tina_craig (Hive Bee)
10-18-04 17:17
No 536365
      First complete and perfect dream....     

swit_c realized this weekend past that he was full of shit.  Had his first actual dream.  Others were evidently a placebo to get him by, but this one was the shit.

157ml glass bottle
4' of clear braided PVC hose
1 Punch balloon
6g pseudo from KOH method
4g fresh MBRP, 2g 2nd time around MBRP
6g I from tinc (I2 was moist so no h20 added)

Mixed I with pseudo with 2g 2nd time round MBRP, mixed until completely homogenous.  Continued adding RP over about 30 minutes time.  Perfectly smooth start.  Attached hose and balloon and let it warm up on its own for about 15 minutes.  Then put in oil bath set at 75 degrees C.  Left it there for 40 minutes until small bubbling stopped.  Started increasing heat to 125 degrees C over 20 minutes, then to 150 over 20 minutes, then temp was slowly raised to 220 degrees C over 30 minutes, then refluxed another 15 minutes to ensure completeness.  Well, flame away because this was the first time that swit_c actually noticed the phases.  The bubble sizes, colors of mix and flask atmosphere.  However, Phase 2 didn't get extremely violent, someone could definitely tell it was happening and could also tell when it was over, but maybe because it was a 6g run it was kind of a downscaled turbulence.  Total time from putting on the hose to taking off of heat was 2 hours 20 minutes, although swit_c thinks it could have been done sooner because was following a write-up about the phases and the temps they start at where the author had listed Farenheite as temp units instead of Celcius so more time was probably spent waiting for Phase 2 at the wrong temp, but perhaps added time at that temp was a good thing because product is supreme although swit_c has no comparison.  Performed standard workup of product, rxn fluid was divided into 3 portions and 3 a/b's per portion for a total of 9 extractions.  Done with 4 and have returned around 2.5-3.0 grams of the strongest shit that swit_c has ever had.  Product dissolved and cleaned with methanol and acetone 3x.  White crystalline flakes, powder and crystals a plenty.  Will rxtallize returns tonight, most likely with ISO & Tone.  IV'ed about 1/8th gram, coughed, spun, twisted and still wired to the max.  Fucking 'A' thank everyone here that made this possible.  Swit_c is also confident now that this can be performed over and over without a problem.  Everything went so fucking smoothly.  Began extracting 6 boxes of 24x60 Saturday night, sampling product Sunday morning.  Everything that the write-ups said would happen did.  This is swit_c's first 100% rxn.  Swit_c thinks he was just letting himself think he saw the signs on prior runs.  Those were probably in the range of 10-30% complete.  Mmm-mmm good nothing like a pseudo high!!!  This last rxn product is the shit.  Finally, motherfucking success, nothing but smiles round here.  Again thx everyone for putting up with swit_c's shit and helping out.  The only advice swit_c can give to anyone on the ability to dream is extreme, undaunting patience.  Patience and just following the "User Manual" that is published here at the Hive.  All shortcuts that swit_c tried fucked him, follow directions and have patience, patience, patience.  If something is suppose to sit for an hour let it sit 1 hour and 20 minutes.  If you let it do it's thing at whatever step of the entire dream you WILL NOT be disappointed.  Patience and following directions IS THE KEY.

Tina Craig worked for me!!
 
 
 
 
    Scottydog
(Hive Addict)
10-19-04 00:28
No 536461
      BEE CAREFUL     

220C? Fast and hot rxns rock but please bee careful! If the rxn ever dehydrates at temps of 180C or higher, you could open the door to phosphine gas production.

If not, you could also end up with burnt tasting gear! Congrats on your success in under an hour? laugh

I once met a d00d in jail who said he would run his rxns with a benzomatic torch! Supposedly he would clamp his flask in place, in an elevated position and torch the bottom of the pyrex off and on keeping the rxn fluid at a steady roll.

It is hazardous and crazy but I don't doubt his successes. I also met a few people that tried his gear and they all said it was great.

The problem with these rxns is if the rxn solution dries out, there could bee potential problems with phosphine.

SWIM doesn't recommend any temps over 170C

Refuse/Resist
 
 
 
 
    geezmeister
(Of Counsel)
10-19-04 00:37
No 536465
      next time     

Next time, add water, cook at lower temperatures for longer times, and compare the difference in quality of the product.

Not knocking what you did, mind you... but steering you to surer successes.

mostly harmless
 
 
 
 
    buz
(Hive Bee)
10-19-04 15:09
No 536585
      patience?     

2 hour rxns aren't a hall mark of patience, though swim doesn't doubt it worked. sounds like you're ready for 24 hours with 4 grams H2O and temps beelow water's boiling point.

if you do, don't worry about the phases, as you may not witness them.

congrats, just the same
 
 
 
 
    tina_craig
(Hive Bee)
10-19-04 16:49
No 536615
      Swit_c meant more about being patient as far...     

Swit_c meant more about being patient as far as the precursor cleaning since of the 4 areas that need to be mastered these appears to be the most difficult.  2 hours 20 mins. cook time, the higher temp was only for the last 15 minutes and Ibee was mistaken, final temp was 200 degrees C, which should have made the inner flask temp 180, correct?  The reason no water was added was because the I was moist already, so moist swit_c was worried it wouldn't take off at all.  Rxn never dried out.  Will be doing a 24 hour soon, then will also try a 48 hour.  The 2 big things ibee accomplished here swit_c thinks is a showing of the signs and smells of success, which was what swit_c was lacking and kept screwing swit_c because swit_c would think, well Ibee thinks that's what they are talking about, but, now ibee knows.  Thx.

Tina Craig worked for me!!
 
 
 
 
    buz
(Hive Bee)
10-19-04 22:43
No 536676
      200F     

200C would bee a problem.
anyway, should you try a slower, wetter rxn, looking for signs may upset you, as there may not bee any.

in a way, if you smell anything, its a bad sign.
 
 
 
 
    geezmeister
(Of Counsel)
10-19-04 23:06
No 536682
      in the flask temps     


final temp was 200 degrees C, which should have made the inner flask temp 180, correct?




Not necessarily. A number of factors may come into play on the difference of temp of the reaction and the temp of the oil bath. There isn't a fixed twenty degree variable. It depends on your set up: flask size, condenser size, coolant temperature, flask depth in the oil bath, depth of reaction contents in the flask... are a few factors I know can affect the in-the-flask temperature variance from the oil bath temperature. The one way to know is to use a thermometer or a temperature sensor in the flask. Do that with each flask and condenser combination you use and remember it for later use. I have some combinations that the temperature variance is about twenty degrees, others about thirty five degrees, and one is between ten and fifteen degrees. I learned by measuring the temperature in the flask.

I've also broken all my thermometers again. crazy


mostly harmless
 
 
 
 
    morpheus
(Hive Addict)
10-20-04 14:55
No 536785
      success     

Congrats T C
Swim doesn't do hot fast dry reactions anymore but
phase 2 does not always happen the way you have
read about or expect it to happen,especially how
exothermic and ready to blow it gets.
Calcium chloride or dam* rid is sold with its own dessicator
so dry the I2 better and do a 48 hour LWR like you plan.
If your excited now just wait.
 
 
 
 
    tina_craig
(Hive Bee)
10-20-04 21:16
No 536845
      Swit_c is a little confused, have read ...     

Swit_c is a little confused, have read write-ups that declare 180 degrees Celsius and max temp on rxn and also seen 180 degrees Farenheit, so which is correct?  Has swit_c totally missed something here?  Looking for the missing link and thx in advance.

Tina Craig worked for me!!
 
 
 
 
    geezmeister
(Of Counsel)
10-20-04 21:48
No 536852
      proposed test     

Run one reaction at 180F, and another at 120C. Compare the results.

mostly harmless
 
 
 
 
    wareami
(Hive Addict)
10-20-04 22:49
No 536861
      Success windows...     

Geez, Actually both temps fall into the safety zone tempwise.
It just takes longer at 82°C.


Time and Temp Window of success with the LWR
48-72hr 82°C=180°F
24-36hr @ 120°C=248°F

Optimal LWR temp and time
30-48hr @ 212°F=100°C
*Note* All temps Internal Flask temp of reactants

While it's highly suspected, There is still no documented hardcore evidence(aside from the collective bioassay experience) that Excess heat is the cause of SpaceDope(shooting star vision/ their out to get ya gear) or whether it could be directly blamed on insufficient H2O in the reaction, combined with excess heat!
But it's just as wise to avoid excess heat, as it is wise to make sure the rxn is plenty hydrated as well, without over diluting of course!

T_C bee: 180°C=356°F falls in that excessive temp range.

Ohhh...and congrats on the success and a special kudo's for taking the time to understand and put into practice the importance of front-side extraction!
Compared to the rxn itself....extracting gaak-free clean feedstock is 90% of the battle!
And remember, There's always room for learning new stuff!

If the shoethrows fits...Ware Itout
 
 
 
 
    geezmeister
(Of Counsel)
10-20-04 23:21
No 536866
      I didn't say they didn't...     

I didn't  say they didn't fall outside the window of success with a LWR.

I thought after he tried one, then tried the other, he wouldn't have the question again. I sure didn't. smile

mostly harmless
 
 
 
 
    buz
(Hive Bee)
10-21-04 00:53
No 536905
      why risk boiling water?     

beeing as the HI rdxn of psuedo-ephidrine can bee accomplished at temps beelow the bp of H2O, why risk it?

gaseous water can make a mess. the water is needed in the rxn vessal. why tempt it to exit?
 
 
 
 
    geezmeister
(Of Counsel)
10-21-04 03:38
No 536919
      repeat     

buz: Post 536852 (geezmeister: "proposed test", Stimulants)

A HI reflux can be done at 120C without difficulty. Someone wanted simple answers to temperature questions without searching for the answers, reading previous posts, or experimenting themselves to see what happened. I suggested they experiment and see the difference. They will remember the answer if they do they experiment themselves. I prefer to react my HI refluxes at about 100C but have taken to increasing the temps toward the end to hedge against the newer gakks.

Is there a problem with my suggestion to them to experiment?

mostly harmless
 
 
 
 
    tina_craig
(Hive Bee)
10-21-04 18:20
No 536974
      Thx geez for the short and sweet, will do...     

Thx geez for the short and sweet, will do experiment soon, don't really like to pursue the higher temp anyway just read that 180 number alot with differing units and figured Celsius would be the most correct being metric.  Rxn never went dry so swit_c must have gotten lucky?  This rxn, however did produce at least 4+ grams of very killer gear out of 6 possible.

Tina Craig worked for me!!
 
 
 
 
    abominator
(Hive Bee)
10-21-04 18:28
No 536975
      180 degrees in a push/pull     


Swit_c is a little confused, have read write-ups that declare 180 degrees Celsius and max temp on rxn and also seen 180 degrees Farenheit, so which is correct?


As noted below in Jacked post, the correct temp for phase 2 is 190 F.

The bees speaking of a 180 degree F temp are probably talking about the push/pull method(not practiced as much anymore due to wider success envelope with the LWR), as that is the temp(inside the flask) that "phase 2" will come on at. This is the temperature a push pull must hit to complete the reduction. After it hits this temp the rxn go on a bit and then will run itself out.

As for the LWR advice what geezmeister and WareamI said are more than enough.


Makes me stand UP/move around

 69
 
 
 
 
    buz
(Hive Bee)
10-21-04 20:57
No 536988
      C and F     

not knowing the difference beetween C and F temperature scales is problematic.

said confusion is not a good sign, considering the details to come, in almost any dream.

one thing we have to go on, even if we are retarded, is that water, in an open containor at sea level, gets very "touchy" about remaing a liquid at the temperatures of 100C and 212F.

true, the mixtures normally dealt with in this 'dream' considerably raise the bp of water.
exterior pressure does, likewise.
Therefore, there is some lee-way on the top temperatures that are stress-free.

but given the average handle shown at this forum, it feels sane and safe to reccomend lwr rxns at sub-H2O bp's.

at the end of a rxn, with containment removed, it might bee benificial to take the heat up, as long as their is ample liquid in the flask.
(do it under adequate venting and away from the pig-like snouts of those whom would foil your plans)

geezar, you seem a bit contentious of late.
know that i am a friendly brother of yours.
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
10-21-04 22:00
No 536995
      actually     

Actually the temp for second phase is 190.. It wont kick until it reaches that magic number.
 I just suggested through PM to now run a reflux and compare the two for quality.. Shouldn't be in any hurry now that a little stash has been put up. Perfect time for a long rxn.

Tighten Up!  (UH)
 
 
 
 
    abominator
(Hive Bee)
10-21-04 22:42
No 537010
      Correction noted     

This bee stands corrected.  He will say that in his experience, if one hits the 180 F temp then the action in the flask will usually bring it UP to the 190 that is needed.  190 F is the magic # for phase 2.

Makes me stand UP/move around

 69