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KrZ Member	posted 10-15-1999 02:11 AM One 160 cubic foot tank of hydrogen was purchased for $225 dollars. A 2L heavy-walled round bottomed flask was purchased, along with a vacuum adaptor and glass stopper. Some big clear tubing with cross-hatched threads was purchased from home depot, teflon tape was wrapped aroung the threads on the H2 tank, and the tubing was just the right size so that it could be twisted and pushed onto the tank, it was sealed with some O-clamps from home depot. Using some pipe adaptors, an adaptor was made to reduce the big tube into the smaller (orange) 300 psi welding tube. The tubing was run through a standard welding pressure gage. This was connected to a t-junction fitted with hose-attachments available in the gas fittings section. One end of the t-valve was fitted with a valve, all the gass connections were aided by teflon tape and O-clamps. The 2L flask was filled with 125g Ephedrine extracted from Ma Huang, 800ml of Everclear, 10g 3% Pd/C, an egg-shaped stirbar, and 20ml of H2SO4 draincleaner. The vacuum adaptor and stopcock were attached. A clamp was placed around the flask neck, and one around the stopcock. These were both secured very tightly. The flask was assembled over a stirplate with a pot of water, which it was immersed in. The water was heated to 60C, and the flask stirred vigorously. The tube from the H2 tank was connected to the vacuum adaptor (teflon tape and O-clamp used here as well). The valve was opened and the atmosphere removed by vacuum (or mouth suction). The valve was then closed. By opening the valve on the H2 tank carefully the pressure was set to 30psi. Stirring and temp were maintained for 120 minutes. When complete the pressure was released through the valve in front of a fan blowing outside. The Pd/C was recovered by filtration. The majority of the EtOh was boiled off (~200ml remained). The 200ml of remaining reaction mix was filtered 3 times to make sure all the Pd/C was removed (you could see some was still in there). This was then dripped into 1L of 8% NaOH (premade and cooled). 125ml of DCM was added and the meth was extracted by heavy shaking for 5minutes, followed by 2 more extraction of 100ml each. The DCM extracts were collected. Dried with Sodium Sulfate. The DCM was then cooled in the freezer and bubbled with HCl gas for 30 minutes. What was recovered was 114g of clean white crystals. These were filtered and dried. The crystals were made into a saturated solution with boiling anhydrous Isopropyl Alcohol. The IPA was cooled in the freezer for 5 hours, and the snowflake crystals were recovered by filtration. Yield after this was 108g of methamphetamine*HCl. And it blew the fucking pants off anything you've ever seen.
spitball Member	posted 10-15-1999 04:49 AM Oh Fuck yeah. Very nice. You paid too much for the hydrogen though. And I think that I should add that REAL pimps recover the Pd/c by scraping it off of the walls. But if you want to do it YOUR way, well, whatever chili. Fucking nice though. So Ghetto lisse although, Do you think that if I were to substitute the O-clamps from Home Depot with ones purchased at Sears, Would this affect the reaction in any way? -spitball- Hydrogenation is fucking pimp as fuck. Oh and just HOW were the gas connections aided by the teflon tape and o clamps? Could they have just assisted maybe? So much to learn....
FMAN Member	posted 10-15-1999 05:58 AM Very well it seems with this method then aPPLAUSE Ok I break the safe then.......... I got two ways to HEADTRICKS... I was on to the divided upside down water glass trick, bust beer bottle off at bottom and clamp down to gortex pad sastured with alch. like a chamane cork. Hydrogen is evoluted in an excess and pressure driven form this advantage point. So ya take salt and water and add goodies. Then ya plug it in and it yep it evolves it is SEALS it in so it is a whole contraption, hydrogen evoluted is mixed equally with clorine evolved there is excess hydrogen leff tover ever time, still havent figured why???Where the oxygen go to? Anyways it the goods are sacked up and placed in the sand quartz works nice so does glass, anyways it is plugged in and it the water is seen to shift from the hydrogen side ot the other side and is escentially clorine over there and NaoH on the other side when dry. Everthing is recycled nothing is used up except water and maybe some air, water is made by combining gas Two toone H@)) Antways the thing is run and with solvent of choice and contraptiosnv ary widely solvent floats usually an ether like substance though mixes work well also, I seen so many different it dont really make seence now anymore to explain, anyways the is run untill the solvent is essentially the only thing left, this is dried sometimes though not usually, if it is its ussually frozen off or out, the solvent chosent is often just alowed to settle off and the water is vaporised into HYDROGEN AND GASS, with the wrong solvent umm bad things can happen for instaance CN deposit on electrode, anyways these things ussually are not noticed because most are real lame and dont recycle all the way, so the gas is recombined and ran through the solvent as dry gass of HCL it the crystals fall out, then it the solvent is either vaporized by uv lamp long and short wave is ussually employed and guy is wearing glasses sun glasses, um the solvent is replaced and the waste gas is alowed to pass back into the resultant mix of the NAOH ya just made earlier at the electrode, this makes salt and water, then this mix is added to the other chamber water and the poles are reversed for posterity and research measurments a small bit of issolated nikle like salt is added and is really never used up anyawys, the stuff the pure water is evolved as before if necessary pertaining to the purity of the operator tap condition, thus it is run again and again over and over and the salt collected time and time again about half was recovered, many different solutions and catalysts and raw meterial were used, a journal is allways dictated into the bug or sound box always available, product is tested on most sensitive test subject available and result is noted, sometimes subject experiences difficulty, this product is no circulated and is rather tossed as trash, to keep the rats happy or well they eat eachother if given the opurtunity you will see I use fish. Anyways along the way a simple method was discovered and it was simpler than the above, much simpler in fact so simple as to be an embarrasment, to most involved. So we continue with simplpicity or rather lets us evolve to the simpler method? A test tube was setup a rather largeish one at first it has been replaced It the mix was essentially good for all everyting ya could seemingly put in there, ti was larned adjunctive process for the earlier experimenteres, thus it can be adjust to various needs so many variables so little time but no hurry????????So the tube was a conglomerate of tubes within tubes and such as to alow the lighter constitutant to basically float though it dont reallt float but this was the disovery process, in essence the tube was divided with two gortex layers alchol water and or ammonia or ether sued used to evolve the free base layer the electrodes being free hanging and placed at the optimial position, so that HCL gas and other evolved slowly through chilled solution thus and with the electrode naoh rain out salt out on nuber one level and a secon stage the etherial salt rained or salted out therupon salt out had become a real bitchy problem untill some idiot decided to distill water with electricity instead of conventional and that soap bitching is unnecesary! It is used to keep help the salt to keep from getting in the wrong layer, um this aint aa question and answer situation no is it a comercial enterprize whatsoever and the stuff pure was/is cut with or made into an alum salt. The great discovery was not how to but what to what inventive process for removing the alum salt that was there to begin with, this was a real bitchy thing, as soapy thing was but aint no more, the trade mark was iridium and it did something special to some of the salt produced, it took 'photographs' of the operator while in "operation" and these were incorporated into the "crystaline substance" by accident. WHHOOPPS:0 ---Amethystium---
randolph carter Member	posted 10-15-1999 07:54 AM you go krz..... nice write-up of a "perrenial" favorite...... destined to bee a classic..... thanx ------------------ randolph carter... the perennial dream questor... "remember, love is real, not fade-away, so, pass some on today..."
Sun_Rah Member	posted 10-15-1999 06:12 PM KRZ---Great write up! Good detail and I am happy for your results. Do you think its the best you've ever had?? I'm smilin for ya ;-)) Spitball how much should he have paid? What is a good price for H2 since I have never priced it. ------------------
FMAN Member	posted 10-16-1999 02:04 AM Um is the vromoly crome contains a necessary for the perfecto run??????????// ---Amethystium---
randolph carter Member	posted 10-20-1999 09:40 AM sheeeeeeeesh.... noone else seems to think this a significant post?????? this is DA BOMB!!!! look again swarm..... ------------------ randolph carter... the perennial dream questor... "remember, love is real, not fade-away, so, pass some on today..."
psychokitty Member	posted 10-20-1999 02:19 PM I'm VERY impressed. But I would like a little more clarification about the potential hazards that may befall anyone attemting this reaction. Is the vacuum adapter (standard glass model, no?) really capable of withstanding the amount of pressure being placed against it from within? How do you keep the whole top of the reaction flask (vacuum adapter and all) from booming off under pressure? (In other words, do the clamps really work that well at holding the vacuum adapter in its place just above the round-bottom flask?). Just a few more detailed details about the construction of the apparatus would be appreciated. Good going! Hey, any plans on adapting your technique to the new microwave-CTH process? Seems like you have everything you need to try it on a small scale. --PK
dwarfer Member	posted 10-21-1999 02:03 PM Super write up: reminiscent of the "Lone Ranger" Shake and Make pressurized experiment i did in the Spring. Do you know what the pH of the alcohol solution was with 20 ML 30% sulf in 800 ml ethanol? =============== 86% yield! Great. ================ Did you extract from plants, or ephedra from health food store. ?? ================ <<<Clapping hands dwarfer
placebo Member	posted 11-04-1999 11:56 AM Hi kiddies, I took the liberty of re-writing Krz's brilliant little write-up, for evil purposes, and was wondering if some smarty bees could peruse it, to check for obvious errors. Also if you could include any tips or special things one should know? My question is can methanol be subbed for ethanol? Can pseudo be used in place of E, I would think so? Catalytic Hydrogenation....H2/PdCl2 Author Topic: The MasterPlan KrZ Member posted 10-15-1999 02:11 AM -------------------------------------------------------------------------------- Cooking Chili Ingredients 1 tank of hydrogen gas with Regulator 125gms Ephedrine 800mLs Ethanol 10gms Pd/C (3%) 20mLs Con. Sulfuric Acid 500mLs NP solvent of choice (DCM, Toluene) 200mLs 20% NaOh solution HCl gas setup (optional) IPA (optional) Equipment 1 Parr Bottle or home made device capable of handling 30psi. 1 set of connectors and hoses and release valve suitable for pressure. 1 Stopcock 1 Pressure gauge 1 mag stirrer and stirbar, or some type of shaker setup. 1 T-junction 1 separatory funnel Assorted filters etc. Method A pressure hose is first connected to the pressure regulator and gauge on the tank, using appropriate fittings that can be bought at any gas distributor. This was connected to a t-junction fitted with hose-attachments. One end of the t-junction was fitted with a valve. The other end is connected to a hose leading to the stopcock and then to our reaction vessel. The reaction vessel was filled with: 125g Ephedrine, 800ml of Ethanol 10g 3% Pd/C, 20ml of Conc. Sulfuric acid Egg-shaped stirbar, if used! The hose to our reaction vessel and stopcock were attached. The reaction vessel was assembled over a stirplate with a pot of water, which it was immersed in. The water was heated to 60C, and the reaction vessel stirred vigorously. The valve on the H2 tank was opened and the atmosphere removed by vacuum (or mouth suction). Making sure our stopcock is open at the vessel. This is called purging the vessel. Then by opening the tap on the regulator, on the H2 tank carefully the pressure was set to 30psi. Stirring and temp were maintained for 120 minutes. When complete the pressure was released through the valve on the T-section in front of a fan blowing outside. (Remember H2 is highly explosive) The Pd/C was recovered by filtration. The 400ml of remaining reaction mix was filtered 3 times to make sure all the Pd/C was removed (wash down walls with a few extra mLs EtOh). Adding half our NP solvent and then basifying the mix with a solution of NaOh (pre-made and cooled) then extracted the Meth. Separate the two layers and put the NP layer aside then add rest of NP and separate again. Pool the NP layers together and then gas with HCl gas, then filter Meth crystals, repeat as necessary. What was recovered was 114g of clean white crystals. These were filtered and dried. The crystals were made into a saturated solution with boiling anhydrous Isopropyl Alcohol. The IPA was cooled in the freezer for 5 hours, and the snowflake crystals were recovered by filtration. Or use crystallization method of choice! Yield after this was 108g of methamphetamine*HCl. And it blew the fucking pants off anything you've ever seen. Hydrogenation is fucking pimp as fuck. 86% yield! Great!! ================ Thanks guys All credit to Krz. Very nice bro'! ------------------ Placebo.... Remember it's all in your mind!
placebo Member	posted 11-08-1999 12:45 PM Yes, I am making this post to bring it back to the top of the thread, sorry Spitty! Krz where are you? Can anyone help me with my questions, or comment on my writeup? What are the feelings about this synth? Why don't more bees try it? It sounds too good! Any comments appreciated! ------------------ Placebo.... Remember it's all in your mind!
KrZ Member	posted 11-08-1999 10:00 PM It's a great write-up placebo. It's referenced well, using a variety of solvents and catalysts. These yields are actually a few % points off the one in the ref. but no big deal. Don't know why no one tried it. Maybe they're afraid of H2,I dunno.
placebo Member	posted 11-09-1999 04:32 AM Thanks for looking Krz, I just rewrote your writeup in my words and made it easier on the eye. A friend has access to the H2 and is just waiting on the Pd/Cl2. So he can try it. I know I'm being lazy but could you just answer my questions or tell me where I can find the refs on the net.(no chem books yet) and I will try it for sure! and of course post my results for all to see! I think this should become a method of choice for many! I will also post pics of setup! ------------------ Placebo.... Remember it's all in your mind!
Wiggenheimer Junior Member	posted 11-09-1999 09:40 AM I have a few questions regarding this synth: Was the freebase of ephedrine used or the hcl salt, or does it not matter? Also, how scaleable is the reaction, could it be done using only about 10-20 g of ephedrine-hcl?
Bright Star Member	posted 11-09-1999 12:32 PM Very nice KrZ. Nice. Write me, would ya? brightstar@hushmail.com
Bright Star Member	posted 11-09-1999 12:33 PM Placebo- I think he used Pd/C (palladium on carbon) Not PdCl2 (palladium chloride)
placebo Member	posted 11-10-1999 04:07 AM Oooops, Good pick up Bright Star, thankyou! Would this make a difference? Which is better as I plan to get Pd/Cl2 for other things anyway! Can Pd/Cl2 be used in this case? I remember reading one is better at reducing primary alcohols and the other better for secondary and tertiary! yes? Why isn't everybody on this like glue? It looks way to cool! Just gotta be careful! ------------------ Placebo.... Remember it's all in your mind!
Xanion Junior Member	posted 11-10-1999 04:37 AM thanks to all you vets out there problem is my chemistry set keeps getting bigger and bigger this will go into my journal for future . ------------------ X anion
dwarfer Member	posted 11-10-1999 12:49 PM This thread has taught me some things that I will employ. I like the summary because a regulator goes on at the tank: a far better setup. I really liked saturating the isopropyl at boiling, and cooling. Never picked up on that before and it could really make a difference, I'll recommend it to a friend. This is one of the 1999 "top ten" threads of CM board IMHO.
placebo Member	posted 11-10-1999 01:27 PM I agree Dwarfer this method looks very good, So lets get some life in here and kick some ideas around! I know you are like me and would love to build such a device for evil purposes! Yeh I just rewrote it so its easier to read, knowing how lazy some bees are! I just need my questions answered to go ahead and I will post pics when its setup!! ------------------ Placebo.... Remember it's all in your mind!
Bright Star Member	posted 11-10-1999 01:31 PM placebo- PdCl2 - the Pd has beed reduced from the metal Pd(0) to Pd(+2) .. a cation ... IE electrons have been taken away. Pd/C has the Pd(0)... in 'metal form' ... The difference between Pd ingot (block o' metal) and Pd/C is that the Pd has been 'spread out' over the surface of the carbon in a weak complexing type bonding ... (its not really bonding ...) The Pd/C has more surface area for the Pd to complex with your double bond ... or electron rich sight (the Oxygen). So ... In general, Pd/C is used for reductions. And in general, Reduced Pd (PdCl2) is used for oxidations. There are journals that actually use the Pd/C as an oxidizing catalyst ... and some articles that use PdCl2 for reductions ... but these are novel. But in general the converse (statement above) holds true. placebo & dwarfer- I think that tanks of H2 gas, and the 'specialty glassware' are keeping people away .. But damn it people ... 1. No nasty chems! 2. Short Reaction time! 3. Ease of work-up ... evap and filter! 4. No mention of the elusive Red P! 5. Did someone say OTC?! So nice! A big hand for the KrZ one.
placebo Member	posted 11-10-1999 02:07 PM Thankyou, Bright Star So I know you can get PdCl2 at photo supply Wher would one get PdC? Is this the stuff metal platers use? I aint scared! I aint silly neither! Do you think 316 SS would handle the small amount of acid? Can methanol be used as the solvent? Is freebase of the E used? and I assume psuedo is allright! Sorry so many questions just want to rule out variables! I have everything but the catalyst! ------------------ Placebo.... Remember it's all in your mind!
randolph carter Member	posted 11-10-1999 03:18 PM Pd an C CAN bee made from PdCl2...... there have been discussions here at the hive and if'n i remember correctly there may bee info on rhods site about just that info..... seek and yee shall find..... ------------------ randolph carter... the perennial dream questor... "remember, love is real, not fade-away, so, pass some on today..."
KrZ Member	posted 11-11-1999 01:08 AM Base or HCl eph. doesn't matter. See all the acid in there? The only speciality glassware are some easy to get adaptors and a simple heavy-walled flask. You can also use a Rossi 1 gallon wine jug, which not-me has actually run up to 80psi H2 during a run without any explosion. This takes some Macgyver skills to hook up though (braided hosing clamped onto the glass threads w. teflon tape). If you do use a regulator, you can set it to maintain 80psi or whatever you want, if its a good one. You can often find used ones of this nature for $50, SWIM got one for $30. But before SWIM got one they tested the flow and pressurizing abilities of the tank valve itself, and finding them to be at least usable, decided to go ahead and write it. An added note, SWIM has indeed had experience running this reaction in SS and there was no noticeable corrosion.
dwarfer Member	posted 11-11-1999 07:02 PM Hey KrZ: another of the neat things about your result is that in doing the "work" in alcohol instead of water you apparently avoided the dimerization I experienced in a similar experiment I did several months ago in aqueous solution. It (my experimant) also used about 20% sulfuric. I do not know why this would make a significant difference: if you can elucidate, I would be appreciative. How did you settle on 60 degrees C as the operative temperature? I think these questions may be related. thanks dwarfer
Frank Needateener Member	posted 11-14-1999 08:42 PM Did someone say good regulator?
Frank Needateener Member	posted 11-15-1999 08:33 PM Don't stop the discussion. This thread is awesome! Don't they see?!?!?!
Barracuda1965 Member	posted 11-16-1999 01:44 AM Just in case you didn't hear me over there: Wow! I'm holding my breath waiting to learn more about this. OK, yes, it's fuckin' awesome. ------------------ 'Cuda65

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