Anhydrous AlCl3 attempt

After seeing chainhit's thread on AlCl3 with a barbeque I thought I'd give it a try.
I used a Ca(OCl)2/HCl chlorine generator through a CaCl2 drying tube then H2SO4 to suck the last of the moisture out, running through 25mm copper pipe in the BBQ with Al foil in it.
Instead of a condenser I attached another length of copper pipe with a damp rag sitting on it, this way it wouldn't clog up as easily and could easily be disconnected and have a cork rammed through to collect the AlCl3.
Here is the setup:


The inlet for the chlorine:


The 'condenser' and makeshift drying tube:


I thought everything was running smoothly until I realized some fumes leaking out of the BBQ. I noticed the chlorine had been reacting with the copper and had eaten a hole through the pipe, I shut off the heat and turned off the chlorine generator.
The pipe was thin enough to tear apart at the hole, it was full of anhydrous copper chloride and a bit of aluminium chloride.


Copper chloride crystals:


I rammed the rod down to clean the foil from the tube. It looks like the copper chloride had been subliming then traveling down the tube to the unreacted Al and reacting to form AlCl3 and coat the foil in copper.


The CuCl in water:


Here is the only AlCl3 I could collect from the condenser:


Does anyone have any ideas as to how I could stop the copper reacting? Was it just too hot for it?
I'm going to buy some more copper pipe and give this another shot, I've left everything set up still.


[Edited on 25-8-2010 by spong]

I wonder what would happen if you used a microwave instead of the bbq

with a glass tube ofcourse. That would be interesting to look at, just to see the reaction going on (hopefully with sparking).

[Edited on 25-8-2010 by Chainhit222]

Ohh yeah sorry about that, if someone could merge this thread with chainhit's that'd be great
Yeah if you look in the third picture I had a female-female joiner to the condenser piece that I pulled out, stuffed a wad of fiberglass in the open reactor tube and then cleaned. I might try and make a jacket because the wet cloth wasn't doing the best job. I found a fluorescent tube on my old fishtank, it's just bigger than 24mm so ground glass with foil should work well
I think it was mostly CuCl2, there was however a layer of white crud that wouldn't wash off the inside of the tube, that could be CuCl. It should change to green eventually if it is. I'm pretty sure what I collected was AlCl3 though, it fumes in water and doesn't show any blue or green colour in the solution.

I suggest a merge also, as it's a direct follow up from chainhit. [edit: can the merge privilege be given to the authors of the threads? That may alleviate some stress on the moderators]

I'm not sure microwaving it would be a good idea. Microwaves tend to reflect off anything metallic, which is somewhat the opposite of why people are trying them in labs now (with charged organics, like double bonded rings with halogens sticking off, they seem to be absorbed fairly well and cause the charge to shift).

Microwave ovens also use the items inside them to limit their load, and 'light' from the magnetron reflecting back at it may upset it over long durations.

If you have major fuming issues, the product certainly won't be anhydrous. It'll retain some degree of Lewis acid potential but, if a significant amount of water gets in, it's not going to do anything positive. A bigger issue than it loosing some of it's Lewis acid potential is it gaining Brønsted-Lowry potential. The former steal electrons, the latter gives away hydrogens. Having the latter floating around will allow the former to begin behaving in ways that you may not want; side products, tar. As you may have seen in my thread, as blogfast, entropy, watson and I debate the matter, I'm fighting off minute quantities of water, and it's still creating issues.

Watson made an excellent reply with the details for producing a dry(er), clean(er) stream by passing it through activated carbon and then silica. That would probably work even better if you used a separate 98% sulphuric drying stage, then the carbon. If it's not dry, odd acids out the end. If it's not going through carbon, sulphuric in the stream (which may be why your pipe began going funny); the solvent in mine has now gone a deep orange / brown, despite the aluminium being clean, the DCM being redistilled from CaCl2 and the entire thing being borosillicate connected with the very best tubing and grease I can buy (sulphuric is creeping in there)

I've been following these threads, thinking about my own (and working on it bit by bit) and wondering if we're not both going about this in a somewhat over complicated way.

The point of mine was to make it clean, avoid the clogging, the baking and preferably end up with something easily pourable / stirrable; whether the halogen came from HCl(g), Cl2, it went straight on just aluminium or aluminium primed with another halogen or salt. And, and, hopefully discover some more about the temperature dependence and other variables.

Here's some technical details with regards to temperature's effect on chemistry

The maths of that finds that a number of reactions already posses their activation energy, but function at a commercially crippling rate when not heated (as you would expect).

One method that seems to be getting overlooked is to purposefully produce the hydrate with hydrochloric, then simply dry it under a stream of HCl(g). It decomposes at 300C; to the oxide in air, and release HCl(g) under inerts. As with hydrated FeCl3, it would likely need to be under a stream of HCl(g) for drying to function; that's not an issue for people who already used to handling that kind of thing in the first place. My hotplate will easily manage 300C.

If it's the hexahydrate as the starting point, that will be a fair amount of gas to carry the moisture off. Theoretically, the direct to anhydrous methods will be using a 1:3 ratio of aluminium to gas. Then you have to factor in for how well it's being absorbed in the first place, and you're not far off the 1:6 of drying.

Only issue with that, for me, is that I expect some clumping will ensue. For fairly obvious reasons, I don't want to fix those with grinding.

Someone also suggested (sorry, can't remember who), ether is a good solvent from anhydrous AlCl3, and can even carry it over in a distillation. That may offer someway to pick up the lumpy results and then drop them back out in a finer, possibly post distillation, form. I haven't had much luck finding it's solubility in a good number of solvents. DCM is not a great solvent at all. Water is...

[Edited on 27-8-2010 by peach]

I had another try with a glass reactor tube and a CO2 generator to push the AlCl3 vapour through the tube. Here it is before the Cl2 was started:


You can see the Al glowing and reacting once the Cl2 was started:


There was heaps of AlCl3 in the copper tube I was using as a condenser, the only problem is that is was stained bright orange with a contaminant from the muffler sealing tape I used to attach two bits of glass tube together. One of them was too small for the copper pipe and the other fit it well. This tape eventually ruined the experiment, lesson learned I suppose. Here is what I got from the first scraping of the tube:


Here's that damned muffler tape:


The reactor tube snapped while I was trying to fix the muffler tape, filling the entire shed with Cl2 and HCl.


I quickly scraped what was left from the condenser, here is the finl yield of the two scrapings that will definitely have to be resublimed to clean up:


My lungs hurt

Quote: Originally posted by spong

My lungs hurt

I know that feeling. Cl2 seems to be even better at producing it, since it seems to go 'smell-less' once I've been breathing it for a while.

Congratulations on the result, get us some picture of the sublimation and end result.

I had my 200g CaCl2 loaded HCl(g) generator sat out in the garden, in the very damp, rainy weather, for three days last week. It was still fuming enough to be a major pain in the ass to when it came to rinsing it out.

You're dead on right about the difference between the two and being alerted. There is no way you'll ever mistake HCl(g) or not notice it, chlorine on the other hand...

At one point I was putting together a mycology laboratory for a company in the US. One of the final things I did to clean it up to something approaching a reasonable standard was to spray and wipe down every single surface in the room, including the ceiling, with 15% industrial bleach (which was greeny / yellow and contained no special additives); wearing my bunny suit, mask, oversocks, gloves and with the flow hood on full. I could easily smell the chlorine.

Two or three hours later, I couldn't smell it. When I left the room, my lungs were a bit sore. A day later, it felt like I'd been whacked in the chest with a baseball bat.

That wouldn't have happened with HCl(g).

I discovered a very handy and cheap method to vastly boost the cleanliness of the room. Buy a big roll of decorators heavy gauge plastic sheeting, glue it to the walls, ceiling and floors, tape up the seams... super smooth, no dust, no leaks, wipe clean.

Chloride ions in the mucus lining of your lungs control the thickness of the mucus. Cystic Fibrosis suffers don't have enough. Breathing chloride donating gases isn't a great idea, and can cause your lungs to flood, encourage pneumonia and so on, but it will also thin out the mucus, for that crisp fresh air feeling the next day.

[Edited on 28-8-2010 by peach]

Urgh your poor lungs :/
I tried again today, at first I had a glass condenser set up made from the same sized tubing as the reactor tube but I broke it as I was putting it all together so I used the copper one again. There was no contamination from the muffler tape this time but it was still a similar yellow colour, probably from small amounts of iron in the foil, it's still better than the black commercial stuff though. The contaminant from the tape was the greyish colour to the yellow powder and the red/orange or black coating on the lumps of powder.
I only got a small amount this time, the gas cylinder ran out just as it was getting started

Yours was off-white wasn't it chainhit? What kind of Al foil did you use?

Yeah it's definitely a viable method, I don't have much DCM to spare, it's impossible to find here so this was the only reasonable way. The main problem with getting it to run continuously(except for cleaning the condenser and replacing the foil) would be the gas generators, particularly the Ca(OCl)2 and HCl generator, once a good amount of liquid above the granules has accumulated the HCl usually just sits near the top, hardly reacting until I swirl it and have it foam like crazy. Bottled gasses or magnetic stirring in the generators would solve this problem. The foil should be able to be replaced relatively easily, the reaction tube is purged of the inert gas, the condenser could be removed and capped or cleaned then the inlet removed and a big log of foil the length of the tube could be quickly slid in, pushing the Al2O3 'ash' out in front of it.
Would it take much moisture to change it to that bright yellow colour? The powder has to be pretty close to anhydrous, it fumes like crazy around moisture, I dumped the AlCl3 and unreacted foil from the last run into a bin and poured in a flask of water, the thick pillar of HCl that erupted from the bin was ridiculous, I should have filmed it.
I'll get some activated carbon at the pet shop and fill another bubbling flask with it as I don't have another tube to use. I'll also get some more gas for the BBQ
I might test some in a Friedel-Crafts alkylation of toluene to mesitylene some time soon to see if the hydrate is much of an issue.

I don't think there is any surfactant, I've been using the same stuff for a while, it's usually just when I leave it dripping and get a large layer of HCl on top and then swirl it because it's not doing anything, then suddenly it all reacts and bubbles up with chlorine, once it even made its way over into the drying tube.
Yeah emptying the broth from the generators was also a pain, having to hold my breath and open the chlorine generator and carry it outside to dump and then refill with hypochlorite wasn't the best, the CO2 generator I used for the last attempts made things easier though, I could just flood the chlorine flask with CO2 and then replace it slightly more safely. Flowback shouldn't be much of an issue though, as long as there is a bit of resistance at the condenser end, temperatures are kept relatively constant and the gas generators are air tight then everything should be ok.
Interchangeable reactor tubes would be ideal, if only I could get some ground glass tubes it would be so much easier, the fluorescent tubes are so fragile and hard to work with, I have to melt the ends to get rid of any sharp edges or cracks and then mould a foil seal to the melted end for the condenser or gas inlet, usually breaking the end and having to remelt it and start over I'm not sure about the optimum temperature, the best estimate I have is 'medium-high' according to the BBQ thermometer, from all 4 burners at full.

@Impy

I haven't heard from you in a loooooooong time.

I've never bothered with stirring the generators, since I use salt all the time and the gunk is far too thick to stir even with an overhead. Never had too many problems with pressure spikes either. The only time that's an issue is when something in the wash bottle is solidifying and then clogs the dip tube. Which almost universally happens when I switch the stir bar off in the flask to see what's happening and what's evolving where. I purposefully leave a stopper unclipped around the generator somewhere, which then pops off if the dip tube clogs.

Neither do I really bother with a carrier gas. One goal should be to keep the dead volume in the flasks and tubing short, so the gas doesn't end up sat in those, doing nothing. Purging it with carrier once it's done would be okay. Again, I tend to just add a tablespoon more salt and sulphuric in the first place to save the effort of sorting the cylinders out.

I find using a carrier gas to be precisely the opposite of what I need. I'm usually struggling to get the gas flow as minute as possible, so the reactive gas won't blow out of the exhaust before it has a chance to get to work.

One could easily set this up to have tubes that are continuously swappable by using an oblique (two way) stop tap on the generator's output, to swap it from one path to another as the tubes are swapped. A more 'fun' prospect is handling them whilst they're roasting hot and the gas is going.

I suspect the temperature it's run at industrially is simply so they can push it through as fast as possible. As I said earlier in the thread, an experimental mind could check the temperature with a high heat variable hot air gun, using that to heat the tube. Or a variable blow lamp for plumbing work.

@spong

Ah right! I thought you were talking about HCl and didn't realise you meant the bleach and chlorine thing. Try shaking the ass out of the bottle of bleach for a while and see if there are persistent bubbles. Pure bleaches are noticeably less 'slippery' when wiped on a surface as well. You could also switch to pool shocks for more gas per unit of flask volume.

The gas is a pain, but it's still not annoying enough for me to spend £15 on a half mask. I have far bigger issues picking things up when I've forgotten how hot they are.

I do not envy you trying to do this with fluorescent tubes. They are stupidly easy to smash, indeed! I see ground glass tubes around all the time. I could pick you some up if you want. Only problem, they're usually about 6" long.

Do a yellow pages for sign makers, specifically neon sign makers. They'll have huge racks of very long borosillicate tubing in whatever size you like. That will be a lot easier than the fluorescents.

I like the temperature setting, "Produce the anhydrous acid on a slow roast, turn and cough frequently"

Oh I have been using pool chlorine, Ca(OCl)2 granules, If I had to use bleach I'd have given up by now, the strongest stuff we can get around here is about 3.5% with a lemon scent, I'd barely be able to smell the chlorine being produced
A 6' reactor tube would work wonders but the shipping wouldn't be too easy. I might have to give the neon sign makers a try though, with slightly thicker glass things would be so much easier, the glass would flare and shrink smoothly instead of getting little dents or lumps in it when I blow or suck from the thin glass heating up too quickly. Plus there's no mercury

Isn't it 5am in Australia?

I'll PM you if I run into any ground tubes.

Quote: Originally posted by peach

Isn't it 5am in Australia? I'll PM you if I run into any ground tubes.

Ooh thanks It would have been about 2AM, left a maths assignment to the last minute
Yeah the powder would probably react too quickly anyway, plus it would want to clump at the bottom of the tube on the glass, foil worked well because it wouldn't be contacting the glass all that much and wouldn't transfer much heat to it as it burnt. Stainless would be good but I don't have the money for it, plus I like being able to see what's going on in there. The cold finger would be better than cramming powder from a tube periodically, you could keep a spare lid so once it's over you just jiggle the finger from outside the lid to shake the last of the powder off, then remove the jar and put a new lid on it. You could probably leave the one jar on for the whole reaction and just disconnect it when it's done and keep filling it the next time you do it. I might try that fir the next run if I can get a nice smooth bend in the glass from the reactor tube, like this:


The only thing I'd be worried about is the reactor tube clogging before it ends in the jar, the stuff sublimes on anything that isn't insanely hot so a lot would probably collect in the tube.

[Edited on 30-8-2010 by spong]

Quote: Originally posted by Chainhit222

If you use a condenser jacket with hot motor oil, how could you heat and recirculate the oil? Would a pump hold up to those temps?

Quote: Originally posted by greenimp

I have built the set up last night waiting for the weekend to run. Using 1/2 inch stainless, the tubes are 1.5 feet long and have quick disconnects to swap the out. Working on a cold finger tonight. I hope to make 500 grams this weekend. Cross your fingers...if it works ill put the part list up.

fucking outstanding
I just hope your stainless does not react... are you using Cl2 or HCl?

[Edited on 2-9-2010 by Chainhit222]

This isn't just industrial, commercial theory either, it's everyday practical reality unfortunately.

Stainless steel scissors


This sink, despite it being old and retired from the kitchen, was clean prior to me using hydrogen chloride near it


The brand new chromed tap is turning green, it doesn't show up very well here, but you can see the stainless is rotting


The thing for doing the cleaning up needs cleaning up


The shiny new regulator has tarnished and features a new, green, colour scheme, despite being metres away


This is all from one or two minute escapes of the bastard. In todays politically correct atmosphere, hydrogen chloride is a bigoted & intolerant character.

It'll probably work, at least for while. However, I would expect some degree of contamination and for the corrosion to occur a lot quicker when the gas is hot.

You may be able to slow the rate down by ensuring the gas is well cleaned up from the generator. That means getting it bone dry and getting the sulphuric out, which will start ruining your Lewis acid anyway.

[Edited on 2-9-2010 by peach]

I had another shot with tubes from a neon light supplier, 25mm glass. It wasn't a huge advantage to the fluro light tube I was using but at least it's a bit sturdier and I'm not being exposed to mercury cleaning them. I didn't use the activated carbon but it still worked ok.
One thing I noticed with a clear condenser was the AlCl3 seemed to just settle as a powder at the bottom of the condenser, to empty it all I had to do was pull it out and give it a slight tap above the jar, much easier than ramming a cork down there. I added it to the small amount I obtained from the last reaction.
here's the first AlCl3 subliming:

The powder settling in the bottom of the tube:

The jar of AlCl3, one day I may fill it up to the top

Do you have activated carbon spong? I can send you out a little scoop to fill a test tube if not, since you're actually doing as opposed to just contemplating. The price tag will be some photos of the setup and result.

I'd be careful with the hissing test. I pulled a little plug of white gunk out of my DCM AlCl3 method, threw it in some water and it hissed. But I wouldn't accept that as proof that it was working.

If it doesn't smell of anything, or much, at first, and then stinks of hydrogen chloride whilst hissing, you're onto a winner. Holding a bit of damp acid indicating paper in the fumes will show it up for MOAR evidence.

It definitely fizzes on contact with water It really heats up a lot too. The fumes are definitely acidic, I had a big solid lump of it left in a flask after a vacuum sublimation of it today and I was playing around with it by adding water and watching it fizz and pouring the dense HCl 'smoke' into flasks and stuff and then I plugged the flask and shook it around to dissolve the HCl into the water in there and dumped it out on the driveway, it fizzed with some carbonates in the gravel we have and a worm that was on the ground wiggled like crazy. Poor thing, I picked it up and rinsed it off but it was dead
I don't have any carbon but I can get some from a pet shop for filters so no need to ship any I will get photos when I do it though
Anyway, here's the pictures from today:
The setup(I need to buy a cold finger next time I get some glassware):

The dirty AlCl3

Cooling and tipi:

Just starting:

Finished:

The crud that was left behind in the flask (a lot of it was AlCl3 as I discovered when I went to clean it )

All I could recover from the receiving flask:

Al turnings would probably be better, I need a good source of them, is there an easy way to make large amounts from a block of Al?

[Edited on 10-9-2010 by spong]

That's absolutely great! We need more pictures and videos and people getting hands on.

I like the stopper in that flask, smooth.

A cold finger would likely be better, but that looks quite good already. Try adding ice / gel packs to the beaker in the meantime.

That vivid yellow has got to be iron chloride.

For turnings, open the yellow pages and call all the guys offering machining, even the guys resurfacing engines may be able to help (Ferrari engine blocks are magnesium, if you can find anyone servicing those ), the scrap dealers will know where to get it as well. The CNC mills and lathes SPEW Al turnings off so quickly they have big augers or conveyors under the table to push all the stuff out into a huge bin on wheels next to the machining centre.

It all goes back to the foundry as comparably high purity precursor to be recast; compared to the ore it's self. But, the machine tools almost always drench the chips and turnings in coolant, which is basically oil in suspension. That lowers it's value a little because the foundry has to then deal with all the smoke and shit burning back off, and clean the alloying up.

Some of the CNC places produce so much of it, they have autobailers that empty the bins into a hydraulic press to squash it into a smaller brick they can stack up as they wait for the scrap guys to turn up, so it's not using up expensive floor space. I've seen some of those bailers with automatic washers on them to rinse the material of coolant prior to squishy the metal into a brick.

I have two billets of aluminium about two foot long each, which I bought from a foundry supplier in Wales (home of very expensive cartons of milk). They'll be pure, but reducing them to shavings, turnings or chips isn't all that easy. Best to go with the scrap I expect.

The most amusing video on youtube of aluminium under pressure

^^^There are also some very funny ones of gigantic 1000 ton hydraulic hammer forges smacking bits of red hot iron into shape

Ohh yeah I could have a hunt around machining places, someone would definitely have some to spare. Magnesium would be great Copper would be handy as well.
Yeah I'd have to wash the oil and whatnot off, I'd definitely have to distill the acetone back with the prices these days, $10 a litre :/

Quote: Originally posted by spong

I'd definitely have to distill the acetone back with the prices these days, $10 a litre :/

I think it's bunnings having their fun with the monopoly everything is expensive, they wanted $100 to order in 4l of toluene!
With turnings it should be much easier to make large amounts, I've just bought a big bottle of hypochlorite and a bag of charcoal so once I get some Al turnings I can have a try at making hundreds of grams, I think the oxide 'ash' the foil leaves behind is preventing the centers of the bunches from reacting, turnings should have a much lower oxide to Al ratio and I could cram hundreds of grams of turnings in the tube.
The new reactor tube will just have a small tube for the hose stuck at one end and the open end for the condenser at the other, very similar to a chromatography column without the stopcock so they should be pretty good if you can find a really long one. It won't be possible to reload it easily while it's running because the oxide would have to be washed out from the small end but with the amounts of Al in there something else will surely go wrong before I run out of Al.
Now to ring around and find some turnings

Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without another 20L of flammable liquids Getting acetone from a chemical supplier is actually cheaper than from the hardware store *facepalm*
I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners.

@Spong

"Someone at some point has decided the general public has no use for paint thinners."

That made me laugh.

If you can squeeze 100g out in one run, I'd be happy with that. That's a perfectly usable quantity and you may find it more effort to spend weeks / months working out a continuous system than you would to just open it up, pour some more in, purge and rerun it. You don't even need a cylinder of inert gas if you're starting the tube from cold, just displace the atmosphere with HCl(g) and warm the tube up.

Look at the solvent problem this way, if you ever need a BBQ on a rainy day, it's not going to be very hard to get the shed going.

20L isn't too bad, just don't drop your cigarettes in the bottles when you're done. And, if the shed is in the sun and it's hot there, those bottles may get fairly warm and fill the shed with vapours, so some ventilation would be an idea.

@Jig pipe

Sell it on eBay.

[Edited on 22-9-2010 by peach]

Quote: Originally posted by peach

Look at the solvent problem this way, if you ever need a BBQ on a rainy day, it's not going to be very hard to get the shed going.

Hehe, or if I ever run out of petrol
I got some turnings today, I'm a big fan of metal recycling businesses, 300g Al, 650g Mg blocks, 200g Cu and 200g steel for $10

Is it possible to make the hexa hydrate anhy?

Quote: Originally posted by spong

Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without another 20L of flammable liquids Getting acetone from a chemical supplier is actually cheaper than from the hardware store *facepalm* I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners.

Quote: Originally posted by starman

Quote: Originally posted by spong   Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without another 20L of flammable liquids Getting acetone from a chemical supplier is actually cheaper than from the hardware store *facepalm* I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners. 20Lt methanol?Is it of reasonable purity.Care to share your source?

Quote: Originally posted by starman

Quote: Originally posted by spong   Yeah I've already bought 20l of toluene and methanol because that's the only reasonable way to get them. The shed is a big enough fire hazard without another 20L of flammable liquids Getting acetone from a chemical supplier is actually cheaper than from the hardware store *facepalm* I think it's mainly Australia. Someone at some point has decided the general public has no use for paint thinners. 20Lt methanol?Is it of reasonable purity.Care to share your source?

http://www.oilchem.com.au/products/alcohols
That's just the alcohols page, they have such a great range of chemicals but they're in 20L minimums, it would be great if some Australians could arrange some kind of a group buy for them, with 10 or 20 people in on it we could get a great deal on some awesome solvents and reagents, I've been looking for benzyl alcohol for ages and they have it...in 20L drums

I just was at toolstation. Having sanded the floor from it's previous nicotine amber stain to pristine white, it's now pitch black, momentarily.

I have a litre of DMSO, but have been so busy I haven't had time to do a lot of chemistry fun. I also need to pick up a new receiver bend before any distilling is happening.

Sorry for not getting back to your PM. I did read it but, as with the experiments, got carried away with tidying up and kept forgetting.

Yes, the repetition is bad.

I don't mind typing the Lewis acid stuff out once or twice, since they're something people usually don't deal with, don't behave as you might expect and have some quirky traits that aren't discussed all that much in what I've read - so I had to gain it first hand, and experience the defunct results with my pocket money.

AlCl3, the discussions of it here, are a prime candidate for compression. This has already been discussed as well. The BBQ method, we have photos of, I'll have a go at forming it with hydrochloric then drying it, and perhaps the DMSO idea as well. Once that's done, the threads all need a battering down into one in the pre-publications section.

[Edited on 17-10-2010 by peach]