03-15-04 06:53
No 495199
Sorry, this post is long (but very complete and detailed). SWIK's first nano was either a moderate failure or a small success, depending on one's point of view. Regardless of how viewed, SWIK learned a lot doing a nano and even managed to obtain a little product in the end. SWIK's sharing this post in the hopes that his lessons learned through making mistakes can help a bee not to make them in the first place.
SWIK's personal definition of a nano batch is something that can be cooked in a test tube. SWIK is in the process of obtaining a shitload of real labware/glassware, but in the meantime he wanted to 1.) Get some experience under his belt before his first non-nano SWR, and 2.) Test the cleanliness of his pseudo beforehand, and 3.) Get a little product to carry him through his first non-nano SWR.
SWIK started with a 15cm long, 1.5cm wide test tube (approximate volume 25ml). To that he added 2.00g pseudo (actually 1.64g pseudo freebase) and 1.00g reagent grade RP. SWIK shook the test tube until the pseudo and RP mixed thoroughly and then placed the test tube in the freezer for 5 minutes or so.
After 5 minutes, SWIK retrieved the test tube and added 1.5ml chilled dH2O. He then added 2.4g reagent grade iodine and quickly slid a medium-sized balloon over the test tube and taped it to the test tube with electrical tape.
SWIK's first big mistake was forgetting/not realizing how hydrophilic and messy iodine is. He used a piece of legal size paper folded sideways as a transfer mechanism for the iodine. After SWIK set the paper down after having transferred the iodine, he noticed that the iodine had fumed through the paper and had now significantly discolored his kitchen table. :-(. A few drops of sodium thiosulfate and lot of scrubbing with a S.O.S pad removed the stains.
SWIK's second big mistake came when he placed the test tube in a Mickey's Big Mouth malt liquor bottle with cooking oil in it heated to 100°C. The oil filled the bottle approximately half-way. The problem, which is now obvious to SWIK, was that SWIK should have heated the test tube gradually, not submersed it directly into a 100°C oil bath! Some reasons that contributed to this mistake were that SWIK was also testing 1.) how high the setting had to be on his new electric skillet to raise the temperature of the oil in the beer bottle to 100°C, and 2.) If the skillet's thermostat was sufficient to keep the temperature of the oil at 100°C without too much deviation. The skillet, by the way, worked fine and held the oil at a rather steady 100°C when the skillet's thermostat was set to 375°F. Temperatures were checked with a candy thermometer.
SWIK's second big mistake resulted in an almost immediate "liquidation" of the reactants followed closely by a massive volume expansion of the reactants that threw up reactants into the balloon, resulting in balloon failure and quite a bit of HI gas escaping into the room. Luckily for SWIK, he had great ventilation and suffered no ill consequences from the HI escaping, save for a little ego damage. SWIK immediately held his breath and pulled the test tube from the beer bottle by the half-attached balloon. SWIK had the foresight to have an ice bath nearby. He put the test tube in the ice bath and re-attached a new balloon (after having added .25 grams more I to jump-start the reaction again). SWIK then carefully attached a clothes pin to the test tube to act as a handle and slowly lowered the test tube into the oil bath once again. The clothes pin served three purposes. First, it was used to center the test tube in the middle of the neck of the beer bottle so the balloon didn't touch the hot glass. Second, the clothes pin served to keep the bottom of the test tube from touching the bottom of the beer bottle. Finally, the clothes pin acted as a convenient handle to remove the test tube from the oil bath for occasional (but brief) close inspection of the reaction/reactants.
No additional "boil overs" occurred after replacing the balloon and putting the test tube back in the oil bath.
SWIK used the opportunity of the reaction proceeding to hone his observation skills. Within a couple of minutes the reactants got even more "liquidy" and the reactants that had been stuck to the side of the test tube began to slide down into the "Jacuzzi" (where the reaction was taking place). SWIK noticed the volume of the reactants actually decreased now, covering only the bottom 3cm or so of the test tube. SWIK noticed that the attached balloon filled with gas and "stood" upright almost immediately upon placing the test tube in the oil. SWIK also noticed that tiny bubbles appeared on the top 2 or 3mm of the reaction fluid. The bubbles reminded SWIK of effervescence. The bubbles were very small and definitely not "violent" in any way. Occasionally the bubbles would drop in height from the 2 or 3mm to only 1mm and occasionally the bubbles would expand in height to the top 7 or 8mm of the reaction fluid. The bubbles waxed and waned slightly at times but basically stayed constant and gentle.
SWIK went to bed after the reaction had proceeded for 4 hours or so. When he awoke 6 hours later he quickly went to observe the reaction. The balloon was still "standing" and the reaction looked like it had six hours later (rather boring, without much happening). SWIK felt the balloon to make sure it wasn't too hot and about to melt. To SWIK's surprise, he felt something in the balloon, like sand (or crystals) stuck to the walls of the balloon. SWIK "kneaded" the balloon, and while he didn't actually see anything falling back into solution, he did notice two things. First the "graininess" in the balloon got less pronounced. Second, the "fizzing", or gentle bubbling at the top of the reactants grew much stronger and taller within the test tube, to the point were it was slightly violent. The increased bubbling that resulted from the "kneading" subsided after a few minutes.
SWIK checked the balloon every hour after that, and found that the "graininess" returned every hour or so. He continued to "kneed" the balloon every hour and always noticed an increase in bubbling that lasted for a few minutes. SWIK knows that he was dislodging some type of crystals every time he "kneaded" the balloon but does not know what the crystals were: pseudo, iodine salts, phosphorous salts, etc.
It was SWIK's firm intention to do a 48 hour SWR. However, SWIK got a call after only 16 hours or so notifying him that his family was dropping by to get him to take him to the hospital to see a dying, close relative. SWIK decided to stop the cooking for four reasons. First, SWIK didn't know if the family was going to come in to his residence. Second, he had concerns about leaving the balloon unattended while he was gone. He'd have no problems leaving a real glassware setup with condenser unattended, but the balloon was a different story. Third, he noticed that the bubbles had got very, very small and their height took up, at most, .05 mm at the top of the reactants--much less than before. Forth, SWIK had noted that for the last two hours or so the balloon would "go limp" for a few minutes and then stand erect again. This "limp"/"erect" balloon phenomenon began to repeat itself every 5 minutes or so. SWIK surmised that the reaction may have gone to completion and he was seeing the signs of such.
SWIK decided to turn off the heat from the beer bottle and let the contents cool slowly (since he was aware the beer bottle is not made of Pyrex glass). After twenty minutes or so SWIK removed the test tube from the oil and set it in a test tube holder until he got back from the hospital and was alone again.
When SWIK arrived back home almost three hours later, he proceeded with the workup. The first thing he did was untape the now-limp balloon from the test tube. To SWIK's great surprise, a considerable amount of HI gas continued to emanate from the test tube and the balloon. Even 10 minutes after having removed the balloon he noted that HI gas continued to be released from both the balloon and the test tube.
SWIK was surprised to see the inner walls of the test tube lined with white crystals when he took off the balloon. The crystals appeared at the top of the test tube and extended down the test tube to about 2 cm from the top.
At this point SWIK decided to go online and double-check the procedures for the workup by referencing Curbshot's procedure as written on Rhodium's web site. To SWIK's surprise, it appears Rhodium removed the article from his web site, which again came as a surprise to SWIK since he had referenced the write-up the night before. Not a big deal, SWIK found plenty of post-reaction workup literature to help him. I guess the article's removal underscores the general sentiment I've been reading about regarding Curbshot's method. Oh well.
SWIK added 20ml of dH2O to the test tube with a squirt bottle, carefully dissolving the crystals that were attached to the top of the test tube. SWIK noted some bubbling as a result. He then capped the test tube and shook it well. To SWIK's surprise, significant bubbling began in the test tube and continued for several minutes. After several minutes, SWIK filtered the solution through a pre-moistened coffee filter in a funnel to remove the RP. Most of the RP was removed, but SWIK noted that he hadn't got all of it. He proceeded to filter once again through a "Charmin Plug". It worked great and SWIK was left with a very pale yellow solution in a 150ml beaker. He added 50ml of xylene to the solution and noticed two layers forming immediately. To this he added previously-created 50% NaOH solution by the eye dropper until the bottom layer turned cloudy and stayed cloudy. He noticed shortly thereafter that something began to precipitate out of the bottom, water layer. SWIK assumes that this precipitant is what is known as "lye lock".
At this point SWIK stirred the two layers together for a few minutes and then allowed the two layers to separate for 15 minutes or so. SWIK then grabbed a 10ml pipette and sucked off the top xylene layer into a funnel lined with dry MgSO4 and another Charmin Plug. The solution dripped into another clean, dry, 150ml beaker. When SWIK got to the point where it was difficult to suck off the top layer without disturbing the bottom layer, he transferred the solution to a test tube which, because of its narrowness, allowed SWIK to get almost all of the xylene solution in his pipette.
SWIK then gassed the xylene using VE's gassing apparatus. The procedure went without incident and the xylene solution turned white with crystals after a couple of squeezes of the gassing bottle. SWIK gave a few additional squeezes for good measure. He then filtered the precipitated crystals through another coffee filter and washed the crystals with cold, dry acetone.
SWIK let the filter cake dry under a heat lamp and then weighed his goodies; a mere .15g of end product was obtained. SWIK was quite disappointed. Obviously there was not enough product to perform a re-crystallization.
SWIK bio-assayed the product and was neither happy nor disappointed with the results. Certainly not "as good as it gets" but not bad either. SWIK sure does wish he could have let the reaction proceed for 48 hours.
On the positive side, no emulsions of any kind appeared during post-reaction workup, indicating to SWIK that he cleaned his pseudo properly. SWIK had also "done it" for the first time, and enjoyed the feeling produced from his product. He's also a little proud of himself. It's been almost two decades since SWIK's felt "the feeling", and he likes it.
So to recap the lessons learned:
1. Remember that iodine is messy to handle and discolors whatever it comes into contact with.
2. Consider using the HCL salt instead of the freebase for nanos since the freebase reacts more violently and the HCL salt should leave a wider margin for "boil over" of the test tube once the reaction begins.
3. Always heat the reaction slowly to get it started, never immerse the test tube directly into hot oil/sand.
4. Make sure you use clean reactants. The pseudo is obviously the hardest for bees like me to obtain and clean. Consider using the tetra trap, followed by 3 x NaOH washes, followed by 1 x dH2O wash, followed by a Japan Drier wash, followed by gassing using VE's gassing apparatus.
5. Strive for a 48 hour cook time.
Questions for knowledgeable bees:
1. SWIK knows "the smell" that occurs upon basing of the post-reactants. The smell that occurred was "the smell", but it was very faint, perhaps because it was overwhelmed by the xylene? Perhaps because the reaction did not go to completion? Perhaps because this was, afterall, a nano?
2. What do bees attribute the poor yield to: technique or cooking time or combination or ???.
3. Obviously quality of product would have increased if left to cook longer. Would yield have increased, too?
4. Regarding SWIK's observations about the "bubbles" during the reaction, do these parallel you observations?
5. Does the slowing/reduction of bubbles indicate a completed reaction?
6. What were the crystals that kept forming within the balloon?
7. What were the crystals that lined the top inner surface of the test tube when SWIK removed the balloon? The same crystals as in #6?
8. When SWIK added 20ml dH2O to the post-reaction solution, it began significant bubbling. What was reacting?
9. Since no emulsion occurred during post-workup and since gassing went without problems, can SWIK assume that his pseudo is clean and "good to go" with a significantly larger reaction?
10. If SWIK wanted to force the reaction to complete in 16 hours, SWIK assumes he could have used less water, resulting a quicker, "drier" reaction, correct? Instead of 1.5ml of dH2O, how much dH2O could/should have been used for the reaction to complete in 16 hours?
11. When SWIK based the polar/honey and dH2O solution, he saw a precipitate form on the bottom layer. Was this "lye lock" as SWIK assumed?
12. Is a beer bottle like the one used really unsuitable if heating/cooling is done slowly? SWIK's friend was supposed to come through with real glassware for him but he's been let down a couple of times now. SWIK is considering "going ghetto" and wants opinions as to the suitability of, say, beer bottles for a reaction vessel. Another post is coming outlining SWIK's plans for a complete ghettoware setup.
Thanks everybody!
--KidClean.
On the hill the stuff was laced with kerosene
But yours was kitchen clean
(Hive Bee)
03-15-04 09:23
No 495216
Hi
You done well. You did it! Now all you have to do is some fine tuning.
Remember, some loss is a percentage (e.g you may lose (say) 20% in an a/b. 1gm decreases to .8gm. 10gms ends up 8gms)
Some loss is mechanical (e.g you may lose (say) .5gm in an a/b. 1gm decreases to .5gm and 10gm decreases 9.5gm)
Some of your loss would have been mechanical. If you reacted 20gms of pseudo, it doesnt mean you would get 1.5gms of meth. It may bee more like (e.g)4-8gms.
So dont think your yield was 7.5%. It may have been 40% but you lost .65gms mechanically.
Its kinda like pouring flour from 1 container to the other. If you have have 1gm of flour in a jar and pour it into the other, .3g might stay behind, stuck to the jar (30% loss). If you have 100gm of flour, .7g might stay behind after transferring it (0.7% loss). The flour that stays behind is mostly 'mechanical' loss.
I am thinking you may have got a little bit more yield if-
-The HI hadnt been lost at the start
-The oil bath was set to about 110-120'c (the temp inside the testube will be lower then the oil temp)
-The rxn was allowed to go for 24hrs
-The post rxn fluid was filtered through the same filter (not a new, charmin plug. The filter, plus the charmin plug, may have been holding 300mg of product!!(??) Remember you are only working with 20mls of fluid!) and then rinsed with another 5-10mls of dh20 afterwards to wash the goodies out
-The xylene was added as ~40mls, stirred really well, waited on 15mins, seperated, add another 40mls, stirred, waited on 30mins, and then added to the first pull
The MgSO4 and additional charmin plug may have stolen another few points, almost every step decreases yield
Maybe a bee could add 20mls dh20 to their meth/xylene, added ~4 drops of acid, SHAKEN LIKE HELL to get the meth to turn to meth hcl, and then sepped and evapped the dh20, and then added another 20mls of dh20 with 1-2 drops of acid, and shaken again, and evapped.
These figures are all around-about
EDIT:
I think the following is something that many will agree on -
a)Newbees want to do nanos, just to 'see if they can do it', and then work up to bigger rxns.
BUT nanos are tricky, and only the experienced bee will be able to pull one off with reasonable yield. Small rxn + inexperience = high chance of failiure
b)Cleverbees will recommend that a newbee should do MINIMUM 10gms. That way after all the first time dramas, a bee will still get some dope. But the newbee just wants to make sure 'he can do it' first (e.g do a nano) before he goes and buys the hotplate, flask & condenser etc, so we go back to a)
its like a) and b) are chasing each others tails...
(formless fortitude?)
03-15-04 09:49
No 495221
Hey, geat job! To get any product at all, on ones first nano, is an impressive acheivement. The idea is not to be concrened about finishing in the top ten. Only to finish, period.
1.5ml chilled dH2O
That's a hell of a lot of H20. S/D uses 2 drops per gram of pseudo. Or aprox 1cc.
Best to forget the oil, and use a pan of damp sand, IMHO.
-S/D
Whenever you find yourself on the side of the majority, it's time to pause and reflect.-Mark Twain
(Hive Addict)
03-15-04 11:17
No 495232
One of the things swim keeps forgetting , due to having cut most any and all connections to the stupid "street trade" fiasco is that nearly anything self produced even if it's relative "crap" compared to the best others might be self making, the odds are that what you have is _still_ better than the average shit sold as meth on the streets.
erections lasting longer than four hours, though rare, require immediate medical attention
(Hive Bee)
03-15-04 12:16
No 495243
Hi
SQUIDIPPY-
"1.5ml chilled dH2O
That's a hell of a lot of H20. S/D uses 2 drops per gram of pseudo. Or aprox 1cc."
I think kidcleans' ratios were for a LWR instead of hot/dry
(formless fortitude?)
03-15-04 13:46
No 495257
lol!
Too much H20 will kill a reaction every time. Too little never will.
If one wants to do a LWR, then after an hour, they can add some H20 and continue with the LWR.
Whenever you find yourself on the side of the majority, it's time to pause and reflect.-Mark Twain
(Newbee)
03-15-04 15:11
No 495269
good to see u ended up with at least something.congrats.
im my experience, very fast reactions in the beginning led to less than 50% yield. I guess that doing long wet refluxes using the amounts/ratios especified here by many bees (0.5 and 0.8) that wont be a problem. I really dont know as i never tried LWR. i will in a near future.
if u have kept all washes and non polars u can recover maybe some more. Just dump the remaining in a big bottle, add some more VERY HOT water to the reaction vessel to clean it again next add all np used and add NaOH. Let it sit for some days or one day or whatever u can wait and then extract it again.
even if u end up with nothing u pratice and u will be moralized to do it since u can actually get some more shit.
peace and good luck for future projects.
(Hive Bee)
03-15-04 21:09
No 495341
S/D
"lol!
Too much H20 will kill a reaction every time. Too little never will.
If one wants to do a LWR, then after an hour, they can add some H20 and continue with the LWR."
2gE - 1gLGRP - 2.4gLGI2 - 1.5mL dH2O
These ratios ARE FINE.
They will not kill a reaction, every time.
They are ratios that suit a LONG, WET REFLUX.
Look here
Post 449625 (geezmeister: "reaction parameters", Stimulants)OR HERE
Post 494412 (geezmeister: "come on....", Stimulants)OR HERE
Post 487707 (geezmeister: "suggested parameters for first LWR", Stimulants)OR HERE
Post 478776 (geezmeister: "Dragan: E:26.5g, I2:39.75g, RP:15.95g, ...", Stimulants)and now tell me im still wrong
(Stranger)
03-16-04 00:34
No 495368
Way to go Kid.As you saw Swu got zip.But doing the GeezWareBeum Nano will net an weighed quarter,or6 gr hc.Though is it not? A salt shaker,small does work,ask Ware.So what did it smoke like?Taste ,colour.Let me know your dream,you will see the results of the GeezWare.It is simple!!I will never attempt any smaller.2 drops\gr=1cc or 1ml,2 gr's right?4 drops=1cc?I had the same blow out!First one knocked the flask in the oil bath,did you keep blowing balloons.?Swu did.Since 12 hrs ago,120C,taped 2 gas leaks at the bottom and top of condenser and did nothing else.Keep posted.Good Luck!
purple people eaters have ears
(Stranger)
03-16-04 01:15
No 495373
How can you have a blow out doing a nano,
Check it out;
Post 451706 (SQUIDIPPY: "ok", Stimulants)
That's 18gr. of pfed, ................no blowout.
huh!!!
(Hive Addict)
03-16-04 01:34
No 495380
Leak no more
Post 349850 (wareami: "Sizing UP...Seizeing UP...& Sizzling UP!", Stimulants)
Good job BTW.
And good lookin out by posting the No-No's!
Some cosmic force musta stole all popi's questions from his thread...musta bean them purplepeephole eaterz!
I know....he editted `em out
a little less conversation, a little more reaction
(Stranger)
03-16-04 01:38
No 495381
> So what did it smoke like? Taste, colour.
To tell you the truth, SWIK's never smoked or injected the stuff in his life. SWIK preferes intranasal ingestion. SWIK remembers reading many years ago in one of Uncle Fester's first editions of SOMM something to the effect of "if snorting doesn't get you as wired as you wanna be you've got a problem", or something similar to that. In reality SWIK just doesn't know why he's never tried smoking the stuff--maybe SWIK will try in the near future.
The appearance of the product was very white, since SWIK washed it liberally with cold, dry acetone. However, since SWIK didn't have enough product to recrystallize, the appearance of the product was that of recently-gassed salt. Don't know if SWIK's alone in producing gassed salt that appears in very thin, large sheets of non-shiny product, but that's what it looked like--almost like someone scrapped a layer off of some gypsum board or something. Oh well.
The bioassay was mixed at best. Way too much of a "sketchy bo bo tweaky biker shit" effect for SWIK's liking. Sure SWIK stayed up all night (in fact SWIK's just now coming down), but there was way too much jaw clenching and leg-locking for a pleasant dream. At least SWIK didn't get paranoid and see DEA agents running around in his back yard!.
--KidClean.
On the hill the stuff was laced with kerosene
But yours was kitchen clean
(Stranger)
05-18-04 06:19
No 507849
once swim has the e,i,rp of maybe say 48+48 pills of 30mg's of pfed, and extract with just s-l-x, then take e-pfed,and put into berlenmyer(flask), then place 10g's of I2, then 3g's of red(p), and place condenser onto top without pump(not necessary for this nano- believe me)..
then gradually work the flask on your hand at room temo for about 20 min till it hits some mud like sol., (if it doesn't turn into mud add heat quickly then take off quickly when the burner is on lowest heat possible), then once it hits mud, mak sure burner temp is 150-160 f.(yes!!!!f not c!!!!!) then put flask right on burner, and take off one minute approx. and mix(turn-turn) then watch---be careful because the r/p cn react if too much heat-then you will have a fire--and pop goes the baloon...with r/p burning you, and the walls(believe me i know), just make sure you are close to the toilet...okay then do this for about 30-45 minutes...which i have seen no more reaction....then swim takes balloon off, and puts cold h20 down the condenser to the flask about 200 ml's, then detach condenser, place flask onto burner at medium fire for (oh say 10-20 min.) then take off---pour off into pyrex bowl, put 100 ml of xzylene, 5-10 tblssppoons of naoh, then pour back into berlyenmeyer(forgive spelling) - flask, and add 200 ml's h20 and place on high heat till boiling...you will see both the h20 layer with the clumps, and the lighter fluid with clearness...untill it boils for about 15 min, or so....the clear xzelene turns yellow to dark brown...
yes!!!!!ahhh haaaa...take the top layer of lighter fluid..
or decant off with hose (small and use your own mouth if in the gheto) and decant off into pyrex bowl...
you now have a lighter fluid brown or yellow sol in the bowl...put on burner on low-med...and do not gas!!!!!
gassing will mess up the powerfullness which can be made...then place 5-15 drops of hydrochrolic acid(muratic acid -29-35% sol.) into the bowl
what you will have left over can be used on foil...and can be taken in a shot glass with 1 oz. of water..
any questions???
if you disagree...tobad it works...and it isthe fastest way...and way better than any street bought p2p i have ever seen.....trust me!!!!!
austintatious-notion-dotion-dude.....tak
07-22-04 12:26
(Rated as: off-topic)
(goat)
07-22-04 17:41
No 520827
(wow...neo's weirder than me)
here's 2 cents on your nano-rxn:
transfering glass containors, especially non-pyrex, from hot to cold enviornments is asking for cracked glass, which can suck.
even adding cold water to a hot rxn can cause breakage. i'd say you got lucky on that aspect.
secondly, unless i read it wrong, you skipped the np wash of the post-rxn aqueous solution, which is easy and quite valuable in eliminating lots of crapola.
i'd say that the violence and the crystals in the balloon, etc, were a case of excess I2 and RP. it has to go somewhere; it can't stay in solution above 50% or so.
it takes some practice to determine optimum ratios, but, once they are found, very little gas will evolve from the rxn vessal; it all stays in the puddle of mud, which is where you want it to bee. even the bubbling is a sign of too much reactants...yet, without some of that, its difficult to ascertain if enough reactants were added. so, a tiny bit too much is needed to mke sure there was enough.
idealy, the balloon won't even inflate, much less 'pop'.
swim agrees that you could mine your left-overs and likely come up with at least as much as you found initially; and the effort is good practice for honing in on extraction comprehension.
(p.s., don't bother smoking the shit, except as a test of purity...its too addictive and too time consuming, and not particulrly efficient. oral is the best and safest; one's digestive system will protect one's brain from some unwanted funk)