distillation

[nitric]

I just got a 14/20 ground glass distillation kit with 2 condensers,5 rb flasks,a 105° bend vacuum adapter,a three way clasien adapter, and a three way 75° adapter for 75$.Help using it. does some one have some advise.

[frosch45]

Thats a great price depending on the capacity of it. Where did u get it?

 

As far as using it, what do you need to know? You should use a flask with a similar capacity for your recieving flask as well as your boiling flask. I trust you have a ring stand? If you don't you can get very cheap but high quality ones from hometrainingtools.com.

 

You might want to grease your joints for a tighter seal, maybe use vasoline. Keck Clamps would be useful to you as well to hold it together tightly.

 

For your condenser, depending on the type and assuming you don't have a pump (although you may), just have a huge bucket of ice water higher from your condenser and "siphon" the water downward through the condenser (using appropriate hosing) and have another bucket underneath the outlet of the condenser to collect the water. Either that or hook up your condenser to a faucet.

 

What exactly do you need to know?

[CaptainPanic]

You will need a heater.

 

Never ever use open fire. In stead, use a water bath (that's basically a pan of hot water) and get electrical heating (for safety reasons). Special lab heating plates are probably the best way to go, but it's probably cheaper to get a simple electrical kitchen stove.

 

If you need temperatures above 100 deg C, put vegetable oil in a pan, and put that on the electric stove. Make sure you measure the temperature (so get a thermometer capable of measuring temperatures up to where you need to work), and never exceed 160-180 deg C, or your oil might catch fire.

 

Wikipedia pretty much shows how to build your distillation setup.

 

edit: I had a look at those electrical heatings I mentioned: Here are the ones I meant. They're actually much too powerful (1.5 kW!) for your little setup... so you might as well ignore that comment. Sorry. Just to give you an idea: this is quite like what I've used in the lab (but that might be too expensive for home use).

Edited August 8, 2008 by CaptainPanic

[insane_alien]

Never ever use open fire.

 

unless your really really careful. seriously, i've done maybe 2 distillations in my life that didn't have an open flame. and thats only because it was carried out in a room with an explosive atmosphere.

[CaptainPanic]

unless your really really careful. seriously, i've done maybe 2 distillations in my life that didn't have an open flame. and thats only because it was carried out in a room with an explosive atmosphere.

Well, our hobby distiller here might be planning on doing some distillation with flammable liquids (like ethanol), and perhaps he is not as careful as you, because it will be his first time!

I will stick to standard safety regulations, and that's the end of it. If people want to take a risk, of course, they can go ahead. But I prefer not to advise someone some risky experiment, especially if there is a relatively cheap and simple solution.

 

"A room with an explosive atmosphere?"

Lol... sorry, but that somehow doesn't seem like a natural environment for human beings. What were the components, and were you in it, or just close to it? My mom always told me never to enter atmospheres that are explosive.

[insane_alien]

no it doesn't sound good and its probably not.

 

it was the organic chem lab and there was lots of ether being used as a solvent.

 

i do agree that ether fumes + fire = AAARRRRGHHHH MY FACE IS BURNING!!!!

[nitric]

what type of coolant should i use for distilling + making nitric acid.

[frosch45]

Depends on your setup. You could just use ice water in a bucket with a water pump, or if you wanted to get it really really cold, use acetone and dry ice.

 

All a "coolant" is is a liquid. You do have to cool the coolant before it will be "cold" via some other cold material (unless you actually do have a set up that can handle the pressure/volume/temperature type of cooling system where those variables are changed to produce a colder area and a hotter area in a system, although I have a hard time believing that)

 

So really, water would be work but overall with pretty poor results, ice water would be like 5-6 C (without addition of NaCl or a similar salt), dry ice in acetone would be like -60 C.

 

Buy a small water pump, have a bucket (or suitable holder for your coolant) pumping the liquid into the bucket from your condenser and have another line out of your bucket going into your condenser but not attached to your pump, only have it hanging in the bucket (if that makes sense).

[person]

Wil your pump still work wile using acetone that "is like -60 deg"

[pioneer]

In terms of operation, if you are distilling ethanol and water, for example, since ethanol has a lower boiling point, a higher ratio of ethanol will boil off than is in the pot, but this richer vapor will still contain water. The reflux ratio is how much of this primary vapor blend you condense and let drip back into the pot from the condensers. The affect of the refluxing is it will strip more water out of the primary vapor that is rising out of the pot. The water will diffusion out of the vapor into the dripping liquid, allowing the ethanol concentration in the primary vapor to get stronger. The more reflux the higher the ethanol at the top. But this lowers the rate at which product will come off the top.

 

If you wish to further increase efficiency, if the distillation column don't already have it, add some type of packing such as glass beams or teflon beads, each will act slightly differently. You are still on reflux, except you get more mixing and therefore more transfer efficiency. The result is your purity will increase, at any reflux ratio.

 

The difference between teflon and glass is based on surface tension. The water will wet glass but bead up on teflon. The alcohol is slightly the other way. It determines which will be the continuous phase and will affect mass transfer between vapor and liquid.

 

What is interesting about ethanol and water is at 95% ethanol you hit what is called an azeotrope. What happens is there is an inversion at 95% and water boils easier than ethanol. There are ways to crack the azeotrope but this denatures the product. You can also use desiccating stones to strip the water from 95% ethanol, but that is not distillation.

[CaptainPanic]

According to wikipedia, you are boiling at 83 deg C... so I'd say normally a condensation at 10 deg C (tap water) is good enough... but it does sound like a particularly nasty reaction, with dangerous fumes (do this in a very well ventilated room!), so a decent cooling will make it safer. Ice + (lots of) salt can become quite cold.

 

I get the feeling that nitric is doing this all at home, so dry ice in acetone is probably not available. Go with lots of ice from your freezer, and add a little water and lots of salt. Submerge the collection flask in that. Also try to connect the cooling (condenser) to some of this ice water. Experiment first with the cooling... and only then play with dangerous chemicals.

 

Step 1 in distillation: test your setup!

[pioneer]

Step 1 in distillation: test your setup!

 

Good suggestion. Practice with to get used to your technique and to gets the leaks and bugs out of the system.

 

An interesting distillation affect is called steam distillation. A good pair is water and kerosene. They will not blend but appear as two phases. If you tried to boil just kerosene it has a relative high boiling point. But if you place it in water, it will vaporize quite readily at the boiling point of water. It is an old engineering energy saver technique.

 

Another consideration when boiling something hazardous like nitric acid or whatever is to avoid superheating. Sometimes the temperature in the pot will get higher than the expected boiling point and then just erupt. It is good to add a few boiling stones before starting to avoid this special affect. The boiling stones provide a surface for bubbles to nucleate. Without that surface potential can build until there is a bubble chain reaction.

[CaptainPanic]

That's another good suggestion

Look up "boiling stones", and get some. Just normal sand will not really do the job (I tried that once).

[frosch45]

The biggest problem is that nitric acid is very volitile when it is concentrated. Just remember, while you have something very hot, you must have something very cold to keep the volitility down, at least until you can transfer it to its container.

 

Also, I would recommend teflon-coated boiling chips. Hot sulfuric/nitric mix (which is what you will have in your boiling flask) would not look to kindly upon certain materials, and if you're not careful, maybe it will even make a nitro compound on your boiling chips!

 

-just a possiblility, and besides, you're smarter than that... right?

[nitric]

I can get dry ice from krogers and acetone from home depot.And i would be distilling a mixture of KNO3+H2O+H2SO4 to make nitric acid

[ivy]

hello is there anyone here?

This is Ivy from China

[CaptainPanic]

Is it going to be your first distillation ever? And you immediately try nitric acid? hmm... I really suggest that you do some practice experiments first. Try to concentrate your wine or something... Just to find out what can go wrong with the experiments, and to find out how stuff works.

 

hello is there anyone here?

This is Ivy from China

 

Hello ivy,

Yes, we're all here!

 

This is a forum, not a chat, so no worries if you don't get an immediate reponse.

 

for saying hello, I can refer you to "The Official "Introduce Yourself" Thread"

[zeldaik]

The biggest problem is that nitric acid is very volitile when it is concentrated. Just remember, while you have something very hot, you must have something very cold to keep the volitility down, at least until you can transfer it to its container.

 

Also, I would recommend teflon-coated boiling chips. Hot sulfuric/nitric mix (which is what you will have in your boiling flask) would not look to kindly upon certain materials, and if you're not careful, maybe it will even make a nitro compound on your boiling chips!

 

-just a possiblility, and besides, you're smarter than that... right?

 

Would non porous clay work as an alternative for the boiling chips?

[DrP]

Would non porous clay work as an alternative for the boiling chips?

 

I don't see why not - anything that creates a site for the bubbles to seed will work: broken splint, glass wool, granuals, scratches in the side of the vessel etc..

 

Something that I used to find useful in a particularly bumpy, small scale, distillation I used to do was to put some glass wool above the vessel at the start of the colunm - It ment that if there was a sudden big bump - the liquid would hit the glas wool 'bung' and not bump all the way over to the collection chamber - instead it would then drip back into the vessel from the wool.

Edited September 10, 2008 by DrP