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[交流]
ICP消解催化剂样品
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想请教若是制备Au/TiO2 用ICP了解Au有多少 一般需要使用哪种消解体系消解样品呢? 我们试过使用纯的硝酸但是 似乎溶的不是很好 Au/TiO2是淡紫色的 在硝酸里泡上一天颜色还是不变 (室温) 是否有经验的人可以来说说要怎么做 [ Last edited by linweiguo0 on 2007-6-6 at 08:58 ] |
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berlin(金币+3):3X
berlin(金币+3):3X
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You weigh it, and put your gold sample in a plastic bottle. You pre-mix HCl and HNO3, either in 3:1 ratio or 1:1 ratio, or 2:1 ratio, roughly, but not precisely. You put the mixed acid into plastic bottle, then you can see the gold is dissolved quickly!! However, at that time, the TiO2 is NOT dissolved! The undissolved TiO2 power will DAMAGE ICP machine. You need to put HF into your plastic bottle, and put the bottle in a water batch at 70 degree for like 30 min. During the initial 30 min, you see some bubbles, meaning that the sample is dissolved. After 30 min, you see there are still some small powders on the bottom of the bottle. You shake the glass bottle a little bit, and then put the bottle in water bath again for some time till it is dissolved. CATUTION: Acids are dangerous! Don't let the temperature higher than 80 degree! DON'T SEAL THE BOTTLE BY USING A COVER! Take a look at your cover! The inner side should be Telfon material, but not a paper material or a Al foil. That will damage the inner side of cover. In particular, if the inner side is Al foil, and you SEAL the cover, the Al will react with acid vaopr, and will change the shape of the plastic bottle, and will even cause accident! Use hood and gloves. HF will damage the fingers quickly! See: A. Horvath, JPCB 110 (2006) 15417. Note: in the above paper, they just used little sample and little acids. You can put more to get a precise result. [ Last edited by zhenmafudan on 2006-12-9 at 03:03 ] |
5楼2006-12-09 03:01:23