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Ciborium
11-02-2013, 06:37 PM
After a long hiatus I am resuming my journey work through the LPN Spagyrics courses. At this point Iím trying to calcine vegetable salt without losing so much material as seems to happen when leeching.

Dubuis recommends a setup with a double crucible setup to contain/enhance the heat on top of a camp stove. Iíve tried this by starting with herbs that are already at a medium grey color on a LP gas powered bunsen burner, but after 2 hours the matter still seems to be no less grey. Any thoughts on what I could be doing wrong?

Here are a few possibilities that have struck me:

Material wasnít grey enough before beginning.
Placement in the flame of the bunsen burner is wrong
Crucibles arenít sealed tightly enough (doing that with a automotive band clamp)
Crucibles are too large (100ml each)


Thanks in advance for any thoughts and suggestions!

Ilos
11-02-2013, 07:58 PM
Hey Ciborium,
Firstly I am going to ask you; did you grind the plant well, into small particles (I think that helps to calcinate better).
Considering the temperature of the heat is good idea to (I am not sure exactly how high but I know that it has to be high enough In order to transfer the ash)

This is also one of the reasons why working with dry plants is again easier.

I have seen small crucibles that have heaters on top and on the sides and were sealed tight.

I also had this theory in my head that for plants about calcination is that the power of the fire and air progress the process better.
the crucible should have some kind of ventilation, even better if it could blow on the residue.

Dr.Zoidberg
11-03-2013, 02:30 PM
What does a double crucible look like?

Ciborium
11-03-2013, 10:45 PM
I started with dried comfry, extracted with spirit of wine with a soxhlet, then burned the matter to a dark grey ash until bits of white began to appear. Dubuis mentions that by using a double crucible the more subtle essences may be captured on the upper crucible (perhaps in a glass-like substance). Additionally, the effective temperature is supposed to double.

Today, I tried the same setup in my home gas oven on broil (500F) for 2 hours. Some more specs of white (purified salt) but at this rate it could take many, many days.

I'm thinking that the crucibles themselves may be overly large each is more than 3" tall. I'll try some smaller ones next. It also seems like a small furnace may be necessary, although I am somewhat limited in space it may be a good investment in the future.

Below are some photos.

Thanks so much for your thoughts! :-)

http://forum.alchemyforums.com/attachment.php?attachmentid=825&d=1383518848
http://forum.alchemyforums.com/attachment.php?attachmentid=826&d=1383518849

Ilos
11-04-2013, 03:38 PM
Hey again,
The crucible looks pretty cool and it does look like it can resist a very high temperature.
500F might just not be enough to penetrate the black ash in that crucible.
It looks like the residue didn't even catch fire.

Id recommend you to build up a fire with a good pile of wood, create as much ember as you can, than place the crucible on the ember layer, stuck the crucible deep in ember and leave it like that, also find some sort of bellow to raise the heat temperature time to time.

I'm guessing that this way in less than 2 hour it should be turned into light grey.
consider to grind it a bit more wile its hot like that,
It is also good to mix it a bit wile its calcining with a wooden spoon, like cooking it. :)

lwowl
11-04-2013, 06:26 PM
Greetings Ciborium,

Dubuis mentions that by using a double crucible the more subtle essences may be captured on the upper crucible (perhaps in a glass-like substance). Additionally, the effective temperature is supposed to double.

Dubius was right about capturing the "subtle essences" that are created at the high temp of calcination. But the double crucible method is inefficient and the azothic matter is mostly lost. You will need to heat the matter to between 900 F 1200 F to evolve the azothic oily sublimate. You must catch it in a receiver. It is the crude philosophical sulfur and along with the azothic mercury the key to transformation.

A gas burner will only get your retort temp to around 600 F. That is high enough to get the azothic mercury which will at first be a clear or yellow or red cloud or vapor (depending on what plant material you use) then condensing into a stinking red oil.


Today, I tried the same setup in my home gas oven on broil (500F) for 2 hours. Some more specs of white (purified salt) but at this rate it could take many, many days.

A conventional oven broiler will not achieve high enough temps to whiten your matters.


It also seems like a small furnace may be necessary, although I am somewhat limited in space it may be a good investment in the future.

That is the best way to go. I use a small kiln interior dimensions: 7.5 x 9 x 9 inches. Fortunately good deals can be found on small kilns here in the USA . Here is an excellent one new:
http://www.theceramicshop.com/store/product/9181/Paragon-Q-11-A/

You can also look around for a used one. Kilns are very versatile for alchemical operations.

Hope this helps.

lwowl

http://forum.alchemyforums.com/attachment.php?attachmentid=827&d=1383589192


http://forum.alchemyforums.com/attachment.php?attachmentid=828&d=1383589194

Ciborium
12-24-2013, 10:17 PM
Sorry for my extremely tardy reply. :-(

The calcined matter was actually quite a bit greyer than it would appear in the photo... For now I have returned to simple calcination and leaching and am considering purchasing a butane burner which purports to get to 1300C (such as http://www.amazon.com/Blazer-GB4101-Brush-Butane-Burner/dp/B000ND10YO). Maybe that would be a stop gap until I make the leap to a furnace?

Ilos, thanks so much for the thoughts. Unfortunately, as I live in a town house I'm pretty limited in the ability to build fires unless I go camping... I love the sound of it though! It's so natural that it is very appealing...

lwowl that is quite fascinating and seems like a great way to go. When I master the basics a bit more I'll give it a try. I really appreciate the photos! On the second photo, is the blue wall to the right your furnace?

Thanks again - I'm so grateful for these forums.

lwowl
12-25-2013, 04:12 PM
Sorry for my extremely tardy reply. :-(

lwowl that is quite fascinating and seems like a great way to go. When I master the basics a bit more I'll give it a try. I really appreciate the photos! On the second photo, is the blue wall to the right your furnace?

Thanks again - I'm so grateful for these forums.


Yes the blue wall is the front of my kiln/furnace. I drilled a 2in. diameter hole in the center of the door so the neck of the reaction flask could extend out and connect with the receiver.

lwowl