Analysis method of 1, 2, 3-tri (2-cyanoethoxy) propane

Abstract

The invention relates to the technical field of analytical chemistry, in particular to an analytical method of 1, 2, 3-tri (2-cyanoethoxy) propane, which adopts gas chromatography for detection, and adopts a hydrogen flame ionization detector as a detector; the capillary chromatographic column is a weak-polarity column or a medium-polarity column; the temperature of a hydrogen flame ionization detector is 300-350 DEG C; the temperature of a sample inlet is 200-250 DEG C; the column temperature of a capillary gas chromatographic column is firstly set to be 40-80 DEG C, the holding time is 5-10 min, then the temperature is increased to 250-300 DEG C at the speed of 10-15 DEG C / min, and the holding time is 20-30 min; the carrier gas is nitrogen or helium. The analysis method is low in operation cost, the chromatographic column has good thermal stability, the peak shape, the separation degree and the repeatability are better, the accuracy is higher, and the method has the characteristics of rapidness, simplicity, accuracy and the like.

Description

Technical Field

[0001] The present invention relates to an analytical method for 1,2,3-tris(2-cyanoethoxy)propane, belonging to the technical field of analytical chemistry. Background Art

[0002] With the continuous expansion of the application scope of lithium-ion batteries, the safety performance of lithium-ion batteries has become a bottleneck restricting development. Battery functional additives have become a new technological development direction, and using a small dosage can specifically change certain properties of the battery. Nitrile compounds are often used as additives in lithium-ion battery electrolytes and can effectively improve the high-temperature cycle and storage performance of the battery. As an additive, 1,2,3-tris(2-cyanoethoxy)propane can be applied to battery electrolytes to reduce the swelling of the battery after high-temperature storage and improve the performance of the battery. Therefore, the testing of 1,2,3-tris(2-cyanoethoxy)propane has important application value. The structural formula of 1,2,3-tris(2-cyanoethoxy)propane is:

[0003]

[0004] Currently, research on 1,2,3-tris(2-cyanoethoxy)propane mostly focuses on synthesis, and there is no reported analytical method for 1,2,3-tris(2-cyanoethoxy)propane. 1,2,3-tris(2-cyanoethoxy)propane is an additive used in electrolytes and has relatively high requirements for the control of impurities. However, during the preparation process of 1,2,3-tris(2-cyanoethoxy)propane, various impurities may be generated. Conventional gas chromatography for detecting 1,2,3-tris(2-cyanoethoxy)propane often has a low resolution, and many impurities cannot be detected, thus unable to provide more help for process research and development.

[0005] Therefore, how to quickly and effectively detect 1,2,3-tris(2-cyanoethoxy)propane has become a problem to be solved. In the production process of 1,2,3-tris(2-cyanoethoxy)propane, some by-products such as monosubstituted compounds, disubstituted compounds, and polymeric impurities will be generated. Therefore, when detecting 1,2,3-tris(2-cyanoethoxy)propane, it is also necessary to detect its monosubstituted compounds, disubstituted compounds, and polymeric impurities to monitor the reaction effect, so as to facilitate the monitoring and quality control of the production process of 1,2,3-tris(2-cyanoethoxy)propane. The impurities that may be involved in the production process of 1,2,3-tris(2-cyanoethoxy)propane include monosubstituted compound 1: Monosubstituted compound 2: Disubstituted compound 1: Disubstituted compound 2: In addition, acrylonitrile, the reaction raw material used for preparing 1,2,3-tris(2-cyanoethoxy)propane, may also produce some polymer impurities with unknown structures under alkaline conditions. If an analytical method for 1,2,3-tris(2-cyanoethoxy)propane can separate various impurities, it can provide more auxiliary information for the development of the preparation process of 1,2,3-tris(2-cyanoethoxy)propane. Summary of the Invention

[0006] Aiming at the deficiencies of the existing technology, the present invention provides an analytical method for 1,2,3-tris(2-cyanoethoxy)propane. The analytical method is simple and rapid to operate, has a high degree of impurity separation, a wide range of instrument applications, low test costs, a long service life of the chromatographic column, high sensitivity, good thermal stability, good repeatability of test data, and high accuracy.

[0007] The technical solution for the present invention to solve the above technical problems is as follows: An analytical method for 1,2,3-tris(2-cyanoethoxy)propane, which is detected by gas chromatography, and the detector is a flame ionization detector; the capillary chromatographic column is a weakly polar column or a medium polar column;

[0008] Temperature of the flame ionization detector: 300°C to 350°C;

[0009] Temperature of the injection port: 200°C to 250°C;

[0010] The capillary gas chromatographic column is first set at a column temperature of 40°C to 80°C for a holding time of 5 min to 10 min, and then set to be heated to 250°C to 300°C at a rate of 10°C / min to 15°C / min for a holding time of 20 min to 30 min;

[0011] The carrier gas is nitrogen or helium, and the carrier gas flow rate is 1 mL / min to 5 mL / min;

[0012] The hydrogen flow rate is 30 mL / min to 40 mL / min;

[0013] The air flow rate is 300 mL / min to 400 mL / min;

[0014] The split ratio is (1:100) to (1:25).

[0015] Furthermore, the stationary phase of the capillary chromatographic column is any one of a combination of 5% phenyl and 95% dimethylpolysiloxane treated by alkali deactivation technology, a combination of 50% phenyl and 50% dimethylpolysiloxane, and a combination of 14% cyanopropylbenzene and 86% dimethylpolysiloxane.

[0016] Preferably, the capillary chromatographic column has a stationary phase composed of a combination of 5% phenyl and 95% dimethyl polysiloxane treated by alkali deactivation technology, with a specification of 30 m × 0.32 mm × 0.25 μm.

[0017] Preferably, the temperature of the hydrogen flame ionization detector is 320 °C; the temperature of the injection port is 250 °C.

[0018] Preferably, the column temperature of the capillary gas chromatographic column is first set at 80 °C for 5 min, and then set to rise to 300 °C at a rate of 10 °C / min for 20 min.

[0019] Preferably, the carrier gas flow rate is 2 mL / min and the split ratio is 1:100.

[0020] Preferably, the hydrogen flow rate is 40 mL / min; the air flow rate is 400 mL / min.

[0021] Preferably, the injection volume is 1.0 μL.

[0022] Furthermore, after the gas chromatograph is stable, the product content error is less than 0.05% for two consecutive injections, and the average value is taken to calculate the content of 1,2,3-tris(2-cyanoethoxy)propane and other impurities. The calculation formula is as follows:

[0023] In the formula, X% is the content percentage of 1,2,3-tris(2-cyanoethoxy)propane and a certain other impurity component, A is the peak area of the corresponding component in the chromatogram; ∑A i is the peak area of all peaks in the chromatogram.

[0024] Furthermore, the gas chromatograph is Aglient technologies 7820A or Aglient technologies 8860, equipped with an FID detector and a split / splitless device.

[0025] The beneficial effects of the present invention are as follows:

[0026] The analysis method of the present invention adopts gas chromatography analysis method, which improves the working efficiency and the separation degree of samples, has good sample repeatability, high accuracy, and reduces the test cost.

[0027] The present invention analyzes the results obtained by the area normalization method using an FID detector on a capillary column treated by an alkali deactivation technique. The operation is simple, fast, accurate, practical, and has a high response value. A second-order temperature programming is established, the temperature of the vaporization chamber is controlled, and an FID detector is used to detect a separation and analysis method for an electrolyte additive 1,2,3-tris(2-cyanoethoxy)propane and its intermediates and other impurities, which can accurately detect the content of the sample and provide a reference for the gas phase testing technology of other high-boiling, easily oxidized, and thermally decomposed compounds.

[0028] The present invention uses a gas chromatography analysis method to quantitatively analyze an electrolyte additive 1,2,3-tris(2-cyanoethoxy)propane and its impurities. The chromatographic peaks have a good shape, the baseline is stable, the separation degree of impurities is high, and the content test is stable. It can accurately detect the content of the sample, especially the content of mono-substituted, di-substituted impurities and polymers. Moreover, the chromatographic column has a long service life and still has good thermal stability at up to 350 °C, providing a technical reference for other high-boiling hydrocarbon compounds. Description of the Drawings

[0029] Figure 1 It is the chromatogram of the blank solution;

[0030] Figure 2 It is the chromatogram of the reference solution in Example 1 (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, B is mono-substituted compound 1, C is mono-substituted compound 2, D is di-substituted compound 1, E is di-substituted compound 2, F is polymeric impurity 1, G is polymeric impurity 2);

[0031] Figure 3 It is the chromatogram of the reference solution in Example 2 (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, B is mono-substituted compound 1, C is mono-substituted compound 2, D is di-substituted compound 1, E is di-substituted compound 2, F is polymeric impurity 1, G is polymeric impurity 2);

[0032] Figure 4 It is the chromatogram of the reference solution in Example 3 (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, B is mono-substituted compound 1, C is mono-substituted compound 2, D is di-substituted compound 1, E is di-substituted compound 2, F is polymeric impurity 1, G is polymeric impurity 2);

[0033] Figure 5 It is the chromatogram of the reference solution in Comparative Example 1 on an HP-5 column (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, D is di-substituted compound 1, E is di-substituted compound 2, F is polymeric impurity 1);

[0034] Figure 6Chromatogram of the reference solution on the HP-50 column in Comparative Example 2 (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, D is disubstituted compound 1, E is disubstituted compound 2, and F is polymeric impurity 1);

[0035] Figure 7 Chromatogram of the reference solution on the 1701 column in Comparative Example 3 (in the figure, A is 1,2,3-tris(2-cyanoethoxy)propane, D is disubstituted compound 1, E is disubstituted compound 2, and F is polymeric impurity 1). Detailed Description of the Invention

[0036] The following provides a detailed description of the specific embodiments of the present invention. The present invention can be implemented in many other ways different from those described herein. Those skilled in the art can make similar improvements without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed.

[0037] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used are only for describing specific embodiments and do not limit the present invention.

[0038] An analytical method for 1,2,3-tris(2-cyanoethoxy)propane, which is detected by gas chromatography. The detector is a flame ionization detector; the capillary chromatographic column is a weakly polar column or a medium polar column;

[0039] Temperature of the flame ionization detector: 300°C to 350°C;

[0040] Temperature of the injection port: 200°C to 250°C;

[0041] The capillary gas chromatographic column is first set at a column temperature of 40°C to 80°C for a holding time of 5 min to 10 min, and then set to be heated to 250°C to 300°C at a rate of 10°C / min to 15°C / min for a holding time of 20 min to 30 min;

[0042] The carrier gas is nitrogen or helium, and the carrier gas flow rate is 1 mL / min to 5 mL / min;

[0043] The hydrogen flow rate is 30 mL / min to 40 mL / min;

[0044] The air flow is 300 mL / min to 400 mL / min;

[0045] The split ratio is (1:100) to (1:25).

[0046] Specifically, the stationary phase of the capillary chromatographic column is any one of a combination of 5% phenyl and 95% dimethylpolysiloxane treated by alkali deactivation technology, a combination of 50% phenyl and 50% dimethylpolysiloxane, and a combination of 14% cyanopropylbenzene and 86% dimethylpolysiloxane.

[0047] A polar chromatographic column means that the stationary phase on the capillary wall is polar. Therefore, the polarity of the column depends on the polarity of the stationary phase, and the structure of the stationary phase determines the polarity of the stationary phase. The structure of the stationary phase is mainly determined by the type of the stationary phase, the polarity of the substituent groups (such as phenyl, cyanopropyl), and the number of the substituent groups. According to the different contents of the substituents, the polarity of the chromatographic column is different. A weakly polar chromatographic column with extremely low column bleed and excellent inertness to active compounds is suitable for the analysis of mixtures, especially samples containing non-polar and polar components.

[0048] Preferably, the stationary phase of the capillary chromatographic column is a combination of 5% phenyl and 95% dimethylpolysiloxane treated by alkali deactivation technology, and the specification is 30m×0.32mm×0.25μm.

[0049] More preferably, the capillary chromatographic column is a weakly polar CP-sil 8CB column, which is a chromatographic column treated by alkali deactivation technology. The stationary phase is 5% phenyl-95% dimethylpolysiloxane, and it still has good thermal stability at up to 350°C, can obtain good peak shapes and fast elution effects, and is suitable for the separation and analysis of various complex samples.

[0050] Preferably, the temperature of the hydrogen flame ionization detector is 320°C; the inlet temperature is 250°C.

[0051] Preferably, the column temperature of the capillary gas chromatographic column is first set to 80°C and maintained for 5 min, and then set to rise to 300°C at a rate of 10°C / min and maintained for 20 min.

[0052] Preferably, the carrier gas flow rate is 2 mL / min and the split ratio is 1:100.

[0053] Preferably, the hydrogen flow rate is 40 mL / min; the air flow rate is 400 mL / min.

[0054] Preferably, the injection volume is 1.0 μL.

[0055] Furthermore, after the gas chromatograph is stable, the product content error is less than 0.05% when injecting samples continuously twice, and the average value is taken to calculate the contents of 1,2,3-tris(2-cyanoethoxy)propane and other impurities. The calculation formula is:

[0056] In the formula, X% is the percentage content of 1,2,3-tris(2-cyanoethoxy)propane and a certain other impurity component, A is the peak area of the corresponding component in the chromatogram; ∑A i is the peak area of all peaks in the chromatogram.

[0057] This calculation method has a small error, the data is parallel and reliable, and the percentage content of different components can be calculated separately, especially the content of the impurities of concern. The operation is simple, fast and accurate.

[0058] Furthermore, the gas chromatograph is Aglient technologies 7820A or Aglient technologies 8860, equipped with an FID detector and a split / splitless device.

[0059] Gas chromatographs of the above models have the advantages of high sensitivity to hydrocarbons and a wide linear range. Analyzing the results of the area normalization method improves work efficiency. Using the split / splitless mode improves the resolution of the samples and reduces the test cost.

[0060] Example 1

[0061] I. Preparation of solutions:

[0062] The blank solution is analytical pure acetonitrile;

[0063] The reference solution is a sample solution obtained by dissolving 0.5 g of the sample (the 1,2,3-tris(2-cyanoethoxy)propane sample to be measured) in 2.5 g of acetonitrile.

[0064] II. Gas chromatography conditions:

[0065] The gas chromatograph is Aglient technologies 8860, the chromatographic column is a weakly polar CP-sil 8CB column (5% phenyl-95% dimethyl polysiloxane treated by alkali deactivation technology), and the chromatographic column specifications are 30 m × 0.25 mm × 0.25 μm.

[0066] The temperature of the hydrogen flame ionization detector is 320 °C; the injection port temperature is 200 °C.

[0067] The capillary gas chromatographic column program: the initial column temperature is 80 °C, the holding time is 5 min, and then it is heated to 300 °C at a rate of 10 °C / min, and the holding time is 20 min.

[0068] The carrier gas is nitrogen, and the flow rate of the carrier gas is 2 mL / min;

[0069] The hydrogen flow rate is 40 mL / min;

[0070] The air flow rate is 400 mL / min;

[0071] Split ratio: 1:100;

[0072] The injection volume is 2.0 μL.

[0073] This analytical method uses the area normalization method to analyze the substance content.

[0074] From Figure 2 it can be seen that through the area percentage report, for sample 1,2,3-tris(2-cyanoethoxy)propane: the content is 99.4619%, for monosubstituted compound 1: the content is 0.0021%, for monosubstituted compound 2: the content is 0.0018%, for disubstituted compound 1: the content is 0.1105%, for disubstituted compound 2: the content is 0.0265%, the content of polymeric impurity 1 with unknown structure is: 0.0697%, and the content of polymeric impurity 2 with unknown structure is: 0.1250%. The calculation formula is as follows:

[0075] Among them, the area of 1,2,3-tris(2-cyanoethoxy)propane is 1.0327e 4 , the total area ∑A i is 1.0383e 4 , the area of monosubstituted compound 1 is 1.2728e -2 , the area of monosubstituted compound 2 is 2.1306e -2 , the area of disubstituted compound 1 is 11.4693e 0 , the area of disubstituted compound 2 is 2.7520e 0 , the area of polymeric impurity 1 is 7.2340e 0 , the area of polymeric impurity 2 is 12.9820e 0 .

[0076] The gas chromatography results show that 1,2,3-tris(2-cyanoethoxy)propane and its impurities can all achieve good baseline separation, and the response values of the main peak and impurities are good, which can meet the actual detection requirements.

[0077] Example 2

[0078] I. Preparation of solutions:

[0079] The blank solution is analytical grade acetonitrile;

[0080] The reference solution is the sample solution obtained by dissolving 0.5 g of the sample in 2.5 g of acetonitrile.

[0081] II. Gas chromatography conditions:

[0082] The gas chromatograph is an Aglient technologies 7820A, and the chromatographic column is a weakly polar CP-sil 8CB column (5% phenyl-95% dimethyl polysiloxane treated by alkali deactivation technology). The specifications of the chromatographic column are 30m×0.32mm×0.25μm.

[0083] The temperature of the hydrogen flame ionization detector is 300°C; the temperature of the injection port is 250°C.

[0084] The capillary gas chromatography column program: the initial column temperature is 40°C, the holding time is 10 min, then it is heated to 250°C at a rate of 15°C / min, and the holding time is 30 min.

[0085] The carrier gas is nitrogen, and the flow rate of the carrier gas is 5 mL / min;

[0086] The flow rate of hydrogen is 30 mL / min;

[0087] The flow rate of air is 300 mL / min;

[0088] The split ratio is 1:50;

[0089] The injection volume is 1.0 μL.

[0090] This analytical method uses the area normalization method to analyze the substance content.

[0091] From Figure 3 it can be seen that through the area percentage report, the sample 1,2,3-tris(2-cyanoethoxy)propane: The content is 99.4754%, the monosubstituted compound 1: The content is 0.0024%, the monosubstituted compound 2: The content is 0.0025%, the disubstituted compound 1: The content is 0.1198%, the disubstituted compound 2: The content is 0.0504%, the content of the unknown structure polymeric impurity 1 is: 0.0735%, and the content of the unknown structure polymeric impurity 2 is: 0.1250%.

[0092] The gas chromatography results show that 1,2,3-tris(2-cyanoethoxy)propane and its impurities can all achieve good baseline separation, and the response values of the main peak and impurities are good, which can meet the actual detection requirements.

[0093] Example 3

[0094] I. Preparation of solutions:

[0095] The blank solution is analytical pure acetonitrile;

[0096] The reference solution is the sample solution obtained by dissolving 0.5 g of the sample in 4.5 g of acetonitrile.

[0097] II. Gas Chromatography Conditions:

[0098] The gas chromatograph is Aglient technologies 8860, and the chromatographic column is a weakly polar CP-sil 8CB column (5% phenyl-95% dimethyl polysiloxane treated by alkali deactivation technology). The specifications of the chromatographic column are 30m×0.32mm×0.25μm.

[0099] The temperature of the hydrogen flame ionization detector is 350°C; the injection port temperature is 250°C.

[0100] The capillary gas chromatography column program: The initial column temperature is 60°C, the holding time is 10 min, and then it is heated to 300°C at a rate of 10°C / min, and the holding time is 30 min.

[0101] The carrier gas is nitrogen, and the flow rate of the carrier gas is 1 mL / min;

[0102] The hydrogen flow rate is 35 mL / min;

[0103] The air flow rate is 350 mL / min;

[0104] The split ratio is 1:25;

[0105] The injection volume is 1.0 μL.

[0106] This analysis method uses the area normalization method to analyze the substance content.

[0107] From Figure 4 it can be seen that through the area percentage report, the sample 1,2,3-tris(2-cyanoethoxy)propane: The content is 99.4808%, the monosubstituted compound 1: The content is 0.0016%, the monosubstituted compound 2: The content is: 0.0016%, the disubstituted compound 1: The content is 0.1213%, the disubstituted compound 2: The content is: 0.0505%, the content of the unknown structure polymeric impurity 1 is: 0.0739%, and the content of the unknown structure polymeric impurity 2 is: 0.1238%.

[0108] The gas chromatography results show that 1,2,3-tris(2-cyanoethoxy)propane and its impurities can all achieve good baseline separation, and the response values of the main peak and impurities are good, which can meet the actual detection requirements.

[0109] Comparative Example 1

[0110] Using the same method as in Example 1 to prepare the reference solution, an Agilent 8860 gas chromatograph was used. The chromatographic column was a weakly polar HP-5 column (30 m × 0.32 mm × 0.25 μm, Agilent). The initial temperature of the programmed temperature rise was 80 °C, maintained for 5 min, then heated to 300 °C at a rate of 10 °C / min and maintained for 30 min; the inlet temperature was 250 °C; the detector temperature was 320 °C; the carrier gas was nitrogen with a flow rate of 2 mL / min;

[0111] the hydrogen flow rate was 40 mL / min; the air flow rate was 400 mL / min; the split ratio was 1:100, and the injection volume was 1.0 μL. As Figure 5 shown, 1,2,3-tris(2-cyanoethoxy)propane and its impurities could not be completely eluted in the gas phase. The separation of impurities and the peak shape were both poor. The main peak was front-extended and bulging, and the baseline was unstable.

[0112] Comparative Example 2

[0113] Using the same method as in Example 1 to prepare the reference solution, an Agilent 8860 gas chromatograph was used. The chromatographic column was a medium polar HP-50 column (30 m × 0.25 mm × 0.25 μm, Agilent). The initial temperature of the programmed temperature rise was 80 °C, maintained for 5 min, then heated to 280 °C at a rate of 15 °C / min and maintained for 30 min; the inlet temperature was 250 °C; the detector temperature was 280 °C; the carrier gas was nitrogen with a flow rate of 2 mL / min; the hydrogen flow rate was 40 mL / min; the air flow rate was 400 mL / min; the split ratio was 1:100, and the injection volume was 1.0 μL. As Figure 6 shown, 1,2,3-tris(2-cyanoethoxy)propane and its impurities could not be completely eluted in the gas phase. The separation of impurities and the peak shape were both poor. The main peak was front-extended and bulging, and the baseline was unstable.

[0114] Comparative Example 3

[0115] Using the same method as in Example 1 to prepare the reference solution, an Agilent 8860 gas chromatograph was used. The chromatographic column was a medium polar DB-1701 column (30 m × 0.32 mm × 0.25 μm, Agilent). The initial temperature of the programmed temperature rise was 80 °C, maintained for 5 min, then heated to 280 °C at a rate of 10 °C / min and maintained for 30 min; the inlet temperature was 250 °C; the detector temperature was 280 °C; the carrier gas was nitrogen with a flow rate of 2 mL / min; the hydrogen flow rate was 40 mL / min; the air flow rate was 400 mL / min; the split ratio was 1:100, and the injection volume was 1.0 μL. As Figure 7 shown, 1,2,3-tris(2-cyanoethoxy)propane and its impurities could not be completely eluted in the gas phase. The separation of impurities and the peak shape were both poor. The main peak was front-extended and bulging, and the baseline was unstable.

[0116] The test results of the different chromatographic columns in Example 1, Comparative Example 1, Comparative Example 2, and Comparative Example 3 are compared in Table 1 below.

[0117] Table 1 Test Results of Different Chromatographic Columns

[0118]

[0119]

[0120] The methodological study of the analysis method of the present invention is as follows:

[0121] 1. Specificity investigation

[0122] Take a blank solution (only the solvent) and a reference solution (the same as that in Example 1), and perform analytical detection according to the chromatographic conditions of Example 1 above, and record the chromatogram. The chromatogram of the blank solution is shown in Figure 1 , and the chromatogram of the reference solution is shown in Figure 2 ; It can be seen from the chromatographic results that under these chromatographic conditions, the sample and the impurities contained therein can be effectively separated, indicating that the method has good specificity.

[0123] 2. Repeatability investigation

[0124] Take a sample solution (the same as that in Example 1), and inject it continuously six times according to the chromatographic conditions of Example 1, and record the chromatogram. The results are shown in Table 2.

[0125] Table 2 Results of Repeatability Investigation

[0126]

[0127] The experimental results show that when the reference solution is injected continuously six times, the RSDs of the retention times and peak areas of 1,2,3-tris(2-cyanoethoxy)propane and its mono-substituted, di-substituted, and polymerized impurities are all less than 5%, indicating good system suitability.

[0128] In summary, the separation and analysis method of an electrolyte additive 1,2,3-tris(2-cyanoethoxy)propane and its impurities provided by the present invention has good sensitivity, specificity, and accuracy, and is simple and efficient to operate.

[0129] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, all possible combinations of the various technical features in the above embodiments are not exhausted. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.

[0130] For those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all fall within the protection scope of the present invention. The protection scope of the present invention shall be subject to the appended claims.

Claims

1. A method for analyzing 1,2,3-tris(2-cyanoethoxy)propane, characterized in that: The detection is carried out by gas chromatography, and the detector is a hydrogen flame ionization detector; the capillary chromatographic column is a weak polar column or a medium polar column; Hydrogen flame ionization detector temperature: 300℃~350℃; Inlet temperature: 200℃~250℃; The column temperature of the capillary gas chromatography column is first set to 40°C to 80°C, maintained for 5 min to 10 min, and then set to increase the temperature to 250°C to 300°C at a rate of 10°C / min to 15°C / min, maintained for 20 min to 30 min; The carrier gas is nitrogen or helium, and the carrier gas flow rate is 1mL / min~5mL / min; The hydrogen flow rate is 30mL / min~40mL / min; Air flow 300mL / min~400mL / min; The split ratio is (1:100) to (1:25).

2. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The stationary phase of the capillary chromatographic column is any one of a combination of 5% phenyl and 95% dimethylpolysiloxane, a combination of 50% phenyl and 50% dimethylpolysiloxane, and a combination of 14% cyanopropylbenzene and 86% dimethylpolysiloxane treated by alkali deactivation technology.

3. The analytical method for 1,2,3-tris(2-cyanoethoxy)propane according to claim 2, characterized in that: The stationary phase of the capillary chromatographic column is a combination of 5% by mass phenyl and 95% by mass dimethylpolysiloxane treated by alkali deactivation technology, and the specification is 30m×0.32mm×0.25μm.

4. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The temperature of the hydrogen flame ionization detector was 320°C; the temperature of the injection port was 250°C.

5. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The column temperature of the capillary gas chromatography column was first set to 80°C and maintained for 5 min, and then set to increase the temperature to 300°C at a rate of 10°C / min and maintained for 20 min.

6. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The carrier gas flow rate is 2 mL / min, and the split ratio is 1:

100.

7. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The hydrogen flow rate is 40 mL / min; the air flow rate is 400 mL / min.

8. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The injection volume is 1.0-2.0 μL.

9. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: After the gas chromatograph is stable, the error of two consecutive injections is less than 1%. The average value is taken to calculate the content of 1,2,3-tris(2-cyanoethoxy)propane and other impurities. The calculation formula is: In the formula, X% is the content percentage of 1,2,3-tris(2-cyanoethoxy)propane and other impurities, and A is the peak area of ​​the corresponding component in the chromatogram; ∑A i is the peak area of ​​all peaks in the chromatogram.

10. The method for analyzing 1,2,3-tris(2-cyanoethoxy)propane according to claim 1, characterized in that: The gas chromatograph was Aglient technologies 7820A or Aglient technologies 8860 equipped with a FID detector and a split / splitless device.

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