February 18, 2009

Grignard in the sonicator

One last trick for this *%$&ing Grignard reaction. Sonication is sometimes used to activate the magnesium surface. Ultra-high frequency sound waves are pulsed in a small pool of water. The reaction vessel is submerged in the water and the sound waves cause small bubbles on the surface of the magnesium. These bubles collapse with considerable localized force, and in an ideal situation, activate the surface of the metal. I'll cut to the chase and mention that this did not work either, frustrating me to no end. I am done with Victor Grignard and his ways.

Just because I am giving up on the Grignard reaction and Rieke magnesium does not mean I am admitting defeat here. The magnesium complex was never an object of attainment, merely a means to an end. The object is to get cobalt on the ligand in a high-yielding manner under reasonable reaction conditions; I simply need to try new means to achieve my end. Next up? We run kitty-corner on the periodic table and pound the ligand with a little lithium.

February 11, 2009

Teflon tape to seal joints

I wanted to find a way to reflux under inert conditions without drawing silicon grease into the reaction flask. I tried using some Teflon tape in between the joints. This sort of worked, but sort of didn't. When I tested the the seal it held better vacuum than ground glass on ground glass, but unfortunately it was not as good as a greased joint. I tried to make a better seal with a little more pressure. With enough pressure the tape in the joint became translucent, looking as thought it almost would form a perfect seal. With a little more pressure I cracked the glass into millions of little pieces, cutting my hand in several places and making a mess of tiny glass shards in my hood. I do not recommend this method.

February 6, 2009

sodium sculpture



These are two pictures of the same solvent pot. The opening of the bomb flask is very small, so only skinny things can fit through, such as the stir bar (the black pill shaped object). To fit the sodium (drying agent) through the hole it was rolled between two fingers in the dry box for form a long skinny cylinder of metal. After stirring for prolonged periods of time, the ends of the soft sodium metal are warped from banging into the sides of the flask to give the unusual shape shown in the pictures above.

February 2, 2009

kosher fake butter

One of the labmates got a rather large shipment of chemical the other day. On the side of this very large bottle was a stamp proclaiming this chemical as kosher.

Interesting, we thought. Most of our chemicals are explicit in stating that these chemicals are for research use only and not to be used for food or drugs. This got the lab chatting a little bit about what was inside. Acetoin (and the very similar diacetyl) are used to give things like margarine their butter-like flavor and smell. It's most recognizable as the smell of microwave popcorn. I considered this for a moment before cautiously sniffing around the outside of the container. I couldn't smell anything so I cracked the lid and made a rookie chemist mistake; I sniffed right in the mouth of the jar. A seasoned chemist would advise not sniffing at all, but when smelling the chemical is absolutely necessary you are supposed to waft the scent towards you. Well, the freshly opened acetoin nearly knocked me flat on my ass. It smelled awful, and only after about five minutes later, when my sense of smell started to clear up, did it start to smell anything like butter.

Some additional trivia... Less than a gram of this compound was needed, but the smallest quantity available is 1 kilogram. Rabbi Gershon Segal certified this particular fake butter flavoring as kosher; thanks, Rabbi.