Author Topic: "True Blue" NH3/Li reduction ie birch  (Read 12263 times)

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Scottydog

  • Guest
Excellent!
« Reply #20 on: May 31, 2004, 11:29:00 PM »
Excellent writeup 24/7/365 days a year! ^^^ Should bee rated as excellent! (IMHO)

Thanks also for writing it in language that even Swim could understand.  8)

One question, what diameter smaller hose are you referring to? (1/4")

Just regular clear tubing, does not have to bee braided?

Lastly, where the big hose connects to the smaller one, can a PVC connector (reducer) with stainless steel hose clamps bee used?

Swim imagines, now that the sobee bottle is half full and already cool in the dry ice/acetone, one could theoretically add the freebase/solvent, Li strips and immediately proceed with the rxn described in the 1st post?  :)

Very nice and all inclusive.


ordinaryguy

  • Guest
hey Big Nut
« Reply #21 on: June 01, 2004, 04:06:00 AM »
I was wondering if my response to your original question number 1 made any type of sense at all. I have been trying to understand how this all takes place but believe some books may be in order. Also I thought I'd mention that every time swim does a "benkeser" with hcl of ephedrine instead of freebase using the 3:1 mole for Li the yield and quality seem to be slightly less. I was wondering if this is due to hidden attachments on the hcl molecule that are not present on the freebase molecule or what.? TIA on any advisement. I think swim has made a decision to stick to the freebase reduction as it is simpler requiring less steps. Also I have a tendency to agree with your thinking on the purity statement previously made. There is a possibility that swim included over/under reduce or other molecular structures in the calculations. I am not sure how the feds calculate purity but it should prove interesting. How does one determine if there is any alkylbenzene present or not and are you aware of how this would affect said rxn? Also I though it warranted mentioning that the reduction under low heat of the NP solvent used to convey the freebase ephedrine is not necessary as long as there is adequate NH3 to displace the NP throught the rxn.(just figured most people are like swim and try and conserve NH3)I was wondering about swim's dream as well. It seems there are many easier pill extraction techniques available with very clean product resulting that propel a higher yield. Just kinda struck me as curious why one would process with all these solvents when these other methods suffice equal quality with a  substantially higher yield% ?


ordinaryguy

  • Guest
The quick NH3 generator
« Reply #22 on: June 01, 2004, 04:25:00 AM »
Just thought I'd add a few safety oriented items for all those fellow bee's that may have read the post on how to assemble a quick NH3 generator. First let me say that it is an excellent example of how easy it really is to obtain NH3. All of the necessary items can be bought OTC no questions asked. The long tube up247365 mentioned to vent the smelly could potentially be put into a bucket of DH20 thus absorbing any odor. Something should be done to prevent suck-back if this is utilized. The other thing I thought worth mentioning is that there should be a vessel midway to the revieving container with something to filter the H2O out. H2O in small quantities reacts violently with Li and also would affect the mole ratio for the rxn. Iv'e heard stories of people coming close to being blinded by trying to dissolve Li into NH3 containing small amounts of ice. Please be careful or add a drying chamber.


ordinaryguy

  • Guest
My comment on freebase
« Reply #23 on: June 01, 2004, 04:35:00 AM »
This goes out to Bigdumbnut. In my original post response to your questions I incorrectly stated that "The only other option to hcl is freebase which is oil". Freebase ephedrine can be brought to crytallization via evaporation if so inclined. I meant specific to the method at hand for the previous post being the only other option as oil.(being suspended in a NP)


Organikum

  • Guest
Li does NOT react violently with water, thats...
« Reply #24 on: June 01, 2004, 11:26:00 AM »
Li does NOT react violently with water, thats a myth.
What does not say that a chunk of Li-metal wettened with water will not start to burn after some time - but for sure not immediately or "violently". Na-metal and K-metal react violently with water thats true. Li-metal doesnt. If it would most Birchers would be dead.


Jade

  • Guest
What?
« Reply #25 on: June 01, 2004, 04:31:00 PM »
Okay, Org, what was that bright flame that swim saw a few times immediately after a very small amount of water hit the lithium?  It may not have been violent but it was pretty damn spontanious.

Then, there's that time that the moth fell in the mixing bowl? ::)


Organikum

  • Guest
As told - it is for sure not a bright idea to...
« Reply #26 on: June 01, 2004, 06:10:00 PM »
As told - it is for sure not a bright idea to wetten a chunk of Li. But it is a complete other thing if one drops a chunk of Li in lots of water or in ammonia containing water - there will not much happen.
A small amount of water alone on the Li will heat up the chunk that it will start reacting with the humidity of the air, Li in solvent also wet will be cooled by this solvent in a way that there will be no violent reaction.
This is not true for Na or K of course.

Sorry if there was some misunderstanding.
ORG

PS:

after a very small amount of water hit the lithium


This is not spontaneous. Spontaneous would say without anything hitting it.
Just for the nitpicking.  ;)




ordinaryguy

  • Guest
Li reacting with H20
« Reply #27 on: June 01, 2004, 06:28:00 PM »
Organikum,
In swims experience, when water droplets come into contact with undisolved Li, the Li turns to a molten state that is hot enough to ignite plastic, furnurature, NP solvents and the like not to mention hot enough to cause third degree burns. If you don't believe me, try swims test. Peel a Li AA battery and set it in the sink. Quickly unravel it(making sure not to short) and sprinkle a few drops of H2O on it. I am sure the results of which will change the tone of your statement. Also when this occurs under the cover of NH3(causing a rapid boil in the immediate area) the result is spewing NH3, which by itself can cause blindness and cold burns to the meat. Please, I hope you wear a face shield and elbow length rubbers before trying this, but try just the same and see for your self. The proof is in the pudding. Then maybe you could share the results with readers of this thread and possibly prevent a tragedy instead of purveying carelessness. No offense meant, just forwarding fact.


ordinaryguy

  • Guest
More food for thought
« Reply #28 on: June 01, 2004, 06:43:00 PM »
ORG,

Taking a strip of Li and dropping it in water is not what is meant. Taking a small amount of water droplets and dropping them on the Li is. Also the fact that there is a refrigerant present really only increases the danger in that splashing will occur. Some have seen this when they failed to properly calculate their mole ratios and quench the reaction with H2O. The result, if the Li present is not properly spent, could surely be catagorized as violent. Unless you take the initiative to try swims test and post the results($2.00 for a battery) this swarm of bee's will have no choice but to hypothesize you having a case of hot air. I am posting in an attempt to prevent personal injury from insueing on others while your posts seem to be motivated to do the opposite. It is kind of offensive to say the least. Please, do the test. A word for fellow bee's.... a $2.00 test sure beats the hell out of ending up bling or disfigured. Best to be safe, than the alternative!


micro

  • Guest
Organikum, if you have any doubts as to how...
« Reply #29 on: June 01, 2004, 06:59:00 PM »
Organikum,no disrespect intended but if you have any doubts as to how violently Li acts with h2o simply pull one of those strips out of its casing and roll it up into a ball and then toss it into a glass jar half filled with water and see what happens....In most cases the jar will  shatter and with the quickness........

Jacked

  • Guest
reply
« Reply #30 on: June 01, 2004, 10:26:00 PM »
I don't know if your question was ever answered but it would be 3 moles of Li to 1 using HCl instead of the freebase..
 Nonpolar solvent would be reduced along with the e wouldn't it? Alcohol would be better to chill the freebase in. Swim adds the NH3 to the reaction vessel with the e already sitting there. Na is by far the better choice for this reaction over Li if you can get it but it is a lot more reactive to H2O than Li is. Na will burn and will lightup a non-polar solvent in the presents of water. Not only that Na will only reduce E one step to the molecule we are looking for Li I
think will reduce 3 steps leaving an overreduced product.. I'm not sure if I said that right but you get the idea I hope..


Scottydog

  • Guest
Drying Chamber?
« Reply #31 on: June 02, 2004, 01:32:00 AM »
Swim has never dreamed with this method but has been UTFSE and researching it in depth.

Swim understands the significance of drying the gas. It keeps the NH3 anhydrous and avoids a "potential" fire or splashing hazard when adding Li, but is this drying really necessary?

"Suppose you do nothing to dry your gas, and that for some reason you end up with say 50% water in you condensation chamber.  Well a very significant portion of that water will be solid, whereas the NH3 will be liquid.  So, SWIS has discovered that if you pour off the NH3 into another flask, that the water chunks and salt shit stays behind."

Post 236310 (missing)

(SynapticGap: "Re: Some ??? about generating NH3", Stimulants)


Would decanting the NH3 from the ice chunks keep the gas anhydrous enough to avoid the hazards?


ordinaryguy

  • Guest
answering jacks questions
« Reply #32 on: June 02, 2004, 02:29:00 AM »
I don't know if your question was ever answered but it would be 3 moles of Li to 1 using HCl instead of the freebase..

Yes, thank you. I was aware. I was inquiring to a differnt thread post bigdumbnut created asking this question long ago and was wondering if ever he recieved the correct answer. Of course this mole would be affected by any unwanted adulterants.

Nonpolar solvent would be reduced along with the e wouldn't it?

Never in swims experience has such a magical thing occurred but good imagination!

Not only that Na will only reduce E one step to the molecule we are looking for Li I
think will reduce 3 steps leaving an overreduced product.


Over-reduced ephedrine in the case of an Li reduction is due to too much Li being present. The reduction takes place in a multi part stage sequence to obtain the Meth molecule. In over reduce, the excess Li present causes the reaction to continue on it's return path of where it originated thus bringing the product back to the under-reduced stage of the process. Please reference posts number

Post 396293 (missing)

(Rhodium: "Birch reaction mechanism", Stimulants)
and

Post 396551 (missing)

(Rhodium: "over-reduction", Stimulants)
from the stimulants faq forum digest which illistrates the reduction and explains what stage under-reduce is nested.

As far as the Na reduction, swim is unfamiliar. Searching the various forums should yield a similar illistration for that rxn as well.

Good luck to ya


ordinaryguy

  • Guest
decanting NH3 from the ice chunks
« Reply #33 on: June 02, 2004, 02:36:00 AM »
scottydog,
first of all if there is ice present then there is a good possibility that the product is not anhydrous (no water)
giggle...just fuckin with ya. decanting the NH3 to a seperate container is not going to remove all the water molecules that would be suspended in the NH3. This means that potentially there still is good reason to believe that these suspended molecules would react with the Li and change the mole. It is very simple to add a drying chamber, and well worth the invested time and effort.


Organikum

  • Guest
It wasnt intended to play down the dangers of...
« Reply #34 on: June 02, 2004, 06:01:00 AM »
It wasnt intended to play down the dangers of Li. But there has to be some space left in definitions for the much more reactive compounds like Na. Somebody who believes Li being overly reactive will hurt himself badly as soon he gets a chunk of Na as he believes that Li already played showed him the crown of reactiveness. This is not true.

And also if a glassjar shatters - this names by no way a violent reaction, jars are made for fruits and not for chemical reactions.

Its not on underestimating Li, but on leaving some headspace and to spare the superlatives for compounds they are right placed. The words have a meaning which is defined well. Its not on the definition to be changed but its your wording which has to be changed if you want to call for safety here.

ORG


ordinaryguy

  • Guest
Thanks for the clarification
« Reply #35 on: June 02, 2004, 07:00:00 AM »
My intention in posting safety oriented statements is for the less than experienced bee's whom might attempt to do some hands on learning. I feel it would be irresponsible to exclude these potential hazards and if someone adds a post to the thread containing less than ideal processes, I feel an obligation to identify this to the population at large. Choice of wording is something I believe becomes more accurate with experience. I will make a concious effort to improve in that area. Thank you for your input and anything additional you may have to offer would definately be appreciated.


Jacked

  • Guest
reply
« Reply #36 on: June 02, 2004, 11:36:00 AM »
I was to understand something different about solvents, I think the real birch was reducing alcohols maybe this is what led me to believe solvents would be reduced too. Any how, its been a long time sense I've read anything on birching and sense swim birches now with Na I might add. We were under the impression that a Li birch was quenched after say 20 min or so of reaction time. It would be quenched with H2O in general. Sense Swim always used Na he let it stir out sometimes after an hour he would quench with iron shavings with no noticeable difference in product than if it was quenched after only 30 min. Swim has seen a 70g batch run blue for over one and a half hours before it slowly started whiting out. So If one used the molar ratio with Li he could let the reaction run to completion on its own without quenching and overreducing his product?
 I must be way off in my thinking about pseudo in the birch. I thought if one got back unreacted pseudo from a failed rxn it could not be ran again, failed either by no reduction at all or by over reducing. What I'm picking up from you is that is a wrong assumption.. I guess I need to UTFSE myself..

 Warning to all Na is dangerous in the presence on H20 about 20 times more reactive, A small peace will dance on the surface of water until it catches fire then with a red flame and intense burning it spits and pops at this point.. Li does not react in this manor when contact with H2o, I notice that Li needs O2 present to get to the point of say catching fire, even though I've never seen Li burn it spits and boils violently also puts off a toxic gas that is as bad as the NH3. Under a layer of solvent Li is way more forgiving to the introduction of water than Na, Under a solvent (No O2 present) Na will cause the solvent to flash when H20 is added. Only if there is Na that hasn't been dissolved left.. When Li is dissolved as with Na it does not react the same in the presents of water like it does when its in a solid form. This is from experience and not asumshion so take it to heart.


Scottydog

  • Guest
Okay, No Shortcuts
« Reply #37 on: June 02, 2004, 03:10:00 PM »
Okay, I stand corrected! Obviously one should not take shortcuts and gamble on avoiding potential hazards.

No one should gamble on safety and freedom.  ::)

My apologies to Ordinary, for the many questions. Swim is trying to get "this down to a science"

After reading this related thread:

Post 485647

(TrickEMethod: "30min/$40 - NH3 generator!", Chemicals & Equipment)


The schematics may bee flawed (concerning the production chamber beeing on ice rather then the receiving vessel) but as far as the drying chamber is concerned, would his internal chamber (within the bug sprayer) work if incorporated with up247365's method for NH3 production?

Swim has searched many threads, some saying CaCl used as a drying agent may react with amines, MgSO4 leaves a shitty taste in end product and NaOH often times clogs and obstructs gas flow through the tubing.

One thread mentioned the use of a water filter for a chamber.

Will the internal chamber work as drawn up in the thread above and if not, anybee have any suggestions providing for maximum efficiency?


ordinaryguy

  • Guest
letting the rxn run it's course
« Reply #38 on: June 02, 2004, 03:12:00 PM »
So If one used the molar ratio with Li he could let the reaction run to completion on its own without quenching and overreducing his product?

Awsome deduction! That is precisely why the moles are so important to adhere to. Otherwise somebod-bee would have to make an educated guess at when to quench with H2O which actually forces the remaing Li to be spent in a hurry. If one uses the proper mole for the beginning product they have chosen to utilize(ie freebase/hcl) including variences for any impurities that may be present, then the rxn when run it's natural course would fail to produce under/over reduce or otherwise damaged molecules. Yes. If you used the proper mole, let the reaction expire naturally, you would have d-methylamphedimine without any over/under mixed in. Isn't this the ultimate goal? A no brainer!


up247365

  • Guest
Water in NH3????
« Reply #39 on: June 03, 2004, 02:14:00 PM »
Swim has always been taught and know first hand that water becomes a solid or frozen at 32 degree's or 0 celcius- Just putting water in the dry ice is going to go from water to ice like right now! Trust me, you can go ahead and make a dry chamber or pre-cooler, but it really is not worth it. Chance for more leaks, etc.. Scottydog: the size hosing Swim uses, and reuses it every time, is about 10ft of 3/4 in. braided,run it str8 up about 7ft and then take and reduce it to 1/2 in. clear and make like 4 coils, it's pretty damn hard for moisture to make it up that high and then through that little maze to effect anything, and then  run the 1/2 in. hose back down to the sobe bottle and in the lid of the sobe bottle, have a thick rubber stopper with two holes in it and like 6in. pieces of 7/16 in. hard plactic hose for reducers and the rest of the ventilation hose is the same which goes into a chimney and mixes with smoke from a fire that's burning.  Swim guarantee's this to work. Some of the best anhydrous ammonia Swim has ever used. Very little risk.  8)