Who is Going To Mark My Report?!

I got my report bound today. It now looks almost half-decent-professional, yay! On the other hand, the completed report reminds me of the following conversation I had with my supervisor while he was marking it...

Supervisor, regarding an equation he'd write differently: "...only people who are interested in the subject will notice that."
Me: "Well, the markers at the university are English majors, and all they look for are grammar and formatting and such."
". . . English majors?!"
"...yeah. That's why we have a technical evaluation."

Needless to say, I made the suggested changes and sent him the revised version, anyway, English majors or not. On the bright side, my supervisor did like my report even without the changes...

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Pictures I Forgot to Post

I can't believe I almost forgot about these pictures.

The ICP gone wrong, taken with a cellphone camera.

A reaction I've been wanting to do ever since I have heard about it. Pretty colours, loud(ish) noises, and bright lights. What more do you want?

[Edited]
Ok, ok, I'll describe what I did in the second picture. Concentrated sulfuric acid on the bottom. Methanol on top. Add a few crystals of solid potassium permanagate, and wait. Give it a swirl if impatient. The reaction is described here and here, though whether the light is due to ozone or manganese (VII) oxide I am not sure. The water bath is there in case something goes wrong.

It's fun to clean up the reaction, too: pouring out the mess causes the methanol to burn all at once, on places like my (fortunately, gloved) finger. What is this safety thing of which you speak?

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Two Stories

Today is my last day of work - I am officially out of a job right now. What better way to spend the remainder of my afternoon than to tell two recent stories from the lab?

Story 1. April 13, 2008. Mid-afternoon.

My project report basically consists of validating a method in the literature that the company is thinking of using. So, before I leave the company, (one of) my supervisor(s) wants me to show her how to actually perform the procedure.

Well. It's an easy procedure. I mean, it's not that hard to use a spectrophotometer after the method has been all set up - just insert the cuvette in the proper slot, close the lid, and push a button.

Of course, first one must fill the cuvette with sample. Usually with a Pasteur pipette. Anybody can do that. But then again...

When I was prepping for the demonstration, guess what? I killed another quartz cuvette. This one also underwent assisted suicide down one meter onto the floor. As it happens, that was the last surviving quartz cuvette in the lab. And it's not like you can just run out to the university chemistry store and buy another one. So my supervisor ended up having to order new ones - they'll take at least a few weeks to get to the worksite. Price tag: $494.90 for a pack of two. Cha-ching! Supervisor: oh well, it's not my money.

So, I ended up doing my demonstration using glass cuvettes. Glass cuvettes, as they absorb in the UV, will guarantee fascinatingly odd spectra in the UV range. They worked fine for practicing, though.

Mid-demonstration, there was a sudden BOOM! The walls shook. Nothing fell from the ceiling (fortunately). That was a blast! (Yes, the company blows up stuff on a regular basis.)

Me: aww, [being in a lab in no windows,] we can't see the "mushroom cloud" from the blast.
Supervisor: maybe not. Let's go.

So we ran to my supervisor's office, where there's a window. Sadly, no cloud is to be seen. Slightly dejected, we returned to the lab and I continued my demonstration.

Anyway, I was filling the cuvette with sample, explaining some of the reasons behind the procedure as I go. Then: clink. One Pasteur pipette down. Bits of glass all over the floor, and on my supervisor. I think I even got glass bits in her hair. Oops. Well, that's what safety glasses are for, right?

Thankfully, my supervisor is a nice sort, and she was lighthearted about it. Then: clink. There goes another Pasteur pipette. *Pause*

At the end of my demonstration, I tried to find all the glass bits, to no avail. Supervisor: don't worry about it, you'll find the glass bits when you step on them.

Um, ok.

---

Story 2. April 15, 2008. Morning.

Every morning, one of my coworkers bring me environmental water samples for pH testing (among other things). Normally, the samples are somewhat basic so that the heavy-metal concentration in the sample stays relatively low. It being my last day, naturally my coworker has to (in another coworker's words) "fuck me over" by bringing a sample that's been spiked with hydrochloric acid.

Well, I know it's 7 a.m. and a little too early to be thinking coherently, but I am not that blind: it is obvious that something is wrong, because the sample bottle lacks a proper label. Being suspicious, I tested a second bottle of the same sample first: it gives a normal(ish) pH. Just in case the small bottle is an ad-hoc sample that nobody's bothered to label (this happens more often than it should), I tested the suspected sample, as well. pH = 2.78. Yep, definitely not a typical water sample.

Upon being told that my coworker is playing a prank on me, I starting thinking (it's my last day, after all). Hmm. I need something that's already in the lab (not the storage room), fairly safe, but unusual. Mercury salts can be colourful, but they are toxic...nah. Potassium permanaganate is nice, but even the tiniest spill of that makes a highly visible purple mess which I'll have to clean up. Potassium dichromate...I don't like anyone dumping chromium (VI) down the drain.

*Looks at the desiccator*.

Hmm. *Adds some sodium thiosulfate to the adulterated sample, a squirt of concentrated hydrochloric acid for good measure, then puts it back in the sample's usual spot*. I wonder what my coworker will think of it when he sees (and smells) all that sulfur when he opens the sample bottle tomorrow morning.

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Back in the Lab...

...for the last time ever. This makes me oddly sad. I think I'll save my "emo-reflective" post for until I get home and have nothing better to do, however.

At least my report is done and submitted (for one week)! Not that my supervisor has even glanced at it yet...this gives me more time to hope that he'll like my report. (It has colourful lines in it...?) Sadly, I can't even buy bribes for him because the city in which I resided in has NO decent chocolate! ! !! !!!

My supervisor also needs to complete the student evaluation form. Darn, I forgot to buy red pens for the entire lab! (Everybody in the lab - except me, naturally - provides input on my evaluation.) On the serious side, I really want to receive some constructive criticism - haven't gotten any in my last work term, except "don't work so hard" (which, as long as one can work safely, is kind of silly). On the lighter side, all my coworkers have made threats about writing weird things on my evaluation, and well, they are certainly weird enough to do it. I want to see those too.

The student evaluation form has some pretty stupid questions though, like those related to "goal setting" and "reflection" (I mean, how is the supervisor supposed to know whether the student has set goals and followed through them? Especially when those goals aren't necessarily strictly work-related?).

Actually, I know of one constructive criticism that is very difficult for me to follow: don't break so much glassware! (Eep.) I think I destroyed several watch glasses, one Erlenmeyer flask, a few beakers of various sizes, one 100 mL volumetric flask, and three quartz cuvettes (the first got cracked overnight while getting dried, probably from falling sideways from an upside-down position; the second had so much colloidal sulfur sticking to it that nothing* in the lab - including aqua regia which doesn't dissolve sulfur anyway - can get the sulfur out; the third slipped and fell to a dramatic death one meter below the counter). Of course, I also killed more Pasteur pipettes than I can count, but at least those are designed with short lifespans in mind. It's a good thing that the ICP torch is plastic, and that I don't usually touch it.

On a tangential vein, despite being April Fool's day, fortunately nothing untoward happened to me personally today. Rather the contrary in fact...I got free breakfast from the company, for no reason. Warm and slightly soggy hash browns, with plenty of grease to reinforce my arteries. Mmm.

My coworkers did pull pranks upon each other, but those were retaliations from earlier pranks. It was kind of fun to watch them, actually. (Tell me where it is! I don't know where it is. Yes you do. No I don't. *repeat, with minor variations*)

*Well. Strictly speaking, the lab has HF, which, if added to some oxidizer, can probably take out the sulfur. But it'll kill the quartz too, and it's not really safe to use HF in the lab because we don't really have the equipment for it.

[Edited]
I forgot to add "ICP nebulizer" (more accurately, that little glass thing connecting the nebulizer to the spray chamber) and "Leco combustion tube" to the list of broken glassware. Maybe this is a sign that I should study theoretical chemistry instead of experimental areas.

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Report Schedule

As usual, I need a schedule to keep me on track in writing my report. To help me stick to the schedule, I am putting it up here.

• March 19 - validation
  
• March 20 - more validation: statistical analyses (Gaussian response models are coming back to haunt me, oh no!)
  
• March 21 - method comparison
• March 22 - references, conclusion, executive summary, appendix
  
• March 23 - editing!
  
• March 24 - final editing, checking for formatting details, etc. (University markers are insanely fussy. They probably do use a caliper to check margin sizes :P.)
  
• March 25 - report due: email to supervisor, say before noon (well, actually, he'll be in the office at 5 am, but I don't get up *that* early).
  

I hope I will make it - this is very, very tight. *Not happy.* My supervisor will be expecting something "impressive" (in his words), too. Boo, hiss.

[Edited]
I just realized that appendices cannot have pictures! This, along with strict word-count/formatting constraints, means that 1/3 of my experiments can't be in my report. Curses!

[Edited again]
Ah, screw it. I'll exceed the word count. Keeping my boss happy takes priority.

[Edited thrice]
Incidentally...what happened to Putnam results? It's mid-March, they should be here soon...(do I want to know?)

[Fourth edit]
I have a nonzero score on the Putnam! A nonzero score! Yay! (Back to work...)

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What Is In This Picture?

The following images might not have pretty colours in them, but they do have rather interesting um, "textures".

Side View:

Top view:

This particular item comes from my lab fridge. You know, the one where sensitive samples are stored...along with food.

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Colourful Plasma in the ICP

As readers probably know, in an ICP-AES machine, the plasma - typically of argon - is normally an eerie sort of white with a greenish tinge (the green is probably due to the viewing port). Unlike the AA, where a randomly coloured flame is by no means unusual and depends on the sample, if the plasma in an ICP is oddly coloured at any time, it usually means something really bad. As in, "the torch is burning" kind of bad.

(I have no idea how the plastic torch normally survives in the ICP, but it does, if properly positioned and aligned. Hmm.)

Well, it was near the end of the workday, and I was running a few samples on the ICP. Usually, I just check that the run started correctly (plasma is ok, autosampler didn't bump into a test tube by accident), then go on my way. I was waiting for the run to finish so I can turn the machine off for the day, and happened to glance at the plasma. Hmm. Looks normal for the most part, but...wait a minute. Was I hallucinating?

The plasma was green-white at the center of the "flame", and dark purple-red-orange at the edges. Pretty cool, actually, and I would probably appreciate it more if I wasn't panicking about the torch. I didn't slam the emergency stop button mainly because the run on the ICP was almost complete, QC results were reasonable, and I was too short on standard solutions (and time) to start another run. But then again, a toasted torch isn't a good thing, either...

After dancing about indecisively for a few seconds, I asked my coworker in the next room to take a look. He did - indeed, he turned off the lights in the room to watch the show.

Surprisingly, the torch (apparently) wasn't actually burning, because the colour is sample-dependent (!): when dilute nitric acid rinse is aspirated into the ICP, the plasma is perfectly normal.

I really wish I can post a picture for this one, but I can't because the (poor-quality) picture is on my cell phone, which has zero connectivity in the province at which my workplace is located. Darn. I'll post the picture when I get back to university (and if I remember). Unless I can get ahold of a nicer picture, anyway.

[Edited]
More recently, during analytical lecture, the professor says that the torch is quartz, not plastic. That, makes much more sense. Now how'd I get the idea that the torch was plastic in the first place? (And, on the other hand, why does the torch get permanently scorched if something bad happened and the ICP arced?)

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*Insert Swear Words Here*

Curses! Glass absorbs in UV. Glass absorbs in UV. Glass absorbs in UV.

Guess what, so does my analyte!

So yes, I do have to use those expensive re-usable quartz cuvettes, and not easy disposable glass ones. I hate washing those things - have to incredibly careful with them, too. Curses!

At least the lab Does actually have quartz cuvettes. Which is much more than I can say for every other lab with a UV-vis that I have been in.

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Fume Hood Story, Sequel

One might recall that the fume hood at my workplace died recently. Well, it's fixed now, which is great, but apparently my luck is just as great as it was when the fume hood died.

Ok. The fume hood died the day before yesterday late in the afternoon. I got a bit of work done.

I was due to leave the worksite yesterday, but weather delays caused the flight to be cancelled. Meanwhile, I have all this time that I could potentially use for my experiments, but I can't do anything because the fume hood is dead all day. The worst? best? thing is, my compound did end up crystallizing beautifully into yellow needles at the bottom of my flask, but I can't filter sans fume hood. No clean product means no data collection. In the end I had to seal up everything using various ad hoc methods (it involved disposable aluminium weighing pans, lots of tape, and paper towels), sadly gazing at the pretty needles while being unable to work with them.

Naturally, today the fume hood got fixed right before I had to fly offsite.

I hope my compound doesn't decompose in my absence, but with my luck, no doubt it will. In two weeks time, we shall see...

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Things Can Always Get Worse. And They Will, Too!

First, thanks to ψ*ψ for her excellent advice on recrystallization! It is very helpful. Now if only the analytical (literally, "wet") lab in which I work has all the requisite equipment...(there's no heating mantle, no RBF, no condenser or distillation column, no absolute ethanol, etc.) Except, of course, things can always get worse.

Background story:
The lab has three fume hoods, one of which is intended for perchlorates. In theory.

In actuality, the contractors who ordered and installed the fume hoods apparently went with the cheapest, flimsiest ones available (the opposite of what the lab director wanted). Thus two of the three fume hoods died within a year of use: the dead hoods literally look and work worse than those first-year fume hoods that's been abused for decades. Only the perchlorate fume hood survived (kind of), and continues to be used to this day. Oh, and the perchlorate hood can't be used for perchlorates because the special safety features don't work properly, so I can use organics in it without causing explosions.

Today, I was trying to get some of what I think is my compound X from the filtrate by very gently heating the filtrate so that the compound just starts to precipitate. (Then I can add enough solvent to dissolve the compound back, cool, etc.) Now, compound X is organic, and has sulfur in it, with all the attendant aromas organic sulfur compounds are justly famous for. Not to mention the toxic potential decomposition products. Naturally, I do the heating in the fume hood, with the sash waaaaaay down.

Somehow, the smell of my compound eventually ended up all over the lab. It took me awhile to notice, so it was some time before I stopped heating. My co-worker wasn't too surprised ("The fume hood sucks. Actually, the problem is that it doesn't suck."). My supervisor, however, well...she walked into the lab at the end of the day, gagged, immediately turned around, slammed herself dramatically against the door with palms and face on the window, and rapidly exited the lab. Then she made a phone call to the safety department.

So now the only kind-of-working fume hood is toast, and nobody is allowed to use it. And I have no data yet! What is coming next? Meteors crashing down onto the lab?

The only good thing is that I figured out the reason for spiky UV-vis spectra. In retrospect, it was a dumb reason: my solutions were too concentrated, so absorbance shot through the roof, resulting in awfully spiky spectra in random places. Dilute the solutions down to the ppm range, and the spectra smooth out beautifully. But now I have another problem: the spectra of all the various species in the mess have peaks in all the same places, but the peak heights are different. This might be because of concentration differences, cross-contamination, or the different substances indeed have similar spectra. Must straighten this out before I leave the worksite tomorrow...it'll be a horrible two weeks off if I leave without any meaningful data to analyse at home. Of course, with the fume hood shot, I'll probably end up with no data, regardless.

Gotta love my workplace.

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Spiky Peaks and Underestimating Simple Tasks

Does anyone know what is wrong if a relatively pure substance gives extremely spiky peaks in a UV-vis spectrum?

(Long) Backstory:
At work, I am trying to develop a method for analyzing a particular process chemical. It is the sodium salt of a weak organic acid; I will call it "X" for now. Unfortunately, compound X decomposes rather readily (it's somewhat light, heat, and air sensitive; it is also hygroscopic). I don't have the reagents or the equipment to synthesize the stuff, so I need to purify the technical grade compound.

According to the literature, the compound can be "readily recrystallized from absolute ethanol or acetone" to give >99% purity. Nobody seems to have more elaborate instructions than that. Well, recrystallizations are easy, right? Heat solvent, add just enough solvent to dissolve sample, let cool to precipitate pure crystals, filter, wash. Even someone organically-illiterate like me can do that. So I did.

The first time I tried heating acetone, it superheated and popped right out of the beaker. It was kind of interesting to watch, actually...one minute there's acetone in a beaker, the next minute there isn't. What happens when using high-purity acetone without boiling stones, I guess (no boiling stones in the lab.)

Anyway, eventually I got the acetone heated up, and dumped some onto my technical grade compound. The technical grade stuff is pale-ish yellow. From memory of an MSDS somewhere, the pure stuff is also pale yellow. But when I poured the acetone in, the mixture was a deep orange slurry, heavy with orange precipitate. Not really a solution at all. Adding more acetone does not help dissolve the orange precipitate. Nor does heating the slurry.

My thoughts:

• Crap, I decomposed my compound! But acetone boils at a relatively low temperature (~56^oC if I recall correctly). And if I did decompose the compound, what is the product?
• Or maybe the orange stuff is a mix of impurities. But that's alot of impurities.

Well, I figured I'll filter the orange precipitate from the hot solution, and see if anything precipitates from the filtrate. Then I can run a UV-vis spectrum on the orange residue, any precipitate from the filtrate, and the technical grade compound, to see which is which. That's nice...in theory. The procedure reminded me just how tedious gravity filtration is. The precipitate clogged up the filter paper very badly, and I have a feeling the acetone evaporation rate is potentially faster than the filtration rate. That's just sad. The only good thing is that the filtrate is yellow. That's a good sign (I hope), and at this stage I need all the good signs I can get.

Odder yet, there are multiple "species" that ended up on the filter paper. The majority is the orange precipitate. However, there's yellow stuff near the top of the filter paper, and some fine white powdery stuff as well. Hmm.

Also, nothing crystallized out of the filtrate. I ended up boiling some filtrate to start the crystallization process. Alas, acetone being acetone, most of the solvent evaporated by the time the boiled filtrate has cooled down to room temperature, leaving a paste-like solid mass. Probably not pure.

So, in the end, I dissolved a bit of everything (separately) in some distilled water, and tried to run a UV-vis spectrum of the samples. But the UV-vis was stubborn and gave oddly spiky peaks, not one of which appeared at where the maximum absorbance is supposed to be. I mean, I'll accept spiky peaks for my botched recrystallization samples, but another coworker managed to get a very nice peak for the technical grade compound which isn't happening now. Unfortunately, the coworker is on holiday at the moment and thus unavailable. The help file wasn't helpful.

In the end, I was getting kicked out of the lab (it's the end of the work day), so I covered everything with parafilm, ineffectually tried to keep them in the dark with paper towels, and left it at that.

What to do, what to do? I can't progress on this project without pure analyte! (Among other things...I can't calibrate the machine with technical grade compound.)

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First Impressions of a Subzero Eastern Province

Yesterday, I flew out from my parents' place to the place where I will be spending my next four months, when not working.

Location: remote small town in an "Eastern province". English-speaking (fortunately). Proud location of the smallest airport I have ever seen. Unfortunately, I didn't get a chance to take a picture.

Surprisingly, it is not as cold as I thought it'd be. Kind of like the coldest sunny day* I have ever had at my university town - which is cold but not exactly winter Arctic conditions. Of course, one day is a statistically insignificant sample size. We shall see whether I freeze in this town or not...

As is common in a remote town, there are very few things to see and/or do, and very few shops. So-called fresh food is extremely expensive around here - even more so than those grocery stores near university campuses. So here I will be living on the classical substance known as instant noodles. Possibly some other stuff to prevent scurvy. Probably little to no coffee, since that's expensive, too. (Noo, need caffeine fix!)

My renting arrangement is basically a room in the landlady's home, with the opportunity to share her kitchen, laundry (etc) as required. This place is a mess. Bad as first-year residence, without the excuse of housing first-year students. But at least it has high-speed Internet. More to the point, it also has:


(Sorry for the blurriness, I know my picture-taking skills sucks. The landlady also has dogs, and those are cute too, but...)

So it's not so bad, after all. Except now I can study physisorption of cat hair on my sweater.

Oh, and since work will begin soon, I might go on a hiatus due to lack of Internet access on the worksite. Can't exactly blog on the company's Internet you know.

*Oddly enough, during the winter in Canada, sunny days are often colder than snowy days (subjectively speaking), especially when windy.

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