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"It's all gone wrong for me"1 - no, not the hungover cry of the ethanol-loving undergraduate, but the familiar wail of another lab cock up.
Mine, sometimes; yours, occasionally; and historic, from time to time.
 
1 Bill Bailey, 2001

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I have just returned from an escapade on the Greenpeace website.

A link came up on my feed and I had a bit of an explore of their Detox Campaign. I hadn't realised this had been going on since 2011 and it definitely included some new facts for me: that clothes are not only made using hazardous chemicals, the waste of which is dumped into drinking water around the world, but that many of these hazardous substances remain in our clothes in small quantities and are admitted to the waterways every time we wash them.

Various tests on clothing found phthalates, carcinogenic amines from azo dyes, and nonylphenol ethoxylates (NPEs), which break down to toxic, hormone-disrupting materials. Worse: in every brand tested, trace levels of NPEs were found.

This particularly interests me because of what my research is about: cleaning up a carcinogen found in waste water, one source of which is the dye industry. It seems like a lot of toxic materials come in pretty colours and have infiltrated our world... Mine is chromium VI, so a bright orange colour. It's actually quite good to see that there are other (non-lab-based) approaches to these problems in the world and that stuff is happening. Better still, it makes my research seem real-world and relevant - and exciting.

Right, back to the grind.
Posted by Rowena Fletcher-Wood on Nov 14, 2013 9:24 AM GMT

Do you know what happens if you put metal in an x-ray diffractometer? If the beam strikes the metal the whole machine could overheat. Thousands of pounds worth of equipment fizzled out in a shot.

But it still seemed worth the risk.

I was in Oxford, downstairs in the Chemical Research Laboratory, and Amber helped me carefully mount my engagement ring and align the beam to strike the diamond. Her first question was whether I thought my fiancé might have bought me a fake diamond and was checking up on him, and she wasn't the first person to ask me that. But in fact the opposite was true. If I hadn't thought the diamonds were real, I would have had no motivation to see their diffraction pattern. I am a doer: I can't just exist, I have to act, so when I was given my beautiful engagement ring, I couldn't just leave it alone on my finger. I had to do something with it: I had to explore it.

We switched on the diffractometer... and waited... The beam struck the stone, the x-rays diffracted, and very slowly this beautiful, simple, but slightly frayed-looking diffraction pattern began to form.


http://static.smallworldlabs.com/myrsc/user_content/photos/000/029/29634/21d04e1005c6e20af815c987febbefe2-original-img_0096.jpg
[Photo courtesy of Amber Thompson, Oxford]

Posted by Rowena Fletcher-Wood on Oct 26, 2013 1:33 PM BST

Today I have been making fused beads. I have made a lot of fused beads lately and I'm reminded how blaise we have become working at extremely high temperatures. Nowadays, the 1050 degrees centigrade furnace we used to melt the flux into glass is unexciting and we feel no sense of fear or trepidation using it, even when reinforced safety rules are in place, like making fused beads a two-person operation.

We just go 1050ºC? Meh, that's not very much. The blow torch gets hotter than that when you shape glassware. Sometimes we run reactions at 1200ºC (but not very often).

They say once burnt twice shy, but in fact the opposite occurs. After you have burnt yourself a dozen or so times you learn that you can live with the consequences of making a mistake... and stop fretting over it. And that means that even when you are swirling molten glass around you never really concern yourself with the possibility of spilling it and that kind of burn being much, much worse.

Don't worry... that's not where I'm going with this.

We were reminded of how insignificant 1050ºC has become when we needed to do a different reaction at 1500ºC. A colleague of mine put a crucible very like our fused bead crucible into a furnace and left it to ramp up to 1500ºC. Once it was up, we went to retrieve it. Normally when you're making fused beads you have one person open the door and the other takes out the crucible with a very long pair of tongs. A heatproof brick sits at the side of the furnace to rest the crucible on whilst it cools. We set up our brick, got our gloves and tongs, and went up to the lab. We opened the door of the furnace.

And it was literally like looking into the sun.

Whilst the 1050ºC furnace emits a reddish glow, a 1500ºC furnace emits a powerful white light. We hesitated for a moment... then closed the furnace door. Suddenly we were faced with an unexpected situation – 1500ºC is actually very hot. It was hotter than the range of “hot” we were normally used to dealing with, and we were going to have to introduce extra safety precautions. Using the blow torch there are some tinted goggles, and I also knew there were some face shields kept in the same lab, the kind you would use for welding. So we fetched two face shields, put them on and went back to the furnace.

Opening the door wearing tinted face shields, the inside of the furnace didn't look like the sun any more. It looked reddish and glowing like the 1050ºC furnace. We got the crucible out, shut the door, turned off the furnace and removed our face masks. The platinum crucible was glowing red around its base, a clear indication of its ertwhile environment. Just in case we were beginning to forget.

Posted by Rowena Fletcher-Wood on Oct 16, 2013 9:51 AM BST

I once wrote a murder mystery game where the killer committed the act by filling a sealed room with bromine gas. I'm not entirely sure it would work, but once when I was in school the physics class removed itself to a chemistry lab to watch a demonstration on gas mechanics, and we used bromine.

“I have to warn you now,” the teacher said, “that bromine is toxic, although we have a very small quantity here, it can still be harmful, especially to the boys in the room, as it can cause male infertility.” A few teenaged boys shuffled uncomfortably. “So,” the teacher continued, “it is my responsibility to tell you that in case of accident, we must all evacuate the room, okay?”

We nodded, reassured that some safety measure was in place, and that it wasn't anything too drastic.

He then went on to outline the experiment. First, he would expose the bromine gas to an “empty” flask and we would time how long it took to diffuse through and look roughly mixed. We were using bromine, he explained, in spite of its hazards, because it was brown, and thus we could see it. This seemed sensible. In our second experiment, we would expose the bromine to a vacuum, whereupon we would see how fast a gas really travels, when it is unencumbered by collisions with other gas molecules!

We completed the first experiment. Obviously it was the less thrilling of the two, and we looked forward to the second, where the gas would shoot through the flask with the promised velocity and we could ooh and ahh appreciably before going back to the physics classroom and doing the maths.

He prepared the second experiment. He opened the valve between the bromine chamber and the vacuum...



“Ah,” he said.

Then, “So now, we shall all vacate the laboratory.”

And there was as sudden mad scramble as all the boys made for the door like bullets.

Posted by Rowena Fletcher-Wood on Oct 2, 2013 3:31 PM BST

Today, I have been inspired to contemplate the concept of science by page 65-66 of my Collins Classics version of 'The Moonstone'.

“Gentlefolks in general have a very awkward rock ahead in life – the rock of their own idleness. Their lives being, for the most part, passed in looking about them for something to do, it is curious to see – especially when their tastes are of what is called the intellectual sort – how often they drift blindfold into some nasty pursuit.”

And he goes on to list some of them.

“[They] catch newts, and beetles, and spiders, and frogs, and come home and stick pins through the miserable wretches, or cut them up, without a pang of remorse, into little pieces....Sometimes, again, you see them occupied for hours together in spoiling a pretty flower with pointed instruments, out of a stupid curiosity to know what the flower is made of. Is its colour any prettier, or its scent any sweeter, when you do know?”

I always love it when I am confronted by a character who really and truly supports this idea, because it fascinates me. Why? Because outlines The Other View. What do I mean by that? I mean, I suppose, the romanticist view rather than the enlightenment view. The view of the church who told Van Helmont he was committing crimes against nature. The let it alone, appreciate it and don't fiddle with it view. The view that you should honour and respect rather than understand and realise. This is emphatically not my view. In this view, you do not ask questions unless you need the answers, which means you never come across unexpected information.

I have noticed two kinds of scientific research in my time: the one asks, how do we do this? And seeks a way of achieving the goal. The other (my preferred kind) asks, what is this thing and how can we use it? The latter is much easier to ask and to follow than the former, it is more productive and moves faster, although it has a funny habit of missing the mark when it comes to priority problems.

And it makes me wonder whether the latter could exist, and if it didn't, or it was much repressed, how that would have retarded science, were there not people like me with the enlightenment view.

That is not to condemn the romanticist view entirely; the romanticists may never have developed penicillin, yet probably would have found nuclear weapons. But they do ask some valid questions. To what extent is the pursuit of science a good idea? Is it not putting the future above the present? It also carries the warnings that we are just beginning to heed for our planet about the consequences of meddling in stuff we don't understand. Put simply, the romanticists worried about the health of our planet before we realised we were harming it.

And there is another question: to what extent would science not have developed were it not for idleness?

Agatha Christie addresses this too in her 'The Moving Finger', but attacked from a different point of view: idolising idleness.

“'Sir Edward Grey,' I said, 'afterwards our foreign minister, was sent down from Oxford for incorrigible idleness. The Duke of Wellington, I have heard, was both dull and inattentive at his books. And has it ever occurred to you, Miss Griffith, that you probably would not be able to take a good express train to London if little Georgie Stephenson had been out with his youth movement instead of lolling about, bored, in his mother's kitchen until the curious behaviour of the kettle lid attracted the attention of his idle mind?'

“Aimee merely snorted.

“'It is a theory of mine,' I said, warming to my theme, 'that we owe most of our great inventions and most of the achievements of genius to idleness - either enforced or voluntary. The human mind prefers to be spoonfed with the thoughts of others, but deprived of such nourishment it will, reluctantly, begin to think for itself - and such thinking, remember, is original thinking and may have valuable results.'”

Well, I am not an advocate of idleness. But it is a good point that to some degree curiosity spouts from idleness. But I do think it is curiosity, not idleness, for you can have a wandering mind very easily when involved in physical work: you may not have the time to carry out experiments, but you can still pursue some science. On the side. Because science is on the side of life, isn't it? We couldn't just explore; we need to do functional things as Wilkie Collins' character observes. Science is not functional most of the time. In fact, when it comes down to it, science has, to some degree, to not often succeed to be pursued. If success were guaranteed, and acquisition of knowledge certain, none of these experiments would have any greater appeal than the opening of a book. It would be learning, rather than playing hide and seek with the world.

Posted by Rowena Fletcher-Wood on Sep 22, 2013 9:17 PM BST

I am good at quite a lot of things, but there is an even larger number of things I am really not any good at at all. For many years, it has been a source of disappointment to me that I am unable to guess the temperature of boiling sugar just by looking at it.

A couple of years ago, I gave up, and got a sugar thermometer.

It was an act of desperation. I had been trying for years to learn the “coats a back of a spoon” consistency with the optimistic expectation that if I just messed up enough times, I would eventually get there. Maybe there just weren't enough attempts. More likely, I needed not to actually see it go right a few times in order to learn. And this hadn't happened yet.

Still, I had my adventures. There was the black toffee which you could hit on a bench and not break, and the stream of suspiciously burnt-smelling sludges which turned to rock instantly on contact with the tongue and/or resulted in the throwing away of several pieces of kitchenware. On one tentative venture, I successfully synthesised glue-your-mouth-shut baklawa (best used on enemies and the very talkative). I got used to lining tins with baking paper to pour my toffees into on the inevitable off chance that it would solidify and need to be chipped off systematically on a night I was procrastinating my tutorial work, or treated repeatedly with strong sodium hydroxide solutions.

Stubbornness, it seems, is not necessarily a winning formula, especially combined with lack of consistency. It never occurred to me to time how long the sugar had been boiling, or if it did, I forgot the number or lost where I'd written it down. I rarely used the same sugars, the same recipes, or even the same kitchens. I was an undergraduate, I moved around, I tried new ideas. And I had made Yorkshire puddings rise, damnit – I should be able to make toffee.

Even after I got the sugar thermometer, it turns out a lot of recipes just don't give numbers.

I had already established that my by-eye judgement was less than useless, so I wasn't giving up. I eventually discovered a winning recipe (ahem, it's a bit long-winded and I skipped a lot of it – it does include numbers, I promise) and one that appeals to the scientist in me. It's worked every time. And, with the wonderful magic of a single scientific instrument, I have created not only cinder toffee, but chewy toffee, honey toffee, hard bonfire toffee made from dark muscovado sugar and caramel toffees for filling chocolates with.

We even gave out some for Christmas, carefully packaged in pretty jars, whereupon it softened slightly under the seasonal glow and cemented together into one giant multi-coloured toffee globule. Still, it tasted right.

Posted by Rowena Fletcher-Wood on Sep 10, 2013 4:35 PM BST

“I am very nervous,” began D. Bessas on Monday, before the International Conference for the Applications of the Mössbauer Effect 2013, Opatija, “because I stand before Mössbauer spectrometers” [scary, methinks, in and of itself] “and I will not talk about Mössbauer and I will not talk about iron.”

“...Actually,” he went on to clarify a little later on, “there is a connection between Nuclear Inelastic Scattering and Mössbauer spectroscopy, otherwise there would be no reason for me to be here.”

But for very subject specific conferences like this, that is always the case. I spoke about chemistry and the application of Mössbauer to assist environmental research; across the week, others have spoken about geology, quantum physics and biological processes. And in all of these research threads, the common application of Mössbauer spectroscopy or similar effects has persisted. Our elucidations have ranged from the poignant to the absurd;

“The high spin to low spin transition can profoundly affect the structural, magnetic and electronic properties of this material and thereby influence our understanding of the earth's core,” says I.S. Lyubutin: understanding very small local changes in materials can have big consequences to our world view. He refers to his work as the “spin chicken and egg problem”, by the way.

What is Mössbauer spectroscopy?

Well, for the unenlightened, Mössbauer spectroscopy is an analytical technique which works by the application of gamma rays to probe nuclear energy levels, which process gives information about the local environment around a Mössbauer-active centre (usually iron. I work with iron. Iron is good). I'm a chemist, so I use it to learn about my products. Or, as F. Berry said, “Chemists make things. Chemists make new things. And that's the central principle to the practice of chemistry.” For others, Mössbauer spectroscopy is useful for solving Einstein's clock problem (trying to discover whether there's a limit on acceleration in nature), or they are piloting synchrotron Mössbauer spectroscopy.

Frank Berry's comment makes another “observation” however: we are all scientists, but we are not all the same kinds of scientists. “I think this is the fight between chemists and physicists, for whatever reason,” says W. R. Scheidt. He's being flippant, but he sounds a little wary all the same. “Yes [this work] is very complex physics,” H. P. Gunnlaugsson acknowledges to his very varied audience. And jokes, “I will now spend the next two hours explaining.” Whilst I'm sure we're all very relieved he didn't, “we all know that Mössbauer spectroscopy is very useful,” even though we value it in different ways, so there is an element of “preaching to the choir,” as D.H. Ryan puts it, and we do have some similar approaches.

 “Now, if we had a neutron audience here, most people would start to panic when they saw this slide,” says J. M. Cadogan as he expounds his neutron research on gadolinium compounds. We stare blankly. But we are appreciative of the subterfuge of J. Lindén, who complains, “Now, if you present hyperfine parameters to non-Mössbauer spectroscopists, they will either be bored or angry. So we have to do something clever.” And nobody so much as blinks when he personifies functions: “whenever there's a Hamiltonian hanging around that nature can use, it will use it.”

Even more crucially, it's important to remember that this is a mobile community; because the mutual field is an analytical technique, rather, say, than a series of related chemical compounds, it is more likely that several members will dip in and out of Mössbauer spectroscopy during their research careers. Mössbauer himself had moved out of the field by the time he died in 2011. We are like antimony, as F. Berry describes it in an answer to a question about synthesis methods: “There are some materials which we use that are very mobile... You try heating antimony in a lab in an open crucible and there's antimony up the walls – it just goes everywhere!” And so do Mössbauer spectroscopists. We go all over research.

[And last night, all over the dance floor]

And after eighty talks and two hundred and twenty-one posters, I'm pretty tired of Mössbauer spectroscopy. The energy this week has been incredible, especially when it came to controversial research. “Lively discussion is very important for this conference, but now we must continue,” insists chair G. Wortmann after a heated debate on the interpretation of Mössbauer spectra of FeSe and related superconducting compounds. Men were actually getting out of their seats to shout across the room, forming, for me, a low rumble of accented English words, bubbling over each other. Over two talks on this subject, we ran 20 minutes late: roughly half the combined lengths of the talks. The debate was carried into coffee time, highlighting the passion and enthusiasm of so many scientists to percolate the “right” view through the research community as theories evolve and camps of opinion develop.

Which is, of course, how science works: it is an idea or theory pool, where its dedicated practitioners devote themselves to substantiating their perspective. But we have to try to keep an open mind, and it's too easy to make assumptions; E. Bill warns us on the dangers of research theory: “Is it valid to talk about iron oxidation states...?” he asks. And adds ominously, “We are deep in metal organic chemistry.” And none of us, I think, want to go there.

“Maybe we should start with a coffee break,” suggests chair K. Schlage, whilst J. M. Cadogan struggles with “the joys of Mac versus Windows.”

But when it comes to mistakes, misappropriated theories and practices, none are so good an example as D. H. Ryan's talk on Moments, fields and magnetismin Eu-based EuTM2X2 compounds, which he subtitled “A cautionary tale.”

He starts by talking about gathering his data at a neutron source, and how they responded to nuclear disaster. “Because this was the fifties and they liked nuclear power back then, they rebuilt it and thought if they put a couple of extra things in place, we can put in a bigger core, rather than scrapping it and walking away from nuclear power for the rest of their lives,” he says, and even though it is integral to his research, there is a certain exasperation in his tone as he reflects on the basis of this decision.

He also has comments on the interface between teaching and research: “If a student gets an answer which is out by an order of magnitude, we typically say that's wrong. So we should really say this is wrong.” “This”, by the way, is the basis of his research, from which he concludes firmly, “It doesn't work for iron; it never really has... It doesn't work for tin... And it doesn't work for europium. Perhaps we should just stop claiming that the hyperfine field tells us what the moment is.”

[this post may also be found on my own blog]

Posted by Rowena Fletcher-Wood on Sep 6, 2013 9:11 AM BST

The practice of science as we know it developed incrementally, mostly from one natural philosopher building on the work of a predecessor and disproving their conclusions with further experiments (you may recognise this same drive in researchers today). And it paid dividends. Not only did the extent of scientific knowledge increase, but so did the rigour of experiments.

Before anyone really understood which materials were fundamental and how things could turn from one substance to another, there was alchemy. Alchemy, whilst meaning “the chemistry” is about as unlike chemistry today as it can be: chemistry starts from the elements of the periodic table and the basis of conservation of mass; the principle of alchemy is that materials are transmutable (which we can't really achieve without nuclear decay). And so hard water, when boiled, left behind limescale, so rock must be made from water. And until people started tinkering around with experiments, it seemed a pretty solid (ahem) theory.

Alchemist Van Helmont went further. He determined that plants were also made of pure water (although after he was arrested in 1634 for “violating God's law” by studying nature, he declined to publish anything whilst alive; strange choice, that). His conclusion is wrong. We know that carbon dioxide plays a part, that plants generate their own food via photosynthesis, but Van Helmont didn't know this, and whilst he was wrong, he was also very thorough.

In a five year experiment, Van Helmont carefully watered a 5lb willow tree stood in a pot containing 200lb of dried soil, before finally reweighing both tree and soil. The soil weight was unchanged, the willow had gained 164lb.

QED. Trees are made of water.

At least, willow trees.

Today, Van Helmont has been dubbed a chemistry pioneer and a founder of pneumatic chemistry. Even though he was wrong.

But the idea of gases evolved, and became of importance to fuel later investigations into the transmutability of water. In 1770, Lavoisier undertook an even more rigorous experiment, weighing a sealed glass flask of distilled water and boiling it off. Through this experiment he was able to show that the evolved “earth” came from the soft glass of the flask, not the water nor air.

Water was, in fact, neither soil nor tree. It was water.

Posted by Rowena Fletcher-Wood on Sep 2, 2013 7:53 AM BST

I've been involved with lots of outreach projects; last week it was Year 12 Experience Days. I haven't heard of them before... so of course I got involved. The principle (in chemistry, anyway) was to put 20 year 12 students in a lab and blow things up. Not the students.

It was an experience for me too, for whilst all I had to do was help with some ratio calculations and chat to keen students about degree options, there were a few bangs. And whooshes. There were also a few explosions of water from very high pressure taps (we had warned them about the taps, but they hadn't quite realised the extent of the danger), but it was the hydrogen bombs which took centre stage ...they, after all, were deliberate.

The Experience was actually a fairly innovative lab designed to teach the value of precision and accuracy in order to get exciting results like very loud bangs and fireworks. This was coupled with a fairly appalling out of date handout, which every single student abandoned in the laboratory.

They started off by choosing a hydrogen:air ratio and measuring out a test tube to be filled with that amount of hydrogen, then they stood in a line lowest:highest hydrogen loading whilst we went past lighting the tubes to give that distinctive squeaky pop. As the hydrogen content increased, the squeaks got quieter, and we explained how the extra fuel couldn't burn without the right amount of oxygen.

After that we got bigger (plastic) bottles and did hydrogen:oxygen ratios; we cleared a long line in the laboratory, mounted them on a crate and set light to the rockets, which projected themselves across the room. We had to wear ear plugs (I always wonder if they're luminous yellow to make them easier to find if they get lost in your ear). The rocket which went the furthest was the only one that had been named.

And after that, we got an even bigger bottle of methanol and oxygen fuel, called a Whoosh Bottle. This experiment is best done in a darkened room. One (slightly nervous) volunteer lit the fuel and we were treated to an array of blue flames which rose up and hit the ceiling with that characteristic whoosh.

It's nice to know that fuel cells are on the A level syllabus, but I doubt they do this one in schools.

Posted by Rowena Fletcher-Wood on Aug 29, 2013 9:04 AM BST

The first flames of my passion for chemistry were ignited in year 10 when I had a very good chemistry teacher. My best friend and I would work together to get finished as quickly as possible and then follow her round the classroom pestering for more work. ...Yes, we were actually that geeky.

I immediately decided that I wanted to do chemistry or something chemistry related at university ...so much for my family who assumed I would do English. It's not that English isn't fun, or you can't get jobs with an English degree, but chemistry not only explains the hows and the whys, but it does it with bangs, flames and vibrant colours and odours.

The particular chemistry teacher I mention was especially good at demonstrating the ease with which practicals that seem to start off well can quickly go up in flames. There were a few incidents.

One I remember was the electrolysis of brine, which she happily told us how to set up, then left us to it. Ten minutes later I asked her how long we should run it, as I was starting to feel dizzy from all the chlorine...

Her lackadaisical approach only made us all the more keen to experiment: I remember one incident when she urged us to cautiously add just a touch of iodine to a solution, just the tip of a spatula. Naturally, one of the boys on the bench next to me had to see what would happen if he threw a whole load in - BANG, and iodine on the ceiling. Which actually remained there the whole time I was at school.

One of the highlights had to be "Mr B's Biology Books". This was a demonstration she ran, and I can't actually remember what it was now, although I suspect it involved ethanol. A dangerous demonstration, she set up the plastic shield between her and us at the front of her desk, while she heated a reflux condenser set up with rubber tubes to feed the water in. Quickly, she realised that the screen base was too high and we couldn't see anything. Scouting around, she spied a pile of A level biology text books, which she nicked to pile up her apparatus on before continuing heating.

The inevitable happened: the rubber tubing caught fire, the rubber tubing lit the biology books. We were all very appreciative and unhelpful in the face of disaster.

She extinguished the fire, leaving the biology books scorched and hiding them on the shelf whilst begging us not to tell Mr B. Of course, he was immediately notified.

Posted by Rowena Fletcher-Wood on Aug 22, 2013 8:48 AM BST
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