A while back I was attempting to chlorinate sulfur in a dry reaction using a test tube mix of sulfur and TCCA. As the mixture was heated it started to
produce a condensible liquid that I capped in a test tube assuming it was mixed sulfur chlorides, and also starting material and other byproducts.
Well, it's been a while and this test tube has sat in a test tube rack at the back of my bench. This evening I decided it was time to dispose of it,
so I took it out back and threw it a distance attempting to break it as I didn't want to smell it. It didn't break, so I walked up to it and hit it
with a stick. POW!!! There was nothing left but the rubber stopper. I figured that it had built up pressure, but what was up with it being so loud
that it left my ears ringing, and when I came in a few minutes later I was asked if I had shot a gun.
So what happened? I know that TCCA mixtures can be unstable, but what was this? It sounded and looked like when I was playing around with nitrogen
trichloride in small amounts. Was this nitrogen trichloride? The test tube just vanished... leaving behind a nasty sulfur smell.
[Edited on 3-8-2016 by Loptr]j_sum1 - 3-8-2016 at 14:55
Sounds to me like you made some NCl3.
It could have gone a lot worse. You were lucky. Good thing your volumes were small. Chalk that one up to a close shave.PHILOU Zrealone - 4-8-2016 at 07:15
The two possible ideal suspects are NCl3 and/or S4N4...
Glass shrapnels cuts and pierce flesh/eyes and are hard to get rid of vs metallic ones because of their transparency...you was under a Lucky star this
time!Loptr - 4-8-2016 at 08:28
The two possible ideal suspects are NCl3 and/or S4N4...
Glass shrapnels cuts and pierce flesh/eyes and are hard to get rid of vs metallic ones because of their transparency...you was under a Lucky star this
time!
Speaking of S4N4 there was a solid precipitate at the bottom of the test tube that was not there when first stored. I thought it was sulfur that had
precipitated since the original volume of liquid had reduced, which I had believed was from reaction with the rubber stopper. The rubber stopper had
become enlarged and significantly deformed and corroded. Sulfur is soluble in disulfur dichloride, so the naive assumption fit at the time.
The color of the precipitate could be described as sulfur-like, but maybe a brighter yellow-gold color, and the distillate itself had turned from a
deep red to orange.
As for the lucky star, it was a pretty long stick and I was on the other side of a tree. I had thrown it aiming at the tree, so when it didn't break I
came around the side and hit it. I am glad I was scared of a pressure build up and getting it on me, and expected a pop, but not a bang. I had minimal
exposure when it went off.
