04-06-04 16:47
No 499430
The following is a work of fiction.
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Hour 1:
On the verge of one more of these reactions. I keep asking myself how many times I'm going to try this and fail before I decide it's too much trouble. How many times do I have to choke on HI gas? How many times do I have to stain everything in my kitchen brown with fumes from iodine crystals, those same fumes doing things unknown to the inside of my body which are presumably worse than some brown tubing. There has been times in this experimentation where I thought that any second then the DEA was going to come knock down my door and cuff me up. But I'm so close to graduating! I tell myself: only an idiot would continue doing something like this when he could just buy it off the streets. Especially when for all he knows it will end up costing the same amount. Something lingers in me that doesn't allow me to give up.
So I'm sitting in my kitchen. The past 7 days I've barely left the house other than for a box of red hots or a can of acetone. The windows are all shut up and covered, the air is dank and astringent and I'm sitting in front of the most beautiful piles of red, white, and purple. Even when I was sleeping the night before I couldn't keep the image of those pearlescent crystals of psuedo that after an overkill session of boils, recrystallizations, preciptiations, acid basing, and gassing must be close to pharmaceutical. Another wave of fear comes over me, have any of my neighbors noticed the paint dissolving fumes billowing from my roof? As I peek out my window I realize the grass is about .5 meter tall and I can't for the life of me remember the last time that I was out there mowing it. That has got to be obvious that something is going on in here, the un-mowed lawn, the covered up window, me huddling in my house with bags of solvents and the wonderful smell of sulfur emitting from my chimney from that monstrous pile of safety matches made even safer by the removal of those terrible little red strips. As the necessary nervousness fades into oblivion I turn back to the glistening iodine, and that sparkling pile of matchbook phosphorus that I've learned to hate so much.
It all started about 9th grade when I was walking down the street one day and I spotted the man who once bunked me $400 dollars worth of acid. After calling up some friends to rendezvous, we confronted this guy. I start yelling at the bastard, telling him he owes me big. "I don't fuck around", he said as he inched a gun from his pocket for all of us to see,” If I owe you, you'll get what you need". Well he didn't have money, but he still was willing to come to an agreement. An hour later I had a big ass pile of tweak. I had never done this shit and didn't even know how to take. A few assays of small amounts and then I must have hit the target as a large whoosh enveloped my central nervous system and I cried out for more. From that day on I knew I had found the drug I was made for, nothing blended so in synch with my psyche that I felt so in synch. This shit made me superman. For someone so unsociable, I was now the life of the party talking 800 words, smoking three cigarettes, grinding my teeth 9.5 times, taking a big deep breath and almost passing out all in the same minute. Nothing ever felt so good, and I fell in love with this drug.
That is, right up until I was crushing up a freshly bought rock when one of my friends told me his mom was coming down stairs and instead of ditching it down the sink I hid it in my nose. Next thing I knew my tongue was blue, my heart was leaping out of my chest and I couldn't breathe. After that I started getting panic attacks all the time and I had to quit most everything: cigarettes, caffeine, weed, mushrooms, lsd, tweak and all the other 300 otc medicines I would insufflate each time I couldn't find a place to get my fix. I joined a basketball team and left the world on the street in order to find a better lifestyle, but that feeling still lingered in my head, and with my obsession with chemistry I knew I would someday be able to make anything I wanted. And would, regardless of whether I took the drugs anymore or not. Many years later, I've read enough chemistry books to overload my shelf, I've spent more time than I'd like to admit reading all the ramblings at the hive, and I've put in so much work that to quit now would be a shame. In the back of my head still lingers the fact that quitting this insanity is probably the best thing for me.
But as I remember the satisfaction in crushing up those rocks, rolling up my bill, smelling that wonderful smell, tasting it's bittersweet seduction, and wincing in the sting of it flying up my nose and waiting for the rush to hit, I can't let go. I need to go that extra mile. First stop: Whacking that piece of shit alcohol group off of that no good pseudoephedrine.
Today is the day when I get to test what I've learned. Today is the examination of my experience with chemistry. Today is the start of my long wet dream.
I've never been more prepared than this. Lg iodine, super pure psue, and, well, the best phosphorus I can come up with. Sure, I've tried before. Each time I've learned something that I should have already known, but over-eager me blew it every time. I think now I've got it down. I think now I realize that I shouldn't try it my way since after all it wasn't me who came up with this synthesis at all. Now I realize I should benefit from those experiences of others and try my best to dodge the failures others have experienced. At least now that I'm not doing that nano-crizap, when I get that uncontrollable urge to put in "just one more scoop of this" or "well I'm almost out of that, how about I throw it all in?", well now that extra is a small percentage of the total and probably willn't fuck up the ratio.
Everything is prepared. I've decided on a 1:1.16:.75:.95 ratio of E:I:MBRP:H2O to be exact. Even after reading all the ratios I couldn't help but throw in a little personalization. I've decided to run it for 40 hours. I've got the condenser flowing, an addition funnel and a balloon at the top, a bucket of ice and a stir plate and my little round bottom thirsty for some reactants.
At the hood, I mix my water and phosphorus. This shit just will not get wet. Swirl here, stir there, scrape it off of the walls once more, stir again. Finally it's more or less in there. The first scoop of iodine and there is little activity. It is reacting: I see little ghosts of dissolving iodine trailing off of the crystals, but compared to when I fumigated my house with HI this is docile (thank you LWR, you are the best). Another scoop, then another, it's heating up all right! another scoop, whoa! here we go! little bubbles white misty HI gas slinking off the surface. Another scoop, more steam, more swirling, more icy bathing. Ah, fuck it, in she goes, and the whole shebang of iodine gets dumped in. Lots of stirring on the plate, lots of dunking in ice and being careful not to let it get out of control and all of it's in there with no crystals and not a singe puff of HI has escaped out the neck. Now for the pseudo. One scoop goes in.. a little bit thicker but not too bad. Another scoop.. little thicker, stir bar still works though. Another scoop.. is this thing heating up or is it just me? Another scoop, whoops, big ass clump comes out of the bottle. So thick now the magnet willn't work, I decide to just say to hell with it like the iodine and throw it all in. A large magnet held up to the flask allows me to at least make a mixture in the flask. A little bit-o-stopcock grease and she's ready for action. Slow increase on the mantle, shit liquefies, stir bar now works. Little more voltage and the stuff has cute little bubbles like I'm making poisonous whipped cream. A little more voltage and it's off with a bang. The stuff almost escapes into the condenser because it increases so much in volume with the little bubbles. I ousted the mantle, waited a minute, things are settling down. A little less voltage now. A little bit over, then a little bit under, back and forth and back and forth. Finally I find my niche at 55.5 VAC on the mantle and it's refluxing nicely. Here goes time ZERO of my 40 wet dream....
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Hour 5
Time is passing faster than I thought and after trying to ignore this masterpiece of mine I walk into the lab to find that it reeks. Hmmm? Smells like sulfur? Maybe sulfur dioxide or something like that? Yuck, it's that fucking punch ball. Yep, that perfectly good-looking punch ball balloon is sweating some illish crap and smells awful. Who the fuck said this was a good idea? Would the ACS approve of this? Well, if it goes through rubber, maybe it won't go through plastic. Ahah, here is a plastic bread bag, on ye go... perfect. Smell is gone and a bread bag has saved the day.
Looking down into the flask... boil boil toil and trouble, this time it's crank in this cauldron bubble :) The little thing looks just like it did before, bubbling away. Each passing moment I lament not having paid more close attention to those at the hive. My stir plate is on its lowest setting but it's stirring pretty fast... am I supposed to stir at all? What the hell is sweating from my balloon? How can I tell if this shit is working? Well at least this thing appears to be taking care of itself, maybe I can worry about something else now and get some work done for the next 43 hours. Fuck, 43 hours! This really does take forever!
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Hour 15
Opening my mouth far a-wide and letting out a yawn, I peer into the humble resting place of my monstrous creating. How did I get myself into this mess? I feel like the scientist in Frankenstein who is too exited about what he can do to realize what might become of it.
Upon closer examination I peer inside.. The bubbles are a little bigger now but the solution still looks about the same volume, not like I could tell really, unless there was a substantial change. Suddenly, DRIP! What the fuck was that? A drip had suddenly fallen from the top of the condenser... hmmm, that's strange, the reflux has been mostly condensing in the bottom 5 cm of the condenser. My eyes slowly scanned upward looking for the origin of the drip, some sign of alternate condensation... hmmm, that's funny: the drip left a trail of driplets that aren't surrounded by condensation at all... HOLY CRAP! OH FUCK! GOD DAMN IT ALL TO HELL! Suddenly the realization strikes me as I peer into the joint of the addition funnel. NO no no, it can't be. Yes, I'm afraid so, the funnel is indeed leaking. This lonely chemist scrambles across the abode. Pipette in hand, the water is extracted from the funnel (why the fuck did I put it there in the first place! never again!!!) The stopcock, which was found to be slightly loose, was tightened just in case.
What have I done? How much water has entered this bustard? What the fuck! With ratios so absolutely delicate in balance, a few milliliters would stop the heart of my creation and render it lifeless... oh my god, how long did it react before getting watered down? What should? I do? The answers escape me as I prepare my things and get ready to go. Prior arrangements necessitate my attending to something alternate for the moment... most people say just let it go, as fucking with things will likely make it worse. But in this case, who knows....
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to be continued...
(Stranger)
04-06-04 16:50
No 499431
The following is a continued work of fiction
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Hour 24
A full day has gone by. My stress and the rate of this reaction are inversely proportional. I fear so terribly that I might blow this project that I decide something must be done. I have two options in my mind: either cook it for longer, or add iodine to raise the concentration once more, hmmm... or both. I guess that is three options. Well, extra time doesn't do shit to a reaction that is not going forward at all due to a low [HI], as far as I know. Extra iodine does in fact increase the reaction rate and yield to a point, but there is no telling how much iodine is necessary as there is no way of telling how much water or even if the reaction has been diluted more than a few drops. For all I know the water was doubled... one really cannot tell in that mass of bubbles and mbrp and psuedo, which take up a lot of space. The reaction I must admit is a mere 8.5g E.
All in all, this chemist turned fool turns to the iodine: maybe a few grams just for luck.
2.4g of iodine were weighed out to place on top of the original 9.78. Opening at the top of the condenser by removing the addition funnel the extra iodine was poured in, in the process a lingering cloud of HI tickles the nostrils, causing me to wince. A bit sticks to the condenser on the way down but most of it made it... quick, just in case the reaction spews gas any second now I had better get that funnel back on stat! Yeah buddy, great frickin idea: once again a few crystals of iodine have landed on the joint grease and stuck... this time they are pretty small and just like when I filled my house with HI I decided that instead of cleaning the damn thing like a decent individual I would try and grind the crystals with the joint small enough to create a seal. Well there are multiple drawbacks to this procedure, other than a leaky joint, as when I was pushing down on the joint the funnel broke off at the stopcock and the residual sharp spike of borosilicate decided to see what it's like to reside on the inside of a human hand. Morals of the story: the stem of a separatory funnel is weaker than you would imagine, the price of not cleaning out the joint of iodine crystals ranges from $45 to the price of the entire reaction, and last but definitely not least, the skin on the palms of an alabaster-white hermit clandestine chemist doesn't stand a chance when placed up against a freshly prepared blade of pyrex.
Quickly, an extra punch ball was placed over the area where now the joint of a sep funnel has taken permanent residence. Blood dripping from the hand was calmly ignored while viewing the progress of the reaction mix. The whole mix seems to have gained in size and the bubbles are larger. Above that the condensation level in the condenser seems to have risen about 1 cm. I'm now sick of watching what is slowly morphing into my long wet nightmare and now that I don't even have the option of adding more iodine I think I'll just stick it out to the end instead of sticking it to my hand.
Maybe I should just end this thread now. Failure seems imminent and ridicule lingers behind every corner...
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Hour 27.15
I just couldn't fucking help it, ok! Another 2g I2 was added.
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Hour 38
Back into the dungeon, the dragon continued to belch away. The bubbles are the same now as they were in the beginning. They haven't gotten any bigger, or smaller. The color almost seems to have gotten a darker red or almost purple, but it may just be the lighting. Even the height in the rbf is the same. Still, the feeling of worthlessness lingers. Can't I do anything right? They say that anyone out of elementary school can synth this stuff but I seem to lack the capability. Fucking stupid sep funnel. I'm glad you broke. Take that. Still iodine crystals stuck to the inside of the condenser where they were poured through last night, minus a few at the bottom that have been effectively refluxed back in. Well, 10 hours till the real disappointment kicks in, might as well just leave it alone.
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Hour 45
It's almost time! It's almost time! The real excitement is kicking in, only dampened by the idea that failure might be moments ahead! Looking at the flask this time was a real surprise. For some reason, in the past 7 hours all the iodine crystals have disappeared! A few <white>?? Crystals have developed in a streak from where the majority of the I2 was stuck. There is no fucking way that the reflux reached such a height though, this stuff barely has water flowing through it and it's still condensing at the very bottom. Something else that's strange... the stuff stuck to the walls of the flask is not where it was when I was here last: before it was about .5 cm from the bubbling mass, now it's .5 cm from the top of the flask! Somehow, when I was gone the whole mass must have gained tremendously in height, somehow licked up all the residual iodine crystals, and then settled back down into the bottom of the flask to the same level it was when I left? Truly confused. There is remarkably less bubbling in the flask now, which is another sign of something definitely being different. The mantle was turned up a few volts, just milking for some extra action. Could this strange activity be a sign of its completion? Was it just a power surge? Hmmm, we don't really get power surges here... Maybe my variac is fucked up, who knows. I am hopeful nonetheless.
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Hour 48
The time has come and the basement chemist delux is here for another round of toil and trouble. The appearance is still the same as it was before. The heating was removed, flask allowed to cool. Opening the flask released ghosts of choking acidic fumes, but none more than this bad boy can handle. At least nowhere near as nasty to my as xylene fumes, barf.
A small sample was sucked out and placed into a test tube then based. The solution turned foggy. A small allotment of toluene was added and swirled, most of the fogginess dissipated. This toluene was sucked off and dried in a watch glass to reveal a small amount of oil. Now this got Lux thinking, if I got an oil I either have meth or some type of intermediate but definitely not pseudo. If there is an intermediate present it is probably halogenated. Someone who is Relux pulled out the copper wire for a little beilstein halide test fun. If the copper wire after dipped in an unknown, when placed within a flame, causes the flame to burn green there is an halide and one unhappy clandestine chemist. A little smearing around in the oil and into the flame: no green flame. Hmm, better make sure this works: wire dipped in untreated reaction mix where halides are known to be present: nice pretty green flame. Back over to the oil, a little smeary smeary on the wire: a small greenish flash... hmmm, could have just been me touching the wire that did that. Not to mention this should only really work if you wash the np with some clean water to flush out the water soluble halides and then dry to be rid of it all, then dry non polar, then test. But there was so little green that there is enough to make me very hopeful indeed!
Set up for a good ol' steam distillation. Mixed up some NaOH. Added some NaOH. Massive load of white chunky nastiness! Looks like curdled milk! What the fuck! This is not what I expected. Did I burn the product? I thought it was supposed to be resistant to concentrated base? What the fuck? Did I come this far to fuck it all up now? This semi milky, but mostly coagulated mix was boiled as per steam distillation, very very little oil in the collection flask. Great, he says, I really fucked up now, he's really done it for good. This far only to be a jackass and add too much base and polymerize all his delicious honey. Why haven't I ever heard of this happening... wait a minute what is the pH? The cap was removed and pH taken: an... an... Acid? pH4. Damn, this shit is still acidic! This must have had a butt load of acid in it (second thought makes Lux go, no shit Sherlock: HI remember, not just basing the product. Fucking idiot.). More base is added: reaction mix gets foggier then clarifies; More: fogginess flashes again, dissipates; More, more, more: Lux decides to pull his patented "No patience base extravaganza" ousts the cap of the bottle, chucks, the pipette and dumps enough concentrated base in to make a bar of soap: A fatty layer of yellow oil floats up from the solution where the cheesy chunks suddenly have disappeared!!! Woo hoo! NOW WE'RE GETTING SOMEWHERE! What the fuck is that smell? ug, that's fucking disgusting. It's as if I washed a hoe's cooch out with some ammonia and then corked it for a week. The set up, then resumed, provides almost an hour of entertaining enjoyment. Bubble after bubble of water pushing a stream of oil through the condenser, drip by drip the collector captures the bane of my existence.
Some unmeasured, but large, amount of water white, but somewhat foggy (most fogginess came over right as the oil in the flask was consumed, so distillation was stopped). Toluene was poured in, swirled (foggy milky upper layer produced), the water then pipetted out. That water then extracted with tol, that tol added to the other collection. Extracted once more from the water. Last drop of water removed from the bottle containing the toluene extracts. The milky toluene solution was heated, totally clearing it up to a pristine water white clear stanky solution. CaCl2 (anhyd) was added, lots of water removed. Tol filtered from CaCl2. Set up for gassing as per the bubble air with aquarium pump through a container with CaCl2 and muriatic. Gas wand (pipette) upon getting closer to the np solution already begins to precipitate loads of white goop. The wand was swirled in the mix, applesauce created, filtered using Buckner/vacuum, gassed again, filtered again, gassed again, filtered again etc. Last gassing produced only a few crystals and Lux decided to fuck going through the trouble of filtering it again. The vacuum was left on for about 5 minutes, the pristine white cake of pearlescent goodness placed on watch glass, and a rush of pure joy flows through this chemist delux. Fucking A, done finally.
I still haven't recrystallized to see what the structure is, or even assayed the material to find out if it is what I expect. I am not a meth user so the urgent need to consume this pile-o-goodness does not really exist. Maybe someday. Next on my to do list: thermos recrystallization, melting point, and IR spec.
And the chemist lived happily ever after.
The end.
(Stranger)
04-06-04 17:16
No 499434
5.20 g were collected. Yield = 66.4%
(Of Counsel)
04-07-04 09:12
No 499532
Excellent essay, makes for a good read, enjoyable, reminds the reviewer of his own experiences, shortcomings, impatience. And the feeling of success. Yes.
Tips are available to increase yield, yes. This is more an essay on the experience than one on the reaction. I have shared this experience, and you convey the feelings I have experienced very well.
A very good, entertaining read.
mostly harmless
(Stranger)
04-07-04 17:21
No 499605
As to that assay... 0.007g were smoked as per aluminum foil method
...YEP! IT WORKS ALRIGHT! Surpisingly free of odor, either as a powder or as the smoke. Very clean taste. Discolors the foil, probably from overheating (dec) and HCL reaction with Al.
Thanks for the praise Geezer, I've always wanted to make a contribution to the colony. It's as if I'm sprouting my wings.
A few more pix for the the visual bees.
The setup. Keeping it simple, just not simple enough (damn sep funnel).
Brewin'
down to new orleans,
brewin'
ain't just lentils or beans,
brewin'
cook it long and sloooow...
Just keep brewing oooooh ooh ooh oh....
Little Miss Muppet
sat on a tuffet
gawking at curds and whey...
Along came some base,
which in it's embrace,
scared all those curds away...
I know, I know, Lux did sort'a push the limits of the size of his flask, but only for the distillation.
(Stranger)
04-08-04 08:08
No 499726
Relux,
if you imagine dumping all reactants and the water in the flask they will make up a certain volume.
Could you give me an estimate how much the volume will increase when the reaction fires off?
(Newbee)
04-08-04 12:08
No 499759
The amount of volume that increased was solely based on how much heat was added. In the very beginning it was very hard to not over heat, especially because I had not yet used or calibrated the mantle and I did not know how much voltage to use. If I would have known how much voltage to use right off the bat I presume the volume would be the same as after I had the mantle set right, which was about 1/3 gain in size. If you look at the photo above of the bubbling red stuff, that is about the height it remained the entire time, which is about 1/3 bigger than when heat is removed.
The increase in volume is really just from tiny little bubbles appearing all throughout your reaction mixture. This is because not only are you heating it externally but the reaction heats from the inside and therefore the reaction gains the capability to all boil at once instead of just from the bottom. I believe this is why some people say that in the beginning you will see many small bubbles and in the end see larger bubbles.
Anyway, so like I said, volume is dependent on temperature. Set the temperature at the lower range for this reaction and you will have almost no gain in volume as far as my experience tells me. Set it for a hot reflux and you just might end up scrambling to take the flask off heat, which works well when it's going out of control. It's a delicate balance between speed of reaction and ease of reaction.
Make sure you have a heat source that will remain stable, that way you can get away and sleep for those 48 hours.
To answer your question most directly, I did not throw in all reactants at once. I put them in in such an order as to not get a huge blast of heat or a house full of HI gas. Then I attached a condenser and started to heat. Also, to really answer your question, when I first started heating the reaction gained about 3-4 times it's original volume because I didn't account for the simultaneous exothermic in the reaction. I wouldn't suggest you do the same.
(Hive Bee)
04-08-04 22:07
No 499847
Good read relux it kept my attention even though i know nothing about meth. Very detailed. I especially liked this part around hour 15
How did I get myself into this mess?
Boy if swim had a nickel everytime he thought that one...
Never take a fox's word that the hens are safe.
(Stranger)
04-21-04 10:18
No 502082
When swim add toluene to the collected FB (after distilling), how should the dissolved FB looks like?
clear like water or still golden? How much Tol must be added (ratio FB/NP)?
thx
wer einmal leckt, der weiß wie`s schmeckt
(Hive Bee)
04-23-04 17:49
No 502582
When swim add toluene to the collected FB (after distilling), how should the dissolved FB looks like?
clear like water or still golden? How much Tol must be added (ratio FB/NP)?
thx
The distillate will be comprised of a thick cloudy cum-like layer atop of a less cloudy water layer.
You then carefully drain your water layer off, and add enough enough NP to dissolve the remaining fb (about 1.5x volume). The NP/fb will be thinner (then fb only) and cloudy/clear.
Then u proceed with your NP washes until both the NP and wash water comes off clear. Then u titrate for the salt, evap, acetone flash, scrape, (sample
), and recrystalise.