Time for an update. A few days before my last post, thermocouples were finally tested. No comment as to why this information isn't already recorded and regularly maintained. Personally I would have thought that this type of task is done annually by first year students.
After that I changed my attention to the dioxin analysis apparatus. Got all parts together and ready for the first fuel combustion, a wheat-municipal waste mixture. Then my first mistake became apparent, the gc inlet liner was too big for the gc-ms. I had simply bought the wrong part; looking back I asked myself, should I check the inlet dimensions? No, they'll have at least two ports won't they? Little did I know how that silly mistake would cost. So I spent subsequent week looking for a machine elsewhere (i.e. another university) to help. Luckily, living near London proved to help me. Refreshing to be able to walk into a lab and start work, none of the risk assessment, safety induction nonsense, can't do attitude here! More bad news: the analysis failed. Despite the best efforts of the technician (a helpful guy), with the standard, no peaks eluted. Then with one of my samples, the desorption was simply too poorly controlled, so the column was overloaded with dirt. Now I know why £15 000 thermal desorption units are invested in; was always risky trying this thermal desorption technique on the cheap without good temperature control to the inlet liner.
Some good news though, managed to obtain some operation time for the combustion of my fuel mixtures, four in total. I know, a pitiful quantity, but this is pilot lab scale, not typical chemistry bench scale work! A little serendipity also came my way; fluidised bed agglomeration forced me to change the bed material, which prompted me to think of this as future journal article content; after all, in the absence of any laboratory work I needed to find content from somewhere. So, whilst awaiting delivery of new (correct!) liners, electron microscopy analysis will be my saviour!
