| Current mood: |  cranky |
| Current music: | Holst - The Planets, “Uranus – The magician” |
999 – The longest working day recorded
On my way home in bus 95, after a long day at work. Today’s date 090909, 9th Sep 2009 can be slanged to 久久久, meaning “long long long”. Indeed today marks a record setting day for the longest working day for me. Arrived in lab at 0645h and left at 2315h, total 17.5h of working hours, as compared to the usual average 14h (0900 – 2300h).
My intention was to perform 3 sets of trial reactions, so that I can work it up in time to prepare the product samples for PXRD. Rationale for the early hours was that I have TA teaching duty from 1000 – 1700h, so practically the whole day is gone for me. Also this week’s PXRD booking is full as the only free slots left were for today afternoon and evening. The plan was to start the 1h reactions at 0700h, followed by about 1h of workup; so should be done by 0900h to prepare the PXRD thin film samples. Then again, as usual things don’t go on as planned… Though I entered lab at 0700h, I spent 30 min to setup the heating mantles and temperature probes in the common fumehoods. Cos tmd, the last user(s) never cleared up the area after use… Haiz, missed those days when I got my own fumehood where I can easily setup everything the night before and just start the reaction proper the next day. So the first reaction was started at 0745h instead and that snowballed the timings. So in the end only managed to complete the workup by 0955h but couldn’t complete the sample preparation. Timings aside… somehow some the unexpected decided to pay a visit again…
Tmd, some nincompoop is smoking behind me at the bus stop and knn the wind direction not in my favour… Thankfully bus 970 arrived in time when I was about to curse and swear…
Anyway back on work… I’m currently working on a new system, temporarily moved away from Bi2S3 for now. New targets suggested by boss are Sb2S3, SnS and SnS2. So I need to synthesize their respective thiobenzoate precursors first. The precursor synthesis should be rather straight forward as they are reported long ago in the literature… but haiz. Sb(SCOPh)3 seems okay as the product appearance looked appropriate, with reasonable yield. However things are not so rosy for the Sn(II) and Sn(IV) precursors… Aragh…
Ccb… How come the fare is 41 cents (after 50 cents rebate)?! It should be 19 cents!! Knn & #@$#%^&!! The stoopid auto fare stage miscalculated my fare again… Not the first time liao… Bloody hell, cheat my 22 cents!!! Diu… Nevermind, shall go for my usual night snack…
Anyway, I’m not certain how come the Sn(II) system is so weird… Sn(SCOPh)2 should be cream coloured but it gradually turns greyish brown over time. Funny thing was that while the colour somehow changed back to cream as I was doing washings with MeOH but again turned brown… The thing is not the entire crop turned brown but some remained cream colour. In short a mixture. Tmd. I prepared SnTeO3 previously and it also gradually turned dark brown over time but further thermal decomposition yielded SnTe cleanly. Whatever it is, I subjected the “Sn(SCOPh)2” precursor under thermal decomposition at 150 deg C, with TOPO and ddT… and I got mixture of dark brown and yellow ppt… Sianz…
The Sn(IV) system wasn’t so bad… but still there are some issues with the precursor. Initially the bright yellow solids were formed which turned darker yellow over time. To up the ante, the filtrate collected was clear bright yellow and upon standing, the entire solution turned cloudy. Obviously incomplete reaction… Anyway, still proceeded to heat the mixture up to drive the reaction to completion but still the solution phase still remained yellow, albeit increase in amount of dark yellow solids formed. Similarly for the Sn(II) system, I kept the filtrate and light yellow solids gradually formed on standing. Thermal decomposition of “Sn(SCOPh)4” yielded dark yellow solids. What is going on…
For once I’m seeing coloured products, after dealing with mainly black products. (Most metal selenides and tellurides are black.) Such that I was initially wondering “no reaction”? Cos the product didn’t turn black? Checking the appearances, SnS and SnS2 are supposed to be dark brown and gold-yellow solids… Hmm… The Sb(III) seems okay. Precursor looks correct. Thermal decomposition product, also looks correct, dark brown, almost black solids but not very well dispersed in PhMe. Only need to run PXRD to check if it is purely Sb2S3. Problem is no slot available… Sianz, how to do research with so many limitations, especially lack of instruments. Haiz.
My 3 reaction mixtures...
[L to R]
White: JR5901 - Sb(SCOPh)3
Brown: JR6001 - Sn(SCOPh)2
Yellow: JR6101 - Sn(SCOPh)4
Anyway, just an update on my work done last week, for preparing t-Se nanorods from amorphous red a-Se. Apparently, the a-Se is thermal sensitive and I cannot do normal high speed centrifugation as the heat generated would convert to the grey t-Se. I got around that by putting the entire centrifuge machine INSIDE the freezer, aka “improvised refrigerated centrifugation”. Somehow that worked but separation ain’t that good. Difficult to let the very fine red a-Se solids settle, as I cannot do prolonged centrifugation. Anyway, subjected a few partially isolated red a-Se for nanorod assembly and low-res SEM images look promising, though monodispersity isn’t too good yet. Still I managed to get rods, which meant that the method worked but need fine tuning.
The choice now is whether to continue to use red a-Se, which ain’t too stable. The entire red suspension in the conical flask was kept in the fridge and the base layer turned grey overnight, which means not recommended for long time storage. Either that I have to really use the toxic H2SeO3 or SeO2, which I been avoiding…
Suddenly it seems as if I have opened up a few new fronts. Hopefully at least one would lead to the Promised Land as I had been hitting stone walls ever since I started. So now the tactic is to divide and conquer.
Just now, stoopid Lappy refused to shut down or hibernate… Even Lappy is trying to be funny… Grr… Anyway, this reminds me to update my “hate-list”, continued from the previous list…
(5) Stoopid and slow Kompooters
I can get rather impatient with machines, especially computers. I can flare up if the stoopid kompooter actually hangs in front of me. In short, “I hate kompooters”.
Remedy: Transform the machine into a living thing which can feel pain, so that I can inflict mortal pain to it… In the meantime, a knock or punch at the machine does help to diffuse the fury…
(6) Mosquitoes
I have no issues if these pests bite and suck blood but doesn’t make me itch. It is the itch that really drives me to hate mosquitoes to the core. Mosquitoes should be eradicated, extinct, wiped out fro our planet. Really no one should miss them… even lizards can turn to other insects for food. There’s one pesky mosquito still lingering in my Ops Room and until I personally kill it, that pest would stop disturbing me, especially in the wee hours… Defences up, mosquito mat, light, repellent are on standby.
Remedy: Anti mosquito repellent. Once I caught the mosquito, I’ll decapitate it, before dismembering it… the wings, legs, everything. Then I’ll mesh it up into a pulp, with added extreme hatred and vengeance… It deserved that…
Time for bed… eyes are shutting down. Later Lappy better be able to shut down… or else.
Music of the day will be Holst’s “Uranus – The magician” from “The Planets”. I really need to perform some magic for my work…
And that as I say, is that. En Garde!
10 0102h
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