阅读说明：本技术 一种气相色谱法测定丁二酸酐纯度的方法 (Method for measuring purity of succinic anhydride by gas chromatography ) 是由 程露 于 2019-10-31 设计创作，主要内容包括：本发明公开了一种气相色谱法测定丁二酸酐纯度的方法,其色谱条件为：色谱柱为非极性毛细管色谱柱,色谱柱程序升温,初始温度为30-100℃,以10-30℃/min升温至90-150℃,保温2-5min,再以10-30℃/min升温至200-250℃,保温2-5min；以氮气为载气,载气流速为250mL/min；进样口温度为200-280℃,检测器温度为200-260℃,进样口的分流比为50-200：1。本发明采用气相色谱法测定丁二酸酐纯度,操作简单,稳定好,准确度高,重现性好。(The invention discloses a method for measuring the purity of succinic anhydride by gas chromatography, which comprises the following chromatographic conditions: the chromatographic column is a nonpolar capillary chromatographic column, the temperature of the chromatographic column is programmed to rise, the initial temperature is 30-100 ℃, the temperature rises to 90-150 ℃ at the speed of 10-30 ℃/min, the temperature is kept for 2-5min, the temperature rises to 200 ℃ at the speed of 10-30 ℃/min, and the temperature is kept for 2-5 min; taking nitrogen as carrier gas, wherein the flow rate of the carrier gas is 250 mL/min; the temperature of the sample inlet is 200-280 ℃, the temperature of the detector is 200-260 ℃, and the split ratio of the sample inlet is 50-200: 1. the method adopts the gas chromatography to measure the purity of the succinic anhydride, and has the advantages of simple operation, good stability, high accuracy and good reproducibility.)

1. A method for measuring the purity of succinic anhydride by gas chromatography is characterized in that the chromatographic conditions are as follows: the chromatographic column is a nonpolar capillary chromatographic column, the temperature of the chromatographic column is programmed to rise, the initial temperature is 30-100 ℃, the temperature rises to 90-150 ℃ at the speed of 10-30 ℃/min, the temperature is kept for 2-5min, the temperature rises to 200 ℃ at the speed of 10-30 ℃/min, and the temperature is kept for 2-5 min; taking nitrogen as carrier gas, wherein the flow rate of the carrier gas is 250 mL/min; the temperature of the sample inlet is 200-280 ℃, the temperature of the detector is 200-260 ℃, and the split ratio of the sample inlet is 50-200: 1.

2. the method for determining purity of succinic anhydride according to claim 1, wherein the column has a size of 30m x 320 μm x 0.25 μm.

3. A method for determining the purity of succinic anhydride according to claim 1 or 2, characterized in that the temperature of the column is programmed to increase initially at 60 ℃, from 15 ℃/min to 90 ℃ for 2min, and from 10 ℃/min to 230 ℃ for 2 min.

4. The method for measuring purity of succinic anhydride according to any one of claims 1 to 3, wherein the hydrogen flow rate is 30mL/min and the air flow rate is 400 mL/min.

5. A method for determining the purity of succinic anhydride according to any one of claims 1-4, characterized in that the injection port temperature is 260 ℃ and the detector temperature is 250 ℃.

6. A method for determining the purity of succinic anhydride according to any one of claims 1 to 5, characterized in that the split ratio of the injection ports is 100: 1.

7. a method for determining the purity of succinic anhydride according to any one of claims 1-6, characterized in that the detector is a hydrogen flame ion detector FID.

8. A method for determining the purity of succinic anhydride according to any one of claims 1 to 7, characterized in that the amount to be sampled is 0.2. mu.L.

9. A method for determining the purity of succinic anhydride according to any one of claims 1-8, characterized in that the purity of nitrogen is not less than 99.999%.

10. The method for determining the purity of succinic anhydride according to any one of claims 1 to 9, wherein an acetone solution having a concentration of 0.2g/mL succinic anhydride is used as the sample solution; preferably, the purity of the succinic anhydride is calculated by adopting an area normalization method; preferably, pharmaceutical grade succinic anhydride is used as a control.

Technical Field

The invention relates to the technical field of chemical product analysis and detection, in particular to a method for determining the purity of succinic anhydride by gas chromatography.

Background

Succinic anhydride is colorless needle-shaped or sheet-shaped crystal, is slightly soluble in cold water and ether, is soluble in hot water and acetone, and is an important fine chemical raw material. Can be widely used in pharmacy, food additive and pharmaceutical intermediate, and can be used for preparing succinimide and other medicines. The purity of the succinic anhydride is generally determined by a titration method, so that the determination period is long, the error is large, and no unified national standard is provided for determining the purity of the succinic anhydride at present.

Disclosure of Invention

Based on the technical problems in the background art, the invention provides a method for measuring the purity of succinic anhydride by using a gas chromatography.

The invention provides a method for measuring the purity of succinic anhydride by gas chromatography, which comprises the following chromatographic conditions: the chromatographic column is a nonpolar capillary chromatographic column, the temperature of the chromatographic column is programmed to rise, the initial temperature is 30-100 ℃, the temperature rises to 90-150 ℃ at the speed of 10-30 ℃/min, the temperature is kept for 2-5min, the temperature rises to 200 ℃ at the speed of 10-30 ℃/min, and the temperature is kept for 2-5 min; taking nitrogen as carrier gas, wherein the flow rate of the carrier gas is 250 mL/min; the temperature of the sample inlet is 200-280 ℃, the temperature of the detector is 200-260 ℃, and the split ratio of the sample inlet is 50-200: 1.

preferably, the column has a size of 30 m.times.320. mu.m.times.0.25. mu.m.

Preferably, the temperature of the chromatographic column is programmed to be raised to 90 ℃ at an initial temperature of 60 ℃ at a rate of 15 ℃/min, and is kept for 2min, and then raised to 230 ℃ at a rate of 10 ℃/min, and is kept for 2 min.

Preferably, the hydrogen flow rate is 30mL/min and the air flow rate is 400 mL/min.

Preferably, the injection port temperature is 260 ℃ and the detector temperature is 250 ℃.

Preferably, the split ratio of the injection port is 100: 1.

preferably, the detector is a hydrogen flame ion detector FID.

Preferably, the sample size is 0.2. mu.L.

Preferably, the purity of the nitrogen is more than or equal to 99.999 percent.

Preferably, an acetone solution with a concentration of 0.2g/mL succinic anhydride is used as the sample solution.

Preferably, the succinic anhydride purity is calculated using area normalization.

Preferably, pharmaceutical grade succinic anhydride is used as a control.

The specific experimental steps are as follows:

preparing a solvent:

blank solvent: acetone.

Qualitative solution: 0.5g of pharmaceutical grade succinic anhydride was dissolved in 2.5mL of acetone.

Sample solution: 0.5g of the technical succinic anhydride to be tested is dissolved in 2.5mL of acetone.

Sample introduction: and (3) respectively taking 0.2 mu L of blank solvent, qualitative solution and sample solution, sequentially injecting samples, recording a chromatogram, and calculating the purity of the succinic anhydride by adopting an area normalization method.

The blank solvent is used to remove the interference of acetone as the solvent, and the qualitative solution is used to determine the retention time of succinic anhydride, i.e., peak location.

The area normalization method is a conventional chromatographic purity calculation method in the field, and comprises the following specific operations: removing a solvent peak, and dividing the succinic anhydride peak area by the sum of the succinic anhydride peak area and the impurity peak area to obtain the purity of the succinic anhydride.

The method adopts the gas chromatography to measure the purity of the succinic anhydride, and has the advantages of simple operation, good stability, high accuracy and good reproducibility.

Detailed Description

The technical solution of the present invention will be described in detail below with reference to specific examples.