromatography, and calculating the content of sodium bisoxalato borate in the solution to be detected according to the standard curve; wherein, the blocking liquid is used for blocking when the solution to be detected is sampled.
The embodiment provides a quantitative detection method for the purity of sodium bis (oxalato) borate, wherein the detection object of the method is sodium bis (oxalato) borate, and the sodium bis (oxalato) borate is an important sodium ion battery additive, and has the characteristics of high ionic conductivity, wide electrochemical stability window, good thermal stability, good cycling stability and the like, and can improve the stability of a negative electrode SEI film, improve the electrochemical performance, high-temperature cycling performance and high safety performance of a battery. Important indexes such as the storage capacity, electrochemical performance, safety performance and the like of the sodium ion battery are closely related to the purity and impurities of electrolyte salt and additives. From this, it is seen that quantitative measurement of battery additives and the like is a key to evaluating/predicting the above-mentioned important indicators of sodium ion batteries.
Further, the conventional method for detecting the content of sodium bisoxalato borate generally adopts a method for respectively measuring the content of sodium, the content of boron and the content of oxalic acid in a product, and the specific method is as follows:
(1) Sodium content determination: roasting sodium bisoxalato borate in a high-temperature furnace by adopting a titration method to completely decompose oxalate, cooling, completely dissolving the burned residues by using water, titrating a solution from yellow green to light purple by using a hydrochloric acid standard solution by using a methyl red-methylene blue indicator solution, and calculating the sodium content; (2) boron content determination: heating a test solution for measuring the sodium content by adopting a titration method, removing carbon dioxide possibly remained, generating boric acid by boron completely, strengthening acidity by mannitol, titrating the solution from yellow green to light purple by using a phenolphthalein indicator by using a sodium hydroxide standard solution, and calculating the boron content; (3) oxalic acid radical content determination: the method comprises the steps of heating a sample in a sulfuric acid-phosphoric acid solution medium by adopting a titration method, reacting oxalate with excessive potassium dichromate, titrating excessive potassium dichromate by using a ferrous ammonium sulfate standard solution by using sodium diphenylamine sulfonate as an indicator, and calculating the oxalate content by using the indication end point that the solution turns from purple to bright green.
The pretreatment operation of the methods is too complex, and the content of the sodium bisoxalato borate is deduced indirectly, so that the content of the sodium bisoxalato borate cannot be reflected directly. The absolute difference of the two parallel measurement results of sodium content is about 0.1%, the absolute difference of the two parallel measurement results of oxalic acid root content is about 0.5%, the absolute difference of the two parallel measurement results of boron content is about 0.1%, and the errors of various test methods are overlapped and larger.
In addition, the methods all adopt a titration method, and the color change of the solution is judged from yellow green to light purple or from purple to bright green according to the subjective judgment of people, so that the judgment of the result is large in artificial tendency, and the method is not suitable for the rapid quantitative detection of high-purity sodium bisoxalato borate. Therefore, aiming at various defects existing in the traditional method for detecting the content of the sodium bisoxalato borate, a new method for directly and quantitatively detecting the purity of the sodium bisoxalato borate, which has high accuracy, short time consumption, convenient test and high efficiency, is needed to be developed.
Based on the problems in the prior art, the invention provides a quantitative detection method for the purity of sodium bisoxalato borate, which can directly and truly reflect the content of sodium bisoxalato borate. However, when the method is applied to quantitative detection of sodium bisoxalato borate, a plurality of problems are faced, for example, the sodium bisoxalato borate has low solubility in an organic solvent system commonly used in ion chromatography; when the purity test is carried out, the mobile phase is a water phase, so that sodium bisoxalato borate is easy to decompose into oxalate, and the purity calculation in the sample test is inaccurate, so that an effective way is needed to avoid the hydrolysis interference of the sample, and the rapid and accurate detection can be realized, and the problems are all the key points of establishing the sodium bisoxalato borate purity containing detection method. The present invention is to solve the above problems, and is mainly improved in the following aspects:
(1) Selecting a proper organic solvent to dissolve sodium bisoxalato borate, wherein the screening standard is as follows: not only can fully dissolve the sodium bisoxalato borate, but also can not cause the decomposition of the bisoxalato borate into oxalate, and can specifically select any one of methanol, ethylene glycol dimethyl ether, ethylene carbonate or propylene carbonate; (2) Because ion chromatography needs to be eluted under the water phase eluent, after the solution to be detected is sampled, a blocking method is adopted by using blocking liquid (the blocking liquid is selected from acetonitrile or dimethyl carbonate, the acetonitrile is of chromatographic grade and the content is more than 99.9 percent), so that the decomposition of the bisoxalato borate is prevented, the accurate detection of the purity of the bisoxalato borate is finally realized, and the technical problems that the operation process is complicated, the error is large and the content of the bisoxalato borate cannot be truly reflected in the traditional bisoxalato borate quantitative detection method are solved. ( And (3) injection: the screening standard of the barrier liquid is as follows: the solubility of the sodium bisoxalato borate is extremely low and the solvent is suitable for a chromatographic system. )
In one embodiment, the mass ratio of the sodium bisoxalato borate to the organic solvent is 1: (500-1500).
In one embodiment, the ion chromatography conditions are:
a detector: a conductivity detector;
chromatographic column: metrosep A support 7;
column temperature: 35-40 ℃; the column temperature is preferably 35 ℃;
flow rate: 0.7mL/min;
quantitative ring: 50. Mu.L.
In a specific embodiment, the quantitative detection method of the purity of the sodium bisoxalato borate comprises the following steps:
s1, preparing a solution to be tested: dissolving the weighed sodium bisoxalato borate in an organic solvent to prepare a solution to be measured;
s2, establishing a standard curve: according to the content of the sodium bisoxalato borate in the solution to be detected, diluting the bisoxalato borate ion standard solution into bisoxalato borate ion standard solutions with different concentration gradients, measuring peak areas by adopting an ion chromatography, and establishing a standard curve by taking the concentration as an abscissa and the corresponding peak area as an ordinate;
s3, quantitative determination of sodium bisoxalato borate: and measuring the solution to be measured by adopting an ion chromatography, blocking by using a blocking liquid after the solution to be measured is injected, measuring the peak area of the solution to be measured under the action of a high-concentration organic phase mobile phase, and calculating the content of sodium bisoxalato borate in the solution to be measured according to the standard curve.
In the above step S3, the mobile phase of the high concentration organic phase is (20.0-30.0) mmol/L sodium carbonate in water, 40% acetonitrile, preferably 30.0mmol/L sodium carbonate in water, 40% acetonitrile. The regeneration liquid used in quantitative detection of sodium bisoxalato borate by ion chromatography is 0.7% -0.8% sulfuric acid aqueous solution.
In order to more clearly and in detail describe the quantitative detection method for purity of sodium bisoxalato borate provided by the embodiment of the invention, the following description will be made with reference to specific embodiments.
Comparative example 1
The comparative example provides a quantitative detection method for purity of sodium bisoxalato borate, which specifically comprises the following steps:
(1) Instrument, reagents and raw materials:
ion chromatograph: universal 930; sodium bis (oxalato) borate: the content is more than or equal to 99 percent, and the preparation is self-made; sodium carbonate: high-grade pure, national medicine group chemical reagent limited company; pure water: ultrapure water, deionized water with the conductivity (25 ℃) not more than 0.0055mS/m, and self-made.
(2) The detection method comprises the following steps:
(2-1) accurately weighing 0.1-0.2g of a sodium bisoxalato borate sample to be measured, dissolving the sodium bisoxalato borate sample to 100mL by using ultrapure water, and fully and uniformly mixing the solution to be measured;
(2-2) testing by ion chromatography under the following conditions:
a detector: a conductivity detector;
chromatographic column: metrosep A support 7;
column temperature: 35 ℃;
flow rate: 0.7mL/min;
quantitative ring: 50. Mu.L.
(3) Detection result:
according to analysis and detection results, the purity of the sodium bisoxalato borate is poor in test precision and poor in repeatability due to the characteristic of decomposition of the sodium bisoxalato borate in water; and the sodium bisoxalato borate is easy to decompose into oxalic acid radical and is easy to be confused with residual oxalic acid radical in a sample, so that the purity calculation error in the sample test is caused.
Example 1
The embodiment provides a method for establishing a standard curve, which specifically comprises the following steps:
(1) 1mL of solution contains 1000 mug of bisoxalato borate as a bisoxalato borate standard solution (prepared in situ), and the bisoxalato borate standard solution is diluted in sequence to obtain a series of standard solutions;
(2) Respectively transferring 0.0mL, 10.0mL, 20.0mL, 50.0mL and 100.0mL of standard solution of bisoxalato borate into 5 volumetric flasks of 100mL by using a proper pipette, diluting to the scale by using water, and shaking uniformly;
(3) And (3) adjusting the ion chromatograph to an optimal working state, sequentially sampling and measuring the working curve solution with the same volume (the ion chromatograph condition is the same as that of the comparative example 1), and drawing a standard curve by taking the concentration of the bisoxalato borate in the working curve solution as an abscissa and the corresponding peak area as an ordinate.
Results: the standard curve is shown in figure 1, the concentration of the bisoxalato borate has good linear relation with the corresponding peak area in a certain range, and the correlation coefficient R of the standard curve 2 ＞0.999。
Example 2
The embodiment provides a quantitative detection method for purity of sodium bisoxalato borate, which is used for measuring sodium bisoxalato borate in samples 1-3, wherein each sample is prepared into 5 parts, and specifically comprises the following steps:
(1) Preparing a solution to be tested: accurately weighing 0.1-0.2g of sample 1, sample 2 and sample 3 respectively, dissolving with methanol to constant volume to 100mL, and fully and uniformly mixing to obtain a solution A to be tested, a solution B to be tested and a solution C to be tested respectively;
(2) Standard curve establishment: establishing a standard curve with reference to the method described in example 1;
(3) Quantitative determination of sodium bisoxalato borate: measuring a solution A to be measured, a solution B to be measured and a solution C to be measured by adopting an ion chromatography (chromatographic conditions are the same as those of comparative example 1), respectively injecting the solution A to be measured, the solution B to be measured and the solution C to be measured, then blocking by using a blocking liquid (acetonitrile, chromatographic grade, content is more than 99.9%), measuring the peak area of the solution to be measured under the action of a high-concentration organic phase mobile phase (30.0 mmol/L aqueous solution of sodium carbonate and 40% acetonitrile), respectively calculating the content (ppm) of sodium bisoxalato borate in the solution A to be measured, the solution B to be measured and the solution C to be measured according to standard curves, calculating the content (%) of sodium bisoxalato borate in each sample according to a preparation method, and counting the content results of sodium bisoxalato borate in samples 1-3 as follows:
table 1 sodium bis (oxalato) borate content in samples 1-3
| Parallel testing | Sample 1 | Sample 2 | Sample 3 |
| Parallel test 1 (%) | 89.04 | 94.09 | 99.45 |
| Parallel test 2 (%) | 89.93 | 94.29 | 98.78 |
| Parallel test 3 (%) | 89.77 | 93.87 | 99.59 |
| Parallel test 4 (%) | 89.60 | 93.98 | 99.14 |
| Parallel test 5 (%) | 90.02 | 94.05 | 99.31 |
| Average (%) | 89.67 | 94.06 | 99.25 |
| Standard Deviation (SD) | 0.39 | 0.16 | 0.31 |
| Relative standard deviation (RSD%) | 0.43 | 0.17 | 0.32 |
As can be seen from the data of Table 1, the content of the bisoxalato borate in the 3 samples selected in the embodiment is respectively in different levels of low, medium and high, the relative standard deviation is respectively 0.43%, 0.16% and 0.32%, the RSD is far lower than 3%, the error requirement is completely met, and the method has high precision, and the accuracy of testing the purity of the bisoxalato borate sodium by using the method is high.
Wherein, the calculation formulas of the standard deviation and the relative standard deviation are as follows:
Relative Standard Deviation (RSD) =standard deviation (SD)/arithmetic mean of the results ×100%
Screening test of sodium bisoxalato borate solvent
Because the solubility of the sodium bisoxalato borate is poor, the selection of a proper solvent is also very critical, and meanwhile, the solubility of the sodium bisoxalato borate in an organic solvent system commonly used in ion chromatography is considered to be small, the aim of the test is to screen a proper organic solvent, and the screening standard is that the selected solvent can fully dissolve the sodium bisoxalato borate, and the decomposition of the bisoxalato borate into oxalate is avoided. Based on the above, the invention selects several solvents including ultrapure water, ethanol, acetonitrile, methanol, ethylene glycol dimethyl ether, ethylene carbonate and propylene carbonate for screening test, and the specific test method and test result are as follows:
the test method comprises the following steps:
accurately weighing a plurality of sodium bisoxalato borate to be measured, each 0.1-0.2g, respectively using ultrapure water, ethanol, acetonitrile, methanol, ethylene glycol dimethyl ether, ethylene carbonate and propylene carbonate to dissolve and fix the volume to 100mL, fully and uniformly mixing to obtain different to-be-measured solutions (named as to-be-measured sample 1, to-be-measured sample 2, to-be-measured sample 3, to-be-measured sample 4, to-be-measured sample 5, to-be-measured sample 6 and to-be-measured sample 7 respectively), and detecting the solubility of the to-be-measured solutions and whether the sodium bisoxalato borate is decomposed into oxalate or not;
test results:
TABLE 2 screening test results of sodium bis (oxalato) borate solvent
As is apparent from the above table analysis results, sodium oxalate borate is insoluble in ethanol and acetonitrile, and is soluble in ultrapure water, methanol, ethylene glycol dimethyl ether, ethylene carbonate and propylene carbonate, and based on the measurement results of the solubility, the above five solvents capable of dissolving sodium oxalate borate are first used as candidate solvents, and further analysis is performed on whether sodium oxalate borate is decomposed into oxalate in the above five solvents, and it is found through the relevant experiments that sodium oxalate borate is not decomposed into oxalate in all of the four solvents, except ultrapure water, methanol, ethylene glycol dimethyl ether, ethylene carbonate and propylene carbonate, and therefore, the present invention quantitatively detects the purity of sodium bisoxalate borate using the four solvents as final solvents, and a person skilled in the art can arbitrarily select among the above four organic solvents according to actual needs.
Claims (8)
1. The quantitative detection method of the purity of the sodium bisoxalato borate is characterized in that firstly, the sodium bisoxalato borate is dissolved in an organic solvent to prepare a solution to be detected, then standard curves are established by using bisoxalato borate ion standard solutions with different concentrations, finally, the peak area of the solution to be detected is measured by adopting an ion chromatography, and the content of the sodium bisoxalato borate in the solution to be detected is calculated according to the standard curves; wherein, the blocking liquid is used for blocking when the solution to be detected is sampled.
2. The quantitative determination method of purity of sodium bisoxalato borate according to claim 1, wherein the mass ratio of the sodium bisoxalato borate to the organic solvent is 1: (500-1500).
3. The quantitative determination method of purity of sodium bisoxalato borate according to claim 1, wherein the organic solvent is selected from any one of methanol, ethylene glycol dimethyl ether, ethylene carbonate or propylene carbonate.
4. The method for quantitatively detecting the purity of the sodium bisoxalato borate according to claim 1, wherein the blocking liquid is selected from acetonitrile or dimethyl carbonate, and the acetonitrile is of chromatographic grade and the content is more than 99.9%.
5. The quantitative determination method of purity of sodium bisoxalato borate according to claim 1, wherein the ion chromatography conditions are:
a detector: a conductivity detector;
chromatographic column: metrosep A support 7;
column temperature: 35-40 ℃;
flow rate: 0.7mL/min;
quantitative ring: 50. Mu.L.
6. The quantitative determination method of purity of sodium bisoxalato borate according to claim 1, comprising the steps of:
preparing a solution to be tested: dissolving the weighed sodium bisoxalato borate in an organic solvent to prepare a solution to be measured;
standard curve establishment: according to the content of the sodium bisoxalato borate in the solution to be detected, diluting the bisoxalato borate ion standard solution into bisoxalato borate ion standard solutions with different concentration gradients, measuring peak areas by adopting an ion chromatography, and establishing a standard curve by taking the concentration as an abscissa and the corresponding peak area as an ordinate;
quantitative determination of sodium bisoxalato borate: and measuring the solution to be measured by adopting an ion chromatography, blocking by using a blocking liquid after the solution to be measured is injected, measuring the peak area of the solution to be measured under the action of a high-concentration organic phase mobile phase, and calculating the content of sodium bisoxalato borate in the solution to be measured according to the standard curve.
7. The method for quantitatively detecting the purity of the sodium bisoxalato borate according to claim 6, wherein the mobile phase of the high-concentration organic phase is (20.0-30.0) mmol/L sodium carbonate aqueous solution, and acetonitrile is 40%.
8. The quantitative determination method of purity of sodium bisoxalato borate according to claim 7, wherein the mobile phase of the high-concentration organic phase is 30.0mmol/L sodium carbonate aqueous solution, 40% acetonitrile.
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| CN116338057A (en) * | 2023-05-29 | 2023-06-27 | 广州天赐高新材料股份有限公司 | Detection and analysis method of difluoro sodium phosphate |
| CN116338057B (en) * | 2023-05-29 | 2023-08-15 | 广州天赐高新材料股份有限公司 | Detection and analysis method of difluoro sodium phosphate |
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