Gas chromatography method for determining purity of methylsulfonyl fluoride

Abstract

The invention discloses a gas chromatography method for determining the purity of methylsulfonyl fluoride. The gas chromatography method comprises the following steps: preparing a standard working solution and a test solution; respectively testing the standard working solution and the test solution by adopting a gas chromatographic method to obtain a standard working solution measurement result and a test solution measurement result; performing standard curve fitting on the measurement result of the standard working solution to obtain the function relationship between the methylsulfonyl fluoride mass and the methylsulfonyl fluoride peak area and the function relationship between the solvent mass and the solvent peak area; and calculating the purity of the methylsulfonyl fluoride in the test solution according to the test result of the test solution and the function relationship. The method is easy to operate, high in accuracy and good in stability, the chromatographic purity of the methylsulfonyl fluoride can be accurately measured, and the defect of a methylsulfonyl fluoride analysis technology is overcome.

Description

Technical Field

[0001] The invention relates to the technical field of fluorine chemical product analysis and detection, and in particular to a gas chromatography method for determining the purity of methylsulfonyl fluoride. Background Art

[0002] Methanesulfonyl fluoride (CH 3 SO 2 F), an important fine chemical raw material, has a wide range of uses in organic synthesis. It is often used as a remover of protective groups of organic compounds such as esters, ethers, and ketones. Methanesulfonyl fluoride can also be used as a chemical reagent, catalyst, initiator for polymerization reactions, etc.

[0003] There is currently no unified national or industry standard to determine the purity of methylsulfonyl fluoride. Summary of the invention

[0004] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a gas chromatography method for determining the purity of methyl sulfonyl fluoride, so as to solve the problem of insufficient technology for determining the purity of methyl sulfonyl fluoride.

[0005] To achieve the above object, the present invention is implemented through the following technical solutions: The present invention provides a gas chromatography method for determining the purity of methylsulfonyl fluoride, comprising the following steps: S1: Prepare standard working solution and test solution; S2: The standard working solution and the test solution are tested respectively by gas chromatography to obtain the test results of the standard working solution and the test solution; S3: Fitting the standard curve of the standard working solution measurement results to obtain the functional relationship between the mass of methylsulfonyl fluoride, the mass of the solvent and the peak area of ​​methylsulfonyl fluoride and the peak area of ​​the solvent; S4: According to the measurement result of the test solution and the functional relationship obtained in step S3, the purity of methylsulfonyl fluoride in the test solution is calculated.

[0006] Preferably, the solvent used to prepare the solution in step S1 is acetone.

[0007] Preferably, the concentration of the test solution is 1-2 g / g.

[0008] Preferably, the conditions of gas chromatography include: the chromatographic column is a capillary column, 30m×0.32mm×0.25μm; the carrier gas flow rate: 20~50L / min; the fuel gas flow rate: 20~50L / min; the auxiliary gas flow rate: 200~400L / min; the chromatographic column temperature: 180~240℃; the injection port temperature: 180~240℃; the split ratio: 40~60:1; the injection volume: 0.4~0.6μL.

[0009] Preferably, the stationary phase of the capillary column is 5% phenyl-95% dimethylpolysiloxane, a weakly polar stationary phase.

[0010] Preferably, the temperature of the chromatographic column is raised by: using programmed temperature rise: the initial temperature is 50-100°C, maintained for 1-5 min; the temperature is raised to 180-240°C at a heating rate of 5-10°C / min, and maintained for 1-5 min.

[0011] Preferably, the carrier gas is nitrogen; the fuel gas is hydrogen; and the combustion-supporting gas is air.

[0012] Preferably, the detector of the gas chromatography is a hydrogen flame ionization detector, and the detector temperature is 200-280°C.

[0013] Preferably, the functional relationship between the mass of methylsulfonyl fluoride, the mass of the solvent and the peak area of ​​methylsulfonyl fluoride and the peak area of ​​the solvent is:

[0014] In the formula, m' 溶剂 is the mass of the solvent standard in the standard working solution; m' 甲基磺酰氟 is the mass of methylsulfonyl fluoride standard in the standard working solution; A' 甲基磺酰氟 is the peak area of ​​methylsulfonyl fluoride standard in the standard working solution; A' 溶剂 is the peak area of ​​the solvent standard in the standard working solution; k is the constant obtained by fitting the gas phase determination results of the standard working solution.

[0015] Preferably, the purity calculation formula of methylsulfonyl fluoride in the test solution is as follows:

[0016] In the formula, m 溶剂 is the mass of the solvent in the test solution; m 样品 is the mass of methylsulfonyl fluoride sample in the test solution; A 甲基磺酰氟 is the peak area of ​​methylsulfonyl fluoride in the test solution; A 溶剂 is the peak area of ​​the solvent in the test solution; k is the constant calculated by fitting the gas phase determination results of the standard working solution.

[0017] The beneficial effects of the present invention are: The invention discloses a gas chromatography method for determining the purity of methylsulfonyl fluoride. The method has the advantages of simple operation, high precision and good stability, and can accurately determine the chromatographic purity of methylsulfonyl fluoride, thus making up for the deficiency of methylsulfonyl fluoride analysis technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings of the embodiment are briefly introduced below.

[0019] Figure 1 The gas chromatogram of the sample solution to be tested in Example 1; Figure 2 It is the gas chromatogram of the sample solution to be tested in Example 2. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] Example 1 A gas chromatography method for determining the purity of methylsulfonyl fluoride comprises the following steps: (1) Preparation of methylsulfonyl fluoride-acetone mixed standard working solution Accurately weigh 5 portions of methylsulfonyl fluoride standard (0.5 g, 1.0 g, 1.5 g, 2.0 g, 3.0 g) to an accuracy of 0.0001 g; dissolve them in 1.0 g of acetone standard to an accuracy of 0.0001 g respectively, and shake well to obtain a mixed standard working solution.

[0022] (2) Prepare the sample solution to be tested Weigh 1.0514 g of sample and dissolve it in 1.0281 g of acetone, accurate to 0.0001 g, and shake well to obtain the sample solution to be tested.

[0023] (3) Determination The standard working solution and the sample solution to be tested are tested respectively by gas chromatography to obtain the gas phase determination result of the standard working solution and the gas phase determination result of the sample solution to be tested.

[0024] Among them, the gas chromatography conditions are: the chromatographic column is a capillary column, the stationary phase is 5% phenyl-95% dimethylpolysiloxane, 30m×0.32mm×0.25μm; nitrogen is the carrier gas, the flow rate is 30L / min; hydrogen is the fuel gas, the flow rate is 30L / min; air is the auxiliary gas, the flow rate is 300L / min; programmed temperature is adopted: the initial temperature is 50℃, maintained for 1min; the temperature is increased to 200℃ at a heating rate of 10℃ / min, and maintained for 1min; the injection port temperature is 200℃; the split ratio is 60:1; the injection volume is 0.5μL; the detector temperature is 240℃.

[0025] (4) Fitting of standard curve According to the gas chromatography measurement results of the methylsulfonyl fluoride-acetone mixed standard working solution, the relationship between the mass of methylsulfonyl fluoride, the mass of acetone and the peak area was obtained by fitting the standard curve, as shown in Table 1: Table 1

[0026]

[0027] In the formula, m' 丙酮 is the mass of acetone standard in the standard working solution; m' 甲基磺酰氟 is the mass of methylsulfonyl fluoride standard in the standard working solution; A' 甲基磺酰氟 is the peak area of ​​methylsulfonyl fluoride standard in the standard working solution; A' 丙酮 is the peak area of ​​acetone standard in the standard working solution; k is the constant obtained by fitting the gas phase determination results of the standard working solution.

[0028] The constant representing the relationship between the mass of the two substances and the peak area was obtained through fitting calculation: k=3.8018.

[0029] (4) Calculate the purity of methylsulfonyl fluoride in the sample to be tested The gas phase determination results of the sample solution are as follows Figure 1 As shown, 3.260min is the retention time of acetone, and the peak area is 78.8306%; 3.894min is the retention time of methylsulfonyl fluoride, and the peak area is 21.1318%. Substitute the data into the chromatographic purity calculation formula of methylsulfonyl fluoride:

[0030]

[0031] The purity of methylsulfonyl fluoride in the sample to be tested was calculated to be 99.65%.

[0032] Example 2 A gas chromatography method for determining the purity of methylsulfonyl fluoride comprises the following steps: (1) Preparation of methylsulfonyl fluoride-acetone mixed standard working solution Accurately weigh 5 portions of methylsulfonyl fluoride standard (0.5059 g, 1.0056 g, 1.4635 g, 1.9638 g, 2.9662 g) to an accuracy of 0.0001 g; dissolve them respectively in about 1.0 g of acetone standard to an accuracy of 0.0001 g, and shake well to obtain a mixed standard working solution.

[0033] (2) Prepare the sample solution to be tested Weigh 1.0514 g of sample and dissolve it in 1.0281 g of acetone, accurate to 0.0001 g, and shake well to obtain the sample solution to be tested.

[0034] (3) Determination The standard working solution and the sample solution to be tested are tested respectively by gas chromatography to obtain the gas phase determination result of the standard working solution and the gas phase determination result of the sample solution to be tested.

[0035] Among them, the gas chromatography conditions are: the chromatographic column is a capillary column, the stationary phase is 5% phenyl-95% dimethylpolysiloxane, 30m×0.32mm×0.25μm; nitrogen is the carrier gas, the flow rate is 30L / min; hydrogen is the fuel gas, the flow rate is 35L / min; air is the auxiliary gas, the flow rate is 350L / min; programmed temperature is adopted: the initial temperature is 50℃, maintained for 1min; the temperature is increased to 200℃ at a heating rate of 10℃ / min, and maintained for 1min; the injection port temperature is 220℃; the split ratio is 60:1; the injection volume is 0.5μL; the detector temperature is 250℃.

[0036] (4) Fitting of standard curve According to the gas chromatography measurement results of the methylsulfonyl fluoride-acetone mixed standard working solution, the relationship between the mass of methylsulfonyl fluoride, the mass of acetone and the peak area was obtained by fitting the standard curve, as shown in Table 2: Table 2

[0037] The constant representing the relationship between the mass of the two substances and the peak area was obtained through fitting calculation: k=3.80005.

[0038] (4) Calculate the purity of methylsulfonyl fluoride in the sample to be tested The gas phase determination results of the sample solution are as follows Figure 2As shown, 3.255min is the retention time of acetone, and the peak area is 78.8245%; 3.927min is the retention time of methylsulfonyl fluoride, and the peak area is 21.1392%. Substitute the data into the chromatographic purity calculation formula of methylsulfonyl fluoride:

[0039]

[0040] The purity of methylsulfonyl fluoride in the sample to be tested was calculated to be 99.66%.

[0041] Compared with Example 1 and Example 2, the measured purity error of methylsulfonyl fluoride in the sample does not exceed 0.1%, indicating that the test method provided by the present invention has high accuracy and good stability.

[0042] It should be noted that the above embodiments all belong to the same inventive concept, and the description of each embodiment has its own focus. For matters that are not described in detail in some embodiments, reference may be made to the description in other embodiments.

[0043] The above-mentioned embodiments only express the implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A gas chromatography method for determining the purity of methylsulfonyl fluoride, characterized in that: The steps include: S1: Prepare standard working solution and test solution; S2: using gas chromatography to test the standard working solution and the test solution respectively, to obtain the measurement results of the standard working solution and the measurement results of the test solution; S3: fitting a standard curve to the measurement results of the standard working solution to obtain a functional relationship between the mass of methylsulfonyl fluoride, the mass of the solvent and the peak area of ​​methylsulfonyl fluoride and the peak area of ​​the solvent; S4: According to the test result of the test solution and the functional relationship obtained in step S3, the purity of methylsulfonyl fluoride in the test solution is calculated.

2. The gas chromatography method for measuring the purity of methylsulfonyl fluoride according to claim 1, characterized in that: The solvent used to prepare the solution in step S1 is acetone.

3. The gas chromatography method for measuring the purity of methylsulfonyl fluoride according to claim 1, characterized in that: The concentration of the test solution is 1~2g / g.

4. The gas chromatography method for measuring the purity of methylsulfonyl fluoride according to claim 1, characterized in that: The gas chromatography conditions include: the chromatographic column is a capillary column, 30m×0.32mm×0.25μm; the carrier gas flow rate is 20~50L / min; the fuel gas flow rate is 20~50L / min; the auxiliary gas flow rate is 200~400L / min; the chromatographic column temperature is 180~240℃; the injection port temperature is 180~240℃; the split ratio is 40~60:1; the injection volume is 0.4~0.6μL.

5. The gas chromatography method for measuring the purity of methylsulfonyl fluoride according to claim 4, characterized in that: The stationary phase of the capillary column is 5% phenyl-95% dimethylpolysiloxane.

6. The gas chromatography method for determining the purity of methylsulfonyl fluoride according to claim 4, characterized in that: The temperature of the chromatographic column is raised in the following manner: programmed heating: the initial temperature is 50-100°C, maintained for 1-5 minutes; the temperature is raised to 180-240°C at a heating rate of 5-10°C / min, maintained for 1-5 minutes.

7. The gas chromatography method for determining the purity of methylsulfonyl fluoride according to claim 4, characterized in that: The carrier gas is nitrogen; the fuel gas is hydrogen; and the supporting gas is air.

8. The gas chromatography method for determining the purity of methylsulfonyl fluoride according to claim 4, characterized in that: The detector of the gas chromatograph is a hydrogen flame ionization detector, and the detector temperature is 200-280°C.

9. The gas chromatography method for determining the purity of methylsulfonyl fluoride according to claim 1, characterized in that: The functional relationship between the mass of methylsulfonyl fluoride, the mass of solvent and the peak area of ​​methylsulfonyl fluoride and the peak area of ​​solvent is: In the formula, m' 溶剂 is the mass of the solvent standard in the standard working solution; m' 甲基磺酰氟 is the mass of methylsulfonyl fluoride standard in the standard working solution; A' 甲基磺酰氟 is the peak area of ​​methylsulfonyl fluoride standard in the standard working solution; A' 溶剂 is the peak area of ​​the solvent standard in the standard working solution; k is the constant obtained by fitting the gas phase determination results of the standard working solution.

10. The gas chromatography method for determining the purity of methylsulfonyl fluoride according to claim 1, characterized in that: The purity calculation formula of methylsulfonyl fluoride in the test solution is as follows: In the formula, m 溶剂 is the mass of the solvent in the test solution; m 样品 is the mass of methylsulfonyl fluoride sample in the test solution; A 甲基磺酰氟 is the peak area of ​​methylsulfonyl fluoride in the test solution; A 溶剂 is the peak area of ​​the solvent in the test solution; k is the constant obtained by fitting the gas phase determination results of the standard working solution.

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