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Hive BB  Methods
Discourse  Proper
Preparation of Al/Hg catalyst
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| Author | Topic: Proper Preparation of Al/Hg catalyst |
| Dr
Quack unregistered |
posted 05-10-98 05:02 PM
In an earlier post, ole Strike baby indicated that poor yields and reaction fuckups in top ten #4 were often the result of improper catalyst preparation. Well, its not enough to just say, "improper catalyst preparation". Come on ducks, give up the goods. Just what the hell does that mean. Reach deep down inside that empathenogenic heart of yours and imagine a world where the honey flows like rivers of gold. Quack thinks it is super important for we bees and ducks to talk about this all important subject. One thing that has always bothered Quack is the "nebulous" "wait for the amalgamation to work somewhere in the window of 15 to 30 minutes". "Quack!!!!" says the duck, that leaves a lot of room for error. Even carefully weighing out 1.300 grams of HgCl2 and 50.00 grams of Al one can run into the inevitable. The inevitable is this: One ends up with most (70%+) of the Al getting pulverized and flushed done the drain during the 4 water washings. The amalgum is very sensitive to air so needs to be covered with a little layer of water at the end of the washings. What can be imagined happening from batch to batch (in theory folks) is a very considerable amount of variability with the quality and amount of amalgum available for the reaction. Quack!!!!!!!! So here are the questions we must answer: What is a more detailed method for the preparation of the amalgum? Is there a targeted, rough, eyeballing percent by mass for the amalgum based on the original 50 g of Al used to start that is needed for this reaction as it is written in TS. (In TS, the batch is 50 g of Al to start and 67 g of sacred ketone)? When and how does one know when to stop the amalgamation before it proceeds to far? How does Shulgin shake off the water from the catalyst and not degrade the catalyst? It sure does degrade quicly when exposed to air. Imagine, Imagine...the world of milk and honey! Smooch! -Quackamation |
| Rhodium Administrator |
posted 05-10-98 06:50 PM
You amalgamate the Al too long. The longer the Al is left in contact with the HgCl2 solution, the more fragile it gets. |
| Ritter Member |
posted 05-11-98 12:33 AM
Well, I havn't a lot of time to explain more than a few basics right now, but one thing I can say which will definitely help you is eliminating the four dH2O washes of the amalgamated aluminum. Its OK to pour all of the HgCl2 soln off of the aluminum once sufficiennt effervenscence is observed. Meaning use a hot soln of HgCl2 and amalgamate for no more than 10 minutes!!!! At this point you better act quick or you're going to have one hell of a fire on your hands--burning AL(Hg) SUCKS!!!!!!! So quickly cover it in some 70% IPA and then add the methylamine and sacred ketone and enough 70% IPA to cover the rest of the exposed Al(Hg) and keep temp <<< Later, |
| Osmium Member |
posted 05-11-98 04:00 AM
Use thicker Al foil, like extra strong or plates for barbeque. Reaction will be less vigorous. Weighing exacting amounts is really not necessary. O. never had amalgamation failures. This is almost foolproof. Drain Hg solution when Al is silvery and gas bubbles are visible on the Al surface. O. used the following procedure. The Al was added to denat. EtOH, maybe 1 wt. % of Hg salt (based on the Al)was dissolved in there, and after some time the aq. MeNH2 and the ketone were added. No washing. |
| Dr
Quack unregistered |
posted 05-12-98 11:56 PM
Quackbation!!!!!!! Ya' know, its little bullshit details like the ones given above that
can only be found here, on the best damn site Thanx. -Quack. |
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