If you say “DIY Chemistry”, you immediately conjure up images of children sticking mints into two litre bottles of fizzy pop, setting fire to various plastics in a mini bonfire in a pit they've dug into the pebbling in the back yard, or boiling fragrant petals in an attempt to distil their extracts. It's not that I didn't do all of these things as a child, it's that that isn't surprising. Kids. No matter how much everybody moans about the cotton wool generation, kids still have a natural tendency to put things in their mouths and set them on fire. Just not at the same time.

When I say “DIY Chemistry”, I'm talking about adults. Because despite the safe and broadly available tools for chemistry and other science experiments that exist in the world today, there's something not only cheaper, but more fun and fundamental about making it yourself. And dangerous too – but hence fun.

Most of the lab-based DIY I encounter is elementary. It comes down to using rubber bands to hold pieces of glassware together (including pieces of glassware being heated, and including post-eruption, which might have warned the chemist, but didn't), and using household appliances or beauty products to do the job of industrial equipment. Some of this is just basic, safe hardware. In my current lab, for example, we have a gun cabinet. In it we keep a Black & Decker heat gun, because the specialist lab ones are too expensive. Not to be outdone, a previous lab I worked in used a hairdrier, and kept in the glovebox a pair of hair straighteners, which were used for sealing aluminium packets by melting the seal down.

Various science teachers and science communicators have gone even more freelance. From homemade squealing jelly baby experiments (once banned because jelly babies are symbolic of humans and this imagery might induce children to torture), erupting volcanoes and hydrogen rockets made of plastic tubs, to ingesting helium, using basic salts to set soya milk, or employing hydrogen gas to set your hand on fire. In the end, they seem risky at the time, but it's not a big risk. It's a domestic level hazard and for someone who's seen her mother accidentally boil the metal on the bottom of an empty pan, it doesn't seem that large. But what do you think? To DIY or not to DIY?

Reproducibility has always been a struggle in experimental papers; we chemists moan about it, but it looks as though medicine may have exposed the underside of the ice berg.

According to Researchers at Bayer's labs, two thirds of papers are just not reproducible. And this is papers which are accepted by the scientific community as valid and quality works. In attempting to replicate 67 of them, Bayer only succeeded fully in replicating 14, and partially replicating a further 8. Naturally, this is not all due to sloppy academia: sometimes these problems are due to the complexity of biological systems, unrecognised flaws or systematic errors - very sensitive changes which may not have been observed or reported. In my experience, lack of experimental details is more often the real problem with reproducibility, but more and more often scientists are being put under pressure to publish one-time positive results because of the need to validate funding and secure promotions.

Some have mooted the idea that it should be the responsibility of peer reviewers to replicate results in journal submissions to check for reproducibility, but where they will get the funding for the equipment, machine time and chemicals for – let alone how they will create the time for this – was not fully explained in the proposal. They probably won't.

I'm a little dubious however, that reproducibility every time is a must-have (though obviously ideal). Wasn't the Rutherford gold foil experiment famously conducted by picking out only certain data – those alpha particles which came back? Or charging a droplet to measure energy quanta?

Source

There was this old 1993 paper, back when I was doing my fourth year project, where they were making potassium chalcogenides by dissolving the alkali metal in ammonia. It was dangerous. Alkali metals are obviously extremely flammable, and it also involved using very volatile, very toxic condensed ammonia, kept so with a dry ice slurry and extremely low pressures. We were trying to make a product for which the potassium chalcogenide might be a possible precursor. My supervisor looked at the method, and I thought he was going to come up with some super new modern way of doing the reaction safely.

But no.

First I did the reaction with him, then he let me do it by myself, and then he started teaching other students to carry it out.

I think something exploded just under half the time. Usually it was the glass flask that would pop, streaming a fast flow of ammonia into the room, obliging you to dash over to the cylinder and rapidly shut it off before backing away to see if anything else would happen (we probably shut off the vacuum too - I don't remember though). Although it kept going wrong, we were empowered by our initial success with it and my supervisor was convinced that we were all so terrified that we would act with maximum caution... so we kept trying. Afterall, it was fairly reliable in that, although disasters were rife and yields were low, you could pretty much guarantee that if you didn't gas the lab you would get exactly the right product you were aiming for.

But I can't help but wonder what inspired this synthesis the first time round. Did they make a habit of melting alkali metals in liquid ammonia and oohing at the pretty gold colour coming out in the deep blue liquid? Did they throw things in to this witches' cauldron and experiment with what came out as the natural course of their research or were they so determined to make potassium chalcogenides that they were driven to extreme set ups? Because if so, why did they never comment on the safety aspects of it?

We broke so much glassware. And the bigger the experiment, the more likely it was to go wrong, and the more dangerous it was when it did.

On one occasion, my supervisor was in the firing line. I wasn't working with him on this occasion - I was in the next lab down, so the first I knew of it was a shout, running footsteps and, by the time I poked my head out of the door, a host of worried faces and a discarded lab coat lying in the corridor. A few questions were enough to extract the relevant details. He had been leaning over the experiment when it went off, and alkali metal got squirted all over him. This was enough to break his blaise risk attitude - he yelled, ran out of the lab and down the corridor, ripping his lab coat from his body whilst yelling, "AM I ON FIRE?"

He was not on fire. And so the next day, we resumed the experiment.

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.

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.


[Photo courtesy of Amber Thompson, Oxford]

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.

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.

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.

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.

“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]