Method for purifying acetonitrile for liquid chromatogram-mass spectrometer
A technology of liquid chromatography and purification method, which is applied in the field of purification of acetonitrile for liquid chromatography-mass spectrometry, can solve the problems of difficult removal of impurities, difficult purification, difficult acetonitrile, etc., to reduce the cost of imports, The effect of expanding the application range and simplifying the production process
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Embodiment 1
[0022] The purification method of acetonitrile for liquid chromatography-mass spectrometry analysis is characterized in that, comprises the following steps:
[0023] a. Take the raw material acetonitrile, add sulfuric acid to it and vibrate to form a sulfate precipitate, and let it stand at -30 ° C. After layering, discard the water layer, and filter the organic layer to remove the sulfate precipitate. , keep the filtrate. Then, activated carbon was added to the filtrate, followed by stirring for 1 hour. After stirring, potassium permanganate is added for oxidation treatment to remove unsaturated hydrocarbon impurities such as acrylonitrile, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, and at the same time neutralize the acidic substances produced by oxidation, and adjust the pH value to 7. After the oxidation treatment, acetonitrile was rapidly distilled off....
Embodiment 2
[0029] The purification method of acetonitrile for liquid chromatography-mass spectrometry analysis is characterized in that, comprises the following steps:
[0030] a. Take the raw material acetonitrile, add sulfuric acid to it and shake it to generate a sulfate ester precipitate, and let it stand at a temperature of 20 ° C. After layering, discard the water layer, and filter the organic layer to remove the sulfate ester precipitate. The filtrate was retained. Then, activated carbon was added to the filtrate, followed by stirring for 2 hours. After stirring, potassium permanganate is added for oxidation treatment to remove unsaturated hydrocarbon impurities such as acrylonitrile, acetamide and other impurities. At the same time of adding potassium permanganate, sodium hydroxide and calcium oxide are added to slow down the oxidation of potassium permanganate, and at the same time neutralize the acidic substances produced by oxidation, and adjust the pH value to 7.5. After th...
Embodiment 3
[0036] The purification method of acetonitrile for liquid chromatography-mass spectrometry analysis is characterized in that, comprises the following steps:
[0037] a. Take the raw material acetonitrile, add sulfuric acid to it and shake to form a sulfate precipitate, and let it stand at -10°C. After layering, discard the water layer, and filter the organic layer to remove the sulfate precipitate. , keep the filtrate. Then, activated carbon was added to the filtrate, followed by stirring for 1.5 hours. After stirring, potassium permanganate is added for oxidation treatment to remove unsaturated hydrocarbon impurities such as acrylonitrile, acetamide and other impurities. While adding potassium permanganate, add sodium hydroxide and calcium oxide to slow down the oxidation of potassium permanganate, and at the same time neutralize the acidic substances produced by oxidation, and adjust the pH value to 7. After the oxidation treatment, acetonitrile was rapidly distilled off. ...
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