October 2005

October 9, 2005

        Note my apparatus that I made for this preparation.  It was constructed of iron pipes, a regular end cap at the bottom and a reducing adaptor at the top, into this was placed the top of a broken off 24/40 adaptor and this was held in place with fireplace cement that had to be fire cured into place, it held up nicely.  With a metal tube fitted with a 24/40 adaptor 48 grams of sulfur, 9 grams of carbon and a pinch of sodium carbonate were added and into the powder was placed 5 hollow aluminum rods to help heat conduction seeing as how aluminum develops a passive coating on reaction with sulfur.

        The prepared apparatus was attached to a normal distillation setup and the exit gasses lead through basified water.  The pipe was sealed and my fingers were crossed and I started heating full blast with a blow torch.  Nothing for some time then white wispy smoke started to appear in the condenser, the still head temperature remained around 30C the whole time despite sulfur condensing out of the smoke.  Eventually the sulfur gas traveled into the condenser and beyond depositing fine sulfur everywhere.  It was nearly and hour later that I started to notice liquid in the still head, at first I thought that the sulfur was super cooling seeing as how the still head was still cool but after noticing the liquid running and collecting I realized that it was indeed carbon disulfide (at least it likely was) that was collecting.  This is around the time the picture above was taken, you can see droplets and different colors of liquid in the still head, some of this is CS2 (white droplets) and some of it is just deposited elemental sulfur.

        Being curious as to how my base wash was fairing I took some powdered copper sulfate and added it in one go to the clear wash bottle liquid.  Instantly the water turned black (lots of hydrogen sulfide I guess!) so I started to get wary of the reaction and after some time it settled leaving the water a dark green, you can see elemental copper in the picture, I guess there was also sulfur dioxide dissolved in the water.  So my wash bottle was actually getting close to saturated.  I added some more KOH to it and kept going but the evolution of carbon disulfide was incredibly slow and my insulation around my distilling pipe caught on fire and smoldered.  So I had to give up.  After 3 hours of work I got maybe 5 ml of carbon disulfide, very disappointing.

October 30, 2005

       Today I tried to prepare potassium metal by reaction of potassium hydroxide with magnesium turnings in kerosene with a alcohol added to help speed the reaction up, the reaction follows the procedure outlined by patent US 4725311 with the exception that the quantities were only 25% of the example first given, roughly 175 ml kerosene, 3 ml isopropyl alcohol, 8 grams of magnesium and 15 grams of KOH.  These were mixed in a 250 ml Erlenmeyer flask and heated with a vigurex column for reflux and the exit gasses were run though KOH pellets to remove water that might make it though to the reaction flask.  The mixture was heated for 4 hours at near boiling and a reaction was apparent via hydrogen evolution and most convincingly by the precipitation of magnesium oxide/hydroxide in the flask as the reaction proceeded, it was evident the magnesium was being consumed.  The mixture was allowed to cool after 4 hours and it was left like that for several hours then stoppered.  

        The next day the mixture was again heated with some more isopropyl alcohol and stirred, a darker brown color had developed that was lacking previously and there was still a few grams of magnesium left unreacted.  After an hour though the amount of magnesium left had not decreased.  The mixture was allowed to cool to manageable levels and poured slowly into a Buckner funnel using fiberglass to filter it.  However no potassium metal was recovered, there was roughly 2 grams of solid magnesium left in the mixture.  However the magnesium was incredibly reactive, a small amount added to some isopropyl alcohol dissolved in kerosene gave a strong effervescence showing that perhaps some potassium was impregnated on its surface.  Still I think this reaction will work great after I get some tert-butyl alcohol which is the recommended alcohol and also if I run it at higher temperatures, then my main concern will be to find a better method of separation.

Current Comments

1 comments so far (post your own)

Regarding the CS2 synth, the old processes used all iron pipe fittings, with the carbon being heated to redness before sulphur lumps were dropped in on top via a long tube sealed with a ceramic plug

The preheating would seem to prevent the sulfur from subliminating before it could react, as it did in your experiment.

Posted by nbk2000 on Saturday, 10.28.06 @ 17:35pm | #38

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