Chromatography Forum

Assumed my colleague knew what he was doing! (and not investigating properly!)
After installing the column in a Shimadzu GCMS he proceeded to analyse a phenol standard and several samples which all also showed phenol. After a week of harassing the supplier on the phone and doubting their quality control I removed the column which had been snapped in the interface to the MS. The first phenol injection had coated the whole system and was appearing in every subsequent injection. Lots of humble pie was consumed

Michael

My first really dumb mistake when I started doing repair work was to install a brand new diffusion pump on an MS with no oil in it.... Second best was removing an old GC column and setting it aside, then picking it up instead of the new one and putting it right back in. Luckily I caught it before I tried to run anything, but it sure did waste a lot of time.

...keeping my 30+ year old calculator alive, see viewtopic.php?f=6&t=15889&start=15

One late afternoon I was busy in my office when our new lab-hand came and told that he ran out of 10% ACN that he needed to reconstitute samples for UPLCMSMS analysis. I was very busy and just told him over my shoulder – Take 100-mL flask, add 10 mL of ACN then top up to volume.

That night we left late, but managed to finish that big batch of urgent samples and loaded them into the UPLCMSMS auto sampler to run overnight.

Next morning I was checking chromatograms – O my God! It was a mess. First peaks were unrecognizable; only very very 1 last peak was sort of OK.

We started investigation, I spent entire day and trace it back to 10% ACN. Our lab-hand did all as he was instructed, took 100-mL volumetric flask, added 10 mL of ACN and toped up to volume with…the same 100% ACN. I did not tell him to top up with water.

Also, topping it off with H2O is not a 10% solution.

One of the most interesting things I find about working in an analytical lab is that if I ask 4 experts to make up 10% ACN, the chances of me getting 4 identical solutions are fairly small. If I make that a 20mM ammonium formate buffer, the chance is miniscule.

How many ways can you think of, to make a 10% ACN solution!?

One of the most interesting things I find about working in an analytical lab is that if I ask 4 experts to make up 10% ACN, the chances of me getting 4 identical solutions are fairly small. If I make that a 20mM ammonium formate buffer, the chance is miniscule.

How many ways can you think of, to make a 10% ACN solution!?

And this is one of the reasons why the compositions of solutions should always be specified in terms of proper units, not percentages. In addition, the mechanics of which goes into the bottle first, having things at the right temperatures and how you read a meniscus are purely technical skills - which is what makes them so important.

Peter

Having been entrusted with one of the first ever hand made glass capillary PLOT columns I placed it onto the chart recorder before installing it into the GC, not realising that the chart recorder was still running - then watching with horror (why does it convert to slow motion?) as it was dispensed over the edge of the recorder and down towards the floor.

Or modifying an old Pye moving wire liquid chromatograph by incorporating an atomiser at the the end of the column to improve the coating of the eluant onto the wire - it worked beautifully for about 20 seconds until the hexane vapours migrated into the FID - setting fire to the whole instrument. Happy days - or happy daze?

Then again, I am currently having to write a 4 page risk assessment on "Boiling a kettle in the lab" (sometimes it is useful to have hot water to dissolve a product ingredient)

That pales into insignificance compared to the person who had to write the risk assessment for a visit to to the local butterfly park, which I found yesterday when I was reviewing the risk assessment files.

At this time of year I remember when I used to bake pizzas in an F30 oven and mince pies and potatoes in 5890s on Christmas eve without a risk assessment - happy daze

We used to get in trouble if the glassware drying oven smelt too strongly of chips on a Monday morning (it ran a bit hot, quite useful). Of course beer bottles in the ice-machine are merely an indication that you work in Germany.
When H&S mania first hit one of my employers, someone wrote a Procedure for Operating a Door (pointing out that doors cause more injuries than anything else in an average building; stairs of course are a genuine issue, although hard to avoid, and sadly do cause some severe injuries). It was followed up with a Procedure to be Followed to avoid Nervous Breakdown on Reading Procedures.

GOM, if you have the courage to do it, sometimes setting fire to your existing instrument can be the best way to get a new one... I've never quite dared, but once (accidentally) totally trashed a rotary evaporator, something I have never regretted. I felt a bit stupid looking at a pile of macerated glass fragments, but its replacement was so very much better. (The original leaked like a sieve, never contained a decent vacuum, so the flasks kept dropping off the end into the water-bath and took a day to dry.. basically it was a machine to keep the scientist out of the way while the sample evaporated through sheer boredom; I never thought a solvent could get up and leave a flask merely because it had become frustrated).

I have accidently dropped a 19L tank that we use for high-throughput prep HPLC purifications, it made an horrible mess in the lab and I have never felt so dumb in my life mopping the floor for hours. At least, the mobile phase was just water!

But there was also another dumb spill accident in my lab where the waste line of our Genevac went out of the waste container right before we decided to defrost and drain the machine that evaporated TFA the night before. The spill left a huge white stain on the floor and even after 2 years and several floor polishings, I can still see some marks from the accident.

During my study, a fellow student hooked up a Bunsen-burner to the water instead of the gas. When he turned it on, he caused a water fountain and showered the entire fumehood...

During my study, a fellow student hooked up a Bunsen-burner to the water instead of the gas. When he turned it on, he caused a water fountain and showered the entire fumehood...

Oh man, that sounds hilarious.

Here are a couple incidents that just happened in the last month.

One co-worker moved her analyses from one HPLC to the other to take advantage of the PDA detector. She set up everything and began running samples. She gave up after a few because she wasn't getting her peaks. She texted me later that evening from home. It suddenly occurred to her that she hadn't adjusted the column switching valve.

That is a common mistake, but this second incident is a classic. One co-worker recently took a trip back to China, but had Visa problems returning. In the meantime, the lab purchased and installed a new UltiMate 3000 HPLC, right next to the dual pump UltiMate 3000 that she is accustomed to work with. When she returned, she wanted to use the new HPLC. So she set up her mobile phase there, installed her column there and everything, then loaded up her samples. She asked me why her runs were being interrupted and moving to the next seconds after they started. I looked and saw she was loading her samples into the first HPLC, and not into the new one. I told her she'd need a longer (and more flexible) sample needle.

Oh, been there, done that, when we got our Waters hplcs upgraded to a workgroup. Co-worker had already purged pumps and got instrument set up ready to go. I logged on, loaded my samples, started the sequence, and heard the other instrument behind me start to make injections.... nothing to stop you using A's computer to control B, and B's computer to control A. It's almost as hilarious as swapping the mouse-cables round in a cramped office.

(which reminds me of the time someone accidentally found the key-combination in Windows for turning the screen display upside down. This means that the mouse also operates upside down, and it's almost impossible to do any useful web-searches for how to solve it when you're searching upside down. Co-worker's solution: balance the monitor upside down and continue as normal...)