(Hive Addict)
03-08-04 17:32
No 493831
(Rated as: good read)
Getting bored with the same procedure I decided to try a different start to my hypo rxns. I found that I could use about half as much hypo as I had been using. Here’s what I did:
Ingredients
15g Pseudoephedrine HCL
9ml Hypophosphorous Acid (approx 50%)
10ml Dh2O
23g Iodine (recycled from previous rxns)
aterials
250ml Erlenmeyer Flask
2’ Air-Cooled Condenser (Made from fluorescent lightbulb)
Electric Hotplate
Balloon
Procedure
The pseudo was put into the flask along with the dh20. The solution was swirled until all the pseudo was dissolved and then the iodine was added and swirled.
The condenser was then attached and hypo was poured into the top in 1ml portions and swirled between each addition.
The balloon was then attached and the flask placed on the hotplate. The temp was slowly increased until the contents began to react. The temp was raised just enough to keep the contents reacting until an internal temp of 110-120C was reached and was left refluxing for about 4 hours.
A large amount of square crystals had formed in the condenser and these were washed down using a syringe filled with dh20. A little over 1ml of dh2o was all that was needed. About 30 minutes later another slightly smaller amount of crystals had formed and these were treated the same as the first. Upon checking an hour later there were again a smaller amount of crystals and these were treated the same way.
After a total of about 8 hours the condenser was removed and the solution was diluted with an equal volume of dh20, based and steam distilled.
The results were as good as it gets for me.
It wasn't Me!
(Chief Bee)
03-08-04 17:35
No 493832
The results were as good as it gets for me.
And that corresponds to what kind of yield?
The Hive - Clandestine Chemists Without Borders
(Hive Addict)
03-08-04 17:45
No 493834
My final results due to not being able to achieve the 90% that many bees claim to obtain. However, since you asked, i just went and weighed the results minus the small amount which was biotested. The yeild was 10.86g.
It wasn't Me!
(Stranger)
03-08-04 18:20
No 493840
Hey,GREAT writeup there SHORTY.
The 9th march 2004 -WILL- be a big part of our incrediBEE HISTORY.
YOU always seem to hit the nail right on the head every time!
The time is right to grab the horse by the reins and go-man-go-man-go-man,GO.HYPO!!!
Thanks SHORTY, there's a collection of literature I have here that YOUR POST is going
on top of.
Hope to see you around the traps, and
ALL-THE-VERY-BEST for sharing your DREAM with the rest of us.
...feeling like i'm outa the hotwater ALREADY!!!
(Chief Bee)
03-08-04 19:16
No 493851
Shorty: Is that 10.86g of freebase oil directly after the steam distillation, or of hydrochloride salt after gassing?
The Hive - Clandestine Chemists Without Borders
(Of Counsel)
03-09-04 08:30
No 493968
You are running a ratio of pseudo:I2:hypo of 1:1.5:0.6 and the hypo is about 50% concentration, diluted to what I guess is about 25% concentration by the addition of the extra water. You run the reaction near the parameters of the phosphorous acid reaction without the phosphorous acid one would add to recycle the I2 to HI. You need heat at this concentration to generate the HI initially. At this heat the recycling of I2 might be done by phosphorous acid created by the oxidation of the hypo acid during the reaction.
I am curious about the PI3 crystals you describe. You are doing a fairly wet reaction with 9 ml of hypo acid and 10 ml of H20. You are refluxing and I assume you are not losing any moisture. There is plenty of water in this reaction. I am used to seeing PI3 formed in dryer reactions and have not seen it myself with wetter reactions, although this could be that the extra moisture keeps washing the PI3 crytsals back into the flask.
I am not familiar with the dynamics of your condenser and the thought comes to mind that the PI3 crystals might be forming in the condenser where not much moisture condenses. This would allow them to accumulate in the condenser. In a dryer rP type reaction these crystals are seen towared the end of a successful reaction. (At least I have never had them appear in an unsuccessful reaction, and they appear during the I have had them appear the reaction is for the most part complete.) That the PI3 is present in quantity sufficient to crystallize in the condenser in this wet of a reaction is a puzzle to me and I am curious what the formation of these crystals says about the conditions of the reaction. I wonder whether their formation may be a result, even if indirect, of most of the reduction having taken place and there being very little intermediate left to reduce to meth? That is well beyond my ability to reason out, and is just a speculation on my part based on the experience of seeing those crystals late in reactions that are high yielding.
You have obviously shown that the amount of hypo needed to produce the HI and to effect the recycling if I2 is smaller than I thought it would be, and have shown that a longer reflux with less hypo acid in the mix will produce results similar to those achieved in a shorter reaction with an excess of the acid present.
Great work! Thanks for the notes. I think I know someone who will try this out very soon.
Geez
mostly harmless
(Hive Addict)
03-09-04 12:26
No 494014
Rhodium, that was the weight of the hcl form.
WizardX's writeup gave me the idea to use less hypo. Actually what i wanted to do was to dissolve all the pseudo in dh20 so that i would know that there was enough water in the rxn to start with. Even with all that water if i didn't swirl the flask as i added the hypo it would immediately begin to react. However, since i make my hypo from sodium hypophosphite, i have no definite way of knowing how strong it is. I estimate it at 50% based on the density which is 1.27g per ml. I also wanted to see what the rxn would bee like if the hypo was added to the iodine and water because i was reading some old chemistry literature which says to add 1 part phosphorous to 10 parts iodine and 4 parts water to make hydriodic acid. Here is what that same literature says about the square crystals:
A number of complicated changes take place during the preparation of this gas, from the reaction of the different substances mixed together and part of the newly formed products.
Small cubical crystals may frequently be seen in the neck of the flask or retort employed; they consist of hydriodic acid and Phosphureted hydrogen, and are rapidly decomposed by water with effervescence, this fluid combining with the hydriodic acid. The hydriodic acid gas is produced by the iodine combining with the hydrogen of a portion of water which is decomposed, the oxygen uniting with the phosphorus.
Heres part of WizardX's writeup about having an excess of hypo:
HYPOPHOSPHOROUS TO HI CALCULATIONS
H3PO2 + H2O + I2 ==>> H3PO3 + 2HI
Hypophosphorous 50% w/w. F.W = 66 g/mol. Density = 1.274 g/ml.
100mls (0.1Lt) of Hypophosphorous 50% w/w contains :
(1.274 / 50)/100 = 0.637 g/ml H3PO2 = 0.00965 mol/ml H3PO2.
0.00965 mol/ml H3PO2 x 100 = 0.965 mol/100ml H3PO2.
OR
(0.637/66) x 1000 = 9.65 moles H3PO2 per 1000 mls. (mol/Lt)
Since we use 100mls (0.1Lt), then 9.65 x 0.1 = 0.965 mol/100ml H3PO2.
Now since the ratio of Ephedrine : HI is 1:3 = (3/1), we require 0.75 moles of HI for every 0.25 moles of ephedrine hydrochloride.
Since we have 0.965 mol of H3PO2 and 0.39 moles of I2 (99/253.8 = 0.39), then the ratio of I2 : HI is 1: 2 = (2/1); so 0.39 moles of I2 reacts with the Hypophosphorous acid to form 0.39 x 2 = 0.78 moles of HI.
Finally, the excess Hypophosphorous acid, H3PO2 is 0.965-0.39 = 0.575 moles of H3PO2 is excess. The ratio for H3PO2 : I2 is 1:1, so only 0.39 moles of H3PO2 is needed to react with 0.39 moles of I2 to form 0.78 moles of HI.
Not only do we have enough HI; 0.78 moles to reduce 0.25 moles of ephedrine hydrochloride, but a large excess of 0.575 moles of H3PO2.
It wasn't Me!
(Chief Bee)
03-09-04 13:57
No 494033
they consist of hydriodic acid and Phosphureted hydrogen
Ah, that's very interesting! It means that the crystals aren't PI3 at all, but rather the hydriodic acid salt of phosphine:
HI(g) + PH3(g) -> PH4+I-(s)
The Hive - Clandestine Chemists Without Borders
(Of Counsel)
03-09-04 14:40
No 494045
And what does that tell us about the reaction? Anything?
mostly harmless
(Chief Bee)
03-10-04 07:35
No 494213
Well, that the crystals should be scraped back into the reaction container, as it is one of the most strongly reducing species formed in the reaction: Post 443818 (ragnaroekk: "Reference on HI reductions", Stimulants)
Maybe it wouldn't sublime and rather stay in solution if more solvent was used (acetic acid, or perhaps water).
Also, after the reaction one should be careful when basifying, as PH4I turns into phosphine gas under basic conditions.
The Hive - Clandestine Chemists Without Borders
(Hive Addict)
03-10-04 09:27
No 494222
I just poke the needle through the balloon and knock them down into the flask by squirting water on them. When they hit the solution they react immediately. Sort of like when water is dropped on a hot skillet. A white smoke fills the flask and condenser for a few minutes and then they start to slowly form again.
Should i be using even more water?
Does the formation of these crystals indicate that the solution is holding all the HI it possibly can hold and therefore the excess forms on the sides of the condenser?
Or does this mean that the pseudo has all been reduced and the rxn is complete?
It wasn't Me!
(Chief Bee)
03-10-04 14:13
No 494257
Does the formation of these crystals indicate that the solution is holding all the HI it possibly can hold and therefore the excess forms on the sides of the condenser? Should i be using even more water?
Could be, it's hard to tell if the formation of these crystals are due to oversaturation of HI in the solution, or if this is something which invariably will happen regardless of solvent volume, without performing some experiments.
I believe it would be very interesting to see if you by increasing the amount of water (or by the addition of some GAA) can minimize the formation of phosphonium iodide crystals, while at the same time keeping yields the same or better. Please do that, and report back the results. Try to keep the workup identical to this reaction, as to minimize interfering variables.
Or does this mean that the pseudo has all been reduced and the rxn is complete?
Nope, not at all.
The Hive - Clandestine Chemists Without Borders
(Hive Addict)
03-10-04 20:48
No 494311
Actually, i have been using the formation of these crystals as an indicator for quite some time. If they didn't form i would add more iodine until they did and when they did form i would wash them down until they no longer formed. So yes, more water will prevent them from forming. As far as GAA is concerned i have never tried it. I have had a few rxns that never formed the cyrstals and didn't notice any difference in quality nor yeild. I have also had some unsuccessful rxns when the crystals did form. In my opinion phosphorous is just a very unpredictable substance as it continues to dissappoint, frustrate, confuse and amaze me.
So do i want to prevent them from forming?
It wasn't Me!
(Hive Addict)
03-10-04 21:08
No 494314
Going on at the Reef...eh SWIMS?
Not too sure about the relevance here but from all observations in the past since doing the LWR, that HI formed and/or created in rxn seemed to do the best reducing when directly in contact with AWE the precursors at the bottom of pool!
This is why Ibee incorpirates the "Checkpoint" walk the plank style knockdowns with the bambouy stick at every
hours.The same white cloud syndrome can be witnessed as everything re-enters the pool as most of the solids collected on the sides are teeming with the h2o that condenses and drips back down! A little prodding by Capt Hooked never hertz...
Shorty's suggestion about the ACCU-puncture technique seems better than a complete opening to prevent gas escaping.
Provided that one can position and aim the squirting to push everything back in the pool!
OHHH YEAH....and provided it doesn't require an excess of h2o to get it AWE back down therebye diluting the reaction to the point of stalling.
a little less conversation, a little more reaction
(Of Counsel)
03-11-04 08:57
No 494420
I know Ware refluxes with less water than I use in my rP reactions. I use less red Phos than he uses. I don't see these crystals, but have near complete reduction in my long wet rP refluxes. More water, less phos, no crystals.
Then Shorty describes a wet hypo cook-- wetter than I am accustomed to running hypo cooks-- with the same ratio of I2 in the reaction. He runs at temperatures I have run the reaction, so I doubt temp is the factor. He gets these crystals toward the end of his reaction. They dissolve in additional water. I have never had them in a hypo cook, but its been a long time since I refluxed a hypo cook for six to eight hours.
I recall having my nasty introductions to phosphine fires when I refluxed for longer times at higher temps; I was using more concentrated hypo solutions than Shorty.
Could these crystals be related to the production of phosphine gas in the reaction, and be a sign that we have created the conditions in the flask to produce it? Or is it perhaps the production of these crystals which could lead to the formation of phosphine gas?
mostly harmless
(Chief Bee)
03-11-04 11:13
No 494444
Could these crystals be related to the production of phosphine gas in the reaction, and be a sign that we have created the conditions in the flask to produce it?
Definitely. They are the result of gaseous phosphine and gaseous hydrogen iodide being present in the flask airspace, and upon contact with the cooler parts they condense into a solid salt.
It's very similar to CTH reductions using ammonium formate as the reducing agent, in which gaseous ammonia and gaseous carbon dioxide is evolved and combine in the condenser to give ammonium carbonate.
Or is it perhaps the production of these crystals which could lead to the formation of phosphine gas?
Chicken or egg?
In this case the phosphine gas was definitely there first, as only gaseous phosphine can evaporate like that.
The Hive - Clandestine Chemists Without Borders
(Of Counsel)
03-11-04 14:21
No 494480
I have understood that phosphine gas production in HI reactions was related to the temperature of the reaction, and that at certain threshold temperatures, phosphine gas could be produced. I seem to recall that temperature as being about 142C, but whether that figure or the source of the information is accurate I do not know. Part of that information was from Law Enforcement information about meth production, which is notoriously misleading and inaccurate.
In my experience, however, phosphine gas was produced in hypo reactions at higher temperatures, during refluxes, and not produced at lower temperatures with the same concentration of hypophosphorous acid. The crystals are seen in dryer, and in hotter, rP reactions than the ones I do. I work at lower temperatures and with more water with rP, and tend to work with higher concentrations of hypo acid but at lower temperatures than Shorty does.
I understand phosphine gas is toxic, and would think that its production should be avoided if possible. It does not appear to be necessary to the reduction process, as both the rP LWR and the lower temp hypo cooks seem to avoid its production. Might this indicate that performing these reactions at lower temperatures than those that seem to produce these crystals is a good idea from a health standpoint, at least for the clandestine chemist?
Does the formation of these crystals in a reaction suggest the temperature of the reaction should be reduced for safety's sake?
mostly harmless
(Chief Bee)
03-11-04 16:46
No 494509
Might this indicate that performing these reactions at lower temperatures than those that seem to produce these crystals is a good idea from a health standpoint, at least for the clandestine chemist?
Does the formation of these crystals in a reaction suggest the temperature of the reaction should be reduced for safety's sake?
Yes on both accounts, at least in my opinion. Any potential reducing agent crystallizing in the condenser won't do much good for the reaction either.
The Hive - Clandestine Chemists Without Borders
(Hive Addict)
03-11-04 16:51
No 494510
Geez: Ibee's best guesses tell him that phosphine gas is a normal result of marrying I2 and RP or Hypo/h3po3/hp3o4...etc.
In AWE The Kidz Daze since becoming Bees, they have never witnessed the xtal formation phenomenon during rxn...
They felt cheated at first and wondered what they might be doing wrong as everybody elses reports of their presence on the flask neck or inside the condensor coinsided with success reports!
The fact that we reflux with adaquate h2o present throughout the LWR doesn't necessarily mean that phosphine isn't present or wasn't created.
It means we can't see iphosphine in the solid salt form because the dryer conditions don't exist for those of us using ample h2o.
I should have been more explicit too on when Ibee reported seeing the white clouds at checkpoints.
They aren't witnessed at every checkpoint. Just toward the very end of the reaction when knocking down what creeped up on the glass. Little wisps of smoke can be seen and Ibee associated that with condensed h2o trapped in reactants or maybe it's HI trapped and the h2o present at the bottom is what kicks the smoke UP!?#
Isn't that white smoke created by the reaction of h2o and HI when dh2o comes in contact with HI?
It's almost always present when adding h2o to the end rxn work-up!
Now as to whether or not excess phosphine gas gets created by conditions such as high heat Ibee doesn't know.
It's possible and that may be what translates into excess impurity associated with SpaceCopter Dope!
Most of the bees early references to neckxtals seem to have had a common theme...hot dry/fast P/P types.
If there is a way to reduce the amount of phosphine created, if indeed it is a bad thing and serves no purpose in the reduction whatsoever, I'd hope that an easy solution could be adopted and incorporated into the LWR for health's sake!
Bee it a shift in time, temp, or ratio or the reactants!
a little less conversation, a little more reaction
(Hive Addict)
03-11-04 17:02
No 494511
Rhodium: I think that some clarification on specific temp might help some if you could suggest...
Bees that follow the LWR do so under the guidance provided to the best of all our knowledge and experience with the LWR.
It doesn't make allowance for temps exceeding 120°C internal temp. Anything above that temp Ibee doesn't consider a LWR.
Now these are observations basted
on health aspects.So.....if I understand correctly, what is being considered here is a further decrease in temp...
From the 120°C to...............????
Any suggestions as a baseline temp considering AWE tha's been discussed here?
a little less conversation, a little more reaction
(Hive Addict)
03-11-04 19:28
No 494546
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.
It wasn't Me!
(Hive Addict)
03-12-04 19:45
No 494774
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.
It wasn't Me!
(Newbee)
03-12-04 20:53
No 494787
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.
(Hive Addict)
03-12-04 22:32
No 494797
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:
../rhodium
/hypotal
It wasn't Me!
(Hive Bee)
03-13-04 09:09
No 494856
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?
I'm not racist,
I hate everyone.
(Hive Addict)
03-13-04 16:41
No 494927
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.
It wasn't Me!
(Hive Bee)
03-13-04 17:31
No 494934
Would the freebase then need to have any washes for it? Would titration of the base be fine at that point?
(Hive Addict)
03-13-04 18:54
No 494952
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.
It wasn't Me!
(Hive Bee)
03-14-04 05:14
No 495027
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.
I'm not racist,
I hate everyone.
(Hive Addict)
03-14-04 06:12
No 495035
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?
It wasn't Me!
(Hive Bee)
03-14-04 20:46
No 495194
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.
I'm not racist,
I hate everyone.
(Hive Addict)
03-15-04 13:45
No 495354
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?
It wasn't Me!
(Popular Author)
03-15-04 18:20
No 495399
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??
(Hive Addict)
03-15-04 19:23
No 495405
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?
It wasn't Me!
03-15-04 20:25
(Rated as: insignificant)
(Hive Bee)
03-16-04 10:23
No 495526
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.
I'm not racist,
I hate everyone.
(Individual)
03-21-04 03:35
No 496428
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!
Regards, Hematite.
(Hive Addict)
03-21-04 12:30
No 496497
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.
It wasn't Me!