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Method for determining the content of acetonitrile in a sample

A sample and acetonitrile technology, applied in the field of determining the content of acetonitrile in the sample, can solve the problems of inability to measure the purity of acetonitrile, the inability to accurately measure the purity of acetonitrile, low acetonitrile, etc.

Active Publication Date: 2021-10-29
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the domestic acetonitrile extraction process, the detection method of acetonitrile content from the cracking C4 to produce butadiene is the enterprise's own standard, which is the subtraction method, that is, the purity of acetonitrile is equal to 100% minus the content of water and dimer , other organic impurities are not detected, and the purity of acetonitrile cannot be accurately measured
And industry standard SHT-1627 " industrial acetonitrile purity and the mensuration of organic impurity " method can measure acetonitrile purity, but this method is only applicable to the acetonitrile that purity is more than 98% by weight, and the FFAP chromatographic column that it uses is polar chromatographic column , C1-C4 hydrocarbons cannot be effectively separated, and SHT-1627 only measures organic components such as acetone, acrylonitrile, and propionitrile, but does not perform qualitative analysis on components such as methanol, ethanol, and isopropanol, so it cannot be determined that the purity is lower than 98% by weight of acetonitrile, and it is impossible to detect in detail the content of dissolved C1-C4 hydrocarbons, methanol, ethanol and isopropanol in acetonitrile

Method used

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  • Method for determining the content of acetonitrile in a sample
  • Method for determining the content of acetonitrile in a sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 0.5 μL of sample 1 to be tested into column 1 for measurement, and control the carrier gas N 2 The flow rate is 3mL / min, the split ratio is 60:1, and the column temperature is controlled at 50°C for 10 minutes, then raised to 230°C at 20°C / min for 5 minutes; then 1 μL of sample 1 to be tested is added to column 2 for determination , control carrier gas N 2 The flow rate is 5mL / min, the split ratio is 5:1, and the column temperature is controlled at 40°C for 5 minutes, then raised to 60°C at 2°C / min, then raised to 100°C at 3°C / min, and then at 10°C ℃ / min rises to 180 ℃ for 7 minutes, and the valve cut time is 4 minutes.

[0030] Then, according to the external standard method, methanol, ethanol, isopropanol, acetone and dimers of known content were added to the column 1 respectively, and measured with the same chromatographic conditions as described above, and then the C1- C4 hydrocarbons were added to column 2 respectively, and measured under the same chromatogra...

Embodiment 2

[0032] Add 0.5 μL of sample 1 to be tested into column 1 for measurement, and control the carrier gas N 2 The flow rate is 2.5mL / min, the split ratio is 60:1, and the column temperature is controlled at 45°C for 11 minutes, and then raised to 225°C at 18°C / min for 4 minutes; then 1 μL of sample 1 to be tested is added to column 2 for Determination, control carrier gas N 2 The flow rate is 4.5mL / min, the split ratio is 5:1, and the column temperature is controlled at 35°C for 6 minutes, then raised to 65°C at 2°C / min, then raised to 105°C at 3°C / min, and then 11 ℃ / min rise to 185 ℃ constant temperature 8 minutes, the valve cut time is 3.8 minutes.

[0033] Then according to the external standard method, add methanol, ethanol, isopropanol, acetone and dimers of known content into column 1 respectively, and measure with the same chromatographic conditions as above, and then add the C1-C4 The hydrocarbons were added to the column 2 respectively, and measured under the same chr...

Embodiment 3

[0035] Add 0.5 μL of sample 1 to be tested into column 1 for measurement, and control the carrier gas N 2 The flow rate is 3.5mL / min, the split ratio is 60:1, and the column temperature is controlled at 55°C for 9 minutes, and then raised to 235°C at 22°C / min for 6 minutes; then 1 μL of sample 1 to be tested is added to column 2 for Determination, control carrier gas N 2 The flow rate is 5.5mL / min, the split ratio is 5:1, and the column temperature is controlled at 45°C for 4 minutes, then raised to 55°C at 1.5°C / min, then raised to 95°C at 2°C / min, and then 9°C / min rises to 175°C for 6 minutes, and the valve cut-off time is 4.2 minutes.

[0036] Then, according to the external standard method, methanol, ethanol, isopropanol, acetone and dimers of known content were added to the column 1 respectively, and measured with the same chromatographic conditions as described above, and then the C1- C4 hydrocarbons are respectively added in the column 2, and are measured with the sam...

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Abstract

The invention relates to the field of chemical testing, and discloses a method for determining the content of acetonitrile in a sample. The sample contains organic impurities and acetonitrile. The method includes: performing gas chromatographic analysis on the sample to determine the content of the organic impurities, and then performing a subtraction method The content of acetonitrile was calculated, and the organic impurities included C1-C4 hydrocarbons, methanol, ethanol, isopropanol, acetone and dimers. By the method of the present invention, it is possible to accurately measure the content of acetonitrile in samples with lower acetonitrile purity (especially the circulating acetonitrile solvent in the process of producing butadiene by the acetonitrile extraction process), and it is also possible to monitor the content of each organic impurity in real time, It is conducive to the stable operation of the extraction process device for a long period of time and high economy.

Description

technical field [0001] The invention relates to the field of chemical testing, in particular to a method for determining the content of acetonitrile in a sample. Background technique [0002] Some domestic enterprises use the acetonitrile extraction process to produce butadiene products, and the quality of the circulating acetonitrile solvent is related to whether the extraction process can operate stably for a long period of time with high economic efficiency, and determines the pressure difference of the extraction tower and the temperature of the distillation tower control. Therefore, accurate determination of the purity of circulating acetonitrile solvent and the content of main organic impurities is very important for improving the solvent quality of the process of extracting butadiene with acetonitrile and ensuring the long-term, high-economic and stable operation of the device. [0003] At present, in the domestic acetonitrile extraction process, the detection method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 贾闯叶华盛徐丽萍邵柯迪蔡方方檀革江
Owner CHINA PETROLEUM & CHEM CORP
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