New procedure for hypo rxns!

[SHORTY]

That the temperature in all my rxns never goes above 120C and usually is 110C or lower.  This is measured with a thermometer which is in the flask and not suspended in the solution.  Whether or not this is relevant i don't know.

However, i will try to avoid the formation of these crystals in future rxns as i now beleive they are a indication of overkill.

I might do one more and take pictures to post in this thread though.

[SHORTY]

What do you know, this time none formed and i decided not to force them to.  However, since i had the camera out i went ahead and snapped a couple pics.  The first is taken about 20 minutes into the rxn and the last 2 are the results of the steam distillation.

[Phlegm]

I almost always had these crystals form in my red phos cooks, regardless of temps or run time. In fact, I was happy to see them, as I always associated them with a good cook. In contrast to Geez all of my phosphine fires occurred when using red phosphorous. I have never seen these crystals appear, nor have I ever had a phosphine fire, when using hypophosphorous acid.

This phosphine business is nothing to fuck around with and emphasizes the absolute necessity for a continuous and strong ventilation system in any clandestine lab.

[SHORTY]

I think the writeup is by Mnkyboy78 but not sure.  Heres where he also mentions the crystals in a hypo rxn.

Once a steady bubbling begins, look for white crystals (HI) in the tubing or in the glass tubing connector in the stopper.  If a fog is forming in the vessel, try to keep it going for a few minuets. 

White smoke should have been noticed faintly flowing into the flask.  Large amounts of 'snow' should be pressent on the glass walls. Add a few mls of dH2O down the tubing or reflux condencer to wash the 'snow' down. Return to the heat source. After 20 - 30 min of the smoke flowing into the reaction vessel, disconnect the tubing at the opposite end of the flask and add a few more ml (1 to 2 ml MAX) of dH2O to assist in washing down the new 'snow'. Work the water down into the flask.  You should start seeing more white smoke flowing into the vessel. Apply heat until the fog flow rate into the flask is clearly obvious and fairly constant.

Heres the link:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/hypotale.html

[8ball]

I do hypo cooks as well but very rarely do i get the crystals forming in my condenser, i think maybe i could count the times they occured on the one hand.
I also use SHORTIES method to make my hypo, but by no means am i very particular in the process either, i don't seem to think you have to be. I also read the article SHORTY mentioned in the above post and funnily enough the first time i ever got the crystals was when i first followed the writeup word for word. This was also the method that produced the most as well, in my lab anyway, but i have only followed this method word for word 3 times
(in a row) and not all produced the crystals, only the first and second. I remember thinking at the time doing the third cook why no crystals this time and all i could put it down to was i was using a different batch of hypo i had made.
As i said earlier i'm not very particular in the process of making my hypo, its just a matter of a 1:1 ratio of the salt and 37% hydrochloric acid soaked for an amount of time depending on how soon i want to start(it's never the same amount of time soaking) then evaporating over very low heat(does'nt boil) with a fan blowing across the top until i think theres approx 1/2 off the solution remaining once the salt crystals have been filtered out once the solution has cooled. For instance(at the start i just go on grams of each ingredient) 100gms of salt and 100gms of acid soaked then evaped and then cooled and filtered normally leaving me around 35-40ml of prepared acid, to this amount of acid i will add 1/3 of the amount of distilled giving approx 50ml or a little more of hypo acid.
As i always vary the ratios of hypo,lab grade iodine and pseudo used and the weight of pseudo cooked is never the same i end up occasionally a few ml of hypo short so instead of making more i will just add distilled to make up for it as long as its not too much and i have never noticed any visible difference because of it.
I imagine for some reason SHORTY to be very particular in the whole process of preparing hypo acid this is maybe why he gets crystals forming majority of the time in his condenser because being particular he does it properly(by this i mean adding what is considered to be enough distilled to hold the needed gases with the reaction to cause a change in molecules).
                       
                          OR

could it be the lengh and type of condenser he uses. If he ever used a liebig or graham were these crystals forming then as well?

[SHORTY]

57% Hydriodic acid has a boiling point of 127C.  Since these crystals form at 80C and up then at 100C in my setup, i don't have a fast reflux going.  I mean it is refluxing, but at a rate of about a drop every 10-15 seconds.  Therefore the entire condenser is not wet as the vapors condenses no more than halfway up.  Its above this point that the crystals form.

In my opinion, rp takes longer because it slowly releases hypo into the solution sort of like when you are hooked up to an I.V. in the hospital that is slowly dripping into your bloodstream.  So when using hypo, it is like getting a higher concentrated shot in the ass of the same substance.

[runne]

Would the freebase then need to have any washes for it? Would titration of the base be fine at that point?

[SHORTY]

Drain the bottom water layer out and add toluene.  I then wash the toluene with fresh dh20 then add about a tablespoon of table salt and wash a few more times.  I then add more dh20 and acidify then evap the water for the meth hcl. Finish up with a dual solvent recrystalization with acetone and methanol.

[8ball]

Drain the bottom water layer out and add toluene.

SHORTY have you ever evapped that drained water layer out?
i did the other day and was surprised at the amount of product remaining in water that seems to hold nothing.

[SHORTY]

However, what was left in mine was definetly not meth or if there was meth in there it was not worth the effort.  I figured it was either some type of gaak or from the naoh.  Are you sure it was product?  How did you test it?

What form was it in?

[8ball]

You are right you get all sorts of crap, sediment from Naoh being the majority and a bit of meth and it does'nt look real temping i must admit. But i scraped up what was there after flashing with acetone, let the whole lot dry then added to clean acetone and brought to boil and added isopropyl alcoholtil meth disolved then filtered through a fluted filter which caught all the garbage from the Naoh and whatever else did'nt disolve. I brought this back to boil and let rextalise. After the first rextal approx 24hrs later out of a 22gm reaction i only got 13gms of dry product and a further 0.6gm of product after 2 rextals. That .6 smoked up maybe a tiny little bit dirtier than the first yeild, but hardly noticable(i just tried then)but its worth putting away for a rainy day.

[SHORTY]

Meth fb is an oil and you don't mention adding any hcl to convert the fb to the salt so what did you flash with acetone?  Am i missing something?

[UncleFester]

Unless I am incredibly dense, this LWR is just the standard HI/RP reduction method that has been in SOMM since SOMM 3 (writing date 1992), so why the new interest in this old reliable method? If I missed something please fill me in...
When I tried the method a few times back in the early 90's, I got smoke in the round bottom flask, but none in the condenser. I was running a standard reflux with liquid reaching maybe just beyond where the the water jacket started on the condenser. The results were all pretty good, with one exception where the early attempts at gakking pills wasn't removed. This is a very simple and reliable method if you can get the ingredients. The attention to hypo is quite justified, but the idea there is the same...to get a 50%+ HI solution with some hypo left over to recycle the iodine liberated during the reaction. If I am just plain dense and missing details, please tell me, but what I can't understand is why such an old and reliable method is now the webpage's rage? It is what it is, and it works. The biggest problem one would have is getting clean feed to put into the reaction...one could say that about any method starting with pills now... Fill me in on why this is the new hot topic of conversation??

[SHORTY]

I'll try to answer your question at least how i see it anyways. 

As you know the push/pull or dry type rxns using only a very small amount of water were popular for the last few years.  However, thanks to Osmium, Geezmeister and Wareami the majority of the older beez have switched to the wetter longer by the book reactions as we have found the results are much better with higher quality and higher yeilds.  Since then we have also learned that the short, dry/hot cooks produce alot of impurities some of which cause undesireable side effects and are potential hazardous to ones health.

However, the newbeez prefer the curbshot nano and other hot/dry rxns because they only look at the time.  They don't want to wait 36-48 hours cause they think they can get it in 1-2 hours.  Therefore, those of us who know the benefits of a long wet reflux are continuously promoting this rxn in order to try and save the newbeez from multiple failures.  With the gaaks in todays pills it is nearly impossible for a newbee to get any useful product from the short/dry rxns. 

So basically, what you are seeing on the boards are the fruits of the seeds we sowed.  In otherwords the newbeez are finally listening to the advice given over and over again.

This is how i see it anyway. Make sense?

[UncleFester]

[8ball]

Sorry mate, yes i just brought the water down with acid to ph of 6-7 then evaporated. Flash with acetone. Then once you start to rextal and your iso/ace solution is boiling, pour through filter to catch all the sediment and discard filter. Now you will have a clean solution to rextal x2.

[Hematite]

Fill me in on why this is the new hot topic of conversation??

I am not trying to be a smartass here Fester, but since you asked.......
It is a topic of conversation because that's what goes on here, conversation about currently used methods/chems/pills/etc etc.
Furthermore;

When I tried the method a few times back in the early 90's,

Presicely!  It is March 2004 and all that this date represents to a bee persuing the hypo cook. I must have 100 of these rxns under my belt and I will still read anything written about it because I dare say my work could benefit from some improvement here and there. hehehe.

Somm offers what, one version of a hypo reduction? I cant remember but regardless, until your book covers the large number of rxns and variations that have been covered here collectively, it is illogical to assume that everyone here will be best served by following your one example of this rxn written in '92.

I got smoke in the round bottom flask, but none in the condenser.

good for you!
Over time I've had smoke as well, along with fire, crystal formation that ignited on contact with air or water, crystal formation that did not self ignite, and yet another type that waited until it met something basic before going off.
I've used hypo so concentrated it was probably a breath of air short of being a solid, and I've used home made stuff at unknown concentration, paying close attention to filtering out any salts, and I've used it two minutes after filtering it just the once after having made it and said fuck salt that'll do! I've had it run 4 hours and be done one day, and 12 hours to reduce the same amount another day and blah blah blah, and that's just me! I'm only one of many with opinions and preferences based on personal experience.
In my estimation, until you too have covered all available aspects of varying this rxn in 2004, how the hell can you comment on what is relevant and what is not?
What about those that now need to manufacture their own acid? what about acid concentrations? importance of reduced pressure distillation for complete removal of salts produced during the manufacture? How about at what stage the acid being concentrated will ignite and cause the unsuspecting bee much grief? And how about if your method in SOMM, and shorty's method here just plain don't suit certain people and the particulr set of circumstances under which they have to do their stuff?
Actually you of all people know damn well the benefit of hive discussion, I'm surprised you asked the question at all, but mostly I'm surprised that I wrote this post.
Hi everybody while I'm here!

[SHORTY]

Letting off a little steam there Hematite? 

I have to agree with you on the varying ways of using hypo.  I used to bee so worried about letting the acid be exposed to air while concentrating it and therefore was doing so under a vacuum.  However, one day my ghetto refrigerator compressor vacuum stopped working and i just started heating the acid enough to get visible steam and haven't noticed any change in the hypo.  After learning more about it, it seems that hypo will decompose when exposed to air but the process is very slow. 

The point i am trying to make here is that just like most things in life, making meth with hypo is only as complicated as you want it to be. Actually, the hardest part is getting the pseudo clean enough.