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[求助]
合成檸檬酸根修飾的磁性納米粒子時遇到的問題
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文獻(xiàn)上的制備方法: 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 A small aliquot of the reaction mixture was withdrawn, diluted to twice its volume and placed on a 0.5 Tesla magnet in a vial.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. 我的疑問: 反應(yīng)在較高溫度下進(jìn)行了很長時間(至少2小時),體系一直在通氬氣,為了保證內(nèi)部氣壓不至于過高,肯定要有出氣孔,這這么高溫度和這么長時間下,體系的水幾乎都揮發(fā)沒了,請問這個問題如何處理? 謝謝,盼指導(dǎo)! |
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