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[求助]
合成柠檬酸根修饰的磁性纳米粒子时遇到的问题
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文献上的制备方法： Magnetite(Fe3O4) particles were prepared by co-precipitation of FeCl2 and FeCl3 (1:2 molar ratio) by the addition of NH4OH. In a typical reaction, 0.86 g FeCl2 and 2.35 g FeCl3 were mixed in 40 ml water and heated to 80º C under argon in a three-necked flask. While vigorously stirring the reaction mixture, 5 ml of NH4OH was introduced by syringe and the heating continued for thirty minutes. After that, 1g of citric acid (CA) in 2ml water was introduced, the temperature raised to 95º C and the stirring continued for an additional ninety minutes. A small aliquot of the reaction mixture was withdrawn, diluted to twice its volume and placed on a 0.5 Tesla magnet in a vial. At the point when the particles did not settle down under the influence of the magnet, the colloidal solution was stable. The as-formed reaction product contained an excess of citric acid. Therefore, the nanoparticle dispersion was subjected to dialysis against water in a 12-14 kD cut-off cellulose membrane (Spectrum Laboratories, Inc., USA) for 72 hours to remove the excess unbound CA. The citric acid coated magnetic particles are abbreviated as MP-CA. 我的疑问： 反应在较高温度下进行了很长时间(至少2小时)，体系一直在通氩气，为了保证内部气压不至于过高，肯定要有出气孔，这这么高温度和这么长时间下，体系的水几乎都挥发没了，请问这个问题如何处理？ 谢谢，盼指导！ |
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3楼2012-05-05 10:22:48
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2楼2012-05-05 10:13:33
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4楼2012-05-05 10:46:12
5楼2012-05-05 10:47:34