Author Topic: "True Blue" NH3/Li reduction ie birch  (Read 11815 times)

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ordinaryguy

  • Guest
"True Blue" NH3/Li reduction ie birch
« on: May 18, 2004, 09:41:00 AM »
This process assumes the reader has some experience regarding a NH3/Li reduction of ephedrine hydrochloride or ephedrine freebase. The quantities of reactants listed are based on 60 grams of clean ephedrine freebase and the presence of any contaminants including waxes or fillers will change the quantity of NH3 and Li needed for the reduction to complete effectively. Please use caution when manipulating the molecular structure of a compound. They enjoy attentive handling. Please read material safety data sheets on all reagents in the processes prior to attepting the process. This basic list of instructions excludes much important data regarding the safe handling of reagents.

A good education is the best safety coordinator.
Please take time to read accordingly.


The BIBLE says in James 3:8 "But no man can tame the tongue. It is an unruly evil, full of deadly poison."

Having all that been said lets get on with it.....

1- add 500ml of NH3 to rxn vessel
2- dissolve 5.5 double a Li strips into NH3 1/4 a piece
   at a time taking approximately 2 minutes per while
   stirring or swirling. 15 minutes later you have a deep
   indigo blue solution with the consistancy of a thin
   soup. If your rxn vessel is not on a ice bath you
   will loose a substantial quantity of NH3 in this
   process.
   Adjust accordingly at the onset of process.
3- slowly, add 250ml of NP
   solvent/ephedrine freebase solution to the rxn
   vessel stirring or swirling the entire time. The NH3
   will displace the NP solvent allowing the Li to
   manipulate the ephedrine reduction directly to
   the freebase molecules. This will hold true as long as
   there is adequate quantities of NH3 present to displace
   the NP. The coolness generated by the NH3
   stabilizes the freebase molecules during the reduction.
4- remove the rxn vessel from the ice bath
5- continue stirring or swirling every 2 minutes for a
   full 15 minutes. This will assure all molecules of the
   freebase have interaction with the Li which is the
   reducing agent.
6- remove top of rxn vessel if fitted and allow
   evaporation of ammonia to begin.
7- Add 250ml of anhydrous NP. Note: if NP is warmer than
   room temperature the evaporation of ammonia will
   accelerate synergistically. Some consider this
   benificial as the reduction has been completed in the
   first 15 minutes and the balance of the time spent
   is waiting for the excess ammonia to evaporate. This
   usually takes about 30-45 minutes but can be done
   quicker via DH20 washing.
8- filter off the reaction fluid being careful not to
   include the solids remaining in the rxn vessel.
9- add 100ml hot NP solvent to rxn vessel and agitate
   for 5 minutes. This should gravitate any freebase
   molecules trapped in the post reduction waste and the
   NP solvent. Let settle 5 minutes then filter again.
10-with a gloved hand placed inside a pantyhose
   stocking, collect the solids from the rxn vessel.
   squeeze these thoroughly through the stocking, above
   the filter into the collected solution until no more
   liquid is released.
   This may contain some freebase oil.
11-add 250ml hot DH2O to the NP/freebase solution. Shake
   violently for several minutes. allow to settle for 10
   minutes. remove the aqueous layer. now add 250ml cold
   DH2O to the NP/freebase solution shaking violently
   again for several minutes and allow to settle for 10
   minutes. remove again the aqueous layer. a third DH2O
   wash will get any residual water soluable contaminants
   such as chlorine or NaOH out of the solution.
12-now you have two choices. either gas or titriate. then
   evaporate or filter and acetone crash and recrystallize.

13-lucky thirteen! 95% pure product at a yield
   of 78% the original mass in weight. 60 grams reduced to
   47 when the a/b was clean and all filtering mediums were
   pre-moistened. swims preferred a/b extraction begins
   with a DH2O soak then taste test filtering prior to NaOH
   push. the NP/freebase solution was then succesively
   washed 3 times with DH2O. the NP/freebase solution was
   then reduced to 25% under very guarded heat(low, low,
   low). the NP/freebase solution(anhydrous) was then
   slowly added to the rxn vessel during the reaction.
   the one drawback is wondering how much product you have
   in the NP/freebase solution.
   swim feels the uncommon yields are due to the minimum
   use of filtering agents and lack of handling the
   crystalline product. this combined with an accurate
   Ph level during the NaOH push is pobabably the
   explaination.

A) the NP/freebase solution was created during a a/b
   extraction of a pill solution that was filtered
   prior to the NaOH push. then three successive DH20
   washes were completed prior to the 25% reduction
   under low heat. this made for a near crystal clear
   solution of NP/freebase stock for the reduction.

B-the whole process took just under an hour. rather than
  wait for the ammonia to evaporate, swim chose to do
  3 successive DH2O washes to remove the ammonia, chlorine
  and NaOH reminants. the Li was spent in the reduction
  process while the NP was retained with the additional
  amount that was added for the final titriation/gassing.
  also it should be noted that the original pills had a
  antihistimine listed under active ingredients. swim
  believes these 2mg per pill were either diminished in the
  rxn environment and released as other by-products or
  account for the 5% impurity.

swim prefers gassing to retrieve HCL needle like crystals
and uses these without acetone crashing or
recrystallization. swim believes these steps to be unnecessary having little or no affect on the final product.

swim also conveyed a therory she has regarding rxn's that are interupted by the addition of DH2O. She theorizes that the DH2O/Li rxn creates an environment that propels and encourages over-reducing. She believes pockets of concentrated Li are accumulated when the DH2O/Li interact creating an environment in which the temperature exceeds a favorable level for the stable reduction of the freebase molecule. The result being small deposits of over-reduced or otherwise damaged molecules. She also stated that the only time she would consider interupting a rxn with DH2O is when there was an excess of Li known to be added to the rxn due to the lack of a scale or having previously failed to identify the required quantity for the rxn to complete. she then would add DH2O because too much Li IS known to cause over-reduction and/or molecular damage. this would result in smaller yields and a less favorable quality. she also has a theory on multi-solvent extractions, alchohol extractions and NP soaks, adding moe contaminants than they remove but we won't go there.

all I know is that swim knows her "True Blue" like a true crystal knows it's proper structure ratio!

the rest can just vaporize..............


weaz1dls

  • Guest
Hey
« Reply #1 on: May 23, 2004, 09:57:00 PM »
I read through this quickly a week or so past and did not notice until this time that the diference is the addition of freebase suspended in NP.  This sadly has been standard in the past.  I do share your excitement and joy for nailing a smooth procedure.  Due to the nature of NH3 and it's availability not many opt to Birch.  SWIW believes it to be fabulous but alas lack of patients and  the existance of close neighbors keeps this dream at bay.  Also keep in mind that quite a few Bee's are having dificulty with pills and your joy may not be welcome company.  Though this procedure may seem in your eyes to be the answer for those Bees, time will tuely be the judge of that.  As most of us are sceptics and believe sucess under any reaction to have it's numbered days until the pill fuckers roll out a new beast.  Again congradulations and if you have any tips for the micro bircher toss me a PM. ;)

WizardX

  • Guest
Ephedrine hydrate
« Reply #2 on: May 24, 2004, 03:35:00 AM »

The quantities of reactants listed are based on 60 grams of clean ephedrine freebase and the presence of any contaminants including waxes or fillers will change the quantity of NH3 and Li needed for the reduction to complete effectively.




The ephedrine freebase MUST BE DRIED before using in a birch reduction as ephedrine forms a hydrate (ephedrine.1/2 H2O). The water on the hydrated ephedrine will react with the Li and diminish the mole ratio of Li.


ordinaryguy

  • Guest
Drying of the ephedrine
« Reply #3 on: May 24, 2004, 08:04:00 AM »
I believe it was mentioned in the original post that the NP/ephedrine freebase solution became anhydrous while reducing the quantity of solvent over low heat. If the solution was not properly "dryed", there may be enough moisture to react in a way that was less than pleasant when it came into contact with the dissolved Li(not to mention changing the rxn ratios a tad) This moisture content is stated to change the ephedrine to a hydrate. That would lead swim to believe that it has become a new compound and that a rxn would be necessary to free the ephedrine of the H2O. I am not a chemist by any means nor is swim. Possibly the addition of a heat source above H2O's boiling point but below the NP's flash point would be in order. If not youv'e got me cuz swim continues to stand by her original post verbatim. Swim is curious as to whether or not you are suggesting that something other than heating need to occur to properly dry the E. Thanks for the response. I appreciate.


ordinaryguy

  • Guest
hey hey
« Reply #4 on: May 24, 2004, 08:18:00 AM »
Hey weaz
Thanks for the thata girl, guy or whatever. I can relate to fellow bee's frustration with extraction inhibitors. I am not sure if swim remebered that these bee's collect honey all over the globe. Sometimes it's easy to assume flying is as easy south of the equator as it is north. Sounds like somebod-bee should post a simple, effective pill extraction technique for the fellow swarmers. Maybe swim has a copy I could post. She is kinda scared of the internet with emails and all required. Personally I don't have anything to hide(other than my stash) I think I'll get a PM to ya sometime in the future. I watched swim perform this rxn on 60 grams in a basement one bedroom apartment without incident. Very confident she is. Not only that but with all the necessary materials needed sold OTC you may just convert with a little coersion. At any rate thanks for the post. I was sure that somebod-bee out there had used suspended freebase before, I was just suprised not to see any posts on it. After all, it does save a substantial amount of excess handling from being required. Any tips on how to create image files so I can send you some good nano pointers?


bigblue

  • Guest
Hey O.G. Swim would like to read some thoughts
« Reply #5 on: May 24, 2004, 01:26:00 PM »
Hey O.G.  Swim would like to read some thoughts on small birch's.  P.m Bigblue as well, or just post it in this topic.  T.I.A

weaz1dls

  • Guest
Pictures
« Reply #6 on: May 24, 2004, 04:23:00 PM »

https://www.the-hive.ws/forum/faq.pl?Cat

=

Also search the server room here st the hive. 8)

ordinaryguy

  • Guest
nano schematic
« Reply #7 on: May 24, 2004, 07:32:00 PM »
Thanks weaz. It's about time somebody saw the value and potential breezy flow of the NH3/Li. I call it this because it really isn't a true birch reduction. A true birch utilizes sodium as a reagent in liu of Li. I do not however recall the actual name, although it has it's own, of the NH3/Li rxn. Keep your eyes peeled in a few days for a few pages of drawings etc that may benifit swiw. It may take me a few days to get this info in a medium that makes any kind of sense at all. Especially in that I am not familiar with the software necessary to get the schematics ready. I'll do my best but I wish I had access to a scanner. Then I could just color a pretty picture and voula...insti map. Also I use the computer in an environment that is within the commons area of the complex where I reside and lots of other tenants seem to slow the process if ya catch my drift. I will not forget you though and If I were you I'd study at Rhodium and search on "The complete Birch" by mister clean. This document has been around for a long time and speaks with lots of hands on experience regarding the rxn as well as generating NH3 on your own from OTC products. Thanks for your patience and understanding. I may have to ask swim to nano a batch of ambition to keep me company.....


ordinaryguy

  • Guest
Thanks for the interest
« Reply #8 on: May 24, 2004, 07:50:00 PM »
Hey Big blue..as with weaz you can keep an eye peeled for a workup in a few days. I'd convert the whole world if I could thus saving me from ingesting those awful post Rp/I crystal imposters. If you have any doubt just look at them under a microscope. A true Methamphetamine crystal has a 3/1 structure ratio as with various other unique characteristics that the imposters don't. A true Rp/I rxn takes well over 48 hours to achieve product even remotely close in uumph and yield. Not to mention that stinky, messy need a home-lab-kit package that comes with it. After all how would swim explain the need for a 1000ml flask, contained heating element, condenser as with the peeling paint and rusted blinds that result. Goooooood luck! He's got Iodine stains on his fingers, Got a silver spoon made of glass, and a grand piano to prop up his mortal remains.... Isn't that a Pink Floyd spin off? Swim would rather play in the stench for an hour,then be done with it, incriminants and all. If done properly one would never even know NH3 was utilized in this process.(at least from a smellers perspective) Then comes "fluff" time or real shards if prefered.


ordinaryguy

  • Guest
T.I.A.
« Reply #9 on: May 24, 2004, 07:53:00 PM »
By the way....Whats this stand for?


jammin

  • Guest
TIA...
« Reply #10 on: May 25, 2004, 05:00:00 AM »
I dont know what lingo you're after, but it does sometimes stand for "Thanks In Advance".

Thats what I use it for anyway.

There might be som chemical abrivation Im not aware of, though...


bigblue

  • Guest
T.I.A
« Reply #11 on: May 25, 2004, 07:24:00 AM »
Jammin is correct on my usage of T.I.A.  Thanks in advance!  Swim is with the OG on the Birch "Like."  Mr.Clean's write up conviced swim of that.  Much shorter reduction.  You can control the smelly.  The li is easily obtainable.  You can make your own juice.  No heat, till gas, then only a small amount.  Dry Ice can control the reduction.   Plus the best part, NH3 and Li don't care  much about binders, gakks, etc..

bigdumbnut

  • Guest
A few anal retentive quesations
« Reply #12 on: May 25, 2004, 09:45:00 PM »
Thanks for the informative process. Being a big dummy I can't fully appreciate something until I understand all the details so I ask the following hopefully without offending
1. Since you use the fb and not in an OH, where does the H come from after cleaving the OH? Not being a chemist I may be confused here but I thought the H from the cleaved OH couldn't be used and that the NP needed to stay intact for extraction
2.How did you determine a purity of 95%?
3. Did I understand correctly that you obtained a yield of 78% final MA HCl from possible E in pills?
4.You mentioned obtaining MA crystals when you gassed. I have only recent gassing experience but I've never obtained crystals. Any suggestions?
5.You mentioned making your E anhydrous by reducing the quantity of NP it was suspended in. What do you use for NP?

Not a question but I beleive the name for this reaction is a "Benkser Reduction" or a "MAS (Metal Ammonia Solution) Reduction"
TIA

ordinaryguy

  • Guest
A response to your polite inquiry
« Reply #13 on: May 27, 2004, 03:17:00 PM »
Thank you for expressing an interest in my original post as well as forwarding the information on the formal names of the rxn. I have yet to research what documentation is available on the "Benkser" or "Mas" but definately appreciate your input!

1. Since you use the fb and not in an OH, where does the H come from after cleaving the OH? Not being a chemist I may be confused here but I thought the H from the cleaved OH couldn't be used and that the NP needed to stay intact for extraction

Having dropped out of high school in the 11th grade(regretably so) and being only recently introduced to "The Hive" as a primary resouce on the subject of chemistry, I believe quite honestly(and humbly) that this question is beyond my current capacity to answer accurately. It's my feeling that your reference to OH would equate Hydroxide.?(OH-) Iv'e personally, nor has swim, ever seen the scientific formulas nor molecular structures modeled for ephedrine or methamphetamine freebase or crystalline forms. Nor do I have a complete understanding of how exactly the molecular changes take place.(although I are facinated by what I have leared so far)I believe there to be a OH branch(is this the correct term) on an ephedrine molecule that gets diminished during the reduction rxn. Also if memory strikes accurate an additional brach is necessary to form a methamphetamine molecule. It appears that your use of the word cleaving is as a transitive verb meaning "the seperation of a structure into distinct groups having divergent views." To me it means put the O's with the O's and the H's with the H's ! The H's I believe become H+ or otherwise known as protons. I believe an H+ is necessary on the additional branch previously mentioned to attain methamphetamine. Sorry if this is long winded but I'm kinda going with myself here. I don't really have any other resource than "The Hive" and I'm obviously tied up in a response message, unable to do research enabling me to answer with conviction. My deepest apologies if this is way off of the facts. I would not deliberately mislead anybody in such a manner. It wouldn't prevent me from doing so with out my knowledge however. So in your question you mentioned being under the impression that the H by-product generated by the cleaving of the OH could not be utilized in the formation of this additional brach. I believe you to be correct.(by memory again) I am unsure of the explaination for why this becomes unusable though. So this would leave the whole equation short a H necessary to complete the structure in forming methamphetamine? If memory again serves, I recall an ephedrine molecule as having a branch of NH2 that gets modified into NH during the reduction rxn. Is it possible that this is where the missing H is generated to complete the branch necessary for the methamphetamine molecule? I bet those wizards at Rhodium would know! We could sure use their expertise and clarity.

The second part of this question was in reference to the NP involved.

At this point in the process, the NP is being utilized as a vehicle to convey the freebase molecules from one container to another. The reduction under low heat should not affect it's properties in a way that would prevent this from occurring successfully. It may, however, change the chemical percentages available within the NP via evaporating some ingredients more than others. In swim's experience, characteristic changes here were unnoticable having no detectable change on the conveyance of the freebase molecules. The addition of NP post rxn was mentioned as a vehicle to facilitate extraction of the freebase methamphetamine molecules.

2.How did you determine a purity of 95%?

The 95% purity figure was determined on two contributing factors. The roughly 47 gram yield was divided into two lots. The extracted NP was roughly split in half.(no formal measurement however the solution was agitated to facilitate equal distribution of the freebase molecules within the solution) One lot was titriated for preferred honey bee's and the balance gassed. The titriated lot yielded 28.33 grams. The gassing yielded 20.02 grams. The total was 48.35 grams. The titriated lot was then recrystallized via natural evaporation.(which takes way too long by the way) The post evaporation crystals were then seperated from a suspect material that was present.(there were distinct color and texture differences) The suspect material was weighed and discarded after a small sample was tested via vaporization. It's weight was 1.35 grams which when discarded brought the yield down to 47 grams. This equated to 5% of the total 28.33 grams. A little hind-site on the 5% assumed to be remaining in the gassed product would bring it's yield down to 19.02 grams for a total yield of 46.002 grams.(assuming the suspect material was equally distributed within the NP solution) We stand corrected. Thank you for identifying this. Also the titriated crystals where the suspect material was not present were vaporized in a very small quantity. It appeared as if only slight oxidation occurred within the glass utencil. So we figured on 5%.

3. Did I understand correctly that you obtained a yield of 78% final MA HCl from possible E in pills?

Yes, you understood correctly however our figures were slightly off due to the above miscalculation. Including the actual figures mentioned above, the actual yield was 76.66% of a return on the invested 60 grams of ephedrine available within the pills utilized. I believe the maximum yield under perfect conditions to be somewhere in the area of 82% due to reduction. It should be noted though that for certain some E was lost in the extraction but that amount remained uncertain. Midway through the E extraction process there was a total of 63 grams available which obviously equated to unclean E. The remaining 50% of the extraction was carried out in solutions. This made it unfeasible to get an accurate figure on what was readily available post cleaning and reduction.

4.You mentioned obtaining MA crystals when you gassed. I have only recent gassing experience but I've never obtained crystals. Any suggestions?

I stand corrected 50% on this issue. Gassed freebase turns into HCL or crystalline. Although it is minute when compared to the titriated/recrystallized product, it is still crystal formations. The only other option would be freebase which is oil. These tiny fluffy crystals form a sort of spun glass looking structure on the filtering medium prior to handling. Under careful observation one will notice needle like characteristics. The comment within the original post was more so referenced to the titriated lot which did fail to get mentioned. I was unaware of the time perameters governing editing of a post.
If in fact you have any experience with gassing, then you have in fact obtained crystals in doing so. They were just tiny.

5.You mentioned making your E anhydrous by reducing the quantity of NP it was suspended in. What do you use for NP?

Swims personal choice for NP is toulene for various reasons. It is substanially less expensive than other solvents, has less impurities, has good evaporation characteristics, is less volitile than some others, is more common as a everyday garage type product, and has such a sweet smell. Also other NP's such as the common camping fuel so many use causes a cotton candy effect rather than crystallization when gassing and is less than desireable.

Thanks again B.D.N for your interest and your questions. I hope I was able to clarify somewhat. I'm not too sure about that first question though. Obviously having these inquiries come from someone as intelligent and polite as yourself eliminated any chance of offense. Please let me know how you do. Many are unaware that titriation is an option to gassing and that they can obtain what many refer to as glass or shards which is a preferred product for marketing. Maybe if they knew they had a choice they would reconsider this process.

P.s-Do yourself a favor and where the proper eye and respratory protection just in case. It may just save your life.

A few notes in closing...

There was a total of 62 grams available in the pills due to the 2 mg per antihistimine.

The extraction process took a full two days and all filtering mediums were flushed with clean solutions to assure maximum product retention.
 
All seperation of fluids were done in lab-grade seperatory funnels and the solutions were allowed to seperate completely prior to dispensing.

All solutions in the process were double checked for missed product.

The amount of Li used in the rxn was tailored specifically for the 2 gram antihistimine addition. The actual quantity required for the reduction of 60 grams is slightly less than that utilized. Any overage of Li would result in over-reducing the product and a decrease in yield and quality.

A glass mesh was positioned above the NP during the low heat reduction to catch any freebase oil that may evaporate(nothing notable collected-it seemed to only slow the already slow evaporation process)

The reduction of NP solvent to 25% of the original quantity would not be necessary if enough NH3 was utilized to displace what was used. This would not slow the rxn significantly as the NH3 evaporates so rapidly. Successive DH2O washes will speed this process.

Iv'e seen this done with relatively similar results approximately eight times. Very impressive.

Iv'e heard of people chucking raw pills into the reaction but am unsure as to how one would accurately equate the required Li to compensate for the non-active ingredients. Not to mention what kind of carcenegenics they may be creating within the product they will be utilizing.


Scottydog

  • Guest
Sounds great but...
« Reply #14 on: May 27, 2004, 08:02:00 PM »
Thanks ordinary for an awesome post! Swim feels this is within his capacity to learn but the problem is with the acquisition of NH3.

He has a friend who got popped stealing NH3 from a huge tank out in the plains. These huge tanks are under surveillance and Swim doesnt believe in stealing.

Swim was checking out posts by Mr Clean and iseebatsdude on the production of NH3 with various ammonia fertilizers that are OTC.

The descriptions although directly spelled out should bee accompanied by pictures.

With Eudragit, the DEA and pharm industry have accomplished the task of limiting the supply of gear on the streets of America.

So don't you bees feel that it is now time to unleash the beast?

The rxn itself is easier then RP, hypo and phosacid.

What we need as a collective is a fully descriptive thread concerning self production of NH3 with PICTURES and captions.

Dwarfer knows the birch and has no shame concerning pics.

Dwarfer?

Aside from Fester's Eudragit cure, NH3 is probably the last straw before settling on racemic product or beeing forced to learn pseudo production via L-PAC?

Someone should unleash the beast and open the flood gates because it is obvious THEY have plans to shut down shop, as we once knew it, regardless.

There is a time and a place for everything, isn't NOW the time?

If not, PM Swim.

Thanks


ordinaryguy

  • Guest
What an excellent post!
« Reply #15 on: May 27, 2004, 09:13:00 PM »
Man! Just gotta dig that enthusiastic post!!$^%&^ Are all of your posts so passionate? Swim gets her NH3 from a daring source that retrieves it from a cooling system in a cold storage facility so she has not too much to offer on NH3 generation. Although the process is relatively simple. It envolves manipulating a base with a more aggressive base which is a minimal rxn! Swim believes the hard part is getting the system to withstand the required amount of pressure without leaking that dasterdly smell. Otherwise the system can be dissasembled into ordinary garage type equipment relatively quickly. The other difficult part would be the time required with focused attention. Mr clean mentioned I believe 8 hours to produce 500ml. Keep in mind, this isn't really that big of investment considering he obtained enough NH3 to reduce 60 Grams of ephedrine freebase. Not a bad return in my eyes. If this could be done in 8 hours then I would imagine one could retro fit the generator with a double rxn chamber thus doubling the production. It would require a bit of Mcgyvering to assure one rxn vessel didn't compete with the other but is very achievable. There are options available to using NH3 to begin with. Keep in mind that the reason the rxn is executed with NH3 is to attain the low temperature required to dissolve the Li. Other than that it plays no role in the actual reduction of the ephedrine molecule. Having this been said, a little bit of leg work on some convicted individuals part, researching the "Benkeser" rxn would identify plenty of alternative cooling reagents that could be either obtained or sythisized as easily as NH3 is extracted from fertilizer. Not only that but the reagents that can be substituted are not as dangerous or as smelly as NH3. NH3 is very dangerous and should never be taken lightly. It can literally steal the H2O from the walls of your lungs leaving you with raisins to breath(or attempt to)-Just figuratively speaking of course. I will be continuing my research on an alternative to NH3 for various reasons. Around here it costs quite a bundle to aquire, and living in the atmosphere swim does generation is just not an option. If swim chose a different site to generate then someone  else would certainly have to aquire knowledge about her activities in the cooler which might not be such a good idea. Too many fingers in the .... you know. Any how the "benkeser" rxn is the correct name for the rxn utilizing NH3/Li and references various other solvents for Li. A little studying need be done but there is definately room for a huge breakthrough here. I hope I beat you to it in spilling the good news amongst the oppressed whom are waiting. Start by doing a body search at "The -Hive" and "Rhodium" on this rxn and go from there. Birch is not the proper name for this rxn. It just has been so commonly misused over the years that it has been deemed an acceptable term. Lets get shit straightened out! Then people can find the information they are searching for instead of some slang missed information. This may be a good thread to post any new information you may discover on this subject. People are beginning to respond. Possibly we can motivate the masses and get the real wizards supporting us on this venture. Thanks again for your enthusiasm. It is quite refreshing and if I was sitting next to you, I'd give you swim's favorite glass toy!


ordinaryguy

  • Guest
the "Benkeser" rxn
« Reply #16 on: May 27, 2004, 09:48:00 PM »
Hey there Biggie, just thought I'd drop you a line and let you know that I discovered the correct spelling of the rxn to be "Benkeser". Not to be critical of your spelling or anything but I figured maybe we could save some fellow "Hivernators" the trouble of searching without success due to one letter. Thanks again for your inquiry and I was wondering if anything I responded on question number one proved to be accurate or not. Also I was wondering if you ever recieved an answer on the proper mole ratio for this rxn using Hcl in liu of freebase. I was looking over your past posts and this seemed to be one that you didn't ever get a straight answer on. TIA for any insite or ridicule you may convey. It's all part of learning in my opinion.


Prepuce

  • Guest
Scotty, SWIP is with you on the timing.
« Reply #17 on: May 27, 2004, 10:50:00 PM »
It's definitely time to explore alternatives, IMHO (SWIM's, that is.) SWIP started to try one of the birch write-ups, and he doesn't recall who the poster was, but it gave instructions on generating NH3 with little or no odorm, using tubing and fittings for an irrigation system. What stopped him from going on with the plan was the painful discovery that the vinyl irrigation parts do not hold up to HI at all. That doesn't mean it would be a problem in a birch, but he decided he wouldn't risk it.

Other than the possibility of a leak, SWIM was wondering if Weaz had thought of venting through a drain pipe, as has so often been discussed wirh regard to RP/I reactions. As long as no huge quantities of NH3 are involved, it would seem to SWIP that the neighbor problem wouldn't be a big one.

Birch sounds like a good shot for many bees. If a really good procedure for generation/containment of the NH3 could be developed there might be a lot more interested bees.

PP

bigdumbnut

  • Guest
Illiterate High Shool Drop Outs
« Reply #18 on: May 28, 2004, 04:12:00 AM »
Just Kidding. I can't remember if I dropped out of school during or after 11th Grade.People will learn what interests them regardless of formal education so long as they don't question their intelligence.
  Sorry about the misspelling. I even rechecked the name (on the Hive of course) while writing that post. I think I'll do better once I learn to use both finger while typing. You seem to be a quick study. You're correct about gassing resulting in crystals Ive just considered it otherwise since I've never seen it in that state that was transparent or tranlucent or dazzling while I have with Titration. The gassing came about with many posts suggesting it superior in the "War on Pill Fuckers" and it does wonders on impatients.
  No offense but I don't think your method of measuring purity is accurate but this from someone who questions any method. When I was a kid everything was supposedly broken down to protons, neutrons, and electrons. I've lost track of how many atomic building blocks there are now, this all falling under the catagory of Quantun Mechanics I believe. The smaller these things become the farther it gets from known physics and closer to mysticism such as "the Dancing Wooly Masters" or Taoism and some highly accredited physicist believe everything brakes down to one common thing(?), a Vibrating String. With this in mind I'm not sure we can quantitatively analize 2 substances and say they are the the same and what they're made of.
  Please excuse my diahrea of the keyboard. I believe it's from recent results to answer (at least to me) this Molarity thing.The best vague answers so far have been:
   1. 2 moles Li / 1 mole pseudo
   2. "  "     " "  " "   pseudo fb = 1 battery /11.2 fb
   3. 3  "     " "  " "   pseudo HCl = " "      / 9.1 HCl
   4. 1 AA batery (.94 gram) / 7 grams pseudo fb -doesn't
      match 1, 2, or 3 and seems like too much excess to
      cover impurities.
Recently I heard of a dream where there was 11.5 grams of what seemed to be clean Pseodoephedrine HCl extracted from white 60's with a ton of crap in them. They were boiled for 10 min (2X)in carb cleaner containing Acetone and Toluene. They were then pulled with 99% isopropal Alcohol 3X with heat allowed to settle somewhat for 1/2 hour and filtered thru 1 coffee filter. Still pretty cloudy but that's OK. Heated to boiling and held there with ice filled cup as cold finger for 1 hour.Right before boiling NaOH (lye)was sprinkled in. As the lye would settle on the bottom after stirring, DH2O was added until most lye dissolved. This can cause a fountain of meat tenderiser all over your body. The ugly on the bottom layer was seperated from the top and discarded. The top layer dryed in Epsom, gassed and recrystalized yeilding 53%.
  Now approximately 300ml of refrigerant grade NH3 with no detectable refrigerant oil (alkylbenzene)was added to a HDPE 2 quart jug nestled in dry ice. Peeled baterries (2)in Camp fuel and the suzy in a container were already in the dry ice getting cold.The suzy was added first and stirred with a rod of UHMW til dissolved (?). About 1/6 of a battry at a time was added till blue stayed for afew seconds the ittybitty pieces until blue stayed a while (10 min this time)Stirred occaisionlly for another 15 min then pulled out of ice put under window with heavy fan flow. Then left the house for 4 hours. 1.2 bateries was used for 11.5 Pseudo HCl which equates to 2.85 moles Li / 1 mole Pseudo HCl. The final yield was not calculated due to too many finger in the pie. It wasn't anything to write home about but the quality iswas beter than I've seen since staying at a lab/ commune in the sixties.
  I know my thoughts here are incomplete and scattered (and forgetabout my spelling)but that's all I'm good for right now

up247365

  • Guest
Homebrew NH3 that works 4 swim---
« Reply #19 on: May 31, 2004, 10:49:00 PM »

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)

Osmium

  • Guest
> Swim has always been taught and know...
« Reply #40 on: June 03, 2004, 03:36:00 PM »
> Swim has always been taught and know first hand that water becomes a
> solid or frozen at 32 degree's or 0 celcius

Seems like you skipped the following science class where the teacher talked about melting points being depressed by stuff being dissolved in water. What do you think is the purpose of antifreeze in your car? And what happens when a little water will be dissolved in a whole lot of NH3?


ordinaryguy

  • Guest
A delayed respose to your questions
« Reply #41 on: June 03, 2004, 08:17:00 PM »
Scottydog,
Swim has never built a NH3 generator out of a bug sprayer. This means it would be irresponsible for swim to advise you in it's safety.(or not) If swim where to build one, swim would use a clean plastic gas can for the rxn chamber like Mr. Clean suggested. The rxn causes pressure to build and swim would not feel very confident that the pressure release on the bug sprayer could withstand it.

If you chose to use NaOH in the drying chamber and utilized glass wool at the entrance to the tubing it would prevent them from plugging.

A water filter is out of the question as NH3 is soluble in H2O. Any generated NH3 would disolve into the H2O instead of condensing. Are you sure the post wasn't refering to filtering the pressure remaining after the NH3 was condensed to filter out the odor?

My suggestion is that you search

https://www.rhodium.ws

for "the complete birch by mr. clean" and read the NH3 generation posts.


Jacked

  • Guest
reply
« Reply #42 on: June 04, 2004, 11:26:00 AM »
I think SD was talking about a water filter with "no water in it".
 H2S04 is used to dry HCl gas would it dry NH3 as well?
 A no brainer? There is nothing in this forum that is a no brainer, or in this thread I might add.


wareami

  • Guest
Suckback
« Reply #43 on: June 04, 2004, 02:52:00 PM »

Something should be done to prevent suck-back if this is utilized.



Ibee learned early on from a Chemistry Book that by simply attaching the tube to an inverted funnel then placing the funnel, basket side down in liquid will help to prevent suckback.


a $2.00 test sure beats the hell out of ending up bling or disfigured



Excuse me, but what's Michael Jackson got to do with this? :o


A no brainer? There is nothing in this forum that is a no brainer, or in this thread I might add.



The Resident Alchemist Deluxe musta forgot about ole Ware stickin his twocents in.....LOL!
Howdy CaveMan!




foxy2

  • Guest
H2S04 is used to dry HCl gas would it dry NH3...
« Reply #44 on: June 06, 2004, 03:47:00 AM »
H2S04 is used to dry HCl gas would it dry NH3 as well?

I wouldn't try that one....


Jacked

  • Guest
reply
« Reply #45 on: June 06, 2004, 05:30:00 AM »
Your right about that one, I don't know what I was thinking about at the time but it wasn't safety, that could be quite a violent adventure. Strike that!


up247365

  • Guest
What works for swim might not work for you
« Reply #46 on: June 07, 2004, 07:19:00 AM »
Every time swim has made his own juice,the only problem he ran in to was the amount of juice needed and the amount produced. Swim can't do a big of rxn's as he would like to but that's it. You can bee as technical and scientific as you want to, no offence, but bottom line is that Swim's way works perfect every time and he has some of the best shit around, maybe not the most, but the best. And he is completely self-sufficient on gathering the ingredients to support his habit and passion.

TURNTABLIST

  • Guest
Anhydrous Ammonia - Freezing Point: -77.7ºC +...
« Reply #47 on: June 09, 2004, 12:24:00 AM »

WizardX

  • Guest
Reaction Tips
« Reply #48 on: June 09, 2004, 10:36:00 PM »
Organic Syntheses, CV 6, 731

2. It is necessary to use a dry ice condenser to shorten the time required to condense the ammonia (4 hours compared with 6 hours without the condenser). The ammonia tank was warmed with an air gun during the distillation. The condenser was removed after the ammonia was collected.
3. It is necessary to use a strong stirring motor since the reaction mixture becomes, temporarily, rather viscous.
4. One should not pour the liquified ammonia directly out of the cylinder since particles of iron compounds might be carried along, catalyzing the formation of sodium amide. For the exclusion of moisture it is also necessary to use a drying tower (potassium hydroxide) between the cylinder and the flask.
5. The sodium should be cut into small particles to increase the speed of dissolution and diminish the danger of stirrer blockage.
6. During this period the reaction mixture might turn white. In this case, another portion of sodium must be added until the solution becomes blue again.


Organic Syntheses, CV 5, 467

3. Only five or six pieces of sodium should be added at one time in order to avoid an almost uncontrollable exothermic reaction. The solution turns blue and then white as the sodium is consumed. When the solution turns white, another portion of sodium may be added. The last 50 g. of sodium may be added without waiting between portions because the reaction is much slower at this point.
4. Because dissolution of the salts is a highly exothermic process, the water should be added slowly. A stream of nitrogen may be passed through the reaction during the addition of the water to ensure that no fire is started by bits of sodium that may be adhering to the upper walls of the flask.


Organic Syntheses, CV 4, 887

5. During the addition of the lithium the solution turns deep blue. After this has occurred (after about one-third of the lithium has been added), the rate of addition can be increased considerably.

TURNTABLIST

  • Guest
Sorry, 28-30% NH3 in Water
« Reply #49 on: June 10, 2004, 11:17:00 PM »
Sorry, 28-30% NH3 in Water freezes @ -77o according to

http://www.usask.ca/chemistry/courses/laboratory/114/msds/ammonium_hydroxide.pdf



And Mr Clean's complete birch says

OOPS: turns out, the freezing point of NH4OH (aqua-ammonia) is 1 degree higher than the freezing point of anhydrous ammonia.




And Anhydrous Ammonia


Freezing point is at -107.9° F (-77.7c); a white crystalline mass forms.


http://www.rmtech.net/Anhydrous%20Ammonia.htm



PRODUCT NAME: Ammonium Hydroxide
CAS NO: 1336-21-6
TRADE NAMES/SYNONYMS: Ammonia Aqueous
FORMULA: NH4OH
FORMULA WEIGHT: 35.05
DOT HAZARD
CLASSIFICATION: Corrosive Material
PIN(UN#,NA#): NA 2672
WHMIS CLASS: Class E
INGREDIENTS: %: 28-30% NH3
TVL: 25 ppm
HAZARD: Corrosive


Ammonium Hydroxide
_________________________________________________________________
PHYSICAL DATA

PHYSICAL STATE: Liquid
VAPOR DENSITY: 0.6 (air=1)
ODOR THRESHOLD: 50 ppm
SPECIFIC GRAVITY: 0.9
FREEZING POINT: -77o


Offline aamer

  • Larvae
  • *
  • Posts: 3
Re: \where is problem
« Reply #50 on: September 16, 2015, 12:11:47 PM »
Swim have five kgs of Ephedra Distachya or Ma-Huang. He extracted alkaloids with two different methods.
 first by Hydro-Diffusion Extraction (also known as percolation) is the newer extraction methods for essential oils..He  fed steam in from the top on to the botanical material in cylinder while in the case of steam distillation, steam is fed from the bottom. When he got the distillate He evaporated it to low bulk after acidifying it by HCL then extracted by toluene then rendered alkaline with lye. After drying he got 100 grams of free base by this method.
Second  with solvent method he added plant material powder in water for two days with good stirring. The mixed extract is filtered and rendered strongly alkaline with sodium carbonate and the mixture again filtered. evaporated to low bulk and The filtrate is saturated with sodium chloride, then alkaloids extracted with toluene he got 100 grams of free base by this method.
.After this he decided for Birch reduction. He carefully collected fb obtained by both methods which is brownish black oily type. Slowly he dried it with low moderate heat under a griller.
 In three necked 5ltr round bottom flask in ice bath with calcium chloride  (super cooling) whilst fitting it into the bucket system. He added NH3 , stirrer ,then added 15 gms of Li metal in and wait 20 minutes for it to dissolve, When Solution turns dark blue he added pre addition 500 ml petroleum ether then he pour freebase gently into the dark solution.
Other 100 gms he put in flask fb first with petroleum ether then poured NH3. Then he poured sodium 45 grams till solution become royal blue.
 After adding water and evaporating NH3 he found brownish black colored residue in the bottom of flask. which is not in the pet ether. In both cases. While a little amount of oil found in solvent. He extracted it and bubbled he got 3 gms of cubic and needle type  small sized crystals. Which is soluble in water but not in alcohol…. He is in hot water. Any one must help him where is the problem. He is sure that plant matter is Ephedra distachya or Ma-Huang

Offline Necrogram

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Re: \
« Reply #51 on: November 16, 2015, 04:16:32 AM »
Is there a simpler route to generating usable NH3 Mister cleans genorator and condenser?
SWIM has not been able to aquire a tank since the late 90's. Since the dawn of the 'SnB and variations of the BIRCH and Benkesser, just starting to dream again has had it's barriers with new gaks.
I am hoping to glean a few more simpler methods.

Thanks Bees!

Also wanting to check out more threads on p2p from Benz aldehyde then to racemic Methamphetamine using sodium borohydrate.