Purification method of acetonitrile for liquid chromatography-mass spectrometer
A technology of liquid chromatography and purification method is applied in the field of purification of acetonitrile used in a liquid chromatography-mass spectrometer, and can solve the problems of difficult to remove impurities, difficult to acetonitrile, difficult to purify, etc., and to reduce the cost required for imports, The production process is simple and the effect of expanding the scope of application
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Embodiment 1
[0022] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:
[0023] a. Take the raw material acetonitrile, add sulfuric acid to it for vibration, generate sulfate ester precipitates, and let it stand at -30°C, discard the water layer after layering, and filter the organic layer to remove sulfate ester precipitates , retain the filtrate. Then activated carbon was added to the filtrate and stirred for 1 hour. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 8. After the oxidation treatment...
Embodiment 2
[0029] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:
[0030] a. Take the raw material acetonitrile, add sulfuric acid and nitric acid to it for oscillation, generate sulfate and nitrate precipitates, and let it stand at 20°C, discard the water layer after layering, and filter the organic layer, The sulfate ester precipitate was removed and the filtrate was retained. Immediately after, activated carbon was added to the filtrate and stirred for 2 hours. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, an...
Embodiment 3
[0036] The method for purifying acetonitrile for liquid chromatography-mass spectrometry is characterized in that it comprises the steps:
[0037] a. Take the raw material acetonitrile, add sulfuric acid to it for vibration, generate sulfate ester precipitates, and let it stand at -10°C, discard the water layer after layering, and filter the organic layer to remove sulfate ester precipitates , retain the filtrate. Immediately after, activated carbon was added to the filtrate and stirred for 1.5 hours. After the stirring is completed, potassium permanganate is added for oxidation treatment to remove impurities containing double bonds such as acrylonitrile, hydrocyanic acid, acrolein, methacrylonitrile, acryl alcohol, oxazole, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, neutralize the acidic substances produced by oxidation, and adjust the pH to 10. After the o...
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