-Regarding xxvampxx000 comment...Like I said before (one should read entire thread before posting)I can easly get 30 gr of fine Redphosphorous from 20€-
Latest Update.
Hi folks,
Well SWIG is still waiting for the glass and Iodine from the chem supplier. It should arrive any moment so let’s wait!:)
In the meantime SWIG has performed another reaction. This time he used some tincture from pharmacies. Much better price/yield ratio. He used to buy in “big surface supermarket” (those who claim to have the lower prices around!:)) but was only 1% I and 2% KI, so he needed some bottles to get at least 3gr Iodine. Now he has founded 7% Iodine, which is best for his porpose I guess. This tincture costs 1€ where the other cost 0.45€, but its worth. All other percurssors we’re lying around from previous week homework.
Chemicals quantities used:
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3.5gr of Pseudoefedrina extracted from A*****d pills.
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6gr of Iodo from 7% tincture which was extracted the day before and dried inside bottle with Calcium Chloride.
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4gr of Redphosphorous from Matches. About 1gr of this phosphorous came from previous reactions.
First goes the Iodine (It was found to be a solid mass so SWIG has reduced it to finer granules using a wood stick)… then he adds the Pfed… Stir the vessel which is a 250 ml glass bottle that reassembles an erlenmeyer. It was the first vessel used and its still rocking. It has some P residues from previous reaction. It was dry thou… He prepares the condom he’s going to use and cuts the tape, black electrical type. Time to add the P so carefully SWIG adds it. Nothing happened right away…Swig looks inside the vessel. Stir the contents and waits for those sometimes dificult to get first bubbles…nothing…well SWIG decides to add water…One drop…nothing yet…but then and catching SWIG from surprise the contents start to react!!!!JESUS LORD! FUUUUUUUUUCKKK…never seen anything like this before!!!! Vessel heated like hell and instantanously burned his hand leaving burning marks (gloves are a must when using above 4 gr of Iodine or at least remember not to grab the vessel…Let me say that SWIG has only performed small reactions, 1 to 2 gr of E doubling this amount with Iodine, and he allways cools vessel prior to add any chems but this time when was more important, he forgot about that!!!).
He stirs the reaction vessel hard enough trying to stop the mess…he tries to see the contents but that turned out to be impossible as there was to many shit in the walls…BIG ORANGE SMOKE…heavy smoke that floats inside vessel and almost reached the condom!!! Its impossible to grab the vessel for more than a few seconds even wearing gloves! This shit is Fukin HOT!
In SWIG’s brain an image occurred….it was a phrase taken from the warlock site I guess “…yellow or red smoke…NOT GOOD…maybe a fire inside…” but then it calms down…everything is liquid now…well it looks like first part of the reaction was done…what was to take 25-30 minutes happened in 20 seconds…
” this can only be bad...sweet dream turned into nightmare”…Reaction has really stoped…nothing is happening and SWIG can inspect better the inside of the vessel now…looks like a metalic yellow/red liquid above the sludge…”Is this the end??…hmmm…no…better is to heat to see…” So in a sand bath, SWIG gently sarts to heat the vessel. (One improvement from previous reactions is the use of a fume hood. No more fumes around and that is a much better/safer condition to work I must say).
Vessel was still hot from the first messy part so heating was not going to do much and really nothing happened for 5 minutes…only one tought strikes SWIG mind –“ DID I TOTALLY FUCKED UP?”-
Some minor bubbling starts then…looks normal but its still very dificult to see inside as to many shit is grabed to the vessel walls…After 10 minutes it starts to melt more and a yellow reflux is now observed…at the 20 minutes mark no signs of calming and the reflux is now much intense with yellow drops,…SWIG awaits the cleaner reflux…normally it takes 30-45 minutes to reach it but after 50 minutes, still no signs of calming down…some white smoke…shit seems to be breathing…much finer bubbles now and that crispid sound from the reflux drops when reaching the sludge…70 minutes and aparently the reflux is much cleaner while the sludge is still bubling, not bravely like before but in larger big bubbles…80 minutes and everything looks calm but there is still bubbling…SWIG decides to shut of the heat and let the bottle inside the sand bath…the contents look pink…well not bright pink but sort of dark pink but brighter then the Phosphorous marron…white smoke everywhere…adding water now…25 ml to start…waiting for the lovely smell…yet another diferent smell is what SWIG gets…it seems close to “that smell” but it has a touch of other odor which SWIG cant identify since he’s not a chemist or something like that. SWIG gently starts to heat the vessel again which contains the sludge and the 25 ml of water. Boil it for some time. Put aside to cool and prepares the funnel, the cotton balls, the coffee filter and the very Basic solution. Back to the reaction vessel, he stirs it like a crazy trying to get all that P…filtering…hmmm…weird….the liquid apart from being cloudy, wasn’t yellow but rather whitish…tan white but defenetly not yellow like before…
no signs of Phoshorous or any other visible particules floating in this white cloudy liquid…re-filter it but didn’t improve…still cloudy…adding NonPolar now, 50 ml…adding basic solution…precipitates a yellow/white shit…adding more basic solution to bring it up closer to Nonpolar…stops when that happened…
Now SWIG has a question for all u experienced bees:
When inspecting the liquid closely and after 15-20 minutes, SWIG comtemples 3 diferent things/layers (well these questions are “general” and not from this particular reaction. This happens all times):
-in the bottom there is the most clear liquid and the salt he added before…
-then right above is the messy yellow/white “dust”
-and then the nonpolar…
What SWIG really wants to know, since he as read it somewhere is:
1 - Can we actually see the Meth?
2 - Is the meth this middle whitish/ yellow sludge layer???
3 - … Or will Meth became invisible by completely dissolving in the nonpolar??
4 - Should this middle layer go along with the nonpolar to the separatory funnel??? When inspecting closer SWIG sees that very little bubbles are going all the way up the Nonpolar and after 30 minutes this bubbling seems to stop and right bellow nonpolar is this “dusty look” layer with brown garbage added, which gets SWIG very apreensive…
SWIG decants the nonpolar and then with eye droper he managed to get all nonpolar but NO DUSTY shit...Another thing is that Nonpolar is yellow...well not yellow yellow but its not transparent as before and it looks like apple juice but not to dark…like diluted apple juice…OK, SWIG decides to wash the nonpolar so he adds half the amount with D-Water…shake but not to much…takes a sample to measure PH…shit! SWIG reads PH=8…damn!! He decides to add water to the bottle where the very basic solution was trying to make a very diluted basic solution. He then adds a little of this solution to the Dwater inside…reads PH above 10 now so he takes this water away and repeats this wash more 2 times allways adding some of the basic solution as PH was allways falling above 10 ( Some fukin weird shit was reserved to happen to SWIG this day I guess…)
SWIG adds now half amount with water and 8 drops of muriatic acid. Set aside and adds same quantity of water but no acid this time adding this extract to the previous extract…repeats once more and with the 3 water extracts now combined, he makes his way to the microwave (he was going to separate those extracts and let 2 of them evap in normal conditions aka above heater with no microwaving but since this reaction was likely to be a complete failure he decided to go way and nuke the MF!… 20 minutes in 30% potency was suficient…opened the microwave and almost sufocate with the INTENSE HCL smoke/smell…ihihihih…a very fine and dry layer was left and the dish was very hot…SWIG didn’t want to dry that much…SWIG adds acetone now which resulted in vigours boiling along with very fine crystal layer…carefully decant this acetone and yielded 0.2g of yellow cristals that didn’t improve in color with further acetone washes…Repeated this all process using another 20ml of Dwater which we’re added at beginning and settled inside the reactions for as long as this procedure took. Yielded 0.4 gr of a much clear product.
Total yield was an insignificant amount of 0.5gr of active stuff…which leads to one conclusion:
RED/ORANGE smoke is probably bad!RESUME of events, signs and variables taken from this experience:
- First part of the reaction was to fast, having a duration of merely 20 seconds instead of 25-30 minutes as stated in most procedures using a ballon/condom. (An ice bath seems to be the way to go on these “above 2gr” of E reactions. SWIG will try not to forget that next time)
- Reaction wasn’t forced to end at the one hour mark as SWIG allways does.
- Resulting fluid wasn’t yellow but rather withish and cloudy.
- Precipitated a “brighter orange dust” instead of the white/brighter yellow SWIG used to get after the basic solution adition.
- Xylene was transparent but has a piss color…yellowing that didn’t get away even after 3 washes
- Washes automaticly droped the PH to 8. A little basic solution had to be added to the washing water.
- Microwave was used at 30% potency to completely evap/dry the dishes filled with water extracts.
- Yield was very BAD. From 3.5 E, 6 I and 4 P only 0.5g was achieved. SHAME!
Ok this one is part of the history by now…I guess main factor to failure was the fast reaction right in the beginning. SWIG will perform another one like this but using this one to correct potential problems that might occur.
See ya next time! PEACE!
