Dear Everyone. I am trying to do the high yield synthesis from ascorbate and copper salt, according to the similar procedures from the literature (0.18M copper ions) I now tried PVA up to 2%, Tween 20 up to 10%, both, none, dropwise addition of ascorbate, burst addition of ascorbate, nitrogen, air atmosphere, temperatures 50, 60, 90 centigrade. I followed a couple of similar syntheses from the literature, nothing works. All the time instead of suspension I get a salmon-colored precipitate that for sure is not a dozen nanometer copper. What do I do wrong?
Thanks a lot for all the hints
Slow addition with continuous stirring (magnetic stirring) is required.
Dear Sengottuvelan,
Thanks for your prompt. However, today I tried a really slow addition (60 uL/min per 50 synthesis) of ascorbate and the particles are huge.
Best regards
Perhaps a lower proportion of the copper precursor or longer reaction times are more convenient.
I tried different concentrations from 1 to 200 mM... An I'd prefer it in high yields as I need a lot of sample (like a gramm altogether)
Are you sure about the purity of the starting materials? It is better to use Analar grade compounds. You need to optimize the condition with small quantity and then scaling up can be done. The solvent volume is also important. If you are employing lesser quantity of the solvent and higher concentration of the starting material, then the particle aggregation results in.
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