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	All 100 posts	Subject: Free Base - The Wet Start Rxn	Page:  First Last

	VideoEditor (Hive Bee) 10-01-02 02:52 No 362507		Free Base - The Wet Start Rxn	Bookmark Reply
			Free Base - The Wet Start Rxn Condensed Version 2 Ratio Used:  1FB / 1.5 I2 / 0.5 RP (1RP if MBRP)       DH2O:  0.5ml per gram of I2    Example:  10.0 grams free base              15.0 grams I2               5.0 grams RP (10.0 if MBRP)               7.5 ml DH2O -Method using the above sample amounts- 01. Place 10 grams free base into a 250ml flask 02. Add 7.5 ml DH20. 03. Mix with a glass rod or bamboo skewer to dampen free base. 04. Add 10 grams I2 and mix to distribute evenly. 05. Add a pinch (~50mg) RP and mix. 06. Let I2 and free base react swirling flask often.       Mixture will separate into water layer and I2 Layer. 07. When the 2 layers combine again the I2 reaction is done.       You should have a thick black liquid. 08. Add 1/3 of the RP and mix for a few minutes. 09. Add remaining RP and mix for a few minutes. 10. Add remaining 5 grams I2 and mix. HI will start to evolve. 11. Connect to scrubber / PP unit. 12. Heat in oil bath to 150F.  Flask will fill with HI. 13. Hold at 150F for 90 minutes. 14. Slowly raise oil temp to 220F.       2nd phase will kick in at approximately 190F. 15. Hold oil at 220F for at least 6 hours. Note: Do not use a condenser. We want the mixture to slowly dehydrate over time. If and/or when PI3 crystals appear in flask neck add 1/2 original DH2O washing them into flask and continue. Workup using VideoEditor: "Easiest Post Rxn Steam & Clean for RP/I " (Stimulants) or other method of choice. Real Men Don't Preview Their Edits
	Rhodium (Chief Bee) 10-01-02 04:15 No 362563		HI is a gas	Bookmark Reply
			There is no such thing as "HI crystals". You might want to edit your post.
	VideoEditor (Hive Bee) 10-01-02 04:36 No 362573		Damn spell checker	Bookmark Reply
			Thanks Rhodium. That would be PI3. Got auto corrected to HI. Thanks for catching the typo. Thats why you're the Chief. Real Men Don't Preview Their Edits
	Rhodium (Chief Bee) 10-01-02 06:57 No 362627		I think it is a nice that you have added water in ...	Bookmark Reply
			I think it is a nice that you have added water in the reaction. But what if you would reflux instead of dehydrating for 6h? To me that makes much more sense, preventing byproduct formation. What are the yields as it is, and how are they using reflux?
	VideoEditor (Hive Bee) 10-01-02 12:11 No 362676		Control	Bookmark Reply
			Rhodium: SWIVE's goal was to use water to control or stall the reaction at the beginning so that nothing had to be chilled and there would be little risk of burning the free base. SWIVE arrived at this by doing seventeen 2 gram test reactions starting with no water, then increasing in 0.25ml increments up to 4.0ml and found that 1.5ml was the threshold he was looking for. This amount stalled the reaction at first, but with heat and evaporation the reaction start was gradual and calm. Using the stated ratios and times, the intent is not to dry out the reaction mixture, but keep the concentration of HI as high as possible. But what if you would reflux instead of dehydrating for 6h? To me that makes much more sense, preventing by product formation. A reflux will also work if you start with less water and go back to chilling the reagents and combining them as prescribed by Jacked in his method to avoid burning up the free base. If you reflux with the amount of water SWIVE is calling for, SWIVE would let it run for 12 hrs instead of 6 hrs insure a more complete conversion. SWIVE does not have the ability to analyze the byproducts of each approach, but a burn test and bio assay suggest that they are about the same. What are the yields as it is, and how are they using reflux? Assuming SWIVE starts with 10 grams of free base. Using steam distillation, extracting with pet ether and then gassing, yields have been around 8 to 8.5 grams of product before crystallization. Approximately 62% to 69%. I have not done an apples to apples comparison to a reflux for yield. Real Men Don't Preview Their Edits
	Rhodium (Chief Bee) 10-01-02 14:25 No 362692		More suggestions...	Bookmark Reply
			Could you please do that? I would even go as far as to suggest the addition of as much as ~25ml water as to ensure that the temperature stays moderate throughout the whole reaction to inhibit byproduct formation. If you have the time, please perform one 6h reflux and one 12h reflux and then compare the yields between those runs and the ones you have done using much less water. For the sake of purity, I believe that the extra time spent using a real aqueous reflux is well worth it. If you are interested I can post GC pictures of the immense amount of impurities that is obtained from a dry RP/I run - look at the picture on page 99 in http://www.rhodium.ws/pdf/meth.impurities.hip.pdf to see how the chromatogram looks after running a proper aqueous reflux - you only find a half-dozen of contaminants, while after a dry run several dozen can be detected, and the amount of "other stuff" definitely outweighs the desired product. I have one more question, and that is your suggested amount of red Phosphorous. As it looks right now, you'd need 5g of LGRP for a reaction, but only 1g MBRP - that certainly must be wrong, right?
	Rhodium (Chief Bee) 10-01-02 16:19 No 362724		Methamphetamine impurity identity profiling	Bookmark Reply
			Here is an article dealing with methamphetamine impurity identity profiling, compare how pure the product from the birch or P2P reduction method is compared to the RP/I, as well as the different Iodine  based syntheses... http://www.rhodium.ws/pdf/meth.impurity.profiling.pdf
	VideoEditor (Hive Bee) 10-01-02 19:11 No 362791		Can do	Bookmark Reply
			Can do Chief. SWIVE said the next time he bakes cookies he'll run some comparisons and report back the results. He also said he may know a few other bees that might be interested in helping compare.  It's good to see more interest in free base growing around here. -peace Real Men Don't Preview Their Edits
	geezmeister (Bee of the Month) 10-01-02 22:38 No 362876		Nice approach	Bookmark Reply
			SWIG has done freebase reactions since he started trials of the STB method. He has done them Jacked's way, controlling the reaction by carefully regulating the temperature through the end of the first phase. He has done them as VE suggested in the "looping reactions" thread with great success. The last three he has had to evaporate to a drier mixture after the first phase of the reaction completed, for different reasons. His best yields and most potent product have come when doing wet reactions, and four and a half hour or longer refluxes. He peceived no difference in quality between the product of four and a half hour and eight hour refluxes, although the opinion is subjective. Yield has been marginally higher with the longer refluxes, but he has not done enough of them under the same or essentially similar cirucmstances to attribute the result to the reflux rather than other factors involved. The information on shortening the length of the reaction and how to do it is welcome information. That information belongs in the data base because the time will come when you have no choice but to hurry things up and close up shop. I have had three such times in the last three months. An injury, an equipment failure, and a brother-in-law were at fault.* Good to have tested methods for achieving the result, with some foreknowledge of the detriment, on the board. Thanks again VE. * The last was the most serious, and the critter appeared, uninvited, just days before inlaw season officially began, and before I had a chance to get my "former mother-in-law" tag for this year. They seem to run in packs with brothers-in-law, and I always try to bag one during the "primitive bludgeon" season. (I do not participate in the archery season or the firearms seasons, due to the over-crowded hunting condtions during those seasons scaring most mother-in-laws into nursing homes or hospitals until the season is over.) Mostly harmless
	Jacked (Ancient Alchemist Delux) 10-02-02 03:08 No 362993		OK	Bookmark Reply
			I'll get into that one too The end result is directly connected to the effort applied
	cthulhujr (Hive Bee) 10-02-02 13:31 No 363192		condenser	Bookmark Reply
			For his hcl of same size, swim will typically use a 500ml flat-round bottom flask with a 6inch west condenser, circulated with ice water, and only slightly less or as much dh2o, 6ml would be bare minimum (often estimated, to swims discredit, so at least 6ml may be overly conservative), in addition to I from tincture which has been rinsed and only wrung out by hand. The condenser is topped with a double thick latex bladder, condom or glove that is. The rxn is brought to temp (190F), over the first 5 hours and held for a further 8-10 hours, depending on the amount of 'work' it appears to be doing. Finally, it's brought to (205-210F) for one more hour or so.    Despite the fact the reaction seems well sealed, it still, usually during the middle of the 8 hour period seems to thicken up quite alot, as if some water had been escaping, and bubble with vigor, the bladder rarely inflates enough to make it much more than half erect. After reading VE's post swim doesn't see why the same formulae won't work for freebase, just splitting up the Rp addition.  Swims FB reactions were run in dry, fast push-pull days and swim never got the hang of initial firing, consequently yields sucked from burn up of FB. After swim began wet refluxing, he was still under the assumption far more water would be required for FB, and evidently got things far to wet, making the reaction a drag, again FB was forgotten,and after one run.   So thanks VE for putting a finer point on it,swim is going to have to re-visit FB, 'cause this little bee is going to have check out the hubub you Big Bees are buzzin about. As far as the difference between the 4 and a half hour + reaction, swim definitly notices the difference in his HCL. Swim was forced to cut one short recently, 4 hours to temp and 5 hours reflux total time 9 hours, the post reaction solution was tinged with dark yellow, and the product was notably less potent. Admittedly, perhaps the same volatile nature, that makes FB take off quick, may shorten reaction times, as well. In that case, it's like apples and oranges, and swim once again puts foot in mouth.   Swim also notes he uses the Rp, I, and HCL, in same ratio as does VE, with FB, so because FB is not as heavy, a little rp and I is conserved in the bargain. right? Iä-R'lyeh! Cthulhu fhtagn! Iä Iä!
	zibarium (Naked) 10-03-02 06:06 No 363534		weight of fb	Bookmark Reply
			part of the freebase mystique could bee attributed to the same ratios beeing used as if it was the HCl salt. it would seem that such a rxn (FB) compared to an Hcl rxn, is necessarily stacked with more I2 and Rp...and is likely to leave a less acidic post rxn slurry than a salt precursor...possibly requiring less base..and the problems of a/b with more base needed.
	VideoEditor (Hive Bee) 10-05-02 12:43 No 364559		Just to clarify	Bookmark Reply
			Rhodium, SWIVE will try some comparative reflux's as soon as his schedule permits, but in the mean time SWIVE just wanted to clarify a few points. After re-reading his original posts and your replys SWIVE got the feeling that he may have been unclear or was confusing on the wetness of the reaction.  He gets the feeling that your impression is that the reaction will end up being dry or dryer than the current methods of RP/I rxn's. This is not the case. If done in the ratios SWIVE has laid out, with the rxn vessel connected to a P/P unit, the reaction will end up about twice as wet as any of the current RP/I methods in use (with the exception of a pure reflux).  If the PI3 crystals are flushed back into the reaction, it will end up being about 3 times wetter.  The specified amount of water is right on what SWIVE calls the stall line. Meaning the difference between starting as a "reaction" or starting as a "reflux". SWIVE believes this extra wetness combined with using free base as a starter is responsible for fewer by-products and a better yield. Jacked convinced SWIVE a while ago that this was the road to follow and It has not been until recently that he has had success in convincing other bees to try this approach. You have definitely sparked SWIVE's curiosity in making a head to head comparison with a true reflux. More data to follow... Real Men Don't Preview Their Edits
	wareami (Hive Addict) 10-05-02 16:49 No 364617		In the Long Run!	Bookmark Reply
			I have one more question, and that is your suggested amount of red Phosphorous. As it looks right now, you'd need 5g of LGRP for a reaction, but only 1g MBRP - that certainly must be wrong, right? Rhodium: That ratio conversion sounds about right. Especially for Ibee since he always reflux's under controlled conditions. He can always add more and cook longer if necessary. His first flaskfire happened as a result of following suggested (higher) MBRP ratios when using second run MBRP! To this day, if a recipe calls for .5g LGRP/1g MBRP, Ibee starts with .75g MBRP instead  of 1g, and because of the timeframe involved, rarely adds more to complete. How's that saying go? "All good things come to those that wait!" For every run, no less than 18hours is set aside. Reflux definately calls for less reactants and this in turn adds up to less impurities being introduced by excess! Since time is of no concern, more attention can be spent on the control issues. Ibee will take the "Less Precursor + More H2O + Time=Fullconversion + HigherYield" route any day. That equation is a no-brainer once it's been experienced! This is using Hcl as starterfeed and looks forward to trying his hand at the FB way. If you reflux with the amount of water SWIVE is calling for, SWIVE would let it run for 12 hrs instead of 6 hrs insure a more complete conversion VE: That statement says it all brother! Ibee is slightly confused about the "leaving off condensor" one though. By this, is it SWIVE's intent to propose an "Open Air" environment to allow for evap of the excess h2o? Peace of the REaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami
	VideoEditor (Hive Bee) 10-05-02 18:42 No 364647		Condensor	Bookmark Reply
			Ibee is slightly confused about the "leaving off condensor" one though. By this, is it SWIVE's intent to propose an "Open Air" environment to allow for evap of the excess h2o? Wareami, No not open air just a simple P/P unit. The reason SWIVE mentioned no condensor was that at the ratios given, a small amount of evaporation from the P/P had been factored in which will not occur with the condensor. Real Men Don't Preview Their Edits
	Rhodium (Chief Bee) 10-06-02 06:43 No 364952		I have no idea about how wet any "usual" HI/P ...	Bookmark Reply
			I have no idea about how wet any "usual" HI/P reaction gets, I have never performed one. I am just advocating common laboratory procedure, to use refluxing 57% HI (or RP/I2/H2O mixed as to form such a solution) so that the reaction temperature won't exceed that of boiling 57% HI (126°C). As I have never before seen any reaction in the literature being performed "dry" like that (except in mw rxns where the reactants is adsorbed on clay or silica gel, and they rarely run for more than 15min), I have a hard time believing that method has any real merit over a reflux (in real organic chemistry, decreased reaction time at the expense of lowered yield and increased amount of impurities is called a failure).
	VideoEditor (Hive Bee) 10-06-02 14:12 No 365030		How wet is wet	Bookmark Reply
			I have no idea about how wet any "usual" HI/P reaction gets, I have never performed one. SWIVE's observations are that alot of rxn failures can be attributed to not using enough water. I am just advocating common laboratory procedure, to use refluxing 57% HI (or RP/I2/H2O mixed as to form such a solution) so that the reaction temperature won't exceed that of boiling 57% HI (126°C). That's great! that's exactly what SWIVE is advocating. As I have never before seen any reaction in the literature being performed "dry" like that (except in mw rxns where the reactants is adsorbed on clay or silica gel, and they rarely run for more than 15min) SWIVE agrees, thats why he thought he had confused you somehow or was being unclear. He was surprised you brought this point up originally, as the method SWIVE is offering is anything but dry. I have a hard time believing that method has any real merit over a reflux (in real organic chemistry, decreased reaction time at the expense of lowered yield and increased amount of impurities is called a failure). SWIVE's goal was not to compare this to a text book reflux. SWIVE wants to improve what bees "actually" do.  SWIVE see's several merits here.  Shorter reaction time is a good one. Fewer impurities is another. Having a method that bees will actually do, that doesn't involve condensers and refrigeration is right up there on the merit list. Increased yields compared to current methods is yet another. SWIVE thought the reason he was going to do a comparison to a reflux for you, was because they've never been compared, so there is no data to draw a conclusion from. SWIVE uses the Ben Wiffen rule of posting.  If SWIVE's pets haven't personally tried it and verified it, SWIVE doesn't talk about it. Period (in real clandestine chemistry, increased reaction time at the expense of longer sentences and increased number of busts is called a failure). Real Men Don't Preview Their Edits
	wareami (Hive Addict) 10-07-02 16:21 No 365484		Threw Confusion...The Light Sprinkles EveryWare!	Bookmark Reply
			VE: Judging by your last response, Ibee gets the impression that you feel Rhodiums statement about merit was directed toward SWIVE's proposed route! As I have never before seen any reaction in the literature being performed "dry" like that (except in mw rxns where the reactants is adsorbed on clay or silica gel, and they rarely run for more than 15min), I have a hard time believing that method has any real merit over a reflux (in real organic chemistry, decreased reaction time at the expense of lowered yield and increased amount of impurities is called a failure). Rhodium will correct me if I'm wrong, but I believe he was refering to "DRY Rxn Methods" having no merit! SWIVE is clearly advocating the alternative, "Correct Method" that In Ibee's opinion should have superceded the "2hour chili run back to the DrawingBoard" method long ago! Ibee says that 15 initial failures "Rains Supreme" in the manual..."Eliminate the Wrong--Wayz to Succeed!" While these were good "FeetWetting" outlines, they hardly hold a candle to the achievable. Ibee regrets not taking the initiative for a proper Right-UP and commends SWIVE for the contribution! Besides, if Ibee were to do the Right-UP...the cost in Wareamiese Decoder Fluid (Tequila)alone would have driven the cost right through the Ghetto! VideoEditor gets Ibee and the Kidz vote of confidence! Peace of the REaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami
	Rhodium (Chief Bee) 10-07-02 16:38 No 365490		Why not?	Bookmark Reply
			One thing I find very strange is that not a single person during the last 15 years has made a large series of microscale tests on the RP/HI or RP/I2 method and with real analytical equipment determined the actual yield of methamphetamine in each run as to fully optimize the synthesis, considering how many tons of meth that get produced in the US alone every year. The increase in yields a single large-scale meth producer would pay for a brand new GC/MS (including a $100/hour wage to the risk-taking analytical chemistry graduate student he would hire for the job) in just a few months, as well as the results could then be of benefit to thousands of others forever.
	PoohBearium (Bear With Me) 10-07-02 20:33 No 365565		But...	Bookmark Reply
			...unless you one who is producing vast amounts, and are able to distribute this very quickly, anything above 50% will satisfy most.  It's a cheap drug, any supply quickly overcomes demand... IMO, PB "Reality is a crutch for people who can't handle drugs." -Lily Tomlin
	Rhodium (Chief Bee) 10-07-02 20:54 No 365572		The world doesn't understand me	Bookmark Reply
			How can 50% be satisfactory for any reaction you intend to repeat more than once? Am I the only person in the world who derive a deep feeling of pride and inner peace by seeing that I have among the millions of combinations of temperature/reaction time/solvent/concentration/reactant ratio/catalyst for a reaction to come as near completion as possible (considering the inherent limitations of practical organic chemistry as opposed to theoretical)? It is not a question of being cheap on starting materials, but rather a drive for being able to outsmart all the forces in nature which are all working against you achieving a perfect yield in every case, even though for many people the former reason is good enough.
	PoohBearium (Bear With Me) 10-07-02 21:16 No 365575		Try telling that...	Bookmark Reply
			...to a toothless Missouri man who can barely read the ingredients on the back of a Sudafed box. Just talking shit, as usual; my theory often holds no water within the scientific community. PB "Reality is a crutch for people who can't handle drugs." -Lily Tomlin
	zibarium (Naked) 10-08-02 16:30 No 366041		not even your mom?	Bookmark Reply
			rhodium, the type of scrutiny, or pride in one's work...that seeking of perfection..its pretty much not available without real equipment and reagents. i'd guess if fate had you scratching matches for rp, for instance, you might bee alot less willing to do experiments purely for the data. (besides, wouldn't those experiments bee illegal?)
	Rhodium (Chief Bee) 10-08-02 20:44 No 366114		If I could as a kid, you can do it now...	Bookmark Reply
			When I was in my teens, I experimented with various peroxide-based primary explosives, and as all the instructions for their preparation available to me at the time were bad anarchist texts from the net, they weren't optimized at all to give a high yield or anything. Starting with procedures yielding 30, or at best 40% yield, I worked my way up by trying different reactant ratios, solvents and acid catalysts, as well as making graphs where I plotted isolated yield against reaction time and somesuch until the yields were more than doubled. With HMTD and TMDD I finally attained molar yields which in both cases actually turned out to be between 5-10% higher than any of the syntheses of the compounds ever indexed in Chemical Abstracts (this was something I found out years later, when finally getting access to a university library). There is nothing magical about that, as optimization scrutiny is not the main priority of most publishing chemists, that is more a thing for process chemists in industry. At this time I was working with hardware store acids/solvents, and reactants extracted and purified from OTC items like Esbit fuel tabs - I was working in my mom's kitchen, stirred all reactions manually, filtered with coffee filters etc, and the only scale I had was a mechanical one only graduated in whole grams, but visual extrapolation gave me an accuracy of ~0.25g. This was the major weakness of my optimization protocol, I always had to run the reactions on about a 10-gram scale to be able to pinpoint yield variations of 2.5%, and when thinking I had a good procedure, I ran duplicate experiments at a 25-gram scale to verify that the procedure was reproducible, as well as getting an accuracy of my yield of 1%. Working in primitive conditions has no other impact on good science than you having to use more chemicals and the need for performing more tests, usually every reaction condition being tested in duplicate and the result averaged to compensate for lower accuracy in your measurements. Just reflect on the laboratory conditions any scientist had to work under in the 1800's, most people here has access to much better reagents and equipment than they did. Did that stop the chemists 150-200 years ago? No, not at all, much good science was done back then, with the occasional superstition lingering here and there, just like among the clandestine chemists of today.
	dwarfer (Hive Addict) 10-08-02 21:44 No 366144		rocket propellants	Bookmark Reply
			Ah yes, the joys of optimization. Now for me, and my c0-conspirator, (in high school..)it was how much more potassium perchlorate and aluminum powder we could put in our rockets before they would blow up (instead of launching ) on the angle iron guide rails we had set up at our secret desert launch pad. (In addition to the boring zinc and sulpher blend, I mean....) Wish I had all that powdered zinc I used to have.. =================== I appreciate your wistful reminiscence and guidance for optimization, Rhodium: but have thought on the same issue and wondered (in my micro-nano way..)  if it would not be better to derive a useful catalytic hydrogenation protocol that could be employable by the masses: Please correct me if I am wrong, but it appears to offer the following advantages: 1.  The reaction, if conditions were right, could run to it's completion without overcooking. If it ran to long it would be a waste of time and nothing else... 2.  The reaction, for reasons not fully understood by me, but referenced in several locations, yields 100% D isomer, instead of lesser %ages from other techniques. 3.  It would not require a gas chromatograph, or outside measuremdent. 4.  It would be more environmentally benign 5.  It could possibly utilize precipitated Ni, or U-Ni, thus being (pretty close) to universally attainable.. ============================== Whaddaya think? dwarfer
	Buster_Hymen (Resident Smart Assium) 10-09-02 01:00 No 366230		>potassium perchlorate and aluminum powder ...	Bookmark Reply
			>potassium perchlorate and aluminum powder >we could put in our rockets >before they would blow up Flashpowder, while suitable for crackers and such, doesn't make a very suitable propellent mixture at all... Are you sure they didn't ALL blow up?   \\|//     ô¿ô    --  Anger management? Fuck that!     \O/       '''
	ChemoSabe (Hive Addict) 10-09-02 01:18 No 366239		Viable E Synth + Catalytic Hydro	Bookmark Reply
			Dwarfer wrote, to derive a useful catalytic hydrogenation protocol that could be employable by the masses: Swim feels like he's on his last leg dealing with extractions of psuedo & RP and feels like a viable E synth and catalytic hydro method are just what the Dr. ordered as far as truly destroying any progress the WOD may have made on smalltime meth production. Swim don't have the know how yet to lead any such movements but will volunteer as a test subject for someone with enough experience and knowhow to blaze this trail. Sans dookie
	dwarfer (Hive Addict) 10-09-02 01:49 No 366246		rocket abuse	Bookmark Reply
			Seems like we tried KMNO4 and aluminum also, but I did not keep notes.. I know we tried a heavy dose of Al and perchlorate loaded first, with the Zn S loaded last: we figgered we'd get a flash of white light and smoke to let us know when the propellant had become exhausted... We were using 1 1/2 and two inch copper pipes if I recall, up to 4' long. The one in question got about 100 feet off the launch pad and announced it had indeed come to the end of the ZnS propellant by blowing its little nose cone off and splatterring the pipe into several different well stretched directions, which being less aerodynamic than usual made a lot of noise while continuing on it's perterbed drag modified tumbling parabolic path... all in all, a success: though we did not make it to orbit, we were well satisfied with the commotion.. Also, it was easy to find, as compared to those which returned to earth somewhere about 3/4 mile away, and which were buried up to their tailfins.. One of our greatest efficiency enhancements was in noting that master brake cylinder pistons, with their cast indentations on both sides, could be readily made into an approximation of a venturi with a hole drilled, and a rat tail file.. though made of aluminum, and therefore subject to significant ablation (understatement) during use, they beat the crap out of the welded or brazed washers we were using previously, (DUH) Our max was between 12000 and 13000 feet upways, but they were more fun when they blew up.  Well, not Really?? ============== We graduated to bombs, but that's a different story... dwarfer
	ChemoSabe (Hive Addict) 10-09-02 02:10 No 366253		Boys & Their Toys	Bookmark Reply
			Seems like there are quite a few in these waters who put their chemistry knowledge towards the development of both drugs and explosives. Not criticizing, just commenting. Edit: Drugs, Explosives and Insect Torture. Sans dookie
	zibarium (Naked) 10-09-02 02:26 No 366254		rhodium: that's why you're the chief bee!	Bookmark Reply
			i understand what you say. zib's that way w/ insects...quite patient and willing to uncover data that would bore most of us to sleep. perhaps its more to do w/ the illegal nature of clandestine chem...swim's never nervous that someone might show up when he's working on his ant-powered generator. even though they might suspect he's nutz.
	dwarfer (Hive Addict) 10-09-02 03:19 No 366286		insect abuse	Bookmark Reply
			My predelictions ran to insect study as well. I had made a gas plasma discharge tube, which required evacuating a fairly large tube, 3" by 12" (Crook's dark spaces and all that, dontchaknow.. ) Anyway, at 42,000 volts i was getting some low grade x rays, or so I was told, though I could not seem to develop any film with a key on it or anything, inside a light proof envelope, (which disappointed me..) but anyway, I investigated the hypothesis that smaller insects would live longer than larger insects in a vacuum, a shitty hypothesis to be sure, but investigated with vigor nonetheless by my adolescent beingness. sure enough, i had to actually give the damn ants a few blasts of ions to persuade them to go to Ant Heaven: those with segmented abdomens, like your basic grasshopper, were more cooperative in displaying the pressure differential they were experiencing. Flys could not fly, in a vacuum: even their buzzes were muted by the absence of conductive media. well: enough about my childhood insect studies: I'm beginning to feel guilty..  OH yeah! dwarfer
	VideoEditor (Hive Bee) 10-09-02 07:15 No 366354		Boy Toys	Bookmark Reply
			When SWIVE was 8 he was getting conc nitric acid from the local university to make gun cotton. It sure was nice of dad to work in such a fun place. SWIVE also be-friended the head of the chemistry wing who was a pyrotechniqes expert and a top consultant to the military on explosives. SWIVE made extra money through high school selling home made fireworks. Some of SWIVE's other projects (up until women, cars and drugs where discovered) included: Telsa Coil 35Kv and 50Kv Organic Liquid Dye Laser Carbon Dioxide Infra Red Laser Radio and TV Jamming device Electro Magnetic Pulse Generator and he built them all before the internet or personal computers. Real Men Don't Preview Their Edits
	geezmeister (Bee of the Month) 10-09-02 20:58 No 366564		how will we start this from rP/I2	Bookmark Reply
			Suppose we intend to reflux from the start, and not from the start of phase two of the reaction, as I have become accustomed to doing after a fairly dry start. My procedure went wetter from the start after I followed VE's freebase notes in the looping reaction thread. It it still not that wet at the start. Whether freebase or HCl from of the precursor is used, I am accustomed to having the rP and I2 make HI and let the reaction proceed from that point. In neither type of reaction do I start with heat until the rP and I2 have made the HI. It seems if I added even more water at the start, it would impede the formation of the HI at the outset. It would seem to me the logical method of proceeding if one wanted to reflux from the outset would be to make the HI by reacting the rP and I2, and when that initial reaction was completed, to add the pseudoephedrine, stir, add additional H2O if needed, then apply heat. Other suggestions on starting from rP/I2 do to a full reflux from the start of the reaction? Mostly harmless
	VideoEditor (Hive Bee) 10-10-02 00:55 No 366634		reflux	Bookmark Reply
			Once your past about 1-2ml DH2O per gram of I2 heat will be nessesary for good HI production. Aproximately 140f will do the trick. Here's another path I've been toying with. I2 and RP in naptha instead of water makes alot of HI especially with a little heat. FYI I2 in naptha alone will make HI with a little heat. Real Men Don't Preview Their Edits
	Leary1 (Stranger) 10-10-02 01:49 No 366653		Hi from I2 and naptha..	Bookmark Reply
			This seems worth experimentation..naptha instead of water introduction in rxn?? Spedrup
	handsfull2 (Hive Bee) 10-10-02 02:14 No 366661		I2 and RP in naptha	Bookmark Reply
			U-got me on your side VE, BUt Im a little uncertain about the Hi from naptha and I2 alone. If I heard you right then the rp would not bee needed is that what your saying? "Go ahead jump  "
	RepVip (Hive Bee) 10-10-02 02:49 No 366671		HI	Bookmark Reply
			I've been trying to figure out how the HI is produced for quite a while.  I would really like to see a balanced equation that shows how the RP + I + ? reacts to form the HI?? I've searched everywhere.  I even checked out a book titled Reductions in Organic Chemistry which talked about HI, but not how it was formed from RP/I2.  The book metioned that pure HI has a boiling point of like -33° (this # isn't exact, but I know it's close) and azeotropic 57% HI has a BP of 126°.  The book mentioned that reduction with HI + Acetic acid greatly increased yields. Oh, I also recognized this passage in that book -------------------------------------------------------------------------------- Hydrogen iodide dissociates at higher temperatures to iodine and hydrogen. The reaction is reversible. Its equilibrium is shifted in favor of the decomposition by the reaction of hydrogen with organic compounds (iodoephedrine in this case) in the reduction, but it can also be affected by removal of iodine. This can be accomplished by allowing iodine to react with phosphorus to form phosphorus triiodide which decomposes in the presence of water to phosphorous acid and hydrogen iodide (a cyclic oxidation of the iodide anion to iodine and reduction of iodine back to the anion by the red phosphorus, the latter being converted to phosphorous or phosphoric acids). In this way, by adding phosphorus to the reaction mixture, hydrogen iodide is recycled and the reducing efficiency of hydriodic acid is enhanced. -------------------------------------------------------------------------------- which is almost word for word from this text at Rhodium's site: http://www.rhodium.ws/chemistry/meth.forensic.html Anyways, I think HI production has something to do with this: H3PO2 + H2O + I2 ==>> H3PO3 + 2HI, and the passage which is bold up above.. I was hoping somebody could show me the balanced equations of how it all interacts?
	Rhodium (Chief Bee) 10-10-02 03:10 No 366681		RP + I2 -> HI	Bookmark Reply
			It is no mystery, it is a simple reaction: 2 P + 3 I2 -> 2 PI3 2 PI3 + 3 H2O -> 6 HI + 2 H3PO3 H3PO3 can also react with I2 at elevated temperatures to form HI according to the formula in my "HI Recycling - RP Substitute" thread. Alcohol, an unconsciousness-expanding drug
	RepVip (Hive Bee) 10-10-02 04:34 No 366703		Thanks	Bookmark Reply
			That was easy. I figured it would be easy.. I was just having a hard time thinking where the 'H' came from, but duh. Would producing HI really work in Naptha?  For what it's worth, the MSDS on VM&P Naptha states: CONDITIONS TO AVOID: Oxidizers, Strong Acids, Heat and other ignition sources
	VideoEditor (Hive Bee) 10-10-02 16:42 No 366917		getting HI'r	Bookmark Reply
			Producing HI in naptha with RP/I2 seems to be no problem. The catch is when / or how to add the free base. It wants to combine with the I2 to form iodopsuedoephedrine which is insoluble in naptha and falls to the bottom. The iodomethamphetamine produced is also insoluble in naptha. SWIVE has tried a few tests using 1/2 naptha and 1/2 water, but can make no claims to any benefit until more research is done. HI from I2 and naptha alone is based on Patent US1380951.  Both RP/I2 in naptha and I2 in naptha require heat to generate HI. Real Men Don't Preview Their Edits
	Jetson (Hive Bee / Eraser) 10-10-02 18:34 No 366944		geez	Bookmark Reply
			"It would seem to me the logical method of proceeding if one wanted to reflux from the outset would be to make the HI by reacting the rP and I2, and when that initial reaction was completed, to add the pseudoephedrine, stir, add additional H2O if needed, then apply heat. " that's how jetson does it.  with a 24hr reflux of course.  the ratios he usually uses are- 3e:3rp:6i2 and 6ml of dh2o.  he adds 6g i2 to 1g lgrp suspended in 6ml dh2o and lets react for about a half hour then adds the psuedo(e) and the rest of the rp and swirls.  all of this while on heat, then finally refluxes for 24hrs with good results.  usually gets about 70% of product back on the average.  not sure of the actual temperature the reflux reaches.  jetson shattered his thermometer and hasn't had a chance to pick another one up yet(lazy bastard).  one point to make though is that after a certain point, probably up into the ounce scale, the h2o addition could probably be scaled back or even ceased all together.  but jetson assures me that these ratios given are tits for small rxns(that's all he does, sorry he's not the west coast supplier) ^the devil is so lonely
	VideoEditor (Hive Bee) 10-10-02 18:56 No 366949		Gotta do a comparison	Bookmark Reply
			Hey Jetson, Using your starter amount of E, that would translate to 3E/1.5RP/4.5I2 and 2.5ml DH2O using the wet start formula. SWIVE has been getting the same yeild of almost 70% but in 7.5 hours.  I wish there was an easy way to compare the impurities in the field. SWIVE's burns clean and has a good melting point within a few degrees. Real Men Don't Preview Their Edits
	Jetson (Hive Bee / Eraser) 10-10-02 19:40 No 366955		that's psuedo.hcl...	Bookmark Reply
			yeah that's psuedo.hcl jetson uses you do realise that correct?  just making sure not trying to push anything, just making sure you know it's not the freebase as jetson didn't specify in the first post hcl.  yup burns clean as can bee.  with a nice long buzz.  haven't had a chance to measure mp either as jetson used to use his thermometer for that also(not sure if it was a real accurate way to do so or not but seemed to come awfully close to the stated mp of substances.)  but after it melts it quickly recrystalizes back into nice beuatiful shards.  that's if it's not all sucked down swij's throat  the 1 to 1 ratio of rp to e may be way overkill in jetsons rxns but one does want to make sure all gets converted. as with is the case for the i2.  probably could scale that one back but what's the sense in skimping and getting a half reduced or unreduced product?  now, swij is just saying in jetson's thought process that's what goes on.  not at all trying to say that it wouldn't work or for everybee to go out and load up there rxn with excess rp and i2.  jetson just goes a little overboard sometimes,  he's out for quality and quantity of returns.  the rp that is left unused is always easily gotten back from the end of a rxn.  ^the devil is so lonely
	handsfull2 (Hive Bee) 10-10-02 20:05 No 366957		6 grams of I2?	Bookmark Reply
			Jetson your numbers do seem a little to much IMHO. Have you tried 1 to 1 ratio for small rxn's ? SWIHFT has'nt tried with higher numbers in a long time, He remembers a few months back when  2 to 1 ratio worked great . "Go ahead jump  "
	PoohBearium (Bear With Me) 10-10-02 20:30 No 366961		Is this...	Bookmark Reply
			2 PI3 + 3 H2O -> 6 HI + 2 H3PO3 Is this reaction reversible (equilibrium), or is there any way the phosphorous can be salvaged with some type of catalyst? I'm sure this is common knowledge to most, but I'm stupid and lazy... PB I AM a dog, but im not humping your leg, so quit kicking me!
	Jetson (Hive Bee / Eraser) 10-10-02 20:44 No 366964		6g i2	Bookmark Reply
			well,  only 1.5 grams overkill.  that's going be the 1:1:1.5 ratio's that alot of people seem to use for smaller rxn's.  now as it's scaled up swij does usually cut back to the acclaimed 1:1:1.5 ratios.  that's for say 10g and up though.  jetson rarely does 10g or up at a time.  why?  who knows, guess he likes spending time in the lab. ^the devil is so lonely
	Rhodium (Chief Bee) 10-10-02 21:48 No 366983		I wish there was an easy way to compare the ...	Bookmark Reply
			I wish there was an easy way to compare the impurities in the field. Video: You sure seem to be a person perfectly capable of running a TLC comparison. Easy & Cheap. Poohbear: What do you mean by "salvaging the phosphorus"? You want to turn what into what? Alcohol, an unconsciousness-expanding drug
	PoohBearium (Bear With Me) 10-10-02 21:58 No 366986		What I mean...	Bookmark Reply
			...is:  Can you convert the phosphorous acid into a usable form for reducing, or is it pretty much pointless to go through such effort, if such effort actually exsists? PB I AM a dog, but im not humping your leg, so quit kicking me!
	RepVip (Hive Bee) 10-10-02 22:05 No 366989		Excellent Patent VE! Any information I can find ...	Bookmark Reply
			Excellent Patent VE!  Any information I can find on HI I eat up like steak! The patent mentioned that I2 in naptha would produce the HI gas..  Is this going to be a problem?  Would you need to capture the gas in water to be able to use it sufficiently?  The only idea I had was if you could use a solvent which was denser than water.  That way, any gass produced could then travel up through a water layer and be catured? Hmm.. the patent mentioned unsaturated solvents worked better, and the patent also preferred using terpene hydrocarbons (C5H10)n.  I think this is worth looking into.
	Rhodium (Chief Bee) 10-10-02 22:15 No 366991		Recycling of iodine	Bookmark Reply
			Pooh: No, when it comes to phosphorous, spent is spent. You can however recover a whole lot of sodium iodide from the basic aqueous phase after the acid/base extraction of the post-reaction solution. Just acidify the aqueous phase using sulfuric or phosphoric acid (not HCl) and precipitate the iodine with hydrogen peroxide using known techniques. How many people here are recycling their iodine like this, and how many are throwing it out? Alcohol, an unconsciousness-expanding drug
	geezmeister (Bee of the Month) 10-10-02 22:57 No 367007		SWIG figured it out	Bookmark Reply
			After trying a bunch of times with HCl without any luck, SWIG acidified the remaining mix with H2SO4 until it foamed the way vinegar and baking soda does. He added a little more acid, to be sure the solution was acidic, and then used bleach, adding a little at a time until the mixture changed color. He let this sit until what he assumes is I2 settled out. Rather than make crystals, he has some black, amorphous powder with chunks or varying sizes, from sand grain to very small pebbles.  He has several ounces of this saved, dried after rinsing well, and plans to sublime it for usable I2. At least a part of it is iodine, as it stains like iodine and if left open will yellow everything around it over time. Those are familiar signs to SWIG. He recently tried with peroxide and had better luck. He got some crystal formation, not as much as he hoped, but he thinks he is getting in the right ballpark. If he can get it to yield I2, at a worthwhile rate, he'll share the technique he used, but right now he's just getting the hang of it. And it isn't like he does this every day. He has learned to just let it sit for several hours, sometimes this has been overnight, as the process seems to be fairly slow. And yes, it is getting harder to get I2 around here. Gotta go, the red P fairy just called....!!!!!!!!!!!!!!!!!!!!!! Mostly harmless
	ChemoSabe (Hive Addict) 10-11-02 02:21 No 367082		Oil bath & Temp Taking	Bookmark Reply
			This recipe calls for an oil bath and temperature taking. Two things swim has no experience with. In dreamland swim does posess a decent collection of mid sized flat bottomed 24/40 flasks, a matching stillhead that is thermometer ready and a lab grade centigrade thermometer that fits the still head. The question on swims' mind is will the above mentioned setup work OK for this rxn? And if so what then to do about the downward pointing joint on the stillhead to keep rxn fluids from distilling out of it? In the recent Newbee Forum thread titled "Oil bath or heating mantle?" terbium stated "You should be taking the accurate temperature readings at the still head at the top of the column not at the boiling flask." The context of this comment had to do with fractional distillation but swim wonders if it would also apply to temperature monitoring in this wet start rxn. Sans dookie
	VideoEditor (Hive Bee) 10-11-02 06:49 No 367163		temps	Bookmark Reply
			ChemoSabe: The main reason SWIVE uses oil bath temps are because he doesn't use a still head for reaction's.  SWIVE uses a column or condensor if refluxing, or a 20/40 hose adaptor if hooked to a P/P unit. SWIVE does'nt have multineck flasks for this purpose. We are not distilling so if your using an internal thermometer, I would think you would want it closer to the reaction mixture. Internal temps are usually 10-15 degrees lower, but there's alot of variables so your glassware may differ. Real Men Don't Preview Their Edits
	ChemoSabe (Hive Addict) 10-11-02 07:31 No 367187		Glassware Setup	Bookmark Reply
			So here's a theoretical setup. 1000ml (or 500ml) flat bottomed flask. Claisen adapter with 2 24/40 necks on top of that. Still head with thermometer in center neck. A 100ml 24/40 round bottom flask is used to plug the still head drip outlet. Stopcock adapter in outer Claisen neck for gas exit. Flask rxn temp is calculated by converting centigrade to farenheit and subtracting 10-15 degrees from farenheit temp. So far given swims current theoretical dream labware this seems to be maybe the setup/strategy to use. Comments/suggestions still appreciated though. Sans dookie
	VideoEditor (Hive Bee) 10-12-02 12:41 No 367619		I'm sure it would work fine	Bookmark Reply
			I'm sure it would work fine ChemoSabe. The worse side effects might be more stuff to clean up later and more places for leaks to develope.  I beelieve 3/4" tubing fits nicely into a 20/40 joint. (it maybe 5/8" dwarfer would know this fer sher). You could just run that out of the reaction vessle and just monitor the oil temp. The temps stated in the reaction are already in farenheit so no need to convert. A +/- 5 degree error is probably acceptable. Your visual observations will tell you if your right or wrong. At the first temp the flask should be filled with dense white HI mist. At the final temp there should be a gentle bubbling (not boiling) with a noticable phase II along the way. Real Men Don't Preview Their Edits
	ChemoSabe (Hive Addict) 10-12-02 17:57 No 367682		More on the oil bath	Bookmark Reply
			While sleeping swim poked around in his REM based alpha wave lab while snoozing last night and discovered he had a rarely used 500ml 3 necked RB flask that would allow the thermometer deeper penetration into it than the flat bottoms. The question for swim then becomes stability. Swim has no lab clamps or proper stand (an old photo enlarger is currently used as a basic rxn "platform") and previous attempts to set up a rxn situation with round bottoms have been very "mousetrap-like" scenarios in which the whole thing had the scary potential to spectacularly and quite dangerously cave in on itself. Also the nighmarish visions of the arrival of the tag team combo of a fire crew and a hazmat team  has swim shudering when considering setting up the oil bath dream. Is there an advantage to using oil over water for this? And what's a recommended type of vessel to house the oil. Sorry for the newbee-esqe line of questioning here but swim has hoping to never have to deal with an oil bath. For some reason it's just reeked too much of danger potential to him. Also, previous mentioning of doing the c to F conversions has to do with swim's thermometer only reading in C. Sans dookie
	zibarium (Naked) 10-12-02 19:10 No 367691		oil bath	Bookmark Reply
			chemosabe; assuming a hot-plate w/out flame or spark, oil bath should bee no problem. it is preferred over water for several reasons...mainly, that it won't evaporate at the temps needed..whereas H2O will...needing to bee re-filled along the way. Rb flasks are sweet, but a slight problem to keep in place..especially because the flask would like to float up from the pan of oil. (btw, oil pan could or should bee a visionware glass pan or similar glass that can handle temp swings well). swiz has dreamt of a camera tri-pod over the pan, with various clamps, to keep things situated in the proper position. the clamps could bee spring clamps from a hardware store, or other similar set up, as long as the clamp doesn't break the glass. so metal shouldn't contact the glass-ware. rb flask should bee immrsed in the oil but not quite touching the bottom of the pan. it is handy to have a quick-release arrangement on your set-up, in case you need to pick up the flask in a hurry. (don't want to bee un-wrapping duct-tape during a tense moment). a bit of fussing and chem-hack ingenuity will get you a good arrangement.
	ChemoSabe (Hive Addict) 10-12-02 21:18 No 367722		Ghetto Setups	Bookmark Reply
			Swim's experience with ghetto setups isn't a good one. And considering what gear he's currently got available doing the oil bath still seems like it would be leaning too much towards ghetto. The reason he invested in the FB flasks was to avoid things like this but maybe it's time again for him to hit up the auction sites. BTW - is olive oil decent for the bath? And no Popeye wisecracks! Sans dookie
	zibarium (Naked) 10-13-02 04:12 No 367801		for the temps needed;	Bookmark Reply
			any oil would do...but it sure is nice to bee able to see thru it. in a long rxn; the water evapping can bee a hassle. partly because the water added should bee brought up to the same temp beefore dropping it in there. (olive oil sounds a bit extravagant...are you italian?) btw, even a fb flask wants to float up, no?  how do you keep it in place? water's damn handy in as much as its such a handy temp indicator when it starts to boil. and because that 100C hardly needs to bee exceeded in this rxn, it could bee the safest way to go if a bee had marginal heat control or thermometers. a bit of salt tossed into the water bath at the end would allow a brief moment of exposure to higher temps. otherwise, oil rocks!
	aztec (Hive Bee) 10-13-02 06:28 No 367827		bath	Bookmark Reply
			Chemosabe, if swic isn't doing oil baths, how would one do long (as in 12 or 24-hour) refluxing? What would one use in a bath to maintain a steady reflux temp? Always looking for more tips. Free Speech Free Choice
	ChemoSabe (Hive Addict) 10-13-02 07:42 No 367849		Floating FB flasks	Bookmark Reply
			Zib inquired, "btw, even a fb flask wants to float up, no?  how do you keep it in place?" Consider yourself privelaged Zib. This is a secret trick that hertofore swim has never told but since he holds you in such high regard as both an elder and a priceless and invaluable living relic of the hippie era he's gonna let this one loose. The key to keeping flat bottomed flasks from floating up when dreaming is....drumroll. Not using an oil bath. So far swim swears by this practice and only once while dreaming under the influence of massive sleep dep did the flask appear to float. Also for Aztec. Swim just told me that in addition to the oil bath he's also never tried long reflux rxn's. He learned his kitchen craft when Worlock's one hour rxn's were all the rage. Swim now refers to his somewhat outdated and habitual procedure "the knee jerk reaction" due to fact that swim could now do it in his sleep. Old habits die hard for swim so this adapting to new methods is like pulling teeth for him. I hear tell that BenWhiffen and his motorcycle chasing angel have a good long reflux writeup somewhere in the archive. Swim just yelled to me that it's now on his priority reading list. Oh and BTW Aztec if you'd like to share a hot oil bath some day I'd be up for it more ways than one Sans dookie
	wareami (Hive Addict) 10-13-02 08:19 No 367858		Oil baths and such!	Bookmark Reply
			High Aztec: Thare you are!!!! Steady temps are critical to control. Maintaining Oilbath temps has always eluded the Kidz because it seems to flux-uate (no pun intended) H20 baths have seemed more stable but the air temp, if say in an Airconditioned evironment, with airflow from the vent, tends to cool at the surface at various intervals! When refluxing, the Kidz just use the warmer from a coffee maker. Put the Flask right on the warmer. It keeps the internal temp at a steady 90°C. Always do a test run on the burner first with just h2o as some warmers may vary at the holding temperature. Since refluxing...the necessary phaseII is seldom seen and is not brought on with higher temp as it is with faster rxns. Higher temps seem to introduce unwanted impurities also. Watched Pots never boil anyway so the Kidz learned to just put everything on just before Ibee Tucks them in for BeddyBye! This brings new meaning to the term "Stirring when the Rooster Crows". Upon Awakening, they check, stir, and Hydrate if necessary. Peace of the REaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami
	zibarium (Naked) 10-13-02 10:02 No 367888		flattered, but still dumb	Bookmark Reply
			chemo? in saying that you don't use an oil bath, should i deduce that you use a water bath? if so, same floaty problem as oil...slightly less, because oils are generally lighter than H2O...but if one is to have a decent surround of heat-transfer medium on their flask (i.e., water or oil) how is the flask not floating up? no bath at all? a very shallow bath which allows a fb flask to sit on the pan? don't worry...i'm often this confused
	ChemoSabe (Hive Addict) 10-13-02 11:10 No 367914		bathing	Bookmark Reply
			The whole reason swim axed about baths was 'cuase of zero bathing experience. Actually swim's maiden voyages into baked goods were done with a small RB flask that was immersed in fine silica sand which was housed in a pyrex measuring cup that sat atop a hotplate. So that might be considered a sand bath of sorts. After that swim graduated into larger FB's on hotplate only. I've never seen an FB that had a thermometer well on it but I saw that swim had one on his Xmas liszt whether they exist or not. Sans dookie
	Chicken (Hive Bee) 10-13-02 11:17 No 367918		It's called a clamp	Bookmark Reply
			You guys ever heard of using a lab stand and a clamp?  Thats will keep it from floating.  You can easily build a stand, just make sure it has enough weight on the bottom.  Also You want it to be floating in the oil, yo don't want it touching the bottom of the bath, you only want the heat transfred from the oil to the flask, not the botton of the pan.  A ring stand can very easily be made. The complete details are givin in the picture above. The base of the ring stand should be cut to shape and covered with a sheet of lead to give it sufficent weight so that the stand will not tip over easily when in use. The top of the base should be covered with the same acid proof paint as the bench above is coated. (see the above formula). The standared is fastened to the base with two nuts as illustrated. The ring is very easy to produce. The wire should be very heavy so it will hold its shape. The method of holding it in the brass peice which slips over the standard is clearly shown. About three of these rings of different sizes should be made for holding different sized dishes and crucibles. Ringstands are very much used around the laboratory not only as a convenient holder for dishes / glass-ware being heated, but also for general apparatus set-ups. BY~ThE WaTcHeR (would give web address, but not sure if it sells stuff or not)
	zibarium (Naked) 10-13-02 18:30 No 368030		no bath? must bee a hippy?	Bookmark Reply
			yeah, zib's dreamt up a homemade lab stand and clamp deal. works well...using camera tripod and clamps. tri-pod even taped to table so it won't slide around. zib keeps flask from touching bottom of oil pan; has thermometer clipped to the oil pan, so it doesn't need to bee in the flask. chemo? wouldn't you prefer round bottom? seems to facilitate a better swirling of gasses, and sliding of goo. only rub is the stand and clamp deal...not hard to arrange. swiz's first attempt was in fb flask (w/fb rxn) and he didn't like the way stuff got stuck on the sides...but had it too dry. anyway, sounds like you know what you're doing...and there sure are alot of ways to do anything. swiz's little dreams are boring. don't even need to babysit the rxn. (probably shouldn't have said that...like asking for trouble...but its true.)
	aztec (Hive Bee) 10-13-02 18:34 No 368032		Don't want to muddy the oil	Bookmark Reply
			I don't want to muddy up VE's great thread so I'll ask just one more question about baths and be on my way. Chicken, that looks very handy and easy to make, as well as more permanent than what swia is using. Although swia rather likes this set-up:  a balloon stainless steel whisk that fits perfectly and tightly over the neck of the flask, suspending it above the pot floor about 2.5 cm. The whisk handle is clipped over the pot handle for easy removal. However, a more permanent set up is probably in swia's best interest. On the other hand, swia is always searching for ways to simplify her life. Oil is messy and given the size of swia's undertakings (no more than 10g in size) I wonder if Wareami has the right idea with simply using a coffee maker warmer in refluxing. Would a small rxn of 10g's suffer that much without the surround of a heat transfer medium if steady and adequate heat is placed directly below the flask? Free Speech Free Choice
	geezmeister (Bee of the Month) 10-13-02 18:37 No 368033		Crock pots	Bookmark Reply
			There is a very handy device at the housewares aisle called a crock pot. If you are convinced that crockpots do not get hot enough for your reflux, buy a small deep fat fryer. You will need to adapt a rheostat for the deep fat friers, as IME they get too hot-- I've never found one with a temperature adjustment with the range I needed.  If you plan on using these, a standard and some rings and  clamps that attach to the standard are invaluable.  SWIG is testing out a new crock pot at this very moment. He told me between sips of his mocha java that he'd be crossing the twelve hour line around dinner time. You have to be from where he's from to know when Sunday dinner is served. I'll check in with him later today and see how things are going. Mostly harmless
	zibarium (Naked) 10-14-02 06:50 No 368336		one temp setting?	Bookmark Reply
			aztek; probably doesn't matter much...but one of the advantages of the bath of oil (or whatever) is its thermal mass...especially if the pan is quite a lot bigger than the flask. this mass of oil is slow to change temperature, in spite of variations from the outside, and the inside, of the flask. in theory, one could carry on with a heating element that had only one setting...the high end of what you want at the end of the rxn. starting with a pan of cold oil, and a flask of cold precursors, one might simply turn on the heat and let it slowly rise, over the course of a few hours, to the reflux temp. seems like glass is much less apt to break when not in contact with hard surfaces of different temperatures. round is good for that. doesn't hardly permit that sort of contact; and has structural integrity that a flat bottom could die for. experiments in sealed containment devices; submerged within an air pocket provided by a cover, with a non-polar layer floating at that portal; all within a large pan of salted water with a tight fitting lid....that's what's up in a nutshell.
	wareami (Hive Addict) 10-14-02 07:29 No 368346		SimpliCITY=Ghetto	Bookmark Reply
			The only reason the Kidz use the coffeewarmer is for simplicity and for unsupervised cooking. Seeings how the Kidz are Boyz, they wouldn't think of using the "LittleSuzieHomeMaker" oven. Basically, their high profile lifestyle comes into play as well. Size Matters as we know too. Depending on the size of the vessel, not all coffeemaker warmers will work because of the HeadRoom being limited by the filterbasket...so this would be a consideration as well! Considering the temps of reflux by this method of the Kidz, the larger variety of hotsauce bottles fall well within the safety threshold and also fit under the filterbasket and since the topic is refluxing/wet controlled rxn, 10g will have the needed headroom inside that vessel! Violent quick reactions and going into phaseII would be a concern with that volumevessel with the 10g`er! Shopping around is all part of the resourcefulness that bees are famous for and finding just the right way that works is what spells success. Peace of the REaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami
	cthulhujr (Hive Bee) 10-16-02 20:05 No 369270		wet rxn + FB	Bookmark Reply
			Swim was messing with FB rxn, and water quantity. Swim has come to no rock solid conclusion, but made an interesting observation, any input would be appreciated. Swim tried out VE's reaction as written at the top of this forum, 10g FB no problems, all went well. Taking into consideration Rhodium's, post that ~25ml of dh2o could possibly be used for a 10g reaction of FBPsuedo. Swim decided on trying a wetter reaction, reflux-wise, start to finish, on a larger scale. 26g FB Pseudo(extracted VE's STB-method) 12g LGRP (new, not re-run) 40g Iodine Crystal ("dried" extracted from tincture) all the ingredients were well dried swim placed the I and FB in a 500ml round/flat bottom flask, and slowly added dh2o with stirring until 50ml was added, the slurry appeared to be the same consistancy of swim's typical HCL reflux (sadly swim eyeballs h2o addition normally, and the exact amount in his HCL reflux, was only estimated, but seemed quite close, and is evidently more than he previously guessed, trying to take into account the solubility differences) The mixture was chilled 10 minutes, in an icewater bath. Swim added 3g of rp slowly with stirring, the mixture was warmed to room temp, and 3g at a time the rp was added with stirring. With the last addition a little white smoke slowly formed, as the rp reacted with some tiny granules of I2 that had not broken up. The flasked was topped with a 12" graham condenser, triple thick latex condoms were taped to the top of the condenser, which was circulated with ice water. The reaction was warmed (oil bath) to 160F over 2 hrs, whispy very thin white smoke circulated over the mixture for the first 2hrs or so. The reaction was held at 160F for 8hrs, raised to 175 for a further 6hrs. Swim noticed no "action", bubbling etc in the reaction, although the rp seemed to slowly rise and fall from the top to bottom of the mix, which was transparent yellow with a red tinge at this point. Swim had a feeling something may be amiss, and raised the temp to 195F, which was held for a further 6hrs, the reaction proceeded the same although lost it's red tinge and appeared only a bit yellowish, the condoms remained about erect, but not expanded during the course of the reaction.  swim raised the heat to 205F for 1 more hour for good measure, then began the final work-up. 150ml hot dh2o was added, swirled, solution was filtered of rp, poured into a 500ml sep funnel, and washed with 80ml of xylene 2 times, the  first xylene took on alot of the yellow, which alarmed swim slightly, the second was only tinged slightly. The mix was water washed 3x with 80ml hot dh2o and 80ml fresh xylene was added. Swim began to basify slowly with cold naoh saturated h2o to ph 13, as the mixtured cooled and was basified, FB Pseudo crystals began to fill the xylene layer and the top of the auqueous layer, 19g of them were recovered from the solution. More may have been present, but swim in frustration was a bit sloppy. A small amount was burn tested and definitly smelled of Psuedo, albiet the odor wasn't quite as potent as freshly extracted psuedo seems to be (perhaps some other forms were present?). Swim "salted" 4 grams to HCL, and reacted with 6g I, 2g lgrp, and 1.5ml dh20, at a simple 190F for 3.5 hrs in a sealed 250ml bottle, after work-up, with no recrystalization and only a acetone rinse, the final product burned almost completely clean and bio-assayed as per norm, with a yeild around 2.3grams! not shabby, considering, (swims scale may give or take .1g) This was done to simply confirm what the pre-reacted feed seemed to consist of. Swim is by no means knocking a FB reaction, with this post. Swim is confident that the same HCL rxn, with the same amount of dh2o, would complete after 16-20hrs reflux, under these conditions. Swim will carefully measure, his dh2o on the next HCL rxn, to confirm this theory. Swim is coming to the opinion that FB may indeed need to be ran with less dh2o, and thought some bee's may interested, or be able to point out any possible, screw-ups swim made (other than using a 26g rxn, to 'experiment'). This hypothesis is based soley on observing this reaction. Should swim have simply let the rxn continue? Just plain old is using to much dh2o? Need to maintain higher temps longer? For whatever it's worth, there it is. PS(edit)-- In the short time since swim posted this, he attempted to more accuratly quantify the amount of dh2o, he typcally uses in HCL dream, it is approx 1.5ml per gram, swim will run a HCL, dream at 2ml per gram, to make certain the increase in h2o won't likewise affect an HCL reaction. Iä-R'lyeh! Cthulhu fhtagn! Iä Iä!
	wareami (Hive Addict) 10-18-02 00:57 No 369717		Fluid Measures and Hip Waders	Bookmark Reply
			cthulhujr: Ibee doesn't know if others bees are experiencing the same observations pertaining to cook times! Complete reduction appears to be stalling around the usual finish line! This has been noticed the past two months on HCL feed reflux rxns and if Ibee were to make an educated guess as to the cause, he would lean towards a pill additive that hinders the conversion! This would line up with what CRAPSHOOT posted a while back concerning the Pharms Foiling the Birch and HI/RP rxns! SWIC seems to have ruled out cleanliness of starting feed as the root of the problem. Most failures are centered around the inactives and a more complete diagnosis hinges on including the strength and the listed ingredients that SWIC started with. Ibee's experience with wet refluxing points to the "Cook Time" as to why SWIC came UP short. Just as he suspected! Judging by SWIC's description, the reactants were in more or less "a solution", correct??? They way Ibee understands it, Wet rxns are refluxed longer to allow for the excess H20 evaporation. This explains why there isn't much activity during wetcooks until the conversion starts taking place when all the reactants come into full contact with each other again! In solution they are like BumperCars(Right BenW???) until the mass thickens again! Even if it takes 5 days, Ibee always waits for the "WAD-Dewd" who always looks like a blob of bubblegum on a hotday! So in answer to the questions: •Should swim have simply let the rxn continue? Yes •Just plain old is using to much dh2o?Could be, but the purpose for wetter rxns seems to less impurities created and the trade off is "Time"! •Need to maintain higher temps longer? This works as long as the temp stays under 95°C, so impurities aren't introduced that have been associated with "ShootingStar Vision" Hope this helps some! Peace of the REaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami
	cthulhujr (Hive Bee) 10-18-02 05:20 No 369806		cook times	Bookmark Reply
			Swim certainly wishes he'd just let the rxn, run at this point swim has never refluxed past 24hrs, and only a few times past 16-18, albiet with a bit less water.   Swim is still planning a HCL reaction under the same conditions, and just extracting a small amount of the solution at the 23hr mark, to check out and let the thing go if need be. The same type of pillstock will be used as well. Swim can't think of why a difference in amount of h2o in FB vs HCL, would be needed. But swim wants to check it out.    Swim has observed, the rxn seeming to thicken as it progresses normally, even though the volume of the rxn appears to change very little. This one did not.   Swim hasn't noticed reactions stalling, until now of course, but wouldn't rule out the possibility. After all, swim has steadly stretched out cook times, over a long period of time, to improve potency of product. It's very difficult to recall whether or not those old 3 or 4 hour cooks were really any less potent than the long ones are today, when all variables are considered. The last 24hrs have revealed swims quicky nano, of some of this unreacted feedstock, is less potent than normal, despite appearences. But then again no recrystalization, (or steaming), will definitly account for much of this.  US Patent 6,359,011 certainly describes reaction inhibitors,and that was written way back in 1999, they must be far more sinister by now.  Swim would think recent pill extractions should certainly remove this stuff, quite effectively. But, whether or not any bees have positively confirmed this with a real analysis of the Psuedo, is not know to swim.  The input is greatly appreciated wareami, by the way, what is the longest reflux swiw has done?  seriously 5 days?? Nearly forgot, swim didn't consider feedstock cleanliness, to strongly, as the feed was extracted via VE's Universal, from the name brand red hots. Swim normally uses his own waterless variation, but used STB when trying the first 10g FB run, as per this thread, just to get as close as possible to what VE's got going on. And since the carbon, cornstarch etc. was ready to go well..., plus swim was short on solvents he typically uses. Previously, both of these methods have been satisfactory, on said pillstock. Iä-R'lyeh! Cthulhu fhtagn! Iä Iä!
	zibarium (Naked) 10-21-02 02:54 No 370634		thoughts on water quantity:	Bookmark Reply
			swiz can see why fb may require less H2O...as well as why many other variables exist in quantifying this essential compound. a small pile of bone-dry fb psuedoephidrine will require less moisture to beecome moist than a pile of its salt that contains the same amount of psuedoephidrine. because its a bigger pile. (not very scientific, but valid) like-wize, should a bee decide to use more bone-dry lgrp or lgI2, this too will require more water to achieve a workable paste than a rxn that used a more minimal amt. of these dry ingrediants. in nano-rxns, its almost hopeless to quantify H2O use. look what happens when you try to store bone-dry rp in a too big jar that was full of air at 90% humidity...it gets lumpy. anyway, if its too wet, and you don't let some evaporate out of the system, how will things improve?
	12345x 10-29-02 08:13		FREE BASE realy ? (Rated as: incomprehensible)	Bookmark Reply
	12345x (Stranger) 10-29-02 12:45 No 374010		HI + phudo ---> meth +I2 ?	Bookmark Reply
			i dont think so! you are robusto! lets overview the major reactions in the P,I,E batch E=ephed or phudo I= iodine P= Red Phos ok first aproxamation (youll have to forgive my spelling here) 1. P4 + I2 ---> PI3 (phosphorous tri iodide) a brown waxy solid that fumes HI gas (on contact with mosture) 2a. PI3 + H2O ---> HI (hydrodic acid)  +H3PO4 (phosphoric acid ) dont ask me where the the extra oxygen comes from just belive me its not hypo or the other one.its the no good to use one the one that flavers your Coke a cola and cleans your toilet anyway anouther PI3 reaction: 2b. PI3 + E --> I-phudo + H3PO4   phosphoric acid and (I-phudo) ..call it iodioephedrne ie: N-methyl-1-iodio-1-phenyl-2-amino-propane now step two 3. (I-phudo) + HI ---> meth and I2   ie N-methyl-1-phenyl-2-amino-propane  and Iodine the I2 formed reacts with more RP and the cycle continues untill the thing runs out of phudo (good) your done or runs out of any of the others RP,I2,water (bad) your stalled. there is one other reaction ....... reaction X: reactionX uses two compounds 1.phudo or ephed  1 part molor 2. PI3            2 or more  parts moler there are Two products 1. Iodioephedrine  2 moles 2. compound X      3 moles compound X is the unknown compound... it is produced in a thjree to two  ratio with meth compoundX all thou its stucture  not known ... is the reasion of lost product ie it not there as meth and its not there as phudo eather many things are known about it such as: compound X doesnt have a nitrogen on it or if it does it doesnt form nonpolor compounds when exposed to strong bases in water.as I-phudo ,phudo and meth does. because it isnt found in np after adding lye nor does it bond to the RP.as swi know has ran rections where there isnt any phosphorous left (or very little) and asssuming that fish smell that is sometimes produced is small carbon chain amines ie ethylamine etc. one must conclude the methyl group was striped off leaving a non amine compound compound X  acts as a solvent in that it allows HI to contact Iodioephedrine (forming meth +I2) in a way that increases the reaction rate compared to how I-phudo and HI contact in its absence. lets rehash the two routes to meth each route has two steps as such the slow high yeald way: pi3 from P and I then Iodioephed from phudo and the PI3 (A1.)  RP + I2 --> PI3 + phudo ---> H3PO4 + I-phudo.(step 1) and HI and phosphoric acid from water and PI3 then to there ions as they defuse into the liquid. (A2.) RP + H2O ---> H3PO4  + HI ---> (H+),(PO4---),(I-)   iodioephed(liquid) and HI gas as it boils out of liquid forms meth and elemental Iodine both soluble in the acidic depolorized water solutions. (A3.)I-phudo(liquid) + HI (boiling gas)--> meth(liquid) + I2 ----------------------------------------------------------- the fast but low yeald(2/5) of theroretcal) way. using large amounts molor wize of rp and Iodine to phudo and no water  form PI3 in larger then moler amounts compared to phudo (B1.)  (RP + I2) ---> (PI3)    phudo reacts with PI3 forming Iodioephedrine B2 phudo + PI3 ---> I-phudo then here to the end is at best a guess X-reaction: I-phudo + PI3 --> X1 compound X1 compound + I-phudo + PI3 ---> X2 compound and god knows what but no water is present nor is there any HI as there isnt any water to form any. then : X2 compound + PI3 +heat --->x2 compound decomposes then to ---> HI + ???(gas) mistery gas or foam (phospine gas?) this 2nd part produces some water (from decomposing X compound ??) it also produces HI assume from the water formed and a lot of HI that must be soluble in the PI3 ,I2 ,I-phudo,xcompound matrix as the conversion to meth occures very quickly and without the nessary bubbling HI in steam as the slow  way has to to finish altho mabie HI gets contact with I-phudo by bubbles but because the bubbles are small (ie foam) the surfice area is increased to a point that there isnt any HI gas left to pressureize the flask when the little bubble finly breaks the surfice. anyway the numbers : if you did it this way the (B. type reaction) you would use dry I2 and  phudo (mabie add a little acettone to melt the I and phudo together ) you would then add dry RP and vent to water trap with reverse back flow prevention ie two bongs the bowls conected to each other the mouth peices one to your flask the other the vent to outside air. you would use I2 ratios in excess of three to one to phudo by wt. and rp in quintys to handle the reactions where there was some left when it was finnised. you would mix all the I and E togeter then you would use the rp to control the reaction rate so the foam wasnt rising out of the flask. but when it wasnt reacting at max rate you would add more then when it wasnt generating enougt heat to boil fercly by its self you would eather add a small amount of water ie: 1 ml for every 15 gms over the 2:1 ratio I to E or if you were close to 2:1 no  water then you would rase heat untill boiling was occuring you would notice the solution is now thinner then before upon inspection is tranparint "can see light thru it" you assume its done. but to be shure you stab it with some I2 "there is still some rp left in the pot" it turns black , it bubbles the water trap , but 2 mins later its as clear as it was before you stabed it if it stays dark its not done you keep the boiling going on anyway when your sure its clear "this is relitive to the cleanleness of your phudo ie: pure =clear as coors beer if your pills not so clean then mabie a dark micro beer but always can see the light ....thru it and adding I2 results in returning to as clear in a copple of mins when continue to boiling you then let cool a little and some water to bring to liquid level up to a workable concintration it is cloudy untill you bring it up to boiling then it clears up to the coors clearty. it doesnt have any RP clumoing to the sides "a sign of unreacted I-phudo. anyway your done mabie you pour off a little base it into np rince with water then add some acid water and dry in the pan for a bio assy. if no pin wheels just streit shards even thou you smell acid as it drys "which tells you you have the good and the bad in the pan" then you finish the rest if not good ie pinwhells you boil out the water you added untill 57% HI/water is realized ...ie un capping produces stong fumes. you then stab it with more I2 and boil,untill its done if you want it done now you stab it with I2 untill its done your product is always clean because you rince the np with dh2o buy shaking and running off twice. and there isnt ever any phudo as there wasnt any Iodioepedrine to turn back into phudo when you lyed it out. your yealds are 3/5 of what you would get going the (a) roght it appers this reaction forms a compound with 5 phudo molucules then breaks down giving 2 meth molucules and eating up 3 phudos. but it does this very fast " ie in less then 10 mins" yes done in < 10 mins. conditions:            no water            I to E >2:1   need more (3,4,5 :1)if unclean phudo            with enough RP to have some afterwords           and enough to not see Iodine cristals forming at top of flask "purple not brown is iodine"                brown is PI3 and or Iodioephed the other way: you make full strengh HI  ...57%HI in water  1. you add to 43ml hot water some RP use 1 part rp to 3 parts I by wt you then add 57gms dry I2 thats rp and 47parts liquid mesure h2o and 57gms by wt I2 " use floz and oz if you want this gives 57% HI in 43% water by wt da.... now that wasnt hard you will note the water level hasnt rissin much from water to 57%hi so you computating mind tells you this liquid is almost twice as hevey as water apx 1.8 gm/ml if i remember anyway you now add some more rp you bring almost to a boil you then add your phudo how much? alot swi know has added enough that it wouldnt all desolve at room temp. anyway you then bring to a boil. with reflux your going to need your hi/water as youll be boiling awile...... 3 days ...... thats 72 hrs note anytime its not boiling the clock has stoped evey bubble of 57%hi(gas),47%(steem) is reacting at the liquid /bubble interface with Iodioephedrine that sits at the interface in the liquid. this produces meth and I2 in the liquid but the bulk of the gas escapes cuz it isnt at the suface of the bubble from here the I2 finds some agitated RP "anouther reason to boil hard" this unuion produces PI3 now this PI3 can do two things A. it will react with unshelded water presnt forming HI and phosphoric acid. B.it will if there isnt any unshelded water.. it will find a phudo molucule and form Iodioephed what i meen by unshelded water is water that has free molucules to break salts,acids,etc into ions. if the water is saturated with acid ie HI 57% or even if a little less but salts are added to eat up any free to desolve things water."ie some salt sits undesolved even at full boil. anyway water in this state "depolorized" will allow the PI3 to exsist long enough to react with phudo this is the mantra ..... the Iodioephed must not bump into more PI3 before it reacts with HI(gas) at the liquid/gas interface in the bubbles. if the phudo goes this route "and it will if you have 57% acid ,no free iodine added and had the rp in and it clear before adding the E. if it goes this route with a lite to normal boil reflux you will need 72 hrs it will never look dark and your yealds will be 100% of theroretal "93% or whatever it is "as im sure you all know meth is lighter then whats it made from" if that iodioephed finds PI3 before it finds HI(gas) it will via Xreaction form meth now! but will eat three molucles for every two meth produced things that screew things up: 1. acid water not depolorized "less then 57% acid without salts added to keep the water saturated at  boil" this condition allows any PI3 formed to react with water which altho increases the HI concintratuion doesnt leve any to react ewith phudo to form Iodioephed and no Iodioephed no reaction with all that HI to form meth.thats why dilute solutions dont just form meth a little slower.ie half strenght acid twice as long to cook ....no...... half strengt acid never cooks. also if the acid isnt saturated it wont be in ant amounts in the bubbles. as the % acid rises very quickly near saturation.if half strengh acid boiled away with half acid stengt it woulnt get stronger but the acid stays in the water thats how boiling results in stronger acid concintration very quickly. well this is bad as with no acid in the steam bubbles means no Iodioephed is finising to meth. and no free I2 is being formed.etc this is why if you fear you arnt at 57& dont reflux your liquids as thjere wont be any concintrating and without that no reaction. and the other way if you spike this bubbling pot with so much as 1/100 free iodine or you bring the HI/water to boil witout RP it will decompose forming free I and if you have the phudo in it and its boiled >3 mins it will be dark then adding RP wont clear it up . and for some reason the presonce of free iodine in a boiling HI solution increases the rate that the HI decomposes in otherwords if its clear with rp it produces very little free iodine thats what you want. but once its dark it takes a lot more rp to get it clear and this increased rate of iodine producxtion will manisfest it self in lots of PI3 and that means the other reaction the quick one . your cook time will  drop dramaticly and your yealds also ex: you heat up your hi with the phudo in it you bring it to a boil.you hear a noise outside you go look theres now one out there. you return and note you forgot to add the rp dam you throw in a whole bunch. you note when you thru it in the water was already dark "you were only gone a min or so. you will find it stays dark and a test at 24hrs finds it clear and done. but after finishing your yeald is 60%-80% the next time the rp goes in first then heated then phudo it never does darken a pull at 24hrs finds almost pure phudo yeck goes your old ladys throte. after 2 days its phudotar ie: drys as supercool liquil "amorphius" and taists just as crapy as the day before its crap but its half way there. after 3 full days a pull conferms its done.clarty wont conferm it never was dark. and adding all the pulls finds 92% by wt impessive little green one. also note if you run a dry one but dont use enough I and RP to react with all the phudo and have more you will use all the I forming Iodioephed with more phudo but no I and without having any water means there isnt any Hi avalble to finish and relise the I that is in the Iodioephed and with out any extra PI3 to form Xreagent there isnt any decomposing to relice any I eather in this case your black sluge doesnt do any thing it has no HI to finish all that I=ephed nor any PI3 in case you add a little water. the only way to fix this is add enough I to form enopugh PI3 to use all the phudo and have some more for Xcompound to start going wit its self hi and water formation or you add a little water to some I and rP  with heat so this forms 57% acid and then with boiling the acid will convert the sludg into meth and relice more I2 etc i hope you are grasping a concept of how this thing works as swi know says all epedrins with halogens go to meth via forming the haloeped. ie chloroeped ,bromoeped,iodioeped the good thing about iodioephed is because the forming I2 is theraly favorale you can reduce iodioeped with HI because I2 is the product, if you try forming mixed halogens ie: trying Hi on chloro or bromoephed  would result in things very unstable like monobromoiodide check merek for mono chloroflorine and see how unstable mixed halos are or using the same halo acid ie Hcl with chloroephed would result in Cl2 a very unstable compound so paledium with H2 is nessary. the gold medal will go to the person who finds a an inhibitor that blocks the the lose 3 for 2 gained side reaction but doesnt interfere with how fast the Xreaction converts phudo to meth "its been done in less then 3 mins!"
	12345x (Stranger) 10-29-02 13:12 No 374016		to those cuts in pills in 2002	Bookmark Reply
			you will find that whatever gets put in pills the effect is the same effect as using less I and rp to  E ratios ie you need twice as much I and E for X pills today as you did a year ago or for the same amount of I andRP you must cook longer to get the same results. note also the addtion of calcium chloride genraric red hots. if you use water to wash the ca-chloride desolves the bases the phudo which will stick with the solids when you filter out the solids.note this is milled in as a dry powder and doest change anything when one takes the pill as his stomgic (?) will reacidfuy the base phudo prety snicky these days a few drops of acid is added to alcohol washes to prevent pill cuts from basing the phudo while its being seporated from the solids also the addtion of metels ie iron oxide(black) will upon reductuion in the pot form iron metel in a very fine powder which forms coloidle solutions when you shake your np with lye water. these days swin doesnt shake anymore just stirrs gently then reextracts from the lye water many times.as shaking forms the dreaded metel chelate or whatever they call it it means goo with almost no mass holds lye water up in the np the thicking is that I rp gobbling up cut. i recomnd doing a alcohol acetone recristal but stoping the addtion of acetone at the point the xcut starts coming out ie you can pull around 40% clean phudo then stop and pour of the liquid and have clean eped that will use an amazing small amount of I and RP if you continue to add aacetone you will see your cristals start to gum togeter and that glue will when cook with leave you gasping how the fucking thing isnt clearing up and youve added enough I and rP to do ones 5 times as big the other 60% of phudo isnt worth the 5 times as much I and RP to cook it clean in a normal time frame.
	Rhodium (Chief Bee) 10-29-02 13:16 No 374018		Am I retarded and everybody else understand what ...	Bookmark Reply
			Am I retarded and everybody else understand what this guy is trying to say, or what?
	Jetson (Title Addict/Eraser) 10-29-02 15:42 No 374051		sorry..	Bookmark Reply
			sorry i had to stop reading it so i don't know..... ^the devil is so lonely
	ballzofsteel (Miss High & Mighty) 10-29-02 16:58 No 374080		12345x	Bookmark Reply
			Ill give you a gold medal if you could re-write that crap into some easier on the eyes format. Id think I was following what you were trying to say,and then kaboomof on another tangent you go a straying. Im serious.You obviously have something to say,and what it is may be usefull to some bees,but dont try to be another cryptospirodopolous,we already have to many.Just spit it out bro,Ill listen to ya.Or are you just talking crap and trying to mask it with your waffle?
	geezmeister (Bee of the Month) 10-29-02 17:43 No 374086		Hope someone can help translate	Bookmark Reply
			I think the difficulty is in translating his thoughts to English sentence structure and syntax. He obviously has some chemistry background and has a good deal of experience with the reaction. He makes a number of observations about the rP/I2 reaction and yields, and correlates these observations to specific variables. Enough of them strike a common chord in SWIG's experience to suggest he has more crediblity than his command of the English language conveys to the reader. The post relates results and yields to reaction times, temps, circumstances, reagent quality and molar ratios. A number of points he discusses, particularly regarding time, yields, visible PI3, dark brown vs. purple coloration, dark vs.light coloration of the reaction fluid, yields-to-time relationships under different conditions of the reaction---are familiar or have been experienced under similar circumstances by SWIG. The fast, low-yield cook he discusses is something SWIG has encountered locally which is becoming popular with local "street" cooks.  SWIG has no idea whether his chemistry makes sense, but some of his conclusions and observations correlate well enough with SWIG's experiences to suggest his credibility has more to do with his langauage skills than his knowlege. I doubt he is Flinger or Fman reincarnate, and he's obviously not Wm_O.  Then again, I have to agree with Dennis Miller. "That's my opinion. I could be wrong." Mostly harmless
	12345x (Stranger) 10-30-02 08:52 No 374429		what im saying to sum it up	Bookmark Reply
			ok 1st concept that phudo gets converted to iodioephedrine ie: the (OH) group on the beta carbon the same carbon that attaches to the benzene gets replaced with an iodine atom. we call this new compound iodioephedrine 2nd concept iodioephedrine or "N-methyl-1-iodio-1-phenyl-2-amino-propane"' gets its iodine atom replaced with a hydrogen atom this new compound  is meth or "N-methyl-1-phenyl-2-amino-propane" my short hand for phudoephedrine (phudo) my short hand for iodioephedrine (I-phudo) "    "    "    "  phosphorous tri iodide (PI3) "    "    "    "   sodium hydroxide NaOH (LYE) "    "    "    "  non polor solvent (NP) "    "    "    "   water         (H2O) the two steps or two reactions that take place to change phudo into meth: A. phudo to (I-phudo)    this is done using a compound called phosphorous tri iodide or (PI3) put phudo  in contact with (PI3) and the (phudo) is converted to (I-phudo) B.(I-phudo) to (meth)    (I-phudo) reacts with hydrodic acid (HI) and is converted to meth. so good so far? now the reason there is a wide varance in yealds is because reaction (b.) "see above" has two differnt ways or routes it can go. lets look at these  two ways (I-phudo) gets changed into meth. b1. (I-phudo) desolved in a saturated acid water solution d contacts boiling (HI) as a gas at the liquids surface the result is the (I-phudo) is changed into meth. ie: (I-phudo) + HI ---> meth now the other way B2.(I-phudo) contacts (PI3) the result im not sure but anyway the result of this reaction is meth is formed. notice this reaction there isnt any mention of HI in saturated acid water solution like there was in reaction (b2) above. the properties of reaction (b1) are a 100% yeald the properties of reaction (b2) are a 40% yeald in a typical cook using RP,(phudo),Iodine and some water both reactions  (B1) and (b2) are occuring depending on the conditions. this fact is why yealds vary. if your conditons are such that the (I-phudo) does not contact any (PI3) but contacts (HI) gas in the bubbles that rise to the surface as the acid water is boiling.this will convert at 100% yeild. if your conditions are such the the (I-phudo) contacts (PI3) and other (I-phudo) molucules an unknown to me reaction will occure that will use up 3 (I-phudo) for every 2 meth molucles formed by used up i mean they are gone they are not phudo they are not something your going to find when you wash your shit up. they have disapeared for all practacal porpouses now if you dont mind geting 2 meth molucules for every 5 phudo molucules and speed of reaction is important then set up the conditions so reaction (b2) occurs. if you are looking for yealds at the expence of much longer reaction times then set up the conditions so reaction (b1) dominates the conditions for reaction (b1): this invovles making clear hydrodic acid 57% in water adding red phos and refluxing for 3 days. then treating the post rxn as normal to make 57% (HI) warm 43ml water with red phos in it add 57gms Iodine cristals boil till clear. then add the phudo while its boiling. put on your refluxing condenser. use 1:1 Iodine to phudo ratio use 1/2:1  red phos to Iodine ratio for conditions to run reaction (b2) use 2.5 :1  Iodine to phudo ratio use 1/2:1   red phos to Iodine ratio mix I and Phudo together add a dash of acetone "to blend the two" cap flask to a push pull water trap add 1/3 of the red phos to flask and cap after reaction slows add 1/3 more red p repeat untill red phos is all in add 1ml water for every 1/2 oz of phudo bring up to good boil. boil till clear. add 5ml water and bring to boil let cool done wash as usule. the ratios of I and P to phudo are flexable at the minunium a ratio of around 1 :1 Iodine /phudo will produce slitly higher yealds due to the liminted (PI3) concitrations but cook times will increase ie from 1 or 2 hrs to a day depending on how close you come to the cut off ratio. increasing the iodine and red phos ratio to phudo will shorten the cook times as the yealds drop to a level of 40% ie: 2 for every 5 and the time for the reaction depending if your push pull can take the volumes of acid gas and flash is large enough so foaming doesnt rise to the top is around 4 to 5 mins  ie if you use 5 parts Iodine 2,5 parts Red phos 1 part phudo you will have clear liquid in around 5 mins. after washing up you will get 2 molucules of meth for every 5 molucules of phudo used. i will leave it at this...... see if this sinks in if so ill give a little more refinments like why acid solutions with less then 57% concintration type (b1) wont cook. why 57% solutions type (b1) with any free iodine will convert much faster then 3 days and suffer from yeald losses   what happens when your type (b2) reactions will.... if using less then the cutoff ratios of Iodine to phudo will... just die ie: forms  a black slug without any acid smell and wont react no matter how long you boil it. and why type (b1) reactions arnt cooking  when they arnt boiling.
	12345x (Stranger) 10-30-02 09:16 No 374437		probley	Bookmark Reply
			i coulnt say but if you think HI + phudo --> meth i could say you dont know much about chemistry
	12345x (Stranger) 10-30-02 09:25 No 374438		you dont get the concept......	Bookmark Reply
			that free base when put into rp + I + water forms the exact same thing as when you use phudo HCL because puting free base phudo into an acid solution will form the salt and red phos + iodine + water + heat qualifys as an acid solution! do you understand what im saying? oh man who names himself the name of an element
	ballzofsteel (Miss High & Mighty) 10-30-02 09:32 No 374442		PI3?	Bookmark Reply
			So you are saying that PI3 and I2 alone will halogenate Phudo to I-Phudo,but HI wont?What makes it easier for PI3 to give up it I?Why?What makes you think this? And what happens when heat is applied to HI? And why the fuck must a P be involved in this equation? Oh, and how come you are the only one that knows all this,and that statements from our top brains refute yours? See,now uyou got me all phluked up and phlustered. Who do I believe? Genuinely Curious
	12345x (Stranger) 10-30-02 12:12 No 374477		it goes like this	Bookmark Reply
			Iodine and phos will form PI3 PI3 will react with phudo to form iodioephedrine and NO HI wont convert any phudo the reason the Iodine from PI3 does it so easly ill guess probely not becase the phudo wants the iodine but probely because the (OH) group that gets replaced gets bonded to the Phosporous forming a very stable compound phosphoric acid. note that the HI is needed ie: to react with the (I-phudo) to form meth and Iodine. also note this reaction is done with the HI as a gas and the (I-phudo) as a liquid. therefore you must boil the liquid to generate HI gas and as the bubble rises thru the liquid the HI gas that sits in  the outer bonderys of the bubble will contact the (I-phudo)thats at the surface of the liquid.where the bubble is at. this fact about the HI reactinmg as a gas is why if you dont have foam or boiling you dont have any meth forming. this is why pressure pots aint the happening thing as they inhibite boiling. the hot setup is boiling chips as more small bubbles has more surface area then a few large bubbles. and just like the phos "its a surface reaction" so decrease the size to increase the surface area and PI3 aint some stange compound   think about how PCl5 "phosphorous pentachloride "is used to make chloroephed and PBr5 phosphorous pentabromide is used to make brmoephedrine they are all halogens bonded to the hydoxy grabing phosphorous atom and why dont your gurus know about this....... they do know .... the question is why they chose to not share these little 1st yr chemistry facts. thats why i thought id mention these facts ....... cuz im sturing up the duky....... they can staiten me out if im wrong........ they can play dumb and bow down or they will throw me out.to shut me up its there call but belive me , when were talking about using halogens to remove that hydroxy group and replace it with hydrogen the only way it happens is via a replacment with a covalently bonded halogen then reduction to hydrogen and HI mite replace the hydroxy group with iodine on an primary alcohol like methyl alcohol or ethyl alcohol but not on a secondary alcohol where the carbon that the (OH) group is connected also connects to a benzene ring  as is the case with phudo and ephedrine.
	12345x (Stranger) 10-30-02 12:35 No 374481		its realy very simple	Bookmark Reply
			if you want better yealds and have a few days make 57% HI just add phos to 43ml water warm then add 57gms Iodine and bring to boil. theres your 57% HI now add youe phudo 1:1 phudo to Iodine with 1/2 RP to Iodine. and boil 3 days. if you get impationt add some Iodine if you want it done now add some more iodine when it clears up its done. if it aint clearing up add more Iodine and it will. if your not sure its done take a pull.and test. thats pour a little from the flask into a glass container add some np . then some lye till it turns white,then a little more then shake and seporate with a squeeze bottle wash the np with water once then add a tsp of water a few drops of pool acid and run the water layer into a vision pan dry and bio test. if its done good if not keep boiling or add more Iodine just never dilute with water unless its fuming to the point of blowing your lid off the flask.OR YOU KNOW ITS DONE" and you just want the liquid more dilute so decanting the liquid from the RP is easer. just remember if you want it to finish sooner and you have some rp in the pot already "this is always a rule " . just add dry iodine. its that simple it realy is. if cuts in the pills are keeping it black way longer then youd like it to be ...... the answer is still the same "ADD MORE IODINE!"                              "KEEP IT BOILING"
	geezmeister (Bee of the Month) 10-30-02 15:41 No 374502		change of opinion	Bookmark Reply
			A few observations after a further read of these posts: 1) Its not a language barrier problem. He speaks English. He does not write well. 2) His principal observations about yield and its relationship to the molar ratios of the reagents and precursors (and solvent) coincide with SWIG's experience. 3) I cannot comment on the validity of his reasons why the yield is affected the way it is, but as a paradigm for the layperson doing this reaction, his observations suggest a protocol that if followed should increase yield and potentcy. 4) His theory does explain why both the short fast cook and the long wet cook produce meth, and why if you start a short fast cook you will have a cap on yields, despite how long you reflux. SWIG has observed the phenomenon trying to persuade a young street cook to improve the quality of his product and the yield by changing his technique...and was unsucessful in increasing yield or potentcy. 5) I also like the description he provides of producing HI in the flask with red P and I2. Mostly harmless
	Jetson (Title Addict/Eraser) 10-30-02 17:53 No 374533		......	Bookmark Reply
			jetson would have to agree that it shouldn't really matter if one were to start a rxn with either the freebase or hcl of psuedo/e as the HI is going to turn it to a salt anyway.  and also jetson as geez does sees validity in a good bit of what can be understood. ^the devil is so lonely
	handsfull2 (Hive Addict) 10-30-02 17:59 No 374535		Yep	Bookmark Reply
			sounds like a guru ' and I'll tell ya the truth he writes better then some I've seen "me included" ' and the points he makes are understandable. I like the way he thinks' so I welcome his thoughts...... producing HI in the flask with red P and I2 'yep I agree geez" sounds like a good one to me. "A work in progress  "
	zibarium (Naked) 10-30-02 18:52 No 374549		about FB/versus the salt:	Bookmark Reply
			sounds correct to zib, what 1234 says about fb beecoming the salt in situ... but why is the fb rxn so much "hotter"? (apologies for not remembering this: when the fb beecomes the salt in the flask, is this highly exothermic?)
	12345x (Stranger) 10-31-02 06:47 No 374830		yup	Bookmark Reply
			yup adding pure free base to stait acid will siszel everytime. mixing rp and iodine with some water is as good as adding strait acid. and with that little heat input well the P and I reacting give off lots of heat in themselfs if you realy want to run a free base reaction set it up so there realy isnt any HI in it by making sure there isnt any water at all because red p and iodine makes PI3 and PI3 will react with water to form HI to do the true base reaction you cant use any water. as any mosture will form HI and then you wont have free base anymore so what you do is make some pI3 alone "no phhudo added yet and do it in a np solvent that the (I-phudo )will be  soluble in and water is not. pick a np that has a farly high boiling point so as some heat can be applyed without all your solvent boiling away. ie throw some iodine in charcol lighter starter fluid thats been water scrubed with dryed epson salts then add dry phos and let it react with the iodine add some phos untill you dont see any solid I or untill adding phos doesnt seem to generate any heat then add your dryed phudo a little at first and see what happens. the reason i say a little at a time is once way back when i was screewing around with rhe PI3 concept and what i did was i added slowly red phos to strait iodine and after it reacted id add more p let it do its thing etc. untill adding p didnt do anything and then i heated it just to make sure and all the time kept a cap on the little jar loose but on it to keep the air from fuming it. then when it was cool it turned to black wax i then warmed the PI3 wax and poured mabie 5 ml into a glass whisler coffie pot i then added or sprinkeled.....i shgould say some phudoHCL  powder on the semi melted pure PI3 and as soon as that phudo hit the wax.... poof it was on fire! i then threw a shit load of water in the pot.. but the  fear of the dreaded white phos forming from the fire got me spooked "ever got any white Phos on your skin? it aint nothin funny belive me! so i didnt fuck with that stuff in the coffie pot "it went down the neahbors sewer but it was kinda intresting if i was to do it again i would make the PI3 in np solvent "to slow things down a little bit" and then add dry phudo powder to it i figure the np would slow that reaction down. then you could just make some 57gms iodine in 43ml water ie: 57% by wt Hi and let the Hi boil with the NP/I-phudo on top with the HI gass bubbles going up thru the np with the anhidress iodioephedrine in it. just like gassing  your shit . but the idea is to keep the water out while forming the iodioephedrine cuz even if you dont add any water "just  P and I and phudo " its still getting water from the mosture inthe air and in the hose line "i already said this part didnt I?" anyway mabie by doing the first reaction ie: phudo --> (I-phudo) in a non water frendly solvent you could stop that side reaction that eats up 3 molucules for every 5 put in but reatain that blazing fast reaction its under 10 mins it realy is get my drift?
	12345x (Stranger) 10-31-02 07:30 No 374848		if you dont belive me check.....	Bookmark Reply
			read post#365357 by repvip here  ill repost it here: without his permission ------------------------------------------------------------I was thinking about the amount of RP that is actually used and decided to run some numbers.  If I have made a mistake please let me know. In my O-chem book they have this balanced equation for the reaction of phosphorus with iodine: 6R-OH + 2P + 3I2 --> 6R-I + 2P(OH)3 Pseudoepherdine HCl MW = about 201.69 g/mol I2 MW = about 253.80 g/mol P MW = 30.97 g/mol Now, using the ratios of the balanced equation: 6R-OH = 1210.14g 2P = 61.94g 3I2 = 761.40g Divide everything by 61.94g and you get: 19.54g 6R-OH : 1g P : 12.30g I2 ------------------------------------------------------------ this part I add to the post note * in the eq. above "6R-OH" is a abbr. for phudo             and "6R-I" is a abbr. for iodioephedrine if HI reduced phudo it would go like this :      2(R-OH) + 2(HI) --> 2(R-H) + I2 now you find this reaction in a book ... and the book states is a valid reaction  with not just primary but also secondary or tetrary alcohols "phudo has a secondary type alcohol group " anyway find this reaction and ill ........ ill......... ill say well hot damm your the phudoephedrine man!
	zibarium (Naked) 10-31-02 08:49 No 374884		1234; whenever such data appears,	Bookmark Reply
			i have to wonder how...or why, bees claim the sucesses they do. its upsetting to have bees making sense like this. even if i don't understand the 'ph' in psuedoephedrine. i'm starting to think all you have to do is follow any sort of mystic rules with enthusiasm and confidnce, and you'll get the magic powder you seek. anyway, thanks for the food for thought. this will bee fun
	Jetson (Title Addict/Eraser) 10-31-02 17:26 No 375016		...	Bookmark Reply
			hmm... swij once posted how he usually does his rxn's by making the HI first and then adding the psuedo and additional rp and i2 but nobody seemed to care.... hmmm... ^the devil is so lonely
	ballzofsteel (Miss High & Mighty) 10-31-02 21:18 No 375121		Oi	Bookmark Reply
			Well,if we are all gonna fall at the mans feet, Can I have a little recognition about my theory concerning pressure and the influence it has on this particular rxn? I feel this is about the greatest explanation as to why you wouldnt want to exert any added.Even if it blows my scheme out of the water. C`mon,some consistancy in your posting.
	ballzofsteel (Miss High & Mighty) 10-31-02 21:40 No 375125		C`mon gurus	Bookmark Reply
			12345x has just made the first solid case as to what is realy happening,that I have seen. He has also issued a challenge to the great ones. Please respond with some sort of structure. Dont go quiet,or Ill start multiple threads about this subject to realy piss everyone off. If what this man says is true,well fuck? Pissed off.
	handsfull2 (Hive Addict) 11-01-02 01:44 No 375205		all you have to do is follow any sort of mystic	Bookmark Reply
			Zib' a prayer to the meth gods 'and a rabbits foot 'can make a difference. but knowledge and practice is probally your best bet ''' hell you know this better then anyone here ' Maybee that's it"" your just too smart..... "A work in progress  "
	geezmeister (Bee of the Month) 11-01-02 02:02 No 375212		my secret	Bookmark Reply
			My secret is the chant and stomp dance while shaking the sacred acid and water in the non-polar. That is what gives Geez good geez. I can feel it in my bones, trust me on this one, and the check is in the mail. Mostly harmless
	zibarium (Naked) 11-01-02 07:42 No 375309		ballsof; what the quiet might mean:	Bookmark Reply
			bees are thinking 1234 mde intersting points; no doubt about it. as mentioned, it is odd that bees have sucesses that, in a sense, they shouldn't bee having...according to late breaking theories. it beecomes difficult to know what to beelieve, especially if what you been doing seems to work well. 'tis a pity that so much chem-hack research has gone into this rxn...and its future is probably more threatened than evr. rp dissapearing; e going fast and gakked to beat the band...even I2 is getting dear. there may not bee time left, for instance, for a decent way to inject tiny amts. of pulverized reactants into a rxn chamber so they needn't have such trouble inter-relating and bogging down on their own weight; perhaps speeding things up quite a bit w/out long reflux. guess i better spice up the old incantations

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