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would you eat this? i would... mesc hcl extract

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#21 smacked12



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Posted 17 July 2007 - 11:09 AM

good work. thanks for posting an improved HCl concentration for salting. I'm about to do a big run, and I had been titrating my acid but I'm gonna just use your ratio this time. Did you arrive at that by trial and error or did you estimate the amount of mesc per pull and do the stoichiometry calculations?

is this THE foaf, originator of foafs tek. if so, :bow:

i came to that ratio by trial and error. 4-4.5ml gave me decent results also. but, i noticed i started picking up impurities much sooner. my first salting would come out as pictured. maybe even the second but, after that i started getting impurites and with each salting the impurities increased.

using 3-3.5 i usually have to do 5 or 6 saltings but they all come out clean. i could increase the amount of water to solvent i use but again i found it grabbed more impurities that way.

Ok, Not to stray off topic, but, I was curious, can one create anhydrous ammonia the same way? Or will the E salt have an adverse effect on the ammonia? THANKS!

anhydrous ammonia is really nasty stuff. from what i understand it's a pretty involved process.

this was taken from another site...
i'm not sure how accurate it is...

CREDIT TO: Eleusis

As stated before, this is only for the truly insane. Please consult all relevant toxicology sources, lab technique manuals, and common sense before attempting this procedure. It is mildly amusing when it works, but a major lethal pain in the ass if, say, you run out of dry ice. Kid's, don't try this at home, really.

There are no good ways to efficiently make ammonia without extensive industrial equipment. Even worse, due to it's low boiling point and corrosive/poisonous nature, there are no good ways to really store it in the home lab either. But, if you need pure ammonia, there is little other choice but to use the following procedure.

Assemble the following glassware or an equivalent in stainless steel:

--------- -----------------
| ----- | | ------------ |
|| || | | ||
/||\ || -- -- 8||
|||| || |xxx| ||
1 -|||| || |xxx| ||
-|||| || |xxx| ||
|||| || |xxx| ||
2 |||| || |xxx| | -------- -
|||| 5|| 6|xxx| --------| | | |
-|||| || |x7x| | | 10| |9
3 -|||| || |xxx| | | | |
|||| || |xxx| | | | |
\||/ || |xxx| | --- |
|| || |xxx| \ /
/\ || |xxx| -- --
--- --- || |xxx| ||
| | || -- -- | ---- ---- |
| 4 | || | | | | 11 | 10|12
| | | ----- | | | | |
| | ---------- | ---------- |
-------- ----------------

(1) is the Supply connection for ice water for the condenser (2) which serves to condense much of the evolved water. (3) is the return line for the cooling water. (4) is the boiling flask where 3% Ammonia solution is placed to boil gently. (5) is glass or teflon tubing. (6) is a glass cylinder or Hempel fractionation column which is packed with (7) Calcium Oxide or Soda Lime to remove remaining water from the ammonia vapor. (8) is teflon tubing to connect the column to the (9) Cold Finger condenser which is charged with (10) a dry ice/acetone slush. (11) is the receiver flask to hold condensed liquid ammonia. (12) is a bowl that contains (10) dry ice/acetone slurry to keep the condensed ammonia in the liquid state.

3% or 28% (if you are *really* lucky to get it) Ammonium Hydroxide solution is placed into a glass container and an equinormal amount of concentrated (31.45% ok) Hydrochloric acid is added to make ammonium chloride. This mixture is then concentrated to about 15% of the original volume by boiling off the excess water (*).

The ammonium chloride/water solution is placed in a flask and chilled to 0°C using an ice/salt bath. An equinormal amount of Sodium Hydroxide solution is then added to convert the ammonium chloride into ammonia and salt. You should add enough water such that the ammonia concentration will be less than 40% (it saturates around 47% at 0°C and allowance must be made for the dissolved salt). Now, the flask contents are gently boiled to liberate ammonia as a gas. The water vapor which comes along is condensed back into the flask and the boiling continues until no more ammonia comes off the cold finger condenser. At this point, the boiling flask can be recharged to continue distillation. The collected ammonia should ideally be used immediately by disconnecting the cold finger from the receiver and performing the reaction requiring liquid ammonia in situ (eg - a Birch Reduction). The collected ammonia will be anhydrous, any water being removed first by the reflux condenser, next by the CaO drier and third by forming ice on contact with the cold finger.

Keep in mind that if you need, say, .5 liter of ammonia, you will have to distill 17 liters of 3% Ammonia solution to get it. This will require a *lot* of dry ice, so get a styrofoam cooler-full ahead of time.

the glassware schematic won't align properly so here is the original link: Eleusis: Preparation of Pure Ammonia

#22 foaf



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Posted 17 July 2007 - 12:06 PM

is this THE foaf


What volume of acid/dwater to you salt with each time, relative to the volume of xylene?

#23 smacked12



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Posted 17 July 2007 - 12:55 PM

normally i salt around 500ml of solvent at a time. well, 596 to be exact. i use that number only because it's the last graduation on my home made sep funnel. i go with a 1 to 5 ratio. so, approx. 120ml of water for 596ml of solvent.

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