October 20, 2004
I was attempting to make bromine by a procedure I had used before, the reaction of sodium bromide with potassium bromate and sulfuric acid:
2KBrO3 + 6H2SO4 + 10NaBr ---> 6Br2 + 6H2O + 5Na2SO4 + K2SO4
So for every mol of potassium bromide 3 mol of Br2 are produced so I've always considered this a good reaction to make bromine. Anyway, the weather was cool but I knew the reaction would heat up and I like to keep my bromine cool so it doesn't get everywhere. So before even adding the H2SO4, with just the solid reagents in the container I added a bunch of crushed ice, and as I added dilute H2SO4 I kept adding ice. When it was over I had the familiar bromine (very bottom, you can barely make it out) and above it a precipitate, I thought at first that it was sulfates crystallizing out of the solution, but when I removed some it immediately melted and released bromine, I had made bromine hydrate which is a crystalline compound stable at less then 4C. It was an interesting side note to this otherwise normal reaction.
October 25, 2004
A continuation of my experiments from May 22, here I once again tried electrolysis of lithium chloride in DMSO. This time though I used a smaller power source over a greater period of time, it was less then 1 A therefore I did not expect, nor did I get any lithium metal. However what I did get was an interesting precipitate, seen floating in the solution and a distinct separation between the solution that occurred. Notice that the top turned a deep red and developed an intense smell, whereas nickel ions formed from the anode dissolving floated straight to the bottom and made their own layer there. I am still wondering about the precipitate though, some condensation reaction, or even something really interesting like methyl lithium? A very interesting reaction despite the fact I only have a small amount of direction as to what is going on.
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