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FraterP.I.
05-14-2013, 02:57 AM
Ok, Week 3 of my Alchemical studies. I have one successful spagyric...that's the up note. :D Now for the good stuff. I received my distillation assembly today and it has been an explosive good time. I thought, like any good alchemist-in-training, that I'd take a few minutes to get the feel for my new resource. Did anybody here know that glass baking dishes are NOT designed for induction burners and ash baths? Fortunately, my flask was amazingly left untouched by the explosion that sent glass as far as my living room. :cool:

Alcohol burns, as we all know, but take said alcohol in a pot when calcinating mint leaves and decide to turn on the heat in the process renders shaving a pointless task. On an up note, I managed to save the herb and even got a moderately decent salt out of it. Not too bad for my second calcination attempt.

And here I was worried about damaging my distillation setup. It's the rest of the house I need to be worried about. Did I mention that I've had two of those baking dishes explode on me? I've come to the conclusion that they are best left for baking. I grow wary of cleaning up tiny glass shards.

Any advice that could be offered that might save me more explosions, burnings, breaks, and all manner of unseemly "fun" times, would be much appreciated and, might I mention, cost efficient. :D

Goldlion973
06-26-2013, 04:11 PM
I just typed up a good half page list of things for this post and lost it as the forum timed me out.

Annoying is not the word.

Andro
06-26-2013, 04:31 PM
I just typed up a good half page list of things for this post and lost it as the forum timed me out.

See Log In Time-Out (http://forum.alchemyforums.com/showthread.php?3415-Log-In-Time-Out).
(http://forum.alchemyforums.com/showthread.php?3415-Log-In-Time-Out)

Kiorionis
06-26-2013, 05:11 PM
And here I was worried about damaging my distillation setup. It's the rest of the house I need to be worried about. Did I mention that I've had two of those baking dishes explode on me? I've come to the conclusion that they are best left for baking. I grow wary of cleaning up tiny glass shards.

Any advice that could be offered that might save me more explosions, burnings, breaks, and all manner of unseemly "fun" times, would be much appreciated and, might I mention, cost efficient. :D

haha, I'm moving into a new apartment here pretty soon and can't wait to make a mess!

how quickly are you heating up your glass dishes? I use pyrex glasswares that are meant for cooking, and over the last year I've only had two or three explode on me. Mostly due to how quickly I heated them up, or how quickly the volatile the matter was heated (such as the first calcination of herbs saturated with alcohol).
Letting the glass adjust to the heat, is a good rule of thumb (or more familiar, "make haste slowly").

Ilos
06-26-2013, 05:23 PM
Hey,
Dubuis, suggests Pyrex glass for distilling. You can probably find Pyrex lab equipment on ebay.
For calcination, its probably best to use those mud dishes.

Krisztian
06-26-2013, 07:08 PM
On an up note, I managed to save the herb and even got a moderately decent salt out of it. Not too bad for my second calcination attempt.

After separation, one can place 'body' in oven at 190 to 200 Celsius for 8 to (even up to) 24 hours. That dries out the mass. Then, you can roast it well (viz., open flame outside), watch the smoke play and leave, then you may close the lid for higher heat. Simple camping gas stove will do it.


And here I was worried about damaging my distillation setup. It's the rest of the house I need to be worried about.

I've had my share of explosions in the beginning, it comes with the territory - good learning. Much of the 'accidents' can also result from impatience, trying to rush Mother Nature's way.

Any advice that could be offered that might save me more explosions, burnings, breaks, . . .

Some alchemists swear by quartz bowls. They can take swinging of extreme temperatures from cold to hot. Take your pick and needs with which size to get.

Donna Matrix
06-27-2013, 05:37 PM
I calcine first in the BBQ outside all burners on high for 4-8 hours. Then I grind up the ask and ut it into a dental lab oven I have in the lab. This oven works great and I calcine foor about a week at 1000C. Then I take it out and grind up the ashes again and leach the salts, separating the soluble from insoluble. I then put them back in the dental oven until the full moon or just before and do another leaching on the insoluble salts, trying to get all the soluble salts out.

My first water bath was attempted in a pyrex bowl with flask kin it. The pyrex got mad and exploded. I will never use glass for calcining or baths. Best of luck.

Dr.Zoidberg
08-01-2013, 06:29 PM
Hello FraterP.I.!

We also are pretty new to the art of alchemy and have created our own amusing (luckily not serious) mishap. We have a glass stopper (no clamp) that acts as a sort of "check valve" above our vigreux column, so if we have a pressure spike it blows off the stopper and creates a volcano instead of exploding the glass. A couple of ways to prevent a pressure buildup in your train is to use a vacuum take off adapter right before your final receiving flask. Also don't attach your receiving flask until a few drops of your distillate have accumulated in your condenser; this prevents pressure buildup from initial heating. We use a beaker in the receiving location just in case drops come over before we realize it is time to connect our flask. The vacuum adapter also allows for you to tube fumes to a safe location depending on what you are working with. I've seen a nifty video of someone routing their vacuum take off to an open vessel in ice water just to catch anything that may be lost. Pretty clever.

Kiorionis
08-02-2013, 02:43 PM
Also don't attach your receiving flask until a few drops of your distillate have accumulated in your condenser; this prevents pressure buildup from initial heating. We use a beaker in the receiving location just in case drops come over before we realize it is time to connect our flask.

When you release the pressure buildup the distillation will run smoother/faster as well. The first time I was using my alembic I had closed everything off, then started the fire. A couple hours later with no distillate I was thinking "why the f isn't my alcohol coming over?" As soon as I removed the receiver there was a rush of escaping air (the internal pressure adjusting) followed by the alcohol from the boiling flask coming over quite quickly.

black
08-03-2013, 01:25 AM
It's much safer to have an open system in any distillation. This alleviates the great danger of pressure buildup. If you use a drying tube this allows the pressure to escape but stops moisture entering into the system. See attachment.

I connect mine to a vacuum takeoff elbow with a piece of rubber hose. I usually fill my tubes with anhydrous Potassium carbonate. These tubes are an easy DIY. Here is a link about drying tubes that might help.

http://www.ce.gxnu.edu.cn/organic/net_course/content/distillation/drying%20tubes.htm

Regards,

Black