Author Topic: LWR question  (Read 14433 times)

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wareami

  • Guest
DH2O
« Reply #20 on: February 23, 2004, 01:50:00 AM »
The window of success can still be peeked through at .05ml per gram of E.
This rxn is a set it forget rxn and Ibee has never had any adverse affects from using that ratio in up to 72hr cooks.
Others use .08ml per 1g E and that's fine as well.
Even though it's set it forget it style, Ibee adopted early on to make 8-10hr check points to squeegee down the flask sides to keep the reactants from building up too much on the glass!
Shorty: Thanx for that link! Don't recall seeing it before.
On my way to check it out!


CharlieBigpotato

  • Guest
24 hrs on small amount ain't hot and fast
« Reply #21 on: February 23, 2004, 04:46:00 AM »
wareami,
i can see that i don't have the strength to furthar debate this.
i'm supposed to bee on the couch, spewing.

btw, why assume dh2o wasn't used?
but i yield, oddly, beeing a fan of slow and wet and boring from awhile back. 

and if swim ever dreams again, it'll bee 49 fucking hours!
even if its only a gram.

i wonder what one of the real chemists would say about this debate?


Phlegm

  • Guest
Two questions always come to my mind
« Reply #22 on: February 23, 2004, 04:59:00 AM »
when reading these thead types. 1) Why is automatically assumed a hot reflux is done dry?  A hot WET reflux of 5-10 hours will produce excellent yields and quality of meth HCl; and without having to piss around with this stuff for 3 days and without having to worry about burning down your house while you sleep.

2) Why does virtually everyone call their long wet thing, incubated at 100 C, a reflux? It certainly is not a reflux. A reflux of a hydriotic acid based reduction will involve a reaction temperature of approximately 127 C.

CharlieBigpotato

  • Guest
evidently not
« Reply #23 on: February 23, 2004, 05:28:00 AM »
even water heated to under 100 c will make vapours  that leave the flask area, condense and drip back down into the action.
i'd like to agree with you, phlegm, beecause you were sorta backing my side of the debate, and i admire your name, but, for some reason, it seems to work beelow that temp. and  with water weight 80% of 'e' weight.

strange thing, really.
what about reflux in low pressure at lower temp?
does it count, or is the heat what counts?


SHORTY

  • Guest
A good analogy
« Reply #24 on: February 23, 2004, 06:04:00 AM »
I think it was Rhodium who said..
"if it takes 10 minutes to boil 1 egg, would it take 20 minutes to boil 2?"

Ware,
I found that doc along time ago and finally got Rhodium to put it on his site.  It really is good information and seems to bee from a reliable source.  Let me know what you think of it.


wareami

  • Guest
Debait???
« Reply #25 on: February 23, 2004, 07:18:00 AM »
First off...the main controversy that surrounds this subject is that few are really equipped mentally to adjust their mindset to practically applying it and doing the comparison tests openmindedly.
It's easier for many to continue achieving what they are accustomed to under the same rxn conditions!
Since I agreed to participate in these so called debates, my aim isn't to let anyone down, even though I'm the worst spokeperson when it comes to expression and brevity.
I'm sure several are falling of their chairs at the display of consise thoroughness devoid of AWE Wareamiese lately, But hey...I'm trying!
I've been against the term "reflux" attached to this rxn style from the outset. But for lack of a better term and the similarities to "refluxing" by definition, whoami to buck the system? :-[  ;)
It works!
All the ARRRRGuments seem to revolve around trying to incorporate every possible way to hang onto the old familiar anyway a bee can and apply it to this rxn style!
I keep telling bees as I have from the GhetGO that the slightest deviations in time and temp result in a different product! Sure it's the one that can be sold or consumed and nodifferent that what they are use to!
They can't tell a superior product until they themselves expose themselves to it!
The only way to do that is by making it themselves cause they sure as hell won't buy it off the street until the majority start cooking it this way!


btw, why assume dh2o wasn't used?



Because that's the essiest, most convenient comparison. It's what the elders handed down to Ibee and what wet his feet!
Unless you take for example the arguement phlegm is trying to propose! Let's address that as well while we're here...


1) Why is automatically assumed a hot reflux is done dry?  A hot WET reflux of 5-10 hours will produce excellent yields and quality of meth HCl; and without having to piss around with this stuff for 3 days and without having to worry about burning down your house while you sleep.



Key words there are HOT!!!! That is the only way a bee can alter the time in this rxn!
The problem with this will only be experienced and noticed by what many describe as "Whacked Out Tweeker" types that for whatever reasons are sensitive to the Psychosis sides associated with hot cooks and certain impurities present!
There has been enough evidence provided here at the hive that confirms that association.
Obviously, if you're not affected by this, how would you know? Ibee knows because he's sensitive to it and can produce product that doesn't affect him in that way if the heat stays low enough! This brings us to the impurities, aziridines, iodosides, dimers, and a slew of others only the forensic and chemists can spew forth with any kind of authority and accuracy.
Ibee associates this missing tweekin syndrome directly with heat in excess during the cooking process and the logical conclusion lay somewhere in the possibility that those side impurities get cooked off over time! What is the exact time window they fall off? Fuck if I know! How many GDamn rxns ever run identical? But to be safe and gaurantee product doneness in a less toxic state, we go with what works.
This LWR rxn has run identical several times for Ibee and that is all the confirming consistancy he needed to warrant taking UP the cross and delving deeper into explaining the benefits and the process itself, the best he can. 
Many have adopted this LWR without question and most every one has claimed it's the best switch they ever made.
As I said....I'm not defending this rxn, per-se. I'm merely answering the questions others are too occupied conceptuallizing why it's inferior to their tried and true method to find out for themselves!
It's almost reminicient of the Tetra-scapades from daze of yore ;D  and trying to convince others of the merits and benefits in applying that solvent to battle polymers and antihistamines in extraction!
Just do the LWR rxn as outlined and if it fits you're liking and tastes, help your brother/sis bees out and spread the word!
If it aint your cup of tea, GO with what ya know!
Ibee certainly won't lose any sleep!
That's gauranteed!
Chuck-E(saycheeze)...luv ya too bro!




WmPerry

  • Guest
Interrupt rxn, Sleep W/both Eyes closed?
« Reply #26 on: February 23, 2004, 03:49:00 PM »
i hesitate to pipsqueek into this thread, but might'nt one simply kill the heat on rxn, go to bed/leave house etc. without fear of catastrophe, and restart when you could pay appropriate attention?
   my last 24 hr rxn's gigantic improvement over12hr proved to me that my next will go 48. But i aint gonna baby sit it 2 days running.
   thanks for the knowledge, all.

clandestine

  • Guest
YES
« Reply #27 on: February 23, 2004, 04:04:00 PM »
There is no problem as far as swim knows..Just keep your condenser capped off and let no vapors escape.

Also keep tabs and dont skimp on the time..  36 hours atleast.

SHORTY

  • Guest
You really don't have to babysit the lwr...
« Reply #28 on: February 23, 2004, 05:51:00 PM »
As long as you keep the temp below 120C and have sufficient water in the rxn then there is no need to babysit the rxn.  Just look in on it every 8 hours or so and you'll be fine.  It's really not much different than your hot water heater or other appliances that are on all the time.  I mean the only problem that could arise is an electrical short circuit in your hotplate but with a decent hotplate with an inline fuse or circuit breaker it should be just as safe as any other appliance. 

Considering you don't have any pets that might get curious and knock your flask over while your gone!


geezmeister

  • Guest
babysitting the LWR
« Reply #29 on: February 23, 2004, 11:20:00 PM »
With care taken to make good seals as needed, equipment in good working order, and a thermally-limited heat source, you can leave a LWR on its own and return after the annointed thirty six or forty eight hours and work up what you have. A bad pump or a leaking seal can ruin the fruits of your pseudo extraction labor, and a heat source without a thermal limit switch could cause a fire.

The heat source I use for untended reactions is a cool-touch deep fat fryer with an attached lid that covers the grease while the unit is in operation. It has its own thermal limit switch. I modified the lid to hold the flask in place with a nylon wire tie snugged  around the neck. The condenser is held by a clamp in a lab stand and I add wire ties to the water hoses to the condenser if I am leaving it unattended. I have never lost a lwr to lack of attention using this setup. I did lose one done on a hotplate when the flask-to-condenser seal failed and the reaction ran dry while I was gone. I would likely have lost this reaction if I had checked it every four hours or so.

My point is that with appropriate equipment and reasonable precaution, the risk from leaving a lwr untended is not that great a risk. It will never be risk-free, and I will never recommend that anyone leave one unattended or unwatched for long periods, because as sure as I did, someone would do one using an electric skillet with a malfunctioning thermostat and burn down the neighborhood, blaming me for saying it was safe to do. There will always be some risk involved in leaving anything like this untended. You can control the nature and type of risk you take.  That said, I have done a number of 36 and 48 hour refluxes without so much as even checking on them once during the reaction. I usually check them at least every eight to ten hours, but rarely do anything besides changing the water in the ice chest for cooler water. If you use your head, good equipment with thermal limit switches, and take reasonable precautions, this type of reaction can be done and done safely without constant supervision. Do the synth several times to find the weaknesses of the system you use, learn the failure points, and get a feel for how the system operates. After you do a few that need no tending, you will feel more secure about letting it run without watching it all the time.

If doing a lwr means the synth must be unattended for periods of time, accept that fact, and plan accordingly. Your equipment can be set up to allow unattended operation. This is  entirely "doable." If you doubt the integrity of the seals or equipment, turn the heat off until you return.
Do not let the idea of having to watch the flask for two days deter you from this method. You will not have anything to watch, nor will you need to watch it. Plan so that you can leave it alone to take care of other things. But use what common sense and good judgment you have in doing it, and think failures out so they are not emergencies.