09-15-04 13:13
No 531438
Well swim is frustrated at his latest attempt. After doing the 48 LWR with all LG and accepted ratios except E which was well cleaned, swim felt confident of success.
Swim was pleased to see what a difference drying the NP before gassing makes! a real snow storm (makes him cry at how much was unwittingly discarded previously).
So swim thinks he has a good yield, only to discover when trying to recrystallise he couldn't grow any "bigguns". Swim had to reduce to saturation and put in the freezer just to get small crystals to form. Bioassay revealed a real shitty buzz that did keep swim awake for a couple of days along with fireworks, jumping at shadows (spacedope)etc. Not happy with his results swim tested with simons reagent and robadope indicators to be sure. The test with robadope was negative indicating no presence of primary amines (amphetamine) which is what swim expected, yet the test with simons was positive! a dark blue stain appeared which indicates a secondary amine (meth-amphetamine) is present!
This has swim puzzled, according to the test he has reduced the Eph (which indicated negative to both simons and robadope)into meth but presumably only partially? as it wouldn't grow large meth crystals only small eph needles and gave a fuckin' shitty buzz when smoked with tweaky symptoms.
This is the 2nd reaction which has produced under-reduced goods. Swims very first time he had partial success when he used a hot sand bath without water and a few times the temp climbed over the 100c he planned on. The next couple he used wet sand constantly topped up with water to keep the temp at 100c max.
So swim thinks while 100c is hot enough for the reaction maybe the temp in the flask didn't reach near this hot when wet sand was used. So swim is gonna invest in a deep fat fryer and set the oil temp at 120c which should get the flask to around 100 or so. Swim believes the reaction temp in the flask was too low and was the culprit.
If left alone will partially reduced Eph/meth not form large crystals?(it was left in the freezer a week!)
(Stranger)
09-15-04 13:30
No 531441
Sorry, your temp just wasn't HIGH enough. Jack it UP to 120-125C. If your scared, go to CHURCH! (UTFSE) for info pertaining to internal/ vs external temps.
Results may vary!
Beyond the Gates
(Hive Bee)
09-15-04 13:34
No 531442
So swim is gonna invest in a deep fat fryer and set the oil temp at 120c which should get the flask to around 100 or so.
As you suggested, the wet sand wont cut it as a heat source for the LWR. The fat fryer (with peanut oil) cranked to 120`C will provide the 100`C reation temp you require. Caliberate the oil-bath setup as in Post 467534 (biotechdude: "Flask and oil bath temps", Stimulants)
Swim believes the reaction temp in the flask was too low and was the culprit. If left alone will partially reduced Eph/meth not form large crystals?(it was left in the freezer a week!)
Correct. When temps are too low you will get partially reduced eph/iodo-eph intermediates/meth that produces the bioassay you describe. Further, the product doesn't crystalise into large crystals.
Recrystalisation of small quantities produces small crystals (especially with 'wet' crystalisations in the freezer). It may be easier (for small batches) to dissolve in clean solvent (alcohol, water, acetone) and leave to slowly evap in the open air undisturbed for a few days or longer.
(Stranger)
09-15-04 14:09
No 531446
Yeah this is a bit redundant but if your sand bath temp only got to 100C then most likely the inside of your flask was around 80C give or take. This is definitely not hot enough.
Also next time post the ratios used and maybe describe what the inside of the flask looked like, eg smoke, bubbling on the surface, as more experiences bees can tell what's going on by these signs.
Your an individual just like everyone else.
(Of Counsel)
09-15-04 16:26
No 531460
Two points that might help:
The temp in the flask needs to be high enough; the precise temperature is less important than hitting the range of temperatures that work. When I started doing long wet refluxes, I measured the in-flask temperatures with a thermometer and watched the reaction at the measured temperatures for visual cues. I found that when the surface of the fluid was about fifty percent covered with small bubbles in the early stages of the reaction, the temperature measured just under 100C. At 105C the surface was nothing but bubbles. Having observed the same thing several times in a row, I began setting the temperature by visual observation of the surface of the reaction fluid in the flask. The temperature of the oil was about 25C higher than the inside of the flask with the combination I was using. This will vary from setup to setup, depending on flask configuration and size, temperature of the condenser cooling water, how full the flask is, how deep the flask is immersed, and probably several other factors I haven't even considered.
The temperature of the reaction can be left as is for the duration. If you have any question that you may have less than pristene pseudo -- if you suspect you may have polymers left in the mix -- I suggest that during the last half of the reflux you increase the temperature. The increased temperature of the reaction could be raised at twenty four hours to the 120C range, at thirty six to the 140C range, at forty two to the 160C range, and at 44 to the 180C range. Other bees report increasing the temp to 200C for the last four hours; one mentioned 220C. None reported adverse effects on the product from increasing the heat at the end of the reflux in this manner; the reports of improved quality of the product are anecdotal, as none of us can be certain how much of which polymer remained in the pseudo. The common anecdotal comment was the increased temp improved quality and yield, but none of us have done controlled studies (at least so far as I am aware) with everything identical except the change in temp. The temp won't overcome all the gakks, but it does combat some of them.
I suspect low temp was your principal problem, but it also is possible that the effect you report is related to the reaction inhibitor included in the Eudragit packet. Its effectiveness is higher at lower temperatures, at least in my experience.
mostly harmless
(Newbee)
09-16-04 10:51
No 531586
Yep, low temps for sure was the problem as the Eph was extracted close to 2 years ago (before all these shitty newer gakks appeared) and saved for "a rainy day"
.Thanks bees!