Chemistry nightmares, and dreaming of chromatography columns

posted
02-Dec-19, 09:48
Avatar for bdupreez086
posted about 1 week ago
My postgraduate journey has been excting and fascinating, but one of much patience as I needed to make very slow progress during my current year of study as a first-year MSc Winemaking student.

I purify wine tannins using a resin called Sephadex LH-20, which I then pass through more chromatography (HPLC), after which I use this data to get enthalpy (of 'heat' or energy of chemical reaction).
This resin should never run dry, and I would never want to jeopardize my own project; yet it did and my column cracked, which would otherwise ruin my seperation of tannins.

My worst chemistry nightmares have come true, and the fact that these chemicals cost so much money (50 grams of this resin cost over 7K) does not make me feel any better.
Despite that, I am defiant that I'll be able to complete six samples before the end of the year (the acquisition of one sample is about eight hours though).

And I need these purified tannins to get those enthalpy values!

I am just wondering if its normal to make this sort of mistakes in this research environment; I never intended to do so, because in the first place I would never want to waste money in the first place because that will require more waiting - my journey already requires so much waiting!

Is it really okay if things do not go according to plan within this environment, even though it is not your intention to do wrong?

When the resin ran dry, I felt like my world caved in.

I really hope this is the first and last time any of my columns crack, because the emotional burden of having wrecked an expensive instrument, weighs heavily down on me as I seek to cope with the rigours of the postgraduate research environment.
posted
02-Dec-19, 12:22
by rewt
Avatar for rewt
posted about 1 week ago
I completely understand your how feeling. I use BioRad Aminex columns for sugars/organic acids quantification which are about 2K each. The bed can easily collapse if cooled too fast especially if left to dry and guess what I have broken 2! I left the first one to cool overnight with a small flowrate and there was a power cut on that floor!!! Next time is used the column I saw the typical signs of bed collapse and I lost one month of my PhD gone waiting for the replacement to get approved!

The second time I collapsed the column bed all by myself. I was trying to rush some experiments and thought I could cool the column faster than the manufacturer recommended. Nope, that way doesn't work. Then I made it worse the next time I used it, when I turned up the flowrate too fast during start up and saw the pressure spike to over 120 bar (normally 40 bar). That was another 2K down the drain as the column went from slightly broken to full blown dead.

I have also broken a microwave reactor by not reading the instructions, dropped 2 glass desiccators (I now have a plastic one), broke a water bath (still don't know how) and broke a 1K piece of glassware while cleaning it.

Each time I felt gutted and that I shouldn't be there. Though breaking things is part of a PhD. One of the technicians told me I wouldn't be working hard enough if I didn't break things. You learn from your mistakes it is okay because a PhD is supposed to be a place for you to learn and from your mistakes. Everyone has set backs during their PhD and no-one's PhD ever goes to plan. I think the trick is to always look forward and not what could have been.
posted
02-Dec-19, 17:03
edited about 1 minute later
by pm133
Avatar for pm133
posted about 1 week ago
I once put some methanol solution in a sealed flask, set the heater to 120 degrees C to try and force some precipitate to dissolve in it and walked away for lunch.
I was rushing and forgot to both check the boiling point of methanol and to provide a release path for the gases produced.
It exploded, taking the fumehood roof and the expensive vacuum glassware with it.
Don't even know how much this cost but it took 2 months to get replacement specialist glass from the USA.

A week beforehand I nearly killed mysellf by sticking a needle into an autoclave at high pressure with a full syringe attached. The syringe exploded and brushed past my ear landing 30 feet away, melted. Couldn't hear properly for a while.

Lost count of the number of rotary evaporators I have allowed to boil dry.

I also left a sink running that I had plugged with paper towels for half an hour. The ensuing flood took hours to clean up and the staff room was directly below the lab.

Everyone makes mistakes. Some former colleagues have scars to prove it. Hint, never throw raw sodium into a sink full of crushed ice to "quench it". I also witnessed a building evacuation during to HF leakage and a colleague had an NMR tube of liquid oxygen blow up in his hand leaving his face scarred.

Chemistry is just too bloody dangerous and needs computational advances ASAP.
posted
02-Dec-19, 21:49
edited about 7 minutes later
Avatar for Jamie_Wizard
posted about 1 week ago
oh dear.

I don't recall breaking anything, but I once curiously sniffed conc. TFA (Trifluoracetic acid), reasoning that it must be like Salt 'n Vinegar crisps but quite a bit stronger as the 3x F atoms are very electronegative making it a very strong acid - actually it has an acid ionisation constant 34,000 that of Acetic acid, lol. On catching me do this, my supervisor exclaimed "Stupid idiot" as I almost took out all my nasal hair.
posted
02-Dec-19, 21:52
edited about 5 minutes later
Avatar for Jamie_Wizard
posted about 1 week ago
I do, however, recall blowing up the contents of my savoury rice in the microwave at work recently. I put the sachet in for 3 mins without making the outlet slit to let the steam out. I heard a pop and the inside was rice covered. I had sufficient yield leftover for my lunch.

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