Monolithic silica gel adsorption column, and solid phase extraction device and application thereof
A technology of extraction device and solid phase extraction column, which is applied in solid solvent extraction, measuring devices, and other chemical processes, can solve problems that have not been reported before, and achieve the effects of ensuring adsorption efficiency, low environmental requirements, and using a small amount of solvent
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[0030] Example 1
[0031] Preparation of silica monolithic adsorption column
[0032] Weigh 1.2830g polyethylene glycol (MW: 10000), dissolve it in 20ml 0.01M acetic acid solution, add 10ml tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. The solized mixture of tetramethylsiloxane is ultrasonically degassed, and then poured into a straight tube mold (the straight tube mold is a glass tube with a diameter of 30 mm and a length of 15 cm). At 40°C, stand for 2hr to gel. Aging for 24hr at the same temperature. Then, it was treated with a 0.01M ammonium hydroxide aqueous solution at 120°C for 9 hours. The wet silica column was soaked in 0.1M HNO3 for 3 hours, water for 2 hours, and 60% (volume ratio) N,N-dimethylformamide aqueous solution for 5 hours. Finally, the wet silica gel column was dried at 60°C for 10 hours and burned at 700°C for 2 hours. Cut out a 1cm long cylinder and set aside.
Example Embodiment
[0033] Example 2
[0034] Preparation of silica monolithic adsorption column
[0035] Weigh 1.2830g polyethylene glycol (MW: 10000), dissolve it in 20ml 0.01M acetic acid solution, add 10ml tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. The solized mixture of tetramethylsiloxane is ultrasonically degassed and poured into a straight tube mold (the straight tube mold is a plastic tube with a diameter of 50 mm and a length of 20 cm). At 45°C, stand for 2hr to gel. Aging for 24hr at the same temperature. Then, it was treated with a 0.01M ammonium hydroxide aqueous solution at 120°C for 9 hours. The wet silica column was soaked in 0.1M HNO3 for 3 hours, water for 2 hours, and 60% (volume ratio) N,N-dimethylformamide aqueous solution for 5 hours. Finally, the wet silica column was dried at a constant temperature of 50°C for 12 hours, and burned at 800°C for 1 hour. Cut a 15cm cylinder and set aside.
Example Embodiment
[0036] Example 3
[0037] Preparation of silica monolithic adsorption column
[0038] Weigh 1.2830g polyethylene glycol (MW: 10000), dissolve it in 20ml 0.01M acetic acid solution, add 10ml tetramethylsiloxane under ice bath, and stir for 40min at the same temperature. The solized mixture of tetramethylsiloxane is ultrasonically degassed and poured into a straight tube mold (the straight tube mold is a metal tube with a diameter of 6 mm and a length of 5 cm). At 40°C, stand for 2hr to gel. Aging for 24hr at the same temperature. Then, it was treated with a 0.01M ammonium hydroxide aqueous solution at 100°C for 11 hr. The wet silica column was soaked in 0.1MHNO3 for 3hr, water for 2hr, and 60% (volume ratio) N,N-dimethylformamide aqueous solution for 5hr. Finally, the wet silica column was dried at 60°C for 10 hours, and burned at 700°C for 2 hours. Cut a 1cm cylinder and set aside.
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