madscientist
National Hazard
Posts: 962
Registered: 19-5-2002
Location: American Midwest
Member Is Offline
Mood: pyrophoric
|
|
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?
I weep at the sight of flaming acetic anhydride.
|
|
|
trinitrotoluene
Hazard to Others
Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline
Mood: paranoid
|
|
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.
TNT
|
|
|
Arthis
Harmless
Posts: 6
Registered: 16-11-2002
Member Is Offline
Mood: No Mood
|
|
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 ?
Who knows ?
|
|
|
Polverone
Now celebrating 21 years of madness
Posts: 3186
Registered: 19-5-2002
Location: The Sunny Pacific Northwest
Member Is Offline
Mood: Waiting for spring
|
|
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.
|
|
|
Organikum
resurrected
Posts: 2337
Registered: 12-10-2002
Location: Europe
Member Is Offline
Mood: frustrated
|
|
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
|
|
|
BASF
Hazard to Others
Posts: 282
Registered: 5-11-2002
Member Is Offline
Mood: hydrophilic
|
|
"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
|
|
|
lucifer
Harmless
Posts: 21
Registered: 23-11-2002
Member Is Offline
Mood: No Mood
|
|
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))
|
|
|
Skean Dhu
Harmless
Posts: 7
Registered: 4-4-2003
Location: Great Lakes
Member Is Offline
Mood: No Mood
|
|
hey BASF, what is PE foil, could heavy duty kitchen AL foil work in its place?
|
|
|
Organikum
resurrected
Posts: 2337
Registered: 12-10-2002
Location: Europe
Member Is Offline
Mood: frustrated
|
|
PE is polyethylene.
Al foil? Why not. If the distilled liquid doesn´t corrode it, ok.
Are plastic bags now forbidden in your country?
|
|
|
Skean Dhu
Harmless
Posts: 7
Registered: 4-4-2003
Location: Great Lakes
Member Is Offline
Mood: No Mood
|
|
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
|
|
|
Blind Angel
National Hazard
Posts: 845
Registered: 24-11-2002
Location: Québec
Member Is Offline
Mood: Meh!
|
|
About fractional distillation equipement, anyone has somewhere where you could buy one cheap or build one...
/}/_//|//) /-\\/|//¬/=/_
My PGP Key Fingerprint: D4EA A609 55E4 7ADD 8529 359D D6E2 33F6 4C76 78ED |
|
|
the timeless
Harmless
Posts: 14
Registered: 3-9-2003
Location: Mirrorland
Member Is Offline
Mood: No Mood
|
|
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.
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....
|
|
|
vulture
Forum Gatekeeper
Posts: 3330
Registered: 25-5-2002
Location: France
Member Is Offline
Mood: No Mood
|
|
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.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
|
|
|
trinitrotoluene
Hazard to Others
Posts: 142
Registered: 17-10-2002
Location: California
Member Is Offline
Mood: paranoid
|
|
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.
TNT
|
|
|
BASF
Hazard to Others
Posts: 282
Registered: 5-11-2002
Member Is Offline
Mood: hydrophilic
|
|
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 
[Edited on 10-9-2003 by BASF]
|
|
|
the timeless
Harmless
Posts: 14
Registered: 3-9-2003
Location: Mirrorland
Member Is Offline
Mood: No Mood
|
|
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.
|
|
|
BASF
Hazard to Others
Posts: 282
Registered: 5-11-2002
Member Is Offline
Mood: hydrophilic
|
|
?? 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.
|
|
|
Mumbles
Hazard to Others
Posts: 436
Registered: 12-3-2003
Location: US
Member Is Offline
Mood: Procrastinating
|
|
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.
|
|
|
the timeless
Harmless
Posts: 14
Registered: 3-9-2003
Location: Mirrorland
Member Is Offline
Mood: No Mood
|
|
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]
The Balance comes like storm.
|
|
|
Mumbles
Hazard to Others
Posts: 436
Registered: 12-3-2003
Location: US
Member Is Offline
Mood: Procrastinating
|
|
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
|
|
|
Hermes_Trismegistus
National Hazard
Posts: 602
Registered: 27-11-2003
Location: Greece, Ancient
Member Is Offline
Mood: conformation:ga
|
|
ONE WORD!
LABX
Arguing on the internet is like running in the special olympics; even if you win: you\'re still retarded.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
