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madscientist
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[*] posted on 18-11-2002 at 14:11
Distillation equipment


I'm considering purchasing a distillation setup from www.unitedglasstech.com. Is there any huge, blatant reason that I'm somehow overlooking as to why I shouldn't buy the smallest distillation setup?

I'm also planning on purchasing an aspirator from www.al-chymist.com. Could someone enlighten me as to how I should hook it up to a faucet or a hose?




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trinitrotoluene
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[*] posted on 18-11-2002 at 16:14


You can get distilling equipment on ebay for even cheaper, i've found a entire setup for $109.00. But for me i make my own distiller with a Flask with rubber stopper. And copper or aluminium tubing for the condensers. I just coil the tubing. I use the aluminium for distilling nitric acid and the copper for other stuff. But for someone that cant afford a distilling setup then maybe its better to build one out of a flask with rubber stopers and tubing for the condensers.



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[*] posted on 21-11-2002 at 03:36
Al-chymist ?


Hey I was wondering about al-chymist, is it a good place to order ? There's no guarantee, and I believe (I didn't look very far though) that you have to send money to get the stuffs back...

No problems with it ? It may be great to avoid giving your visa number, but you're never really sure about what you get back.

I'm trying to find a shop in my country, it's easier, you go there, buy with bucks, no cheque nor credit card, no problems... But online shop may have many stuffs you cannot find elsewhere.

BTW, I have one so no problems, but wasn't distilling equipment forbidden to the public ?




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[*] posted on 21-11-2002 at 11:42


The al-chymist has treated me well. I don't know if they will do international orders, though, and shipping will of course be more expensive. Some distillation apparatus is regulated (taxed by the BATF since it could be used to purify alcohol). Texas and maybe a few other states regulate glassware on the state level in an effort to thwart clandestine drug chemists. Speaking of drug chemists, if you visit the Hive there is an excellent thread under the Acquisition forum (you must register to see this forum) about constructing a high-quality condenser using low-cost parts that are easily obtained.
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[*] posted on 24-11-2002 at 00:57
distillation setup


On Rhodiums page at
http://www.rhodium.ws/chemistry/index.html
you can find a downloadable pdf on building a sophisticated fractionating still by mostly standard copper tubing.
IMHO this is the best what a interested amateur can get - for small money is understood.
I dunno if the direct link works, if not you´ll have to go over the page.
direct:
http://www.rhodium.ws/pdf/still.pdf
ORGY
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[*] posted on 21-1-2003 at 17:55
"retro-engineering" setups


I want to point your attraction to the fact, that these common lab-setups are not always necessary.

You can make a useable distillation-setup out of junk, like marmelade-glasses, PE-foil and a pot for a water bath.

PPl from the E&W-forum derived this setup from the well known "you are in a desert, you have to piss, but you don´t want to lose any water"-trick(brought up by kingspaz).

Actually, this is not new.

http://cannabis-archiv.de/anbau/alchimie.html

I am sorry this page is in german, but it is a further good example that this design is widespread among back-yard THC-chemists and works well, especially when using containers with a big surface(where the liquid-to-inner-surface-ratio is low) for distilling organic solvents.

To make the whole thing less vague:

Imagine a big marmelade-glass, wherein a smaller one is placed on a small platform.

The big glass is sealed with a thick, or multiple layer PE-foil, which is hanging into the glass in the form of a cone(ideally the cone is hanging nearly to the ground and has a big surface); the cone is cooled with ice, or a slow coherent flow of water.
The room between the two marmelade-glasses is to fill with the liquid you want to distill.

This is all together placed on a warm/hot water-bath, ideally with a suitable thermometer in it.

Even the distillation of anhydrous nitric acid can be accomplished with this setup, although distillation-times as long as 1 or 2 days have to be accepted(look up the "easy nitric"-thread in the nitric acid section of E&W).

And this is exactly the point i´d like to make:

you can even use such a setup for actions that would normally call for a vacuum distillation-setup, but as long as you don´t heat the water bath too much(e.g. when 100%nitric acid decomposes at ~85°C then you have to keep the temp of your water bath below this temperatur), and you only have a little time, there is no problem at all.

Always remember:

you don´t have to bring a substance to boil to vapourize it!

Boiling only means that the rate of vapourization has reached a good rate because the vapour pressure is now equal to the atmospheric pressure-the liquid boils.
(any substance has a specific vapour pressure that applies to a specific temperature)

Considering these setups don´t need much surveillance, they are quite worth a thought for all thinking they would need an expensive distillation setup out of lab-glass for their nitric.

I dare to say, that even such operations like distillation of perchloric acid out of NaClO4/H2SO4, normally calling for vacuum distillation, are possible, given the PE-foil is replaced by a glass funnel or something else suitable.

The only advantages of the complicated and expensive glassware-setups are:

They are much faster, lab procedures can be followed more easily due to
standardisation; and naturally, they can be used more universally.

HLR




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[*] posted on 22-1-2003 at 14:13


I wouldn’t buy the smallest one, 1 liter is nice,
I have a ½ liter, 1 liter and a 4 liter setup.
I mostly use the one liter,
When distilling hno3 and for concentrating H2SO4 I use the 4 liter.
If you take a smaller setup it takes a lot more work to get the same quantity, (cleaning the glass, drying and reassembling))
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[*] posted on 11-4-2003 at 14:52


hey BASF, what is PE foil, could heavy duty kitchen AL foil work in its place?



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[*] posted on 12-4-2003 at 10:22


PE is polyethylene.
Al foil? Why not. If the distilled liquid doesn´t corrode it, ok.
Are plastic bags now forbidden in your country?
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[*] posted on 28-4-2003 at 21:19


https://www.scientificsonline.com/EC/Products/Display.cfm?ca...

little bit of a rip off compared to what some people have found but its a high quality, all glass setup. 129.95 USD




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[*] posted on 29-4-2003 at 16:35


About fractional distillation equipement, anyone has somewhere where you could buy one cheap or build one...



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[*] posted on 9-9-2003 at 01:11
distillation


You dont need a professional-style equipment for a simple distilling. For example, HNO3 and other two-fraction distillations can be carried out with simple flask-and-cooler-type equipment. Of course the case is a bit different if you are trying to fractionate a mixture with ten substances which have less than a one-degree differences in their boiling points.:D PS: By the way, I myself can make all my synths with very few pieces of equipment, because I simply rip the old system apart and make a new one. And besides,for example in many universities the simple beakers are counted very seldom, as bigger sets like fraction distillers are counted every time when you leave the lab after you have made your analyzing assignments....;)
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[*] posted on 9-9-2003 at 03:11


Don't use fractionating coloms with liquids like HNO3 that will decompose when heated! When using a fractionating column you'll have to heat considerably more, rapidly accelerating decomposition.



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[*] posted on 9-9-2003 at 20:29


I have my plan set to slowly aquire the componets for a 24/40 distillation setup. My 300mm graham condenser arrived today with 24/40 joints.It cost me $50 at an ebay auction,and I also aquired a 500ml erlin flask 24/40. Some parts I will get from ebay auctions at lower prices, the rest I will get off of unitedglasstech. I did my math ,it will be cheaper then buying a complete still from unitedglasstech.



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[*] posted on 10-9-2003 at 02:40


I can only say i´ve tried both professional glassware and the improvised method using a stainless steel pot with receiving beaker in it, tightly sealed with the mentioned PE-foil, which was filled with crushed ice(the deeper the foil hangs in the faster the distillation!).
- The improvised method is in many cases as good as glassware, BUT it has a considerable ADVANTAGE:

it is airtight(when fixed with a suitable rubber-band or similar) and no poisonous fumes have to be struggled with while working.
- On the other hand, if the pressure inside should get too high, the ice on the foil falls into the hot water bath and cools it down automatically.

I have not tried anything else than a simple glass-beaker inside for the receiving, and thus a good portion of the received liquid revapourizes, so using an insulating beaker for instance would surely improve the speed of distillation.

It has also been proposed not to mix the reactants stoicheometrically(H2SO4+KNO3>KHSO4+HNO3), but to dissolve the nitrate in an excess of H2SO4. - This has been proven to be a good idea....less decomposition, quicker distilling :P

[Edited on 10-9-2003 by BASF]




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[*] posted on 12-9-2003 at 01:14
Excess H2SO4 spared


Yes it is useful to distill a solution with a small amount of excess H2SO4, because it will prevent the decomposition. But if you don´t want to loose the excess amount of H2SO4 just let the solution to boil until the white fumes appear. This conc. H2SO4 is good enogh to be the base for a new distillation of HNO3, and like this the H2SO4 wont´t be wasted. Of course it is sensible to throw the leavings away once and a while, so that there isn´t a huge amount of sulphates in your solution of HNO3 and H2SO4.
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[*] posted on 13-9-2003 at 07:50


?? How is that meant?

After the distillation is complete, and the mix cools down(or is cooled down, preferably) KHSO4 precipitates.
You want to boil the solution??
This would only increase the solubility of KHSO4...

I am not sure what your thought exactly was...maybe the KHSO4 is supposed to decompose, yielding the pyrosulfate, which is possibly less soluble??

But sulfuric acid is cheap, isn´t it? - The nitrate always used to be the cost-intensive part.




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[*] posted on 13-9-2003 at 09:26


I believe what he is saying is that he wants to reboil the liquid left over. Thus reconcentrating the amount of Sulfuric still left due to the excess. The only thing I don't get is, wouldn't the acid still be near azeotropic, assuming the Nitric acid doesn't decompose? My guess is that a fair percentage of the water left from the already reacted Sulfuric acid is distilled over with the Nitric Acid.

I don't really see this as neccesary. I wouldn't waste all that extra effort to get an extra 20mL of heavily contaminated acid. Although I guess it would be one way to knock the production price down a bit.

I suppose to recover the most amount of acid possible you could take the pyrosulfate decomp route and bubble the resulting SO<sub>3</sub> into the left over liquid, then concentrate/dilute from there.
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[*] posted on 14-9-2003 at 23:59


Of course it is useless if you use a nitrate like KNO3, which will convert to a near insoluble substance in the process. But if you use a nitrate like NH4NO3, it won´t precipitate until you have boiled it down to a concentrated acid AND then maybe also cool the solution down to get more waste salt out of the solution. This will make the process only a little bit more economical, that is right. But at least here in Mirroland the cost of H2SO4 is in fact quite high, because you cannot buy it in a cheap form like battery acid. (Here you probably would have to buy the whole battery to get H2SO4 that way) Another problem is sometimes even to be able to buy it in the first place, the availability is very poor without a licence.

[Edited on 15-9-2003 by the timeless]




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[*] posted on 28-9-2003 at 14:31


My distilation apparatus is now complete(sorta). It has all pieces necesary for distilling. I currently have a rubber stopper as my thermometer adapter. I'll have to invest in some teflon, or a glass stopper eventually. The whole thing ended up costing about $100. I probably could of gotten it cheaper, but I broke down and bought the adapters from UGT. I'll try it out probably this week, I need to get a water pump for the water jacket.

On that note, can anyone suggest how strong of a pump I should get. They range from 10gallons per hour to probably 600. Tap water here on full blast pulls about 120-180 gallons per hour. I was thinking somewhere along the lines of 60 or 70 gph. There are several pond pumps that I'm looking at. Eventually I'll also make an aspirator pump. The basic design can be seen here: http://www.rhodium.ws/chemistry/equipment/aspirator.html
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[*] posted on 28-11-2003 at 01:11


ONE WORD!

LABX




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