SHORTY (Hive Addict)
12-30-03 14:17
No 479838
      Is the minimum temp 120C?     

I noticed when reading this document ../rhodium /hi-rp.mechanism.html on Rhodiums site the following sentence.

Actually, hydriodic acid dissociates by a reversible reaction at high temperature (120°C) to iodine and hydrogen which is the reducing reagent.

Does this mean that the minimum temperature in the HI synthesis's is 120C?

It wasn't Me!
 
 
 
 
    WizardX
(Wizard Master)
12-30-03 16:32
No 479861
      Azeotropic B.P     


57% HI SOLUTION (HYDRIODIC ACID) : B.p 125.5-126.5 deg C/760mm Hg ;Density 1.70 gr/ml ;  55-57%  w/w HI is 0.936 to 0.99  grams of HI per ml.




Minimum temperature in the HI synthesis is B.P 125.5-126.5 deg C/760mm Hg

 
 
 
 
    SHORTY
(Hive Addict)
12-30-03 22:19
No 479920
      Thanks Wizardx,     

But how is it that many bees claim to keep the temp at 100C with good results.  Does a longer rxn time compensate for the lower temp?

I have always assumed that a longer rxn could bee carried out at a lower temperature.  However, that sentence, gives me the impression that unless the temp reaches 120C then the HI is not being used to its potential.

It wasn't Me!
 
 
 
 
    Rhodium
(Chief Bee)
12-30-03 22:24
No 479923
      time vs. temp     

Does a longer rxn time compensate for the lower temp?

Yes, to a certain extent, but likely not fully.

However, that sentence, gives me the impression that unless the temp reaches 120C then the HI is not being used to its potential.

That is definitely included in my belief system too.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    geezmeister
(Of Counsel)
12-31-03 00:30
No 479948
      Think of it like Congress
(Rated as: excellent)
    

There are some things we may prefer not operate at their full potential. Congress comes to mind right away. Local law enforcement is another institution I have no interest in being operated at its full potential. The Jehovah's Witnesses, Al Sharpton, and George Bush are a few thing I hope never operate up to potential. A friend's car is capable of speeds in excess of 150 mph. He best not operate the vehicle to its full potential, because he had too few points left on his license right now. HI might be another thing that really needn't be used at its maximum potential.

I'm only half joking, and I know none of the analogies are chemistry analogies.

I noticed long ago there was direct correlation between hot cooks and tweaky dope. I learned later that part of tweak is the result of the dry-hot-fast start. Not all of it. Most of the more notorious by-product side effects-- the real tweaker stuff--is produced in hot cooks. Black helicopters, shooting sparks, faces in the woods, voices in the air ducts, people talking outside the fourth floor windows... all seem tied to hot cooks. How hot is hot? Hot is hotter than 120C. Even at 120, some tweaker characteristics start showing up.

At one point, I noted the temperature of the reactions I did to determine the effect of temperature on tweaker characteristics. As them temps went down in my admittedly drier and shorter push-pull type cooks, the tweaker effects dropped out. Sparks disappeared first, helicopters next, then the faces in the woods and general paranoia disappeared (at least until sleep deprivation supplied the effects.) The voices and shadow peeps all took leave of my dope in the range under 120C. Around 120C or a little above, the product would have tweaky effects. Below the 120 mark, there were fewer such problems, and the problems disappeared as the temperature fell to the 100C range. Doing a number of six hour cooks that were still too dry, I concluded that quality meth could be produced in reactions done below 100C which would not have the tweaker characteristics. I learned that if I increased the temperature to the 110-115C range, the tweaky effects began recurring, and any temperature higher than 120 seemed to guarantee such effects. 

I finally listened to reason and did a wet reflux, then a long wet reflux, then did one with no noticeable activity to start, no real show or smoke or drama. Just a wet reflux for 36 hours or 48 hours, at an easy, just below 100C temperature. The product of such a reaction done with clean pseudoephedrine is superb. The product lacks any adverse tweaker characteristics. It can produced consistently at this quality without difficulty and without a great deal of experience. Low temperature is one key to the quality and absence of unwanted side effects.

I have not duplicated the side effect experiments doing the long wet reflux, as I frankly have had no reason to repeat them. A 100C temperature produces meth that is as good as it gets with the red phosphorous method.

I started doing hypo synths, and learned quickly to keep the temperature low for that synth. I did not reflux for several hours while doing those, but concentrated the hypo and did a slash and burn fast reduction that was remarkably complete compared to my red phos reactions at the time. I never did the hypo synth as high as 120C without having a phosphine fire at some point.

When I started doing the phosphorous acid synth, I was using a deep fat fryer that would not bring the temperature in the flask to 120C at it hottest setting. The maximum temperature I could attain was 115C. Yet the product was unmistakably excellent. I noticed, however, that even with a longer reflux, temperatures lower than 110C did not give me the quality of product that I obtained at 115, and finally 120C. I changed heat sources and refluxed the phos acid reaction twelve hours at 120C; I was delighted with the results. I had very good product and an excellent yield. My most recent phosphorous acid reaction was done with with very well cleaned freebase pseudo at the higher temperature range, measured by the hot plate settings and the observed activity in the flask. I did not set a thermometer up to test, as I have-- once again-- broken all of them. The last reaction yielded meth that was as good as any I have produced in the last year. No tweak. Solid meth. Clean, smooth, and effective.

I am of the opinion that the phosphorous acid synth does its best work in the 120C range. I am not so inclined with the hypo synth, but my opinions there are tied to instances of phosphine fires. As to the red phosphorous method, at least for the long wet reflux done with actually clean pseudo, I believe that a 120C temp might be an optimal temp. I also believe that unless the pseudo is very clean (and I am of the opinion that very few cooks actually have very clean pseudo) a red phos cook done above 110-115C is an invitation to tweaker dope. Make the red phos reaction a drier push-pull reaction, and 120C guarantees tweaky characteristics. At least in my experience.

Maybe the fact that the typical clandestine meth cook is done with less that perfect precursors under less than optimal conditions mitigates against pushing the temperature of the red phos reaction to the optimal range. This observation could be a misunderstanding of what I have observed over time doing these synths. I belive the tweaky street dope is like that partially because the feedstock pseudo is not as clean as the cook thinks. The balance of the tweaker characteristics are, in my opinon, realted to the temperature of the cook. The STE, STB, and Tetra trap methods, as well as the EGull and derivatives, do not routinely yield completely clean pseudo feedstock. There has to be some workup beyond the base techniques with most OTC pseudo sources.  The pseudo obtained by faster extraction methods will react pretty well, but will usually contain something in addition to pseudo. Few street cooks clean the pseudo to an actually clean state. I know a number of bees who have never really gotten pseudo all the way clean, and who would likely not recognize really clean pseudo when they saw it. The pseudo's purity must be considered when you mull running the HI reaction at its maximum potential.

If you admit that most of the synths, and in particular the red phosphorous synths, are done in less than ideal conditions with less-than-pure precursors, cranking the heat up to 120C to optimize the HI may very well do nothing of benefit to the product made by these cooks. It may be better to back off ten or fifteen or twenty degrees, take more time, and be patient. I for one will likely continue to do red phosphorous reactions under the 120C mark, and will do the phosphorous acid cooks at the 120C mark. I do that based on my experience doing these synths, and evaluating the product produced.

It could easily be true that the clandestine cook does not really want to do this reaction at its optimum potential. That may be one of those things that we don't realy want to work to to its potential in real world conditions. The idea that there is a temperature at which the reaction will work best or at its highest potential does not necessarily mean that the clandestine cook, or his product, would be advised to crank the heat up to that temperature.

Then again I could be completely wrong. It would not be the first time, by any stretch of my imagination.

mostly harmless
 
 
 
 
    SHORTY
(Hive Addict)
12-31-03 01:33
No 479954
      Good answer geez,     

The reason i brought this up is that recently I have been getting not so good results and after many hours of checking this and that and for a while i blamed it on the homemade hypo.

During this testing time i was under the impression that i was keeping the temp of the rxn at around 120C.  However, i didn't measure the temp due to not having a thermometer due to similar episodes to geez and his thermometers.

I tried increasing the rxn times but always kept the hotplate on or below the number that i had previously measured as being 120C. 

Anyways after much hair pulling i finally remembered to pick up a new thermometer while at the chem supply.  What i found was that i had been cooking at about 100C all this time.  I just finished a 13g cook which i kept between 120C -130C for 12 hours and i am now feeling what i have been after for what seems like a lifetime.

After reading geez's reply, i now think that i when i make the hypo and evaporate the water off, a good portion of my hypo is oxidizing to phosphorous acid which is most likely the reason for needing higher temps than those geez used in his hypo rxns.  I also try to get my hypo to about 50% whereas geez would concentrate his to 85%+. 

Nevertheless, i finally found the answer to my problem and will make sure to have a working thermometer from now on.

It wasn't Me!
 
 
 
 
    wareami
(Hive Addict)
12-31-03 04:40
No 479968
      Time and Temp     

>I have not duplicated the experiments with temperature variations with the long wet reflux.

Ibee has!
Back before the LWR really took hold as a viable alternative to the more popular Hot/Fast P/P, Ibeeware did many tests in his quest for thesholds and absolutes.
It was easy to discern some of the differences in quality and the relationships associated to time/temp/hydration during bio-assay.
However, the lack of formal chemistry knowledge presented some pitfalls that demanded recreating unpleasant samples to arrive at consistant data and their possible causes.

We know that the aziderines(iodosides?) and impurities created during Hot/Fast rxn are many and from what I gather now, it's becoming more clear that most are likely created by that dissociation described above.
When one looks at the principal behind what's described as taking place, high temperature (120°C) to iodine and hydrogen, it conjurs UP some pretty vivid images and finally a smidgen of understanding.
At least for me.
Not having the mental aptitude to play out rxns in my mind, prevents me from further expounding on the intricacies in depth.
But We do know that HI recycles and I've seen diagrams of what is suppose to take place in the creation of hydriotic acid.
The above quoted statement is true but it would also be influenced by the Dissociation constant that would be effected by variables introduced.
Those variables seem to bee the topics of the most debate as of late regarding the two main factors, hydration and temperature. Well, three actually when time is factored in.
It's also a well known fact that higher temps applied to the rxn will bring it to completion sooner.
This fact supports the findings in the above quoted statement. But that statement by itself leaves out the important factors that influence the product produced and the amount of impurities imparted above that 120°C temp.
Therefore it still stands to reason that a controlled longer rxn utilizing a less harsh/reactive reducing agent (inder it's full potential) is gentler on the end result.
I still like Rhodiums analogy about the turkey in the oven at 500°F for an hour compared to the turkey in the oven for 3 hours at 350°F.
Which would you eat?
Not only that but lets go a step further because some think this way without considering the bigger picture(I know I did...)
As opposed to cooking the bird at that time/temp rule above, let's factor in the other variables:
Temp + Time per pound(rxn size)
Stuffed(gaaked) or UnStuffed(pristeenclean)
Okay...I'd apologize for rambling but the turkey needed to get all that off his chestlaugh

Either I'm halucinating or Geez editted his reply since I read it first and started this one!wink
Either way we both agree that the LWR produces superior end result!
How and why is left UP to the scientific minds to discern!

Peace of the RXN
Have FUN-Bee SAFE
 
 
 
 
    CharlieBigpotato
(goat)
12-31-03 05:54
No 479979
      question for geez     

hey, bud?

may i ask where you take the temp?
in the bath?
in the flask?
have you tested the thermometer against a known (i.e., boiling water)?

just curious about this strange data

zib
 
 
 
 
    geezmeister
(Of Counsel)
12-31-03 09:51
No 480018
      temps     

Temps were in the flask. Thermometers were considered as accurate. (By golly, water boiled right at 100C on most all of them.)

I do not suggest that my measurements are perfect, nor my memory as good as I like to think, and admit that I break thermometers with the deft skill of the inherently clumsy.

mostly harmless
 
 
 
 
    fierceness
(Hive Addict)
01-03-04 10:10
No 480262
      SWIF can attest to this being true also.     

SWIF can attest to this being true also.  When he was a newbee, he started a reaction and set it on too high, making it reflux  too quickly.  Long story short, there was a volcanic eruption of HI from the flask.  So the next time, he made it only slightly refluxing (~100C).  After 14h, no substantial product at ALL -- All he got was pseudo/ephedrine back.
 
 
 
 
    barkingburro
(Hive Bee)
01-03-04 11:20
No 480273
      all swibb can attest to is h3po3     

swibb can cooberate geez's observations as well. in his experience an hp3o3 rxn is definately something that needs the higher heats. swibb has run the rxn as high as 130C or so for 3 hours in reflux with good yield results (though he did notice a twinge of the creepies) and conversly has run a similarly sized batch at 100C for 8 hours in reflux an came back with half assed dope. swibb DID however notice a pretty marked difference in quality when he drove the rxn to 130C then dropped the temp down to 100C for reflux, and also xerimened with bouncing the temp between 100C and 130C at regular (45min) intervals. both of those rxns had better results than the rxn where the temp was kept at 100C, but all three rxn's that involved reflux at 100C were of lower quality overall tha the rxn that sustained 130C.

as a side note the bouncing temp rxn was also used in an additional experiment for running a sealed rxn. this yielded even better results than all other rxns tested and in 2/3 the time, but sealed rxns gave swibb hell in he form of flying shards of pyrex so he has pretty much abandoned the sealed reaction route.

also, one thing that swibb forgot to mention, at the higher temp swibb started using boiling stones (swibb knows that other hav mentioned using peces of glass etc). at first swibb tried using a small glass marble as a boiling stone, ut the problem with that is that glass makes a horrible boiling stone. it is too smooth. the only reason that broken glass works at all is because of the rough broken edges. swib made his boiling stones from sall glass marbles that he then ground using a carbide tile cuttig tip and his trusty dremel. it is iimportant to grind all smooth area on the marble. now every rxn that swibb does he adds atleast 2 stones (no more tha 2 needed until you get in the 224g p/fed range). the use of these stones has increased the speed of swibb's rxn's dramatically and yield has even gone up slightly. for explanation of the reasoning is from the organic chem lab survival manual by james w. zubrick
A close up comparison between a boiling stone and the inner wals of a typical glass vessel reveals tousads of tiny nucleating points on the stone where vaporation can take place, in contrast to e smooth glass surface that can hide unsightly hot spots and lead to bumping, a massive instantaneous vaporation that will throw your product all over.
 
 
 
 
    WizardX
(Wizard Master)
01-04-04 02:47
No 480353
      Super heating     


When he was a newbee, he started a reaction and set it on too high, making it reflux  too quickly.  Long story short, there was a volcanic eruption of HI from the flask.




This is super heating. Use glass boiling chips to minimize super heating.

 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-08-04 18:55
No 481331
      Juses chreest! Are we back on the 120c+ ...     

Juses chreest!

Are we back on the 120c+ movement again???
Have thing come full circle or what??

WHy does HI need to disasicoiate at it natural disasociation temp for it to reduce iodoeph?
120c min?Are you sure?

Why not 80degC?
Why not Warm weather.Ask worlock If yer game.

Yeah 120 deg is where the two split if heated in a pot,
but what of the natural forces we encounter when ephedrine is introduced then halogenated?

Has anyone ever timed how long it takes for HI to halogenate?
How is hydrogen and iodine going to form the intermediate?
Im sure a little coaxing is required,but surely we dont need to slam them moles appart with such ferocity in order to accomplish a reduction.

If 120deg is the minimum,am swmIm ingesting something other than meth as a result of sub100deg cooks?
80-90degrres and TIME has always done it.Fuck the bubbles,
all they do is make me feel like a chemist anyway.

Who said we need a reflux?
Is it the temp of the HI, the H20 or the ephedrine which counts?
Back to reactions under vaccum then,that is if bubbling is all that matters,or if dissasociation is what makes our meth.
Suck that atmosphere out and let it boil at 20 degreez should do it.

We could hydrogenate using iodine as a catalyst perhaps and water as a solvent.

Are these truely the principles behind this rxn, or is this just more stabbing at shaddows?
tongue


Ahhhh to ponder on such whimsicle thoughts.



Rhod, It was your "excellent idea" that led swim to warm and not cook her rxns in the first place.
NOW YOU GONNA TELL ME I BEEN SNORTIN PSEUDO and IODINE ALL THIS TIME??
Explains them nasty sores and wind tunnel sinuses I spose.
I swear the pinweels swlI get from her warm cooks will rival the best of the best,even if they are kinda yellow.



Happy new year lovely bees.
Stay safe.
B.O.S.
 
 
 
 
    Rhodium
(Chief Bee)
01-09-04 19:45
No 481548
      huh?     

Rhod, It was your "excellent idea" that led swim to warm and not cook her rxns in the first place.

What are you talking about here? Haven't I always told you to reflux the reaction overnight using a lot of water?

I think you are confusing my statement "never run hot and dry" with the incorrect interpretation "don't heat to reflux".

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    LoRE
(Newbee)
01-10-04 11:46
No 481632
      50% hypo what is the rest does it contain,...     

50% hypo what is the rest does it contain, water? from what ive read it does if this is correct then no addition of H2O is required it would only hinder the reaction dropping the HI concetration down to under %50 therefor halting the reaction. Rhodium told me not to add more H2O than you have Iodine does this mean to take into account the H20 already in the hypo. so a reaction that 100ml hypo 50%  0.965mol + min of 0.78mol of I2(= 197g 0.78*2 =1.56mol HI 199.5g enough to reduce 0.5mol of e .5*201= 100.5 g   with exces of .185mol H3PO2 = 12.2g+what ever water was left in the reaction

sorry if that doesnt make sense im tryin and ive been up for a few days
um what is the mol of H3PO3?

maybee i should get some sleep
 
 
 
 
    Rhodium
(Chief Bee)
01-10-04 12:24
No 481639
      Yes     

50% hypo what is the rest does it contain, water? from what ive read it does if this is correct then no addition of H2O is required it would only hinder the reaction dropping the HI concetration down to under %50 therefor halting the reaction.

Precisely.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    wareami
(Hive Addict)
01-10-04 17:31
No 481692
      Moles or Hamsters...take yer pick!     

um what is the mol of H3PO3?

LoRE: See Post 481689 (wareami: "Calculating moles software", Chemistry Discourse)


Peace of the reaction

Have FUN-Bee SAFE
 
 
 
 
    DarkSky
(Stranger)
01-10-04 17:57
No 481700
      ballzofsteel, You have "pinwheels"...     

ballzofsteel, you have "pinwheels" after you finish your rxn's??? This confuses SWID, pinwheels ARE un-reduced psuedo and definitely NOT something you want in your final product, that is not unless you enjoy doing psuedo. The meth crystal is NOT a pinwheel, not even close.
 
 
 
 
    Kinetic
(Hive Bee)
01-10-04 18:02
No 481703
      Excellent ideas     

Rhod, I suspect ballz is referring to the suggestion you made a while back in Post 352969 (Rhodium: "Hypophosphorous acid reduction with 100% yield?", Stimulants).

I too wondered whether the 120oC required for the dissociation of HI to H2 and I2 was significant. I had thought the dissociation was necessary in order to provide a 'hydride ion' to reduce the iodoephedrine to methamphetamine; the reason being for this was that otherwise the only 'H' source would be the protons in the acidic solution which, with no electrons, would not be nucleophilic and would surely be unable to displace the iodide ion.

But then there are trusted bees who perform this reduction well below the dissociation temperature of HI; geezemeister has attested to this above, and there are reports in the scientific literature where such reductions are performed well below this temperature too, sometimes as low as 60oC, for example in the article Tetrahedron Letters 42 (2001) 831–833 (../rhodium/excellent.ideas/h3po2.i2.reduction-2.pdf)

Reduction of 4-methylbenzhydrol (representative reaction):


Iodine (1.00 g; 4.0 mmol), 4-methylbenzhydrol (0.79 g; 4.03 mmol), and acetic acid (25 mL) were stirred under nitrogen in a flask equipped with condenser. Hypophosphorous acid (50% aq.; 2 mL; 19.3mmol) was added and the mixture was heated to 60°C. The mixture was stirred for 24 h, diluted with water, and extracted with hexane. The hexane was dried over MgSO4 and removed under reduced pressure. Analysis by GC–MS showed only a single constituent, 4-methyldiphenylmethane, produced in 100% yield.



So where does this leave us? There is obviously still confusion: this thread's very existence and the views expressed within it are proof enough of that. Attempting to put things in perspective, however:

120oC is obviously not the minimum temperature for the reduction of compounds by HI. As HI doesn't dissociate below this temperature, the reasoning must be, as with most things in chemistry, that the mechanism isn't as clear cut as the simplistic representation we use to enable our understanding of it. It could be that a partial dissociation is able to occur, possibly only in the presence of a reducible substrate, at a significantly lower temperature. It could be that the proposed mechanism needs a little modification: the Final Word on the HI/P reduction mechanism (../rhodium /hi-rp.mechanism.html) is probably the most up to date and definitive proposal we have, but there is always the possiblity it isn't entirely accurate or complete.

It could just be that I've missed the point entirely, but this is the best it's going to get for me tonight.

Any thoughts?
 
 
 
 
    Rhodium
(Chief Bee)
01-12-04 14:27
No 482077
      Direct reduction mechanistically possible?     

Is it possible for hypophosphorous acid to reduce iodoephedrine directly at lower temps without going through HI?

If hypo can reduce iodine to HI and HI can reduce iodoephedrine to meth, it should at least be theoretically possible for hypo to do it too, provided that there is a mechanism for it. That I don't know, but it would explain some special circumstances surrounding the hypo procedures in particular (as opposed to HI/P).

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    WizardX
(Wizard Master)
01-13-04 01:28
No 482148
      The Mechanism.     


If hypo can reduce iodine to HI and HI can reduce iodoephedrine to meth, it should at least be theoretically possible for hypo to do it too, provided that there is a mechanism for it.




C6H5-CH(-I)-CH(-NHCH3)-CH3 + H3PO2 + H2O ==> C6H5-CH(-H)-CH(-NHCH3)-CH3 + H3PO3 +HI

 
 
 
 
    BOS
(Newbee)
01-13-04 02:04
No 482152
      Should this work with say bromoephedrine or...     

Should this work with say bromoephedrine or chloroephedrine?
 
 
 
 
    SHORTY
(Hive Addict)
01-13-04 02:42
No 482159
      Is this possibly what happens...     

Since rp releases hypo at a slow rate then is that why it takes longer than hypo?  What i mean is that as the rp releases hypo it is making HI and phosphorous acid.  The phosphorous acid can then generate more HI. Therefore the concenctration of Hypo is probably not high enough when using rp so the HI has to do most of the reducing and therefore takes longer to complete.

I think i have a similar problem with my homemade hypo because it takes longer to complete than most of the hypo synths I have seen.  I think that by not evaporating under vaccumm, alot of the hypo is oxidizing.  This would explain why it takes 8-12 hours of refluxing to complete the rxn.

 So although its faster than rp, it is slower than lg hypo.

Does this make any sense?

It wasn't Me!
 
 
 
 
    SHORTY
(Hive Addict)
01-13-04 21:07
No 482312
      Rhodium,     

Rhodium,
You might want to put a copy of this pdf on your website, It has good, fairly current info about research on rp.

http://ecb.jrc.it/classlab/0900_IND5_red-phosphorous.pdf

It wasn't Me!
 
 
 
 
    Rhodium
(Chief Bee)
01-14-04 07:39
No 482373
      Done.     

It now resides at ../rhodium/pdf /chemical_behaviour_of_red_phosphorus_in_water.pdf and is linked from the Inorganic Precursors section.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    placebo
(arrogant bee of the day)
01-15-04 05:13
No 482566
      Geez, Re: I noticed long ago there was direct...     

Geez,

I noticed long ago there was direct correlation between hot cooks and tweaky dope.




I noticed long ago there was direct correlation between unclean meth and tweaky dope.

I don't disagree with anything you said above except that statement. And it's not really that I disagree with it, as it may be true, it's just not the whole truth. I think what you mean is that hot cooks give rise to more side reactions and by-products which when not cleaned properly results in tweaky dope.
But, no matter how you cook it, clean, dirty, hot, cold, fast, slow, birch, I/RP, I/hypo or I/H3PO3. If the end product is isolated and cleaned properly, it will all be as good as eachother although yields will vary.

I, as we all have, have had some major fuck-ups and catastrophes, (only way to learn) and extracted the goods from the most disgusting looking black mess, but upon copious, laborious cleaning processes it always turned out as good as any other batch.

Oh and I too have the thermometer curse The worst was breaking a nice $88 0-400c thermometer 10 mins after unwrapping it.


I'm not fat, I'm just too short for my weight.
http://www.whatreallyhappened.com
 
 
 
 
    wareami
(Hive Addict)
01-15-04 05:41
No 482569
      Riddle me this....     

I'm going to let Geez have the first shot here, as it's his statement with which you disagree....
I've done extensive study and experimentation in an effort to reveal more about cooking conditions and how they relate to the effects of this drug, before and after refinement processes.
[quote]Because lets face it, no matter how you cook it, clean, dirty, hot, cold, fast, slow, birch, I/RP, I/hypo or I/H3PO3. If the end product is isolated and cleaned properly, it will all be as good as eachother although yields will vary.

I find that statement false, misleading and misinforming.
I'll let geez speak for himself before I explain why you're incorrect.

Peace of the RXN
Have FUN-Bee SAFE
 
 
 
 
    geezmeister
(Of Counsel)
01-15-04 07:56
No 482579
      I agree w/ arrogant one     

I agree with Placebo. I am saying in shorthand (remember shorthand?) what he said in a few more words. He is correct. High temperature doesn't make meth tweaky. Meth is meth. There isn't a thing about the meth molecule that makes it tweaky. If its meth, its meth. And pure meth isn't tweaky. You can clean most of the tweak out of street meth with multiple recrystallizations, at the expense of the weight of tweaker substances in the meth. 

The real "tweaky" crank I have had has been associated with hot cooks and less-than-stellar post-reaction workups. I agree the tweak comes from by-products for the most part, and in part from intermediates, and not from the meth itself. Meth is meth. The chemcials that make crank tweaky are not meth, they are something else. Its these other things in the mix that make you go nuts, induce paranoia, make you hear the folks outside the third floor window, and see the DEA surveillance team in the trees. (I remember the night I was certain Santa Anna and the entire Mexican Army was hiding in a field behind my lab, waiting for dawn to attack.)

High reaction temperatures help create the by products that taint meth and make it crank, or make it tweaker dope. They can combine with meth to make a product that keeps you up but gives you tweaker's paranoia and insanity. 

I am less prone to concur with Placebo that less-than-clean feedstock is the source of the problem. I am not saying that it cannot be a contributing factor, but from experience I know that even with very clean feedstock, hot cooks (particularly the dry, hot, and fast cooks) will yield a product full of tweaker characteristics. I've had it happen with feedstock from a very clean pill source, and with feedstock pulled from a two-inactive pill formulated to be pulled pulled with MeOH alone which was recrystallized twice after an alcohol extraction. I've had it happen with feedstock extracted from the same pills by an a/b, which also was recrystallized before reacting it. I recognize that less than pure pseudo may contribute to the byproduct formation in the meth reaction; I merely emphasize that heat, particularly in conjunction with a drier type rection, is a primary contributor to the tweak often found with methamphetamine.

I agree completely with Placebo's comment, "No matter how you cook it, clean, dirty, hot, cold, fast, slow, birch, I/RP, I/hypo or I/H3PO3. If the end product is isolated and cleaned properly, it will all be as good as each other although yields will vary."

I will note some of the by products have virtually the same solubilities as meth, and are difficult for the clandestine cook to isolate and remove. You can clean most of them out by simple recrystallization techniques... and the number of tweakers I have known that prefer their meth straight from the evap dish before recrystallization confirms the fact that you can separate most of tweaky by products from the real meth post reaction. I remain of the opinion that the best route to really clean meth is to avoid making the byproducts in the first place, and the best way to do that in an rP reaction is with a long wet reflux at a reasonable temperature.

Damn. I agree with Placebo again. I must be getting old, or something like that. laugh And I recently discovered the newest themometer I had at my disposal neatly disposed in two pieces on the floor. How it got there is a mystery to me. Must be the curse acting up again.

mostly harmless
 
 
 
 
    placebo
(arrogant bee of the day)
01-15-04 09:37
No 482595
      Wareami, I'm waiting, enlighten me.     

Wareami,
I'm waiting, enlighten me.

I'm not fat, I'm just too short for my weight.
http://www.whatreallyhappened.com
 
 
 
 
    CharlieBigpotato
(goat)
01-15-04 11:40
No 482622
      what a break!     

geez,
i was wantin' to chirp up for ol' placebo on this, but didn't want to piss you off, on account of what a sweetie-pie you are, and generally speaking, how caustic dear placebo is (or has been capable of in the past, bless his heart)

so i offer this imagery to the rap:
in the fucking '60's, of which i am a child-codger, meth was plentiful, cheap, pretty god-damned pure, and sort-of frowned upon, especially in hipper circles that were tripping.

yet, even back then when nobody had to put up with shitty meth, there were all the same tales of the speed freak and his paranoia.
frank zappa did radio public service raps on it.
r.crumb created vivid characters based on it.

perhaps the l&d ratio back then was in favor of the l side; compared to now, and its that side that encourages one to stay awake far too long; not eat or drink or bathe; and generate verbose theories.

geez, you must know that i've been 'around'.
here's a weird one from biz's anecdotal history, with clear gear; beefore he knew any better:

the dumb fuck would sprinkle a line into a joint of leaf, and torch it and smoke it.
what an amazing no-no that was, in terms of various meth-monster side chains and azirides and such.

and yet, to this day, he must admit, that the buzz from that goofy-ass means of ingestion, was absolutely identical to any other means the old fool tried later on, when he got more edu-macated.

god bless the placebo effect
 
 
 
 
    geezmeister
(Of Counsel)
01-15-04 15:07
No 482652
      Speed kills?     

As an old Dead Head myself, I assure you that I recall the slogan that "speed kills" although I frankly have forgotten what it meant. The speed I did in the sixites was most often done during finals week. I either did benzedrine by the handfull, Black Mollies (those lovely Biphetamine capsules the long haul truckers loved so much), or some of that nasty methamphetamine a roomie of mine who was a chemistry major made for us at the university lab. I recall giving him the small amount of money it took to buy his supplies and watching him set up the reaction and start it one time. I believe I doing acid at the time and got off on something else before he finished.

it isn't so much how you ingest it that makes it tweaker stuff, its how its made. Tweaker dope will make you tweak whether you smoke it, snort it, eat it or fire it. Placebo's comments are well taken. Tweaker dope is meth that needs to be cleaned carefully because it has other chemicals in it, by products of the reaction for the most part, that give it the weirdness that leads to the paranoia and adverse side effects we call tweaking.

In fact, I never had particularly tweaky dope making it with hypophosphorous acid, although I ran a few batches pretty hot before I learned what a phosphine fire was. I have run H3PO3 reactions as hot as the hotplate or oilbath will go. I have noticed in these only a slight edge to the meth that I do not have with LWR rP/I2 dope. Nothing like tweaker dope, although the inner flask temp has to be pretty high. The tweaky dope I have made, and that that I have obtained from others, was to the best of my current recollection dope made from red phosphorous and I2, both  of questionable purity, cooked hot and with very little water and "finished" in an hour to an hour and a half. The methods all employed a vigorous, smoky, exothermic start to the reaction that filled the flask or coffeepot with thick, yellowish smoke.

Very little of the tweaker dope I have done was at all clean, and what was was very strong stuff indeed. I know the strongest real "tweaker dope" of this kind was cleaned repeatedly with acetone but never recrystallized. When I was doing push-pull type reactions, or low water reactions,  I recrystallized without fail; there were noticable decreases in the tweaky characteristics of the dope, with a noted decrease in yield on recrystallization.
The uneventful-start-fairly-low-temp-long-wet-rP/I2-reflux- for-36- to-48-hours gives dope out of the evap dish that is not tweaky at all, even though it is very strong. With that dope there is minimal loss of weight in the recrystallization step, and the improvement in quality is very limited.

I may be in error in my overall recollection, but I think it  entirely possible that the tweaky meth I am familiar with may be red p/I2 dope cooked with little water, and the norm for such cooks in my area would include high heat. I can tell dope that has been cooked hot by the tweaker characteristics and feeling of it; it may well be that the by products I do not like and the tweakers prefer may actually be the result of the fast hot smoky start making by-products and the hot dry cook making others. I have no doubt that heat is involved in making rP/I2 reactions yield tweaker dope; in retrospect a good part of that may come from the smoky, hot, exothermic start.

I don't recall in my limited experiences with birch dope ever having any partiucularly tweaky birch dope, although some of it has been pretty nasty stuff.

mostly harmless
 
 
 
 
    wareami
(Hive Addict)
01-15-04 18:32
No 482710
      Wait no longer...     

Okay, I'll agree with Geez here in regards to when the end product being produced is 100% meth
Then the drug won't have the side-impurities that produce the effects were talking about when discussing "Tweakermeth/SpaceDope".
 
But from what I gather, placebo is talking about any end-result from any rxn, under any condition, that is suppose to reduce pfed to meth,
and as the last recourse this end product can be supposedly cleaned post-rxn and refined to exclude all impurities associated with Tweakermeth .

Because lets face it, no matter how you cook it, clean, dirty, hot, cold, fast, slow, birch, I/RP, I/hypo or I/H3PO3. If the end product is isolated and cleaned properly, it will all be as good as eachother although yields will vary.





I believe that statement is incorrect primarily because the intermediates that get introduced via the reduction in hot/fast start/fast finish/ HI/RP cannot simply be cleaned away once those impurities are created along side and bonded to the meth via rxn. Be it extraction through steam distillation, a/b,  or further refined by recrystallization.
Some impurities, I like to refer to as intermediates because they form in a neccesary stage whether we like them to or not, are not easily removed by post-rxn cleaning, IMHO.
When looking at the individual processes that go into all that's involved, it's clear to see there are conditions that effect yield and purity.
If it's as Placebo suggests, one should be able to take any method on this board, throw in dirty pills, halfassed cleaned precursors, run the rxn, then proceed to do final  cleaning via steam distill followed by several re-xtallings, and walk away a happy camper never to hide from the bushes again.
I fail to see the logic...
Maybe it's just me!
Maybe I took that statement too literally?
If so placebo, please correct me.
I just don't see the good in handing down that kind of info when there are clearly several better, more effective ways to address the removal of most bad impurities in-situ.
We are a few steps closer to understanding the mechanisms that produce those unpleasant side-effects and then I see a statement like that which clearly undermines the findings and confirmations disscussed on this board.
I'd like to continue moving ahead and advancing in learning more about what makes meth tick, the psychoactive effects produced, and refining the product further. In that process Ibee has duplicated several unpleasant conditions that confirm what everyone suspected about hot HI/RP rxns.

By no means are my findings a definative, but they are as close to an understanding of the 'what's, how's, and why's, as I can manage. These based on individual findings through research fueled by the determinaton to achieve purity since success was only a taste considering the bigger picture here.
Placebo, You do know that my reply wasn't meant to offend, but rather to reach a collective understanding of the processes and conditions bees are beeing handed down as new information becomes available through exploration of new avenues and refinement techniques.


a little less conversation, a little more reaction
 
 
 
 
    Dragontail
(Stranger)
01-15-04 18:43
No 482715
      Tweaked Birch Dope     

Geez
Swim has used alot of Birch dope and every time it always had extreem tweaky side effects. This dope comes from the north-western part of the US and is made from pills bought localy in that area that only have two inactive ingredeints and pull easily with alcohol. Swim has thought that mabie it was due to exessive lithium or that mabie the Anny never fully evaped before adding NP. Swim always beleived that the NP used was ether because after three of four puffs, swim felt real "spaced out" as well as high. Also upon IV use, intense hallucinations would fallow for about ten to fifteen seconds! Swim can remember doing a shot and looking out the window and watching trees wave back and fourth like a belly dancer! Was that the ether or effects of impurities?
Weather smoking or shooting this dope, Swim always ended up having to deal with transparent hellicopters, shadow people and cops in the trees with binoculars. Needles to say that Swim no longer chooses to use this dope, nor does he need to because of all he's learned on the Hive!
 
 
 
 
    SHORTY
(Hive Addict)
01-15-04 18:58
No 482720
      Makes Sense to me..     

In my opinion this just happens to bee on of those rare occasions where for the most part everyone is right.  I have dealt with "tweaker meth" which i beleive was due to getting the rxn too hot and at least for me it was very difficult and usually impossible to rid it of all the side effects like jaw clenching or even worse the one that makes you do things with your mouth and tongue that cause you to make some weird ass faces without know it.  Even after several recrystalizations it would still be there.  I beleive that many of the impurities or intermediates which cause this are very similar to meth as far as solubility and other properties are concerned.

But as Wareami pointed out, for the best results the pseudo should bee as clean as possible in order to avoid these problems as well as avoiding excessively high rxn temps.

It took a long time for me to understand why my meth was never the same from batch to batch although the answer is simple enough.  It seems to me that the best way to avoid the impurities and intermediates is clean pills and longer cook times both are keys to the best meth possible.  Falling short on either of these will have the most effect on the quality of the results.

It wasn't Me!
 
 
 
 
    placebo
(arrogant bee of the day)
01-15-04 19:17
No 482725
      At no point did I condone or promote laziness...     

At no point did I condone or promote laziness and dirty reactions/meth, in fact the opposite. You are reading shit that aint there.

I simply made the observation that regardless of method, dirty meth can be made one way or another, but upon thorough cleaning it should all be good. Obviously if you take the steps to have the cleanest product possible after the reaction, you'll have less work to do in the cleaning, and hopefully a higher yield to boot.

My point is that you dont belittle others methods, as all can produce good meth. Some methods may suit others better in their particular circumstance. You can't make everybody cook your way, it aint practical for some.

I only posted to correct/reword geezmeister's post, which was not a mistake, merely misworded or abbreviated. I know, he knows his shit, I just thought I'd throw a little something in for the newbees to understand better. But you seem to have misunderstood me.

I'm not fat, I'm just too short for my weight.
http://www.whatreallyhappened.com
 
 
 
 
    katsogiannos
(Hive Bee)
01-15-04 19:28
No 482728
      Why use pseudoephedrine?     

Why not just use ephedrine hcl? Not that pseudoeph crap that is in sudafed. Do you still get a lot of impurities/tweaky side effects if you use ephedrine hcl?
 
 
 
 
    spectralshift
(Hive Bee)
01-15-04 20:06
No 482735
      a quick question or 2     

This is what isn't making sense to me, I've read from Shorty and others that hot reactions can produce "tweaky" meth, but meth is the final product of the reduction?

A hot and quick reaction, or a hot and dilute reaction would make sense, but to say the same for a warm and quick, or a warm and dilute reaction would make more sense--that would produce more partially reduced rubbish and by-product.

Heat is actually a positive factor if the other factors are right isn't it?
 
 
 
 
    Rhodium
(Chief Bee)
01-15-04 20:09
No 482736
      It's a supply issue     

Why not just use ephedrine hcl? Not that pseudoeph crap that is in sudafed.

It is a lot less readily available to people, as only pseudoephedrine is found in OTC medications nowadays.
 
Do you still get a lot of impurities/tweaky side effects if you use ephedrine hcl?

Maybe not to the same extent, but the problem is still there with sloppy technique.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    biotechdude
(Hive Bee)
01-16-04 01:47
No 482785
      Things that make you go Mmmm     

Well done lads; a great little read over a spicy thai dinner..

Now it is clear that a 100% pure meth molecule from one synth will be the same as a 100% pure meth molecule from another synth.  This is regardless of whether a hot cook, long cook, etc etc.

HOWEVER, it is worth noting that regardless of method or post reaction cleaning; it is very near impossible that ANYONE will produce a 100% clean meth molecule.

So for the sake of the 'tweaker dope' arguement, we will say that ALL meth that anyone here has produced has impurities present.  Now the discussion boils down to the fact that different methods and factors produce different ammounts of the 'substance(s)' that cause tweaker characteristics.  Now this 'substance' seems to be produced in higher ammounts in
- higher temps (rxn/production rate of 'substance' production increases with temp)
- shorter or 'harder' rxn times (substance produced quickly but then can 'die' off (eg with LWR))
- dirty precursers (tweaker substance can be produced from all production methods.  Therefore 'substance' must be produced from impurtity common to many different precursers eg RP, Li, pseudo)

The 'substance' that produces tweaker behavior must have very very similar properties to meth; in that it is very hard to remove once 'produced' via one of the aforementioned factors.  Additionally, it must be produced in very very low levels (to avoid detection on HPLC) or that close structurally to meth or another impurity to avoid disciminative detection. 

In summary, swix believes that 'tweaker' effects are produced a chemical molecule produced when the factors are best for its production eg. hot, fast and hard, unclean precursers.  This tweaker molecule has near identical properties to meth and hence make its removal very difficult.  Perhaps this tweaker molecule is a structural derivative of meth or a molecule derived from an impurity present across many meth-production techniques.  This molecule could perhaps one day become a new 'drug'; because it is apparent its effects are extremely psycho-active, even in extrememly low levels.

Imagine -
To produce '1g of TWEAKER'
Ingredients - dirty ass pseudo, RP I. 
Reflux for 1min at 250`C

"Ripped off!, this TWEAKER has been cut with meth!"
 
 
 
 
    Osmium
(Stoni's sexual toy)
01-16-04 02:05
No 482792
      > Now it is clear that a 100% pure meth...     

> Now it is clear that a 100% pure meth molecule from one
> synth will be the same as a 100% pure meth molecule from
> another synth.  This is regardless of whether a hot cook,
> long cook, etc etc.

Wow, what a revelation!
I thought that was clear for at least 150 years?

I'm not fat just horizontally disproportionate.
http://tinyurl.com/3kdu
 
 
 
 
    CharlieBigpotato
(goat)
01-16-04 05:42
No 482817
      why, rhodium?     

did you imply that eph-hcl was less apt to reduce poorly than psuedo-eph?
other than added inactives, wouldn't they reduce identicly?

btw, bees, regarding tweeky twitches and the like:
swim has had ritalin and adderal a couple times (seperately) and found both drugs to cause amazing mouth gyrations and toungue waggling...even in single pill doses.

never had those effects on meth; even when it was torched in a joint.
 
 
 
 
    Rhodium
(Chief Bee)
01-16-04 15:13
No 482913
      there is some difference between them     

Due to the orientation of the alcohol and amino groups in ephedrine vs. pseudoephedrine, the former is usually easier to reduce as there is less steric hindrance. I don't have the literature proofs handy at the moment, but anyone who has used both starting materials can vouch for this being true. And - as it's easier for it to be reduced to the desired end product, the less time the intermediates has to react some other way and form by-products...

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    ballzofsteel
(Miss High & Mighty)
01-16-04 22:31
No 482969
      Again, Does the mechanism Wizard X describe...     

Again,

Does the mechanism Wizard X describe hold true for
all haloephedrines, or only iodo-ephedrine???

Sorry to get off topic,but what the fuck is the topic again?
 
 
 
 
    cycosyince
(Stranger)
01-17-04 14:42
No 483082
      I think     

I think it had to do with temps/reflux/and the qualities rendered therein.

I keep reading about impurities causing undesirable (?) effects. However, from my end of the kaleidiscope, alot of the "voices" "DEA-behind-the-clubhouse", tweezer adventures upon the skin, talking with the pals in the A.C. unit, are more often the result of a meth induced psycosis, pure OR tweeky notwithstanding. Now for me what is REALLY interesting is how birch manages to transform the lowly psudo to a lofty position in the land o' meth with a temprature that is sub freezing, and in about an hour. Meth for those on the...(ahem) GO. At any rate, lower the dosage, and get plenty of sleep between the romps and the incedents of audio and/or visual hallucinogenaria should become less pronounced, (with the krappy dope) and go away altogether with the better quality bags.

uh, you know, stuff.
 
 
 
 
    WizardX
(Wizard Master)
01-17-04 15:50
No 483102
      YES     


Does the mechanism Wizard X describe hold true for all haloephedrines, or only iodo-ephedrine???




YES. However the chloro and bromo will give poor yields as these halogen will not leave the ephedrine benzylic C atom as easy as I

 
 
 
 
    biotechdude
(Hive Bee)
01-19-04 06:42
No 483317
      Osmium     

> Now it is clear that a 100% pure meth molecule from one
> synth will be the same as a 100% pure meth molecule from
> another synth.  This is regardless of whether a hot cook,
> long cook, etc etc.

Wow, what a revelation!
I thought that was clear for at least 150 years?


One shouldn't consider it a revelation when the statement was obviously toned to be post-revelation comment through the use of the phrase 'it is clear'.  It was establishing the background information necessary for the smooth literary flow into the coments that followed.

Methamphetamine was first manufactured by the Germans in 1887.  Thats 117 years of meth production technology and validation.  Additionally, the theory of this 'revelation' would of been realised centuries before.

So perhaps you could add your esteemed input into this forum through relevant comments showing your much respected intelligence and experience.  Not 'cheap shots' that highlight your flippant literary humour and erroneous mathematic and history skills.

<<no offence taken or given>>
 
 
 
 
    CharlieBigpotato
(goat)
01-19-04 07:18
No 483321
      2 more cents     

last attempt to explain something that is bothering me about this:

the effort towards producing pure product is laudable, but the growing notion that said product is 'mostly harmless' is dangerous, imho.

geezmeister is the sort of level-headed, decent bloke that one could probably lend his sports car to, and get back with extra gasoline and an oil change.

yet give a few grams of the purest meth in the world to some other type fella(s), and they'll stay up for days, get dirty, see helicoptors, pick at non-existant zits, not eat, get paranoid, etc, etc, etc...just like if they had gotten ahold of the mysterious 'tweeker dope'

meth ain't no health food. i don't care how pure it is.
check your blood pressure, for instance, beefore and after having some.

it puts you 'under pressure'!


fuck, if it didn't fuck up a bee, why would they bother with it at all?

its a good tool;

its a bad habit
 
 
 
 
    cycosyince
(Stranger)
02-01-04 19:39
No 485951
      topically speaking     

So then in review, I assume we can round the figures to: Very high temps, (red heat, major flammage) is generally bad, and will destroy a batch.
High temps, (close to red heat, and 'Ow fuck that charred me skin white!) is quite likely to ruin a batch, or at the very least, wreck the yeilds to around a Qtr. of what went in.
The RIGHT temp. (The temp that works whilst refluxing, resulting in excellent quality/yields) Oh, this is the temp to use!
No temp/room temp, yeah whatever.
-70 with an ammonia odor, (along with some battery strips) You are clear for take-off, houston out.

Got it? Then



COOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOK!

uh, you know, stuff.
 
 
 
 
    gluecifer69
(Hive Bee)
02-03-04 21:42
No 486290
      Swim's push/pulls never reach 120C, so does...     

Swim's push/pulls never reach 120C, so does the lower temperature offer more highly concentrated HI or what.

The highest temp his push/pulls have ever seen was 200 F, which is 93.3333 C. 

Could anybee shed some light on this, because SWIM knows he gets quality gear from the push/pull with high purity. MP tests have been done and they are right on the money. No fucking undreduced shit in this bees gear!

Just wondering all input will be greatly appreciated.

EDIT  I just read that lower temps. to offer higher HI concentrations.  Somebee correct me if am wrong.

absorb what is useful, reject what is useless
 
 
 
 
    WizardX
(Wizard Master)
02-04-04 05:32
No 486325
      Reaction Rate     

The Reaction Rate reduction of ephedrine to meth with HI is directly proportional to the concentration of HI and temperature.

What does this really mean you ask?

Well, if you put ephedrine in a 57% HI solution in a dark place (so photo-dissociation does not occur) at room temperature, 25 oC, you will get after considerable time some iodoephedrine (minor quantities). However, to convert the iodoephedrine to meth requires energy (heat) to force the reaction along by reaching the activation enery and thus increase the reaction rate.
 
 
 
 
    livid
(Newbee)
02-05-04 00:49
No 486539
      re; temps     

gluecifer is  right on the money.