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Method for determining purity of succinic anhydride by adopting gas chromatographic method

A technology of gas chromatography and succinic anhydride, which is applied in the field of analysis and detection of chemical products, can solve the problems of measuring the purity of succinic anhydride, long measurement cycle, large error, etc., and achieve the effect of good stability, high accuracy and simple operation

Inactive Publication Date: 2020-03-17
ANHUI GUOFENG PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the determination of the purity of succinic anhydride generally adopts the titration method, the measurement period is long and the error is large, and there is no unified national standard to determine the purity of succinic anhydride.

Method used

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  • Method for determining purity of succinic anhydride by adopting gas chromatographic method

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Experimental program
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Effect test

Embodiment 1

[0027] A method for measuring the purity of succinic anhydride by gas chromatography, its chromatographic condition is:

[0028] The chromatographic column is a non-polar capillary column with a specification of 30m×320μm×0.25μm.

[0029] The temperature of the chromatographic column is programmed, the initial temperature is 30°C, the temperature is raised to 90°C at 10°C / min, and kept for 5 minutes, then the temperature is raised to 200°C at 10°C / min, and kept for 5 minutes;

[0030] Nitrogen is used as the carrier gas, the carrier gas flow rate is 250mL / min, the hydrogen flow rate is 30mL / min, and the air flow rate is 400mL / min;

[0031] The inlet temperature was 220°C, the detector temperature was 250°C, the split ratio of the inlet was 50:1, and the detector was a hydrogen flame ion detector (FID).

[0032] Preparation solvent:

[0033] Blank solvent: acetone.

[0034] Qualitative solution: Dissolve 0.5g of pharmaceutical grade succinic anhydride in 2.5mL of acetone.

...

Embodiment 2

[0038] A method for measuring the purity of succinic anhydride by gas chromatography, its chromatographic condition is:

[0039] The chromatographic column is a non-polar capillary column with a specification of 30m×320μm×0.25μm.

[0040] The temperature of the chromatographic column is programmed, the initial temperature is 100°C, the temperature is raised to 150°C at 30°C / min, and kept for 2 minutes, then the temperature is raised to 250°C at 30°C / min, and kept for 2 minutes;

[0041] Nitrogen is used as the carrier gas, the carrier gas flow rate is 250mL / min, the hydrogen flow rate is 30mL / min, and the air flow rate is 400mL / min;

[0042] The inlet temperature was 250°C, the detector temperature was 250°C, the split ratio of the inlet was 150:1, and the detector was a hydrogen flame ion detector (FID).

[0043] Preparation of solvent and injection are the same as in Example 1.

Embodiment 3

[0045] A method for measuring the purity of succinic anhydride by gas chromatography, its chromatographic condition is:

[0046] The chromatographic column is a non-polar capillary column with a specification of 30m×320μm×0.25μm.

[0047] The temperature of the chromatographic column is programmed, the initial temperature is 50°C, the temperature is raised to 120°C at 15°C / min, and the temperature is kept for 3 minutes, and then the temperature is raised to 220°C at 15°C / min, and the temperature is kept for 3 minutes;

[0048] Nitrogen is used as the carrier gas, the carrier gas flow rate is 250mL / min, the hydrogen flow rate is 30mL / min, and the air flow rate is 400mL / min;

[0049] The inlet temperature was 200°C, the detector temperature was 250°C, the split ratio of the inlet was 50:1, and the detector was a hydrogen flame ion detector (FID).

[0050] Preparation of solvent and injection are the same as in Example 1.

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Abstract

The invention discloses a method for determining purity of succinic anhydride by adopting a gas chromatographic method. The method has the chromatographic conditions that: a chromatographic column isa non-polar capillary chromatographic column, the temperature of the chromatographic column is raised in a programmed manner, the initial temperature is 30-100 DEG C, the temperature of the chromatographic column rises in a programmed manner, the initial temperature is 30-100 DEG C and is raised to 90-150 DEG C at a speed of 10-30 DEG C / min, heat preservation is performed for 2-5 min, then the temperature is raised to 200-250 DEG C at a speed of 10-30 DEG C / min, and heat preservation is performed for 2-5 min; a nitrogen gas serves as a carrier gas, wherein a flow rate of the carrier gas is 250mL / min; and the temperature of a sample inlet is 200-280 DEG C, the temperature of a detector is 200-260 DEG C, and a split ratio of the sample inlet is 50-200:1. According to the method, the purityof succinic anhydride is determined by adopting the gas chromatographic method, the operation is simple, the stability is good, the precision is high, and the reproducibility is good.

Description

technical field [0001] The invention relates to the technical field of chemical product analysis and detection technology, in particular to a method for measuring the purity of succinic anhydride by gas chromatography. Background technique [0002] Succinic anhydride is a colorless needle-like or flaky crystal, slightly soluble in cold water and ether, soluble in hot water and acetone, and is an important fine chemical raw material. It is widely used in pharmaceuticals, food additives and pharmaceutical intermediates, and can be used to manufacture succinimide and other drugs. Since the determination of the purity of succinic anhydride is generally carried out by titration, the measurement cycle is long and the error is large, and there is no unified national standard to determine the purity of succinic anhydride. Contents of the invention [0003] Based on the technical problems existing in the background technology, the present invention proposes a method for measuring ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 程露
Owner ANHUI GUOFENG PLASTIC
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