Author Topic: Bath Temp for LWR  (Read 5625 times)

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kris_1108

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Bath Temp for LWR
« on: December 20, 2003, 03:56:00 PM »
Hi,
ooooohhhh i reckon ill get an utfse for this one :-s
there is so much stuff in tfse now its hard to sift through it all.
Anyway its a fairly simple question.

Swik has a nice 240v hotplate now and a rxn is in sight. And this newbee has decided on the Long Wet Reflux; 24hrs at 100C (celcius, which is 212 degrees F!).
Ok so there will be a thermometer in the oil, reading 100c, however will the internal flask temp be close enough to the same (100c)?.
I imagine this depends on stuff like flask size(250mL), oil volume, level of flask submersion, ambient temp, etc.)
Anyway that will bee followed up with a steam distill so this procedure should hopefully be fairly successful.
Anyway Thanks

biotechdude

  • Guest
Indeed depends
« Reply #1 on: December 20, 2003, 04:27:00 PM »
Swix's setup has a 25'C temp difference from oil to flask solution.  For other bees it is 10-15-20'C etc...really depends.

EASY SOLUTION - put some plain jane water in your flask and heat the oil up slowly.....when the water starts to boil, read the oil temp (eg 120'C) and minus 100 (120-100=20'C).  Thats the temp difference (for your personal setup). YAY!

Rhodium

  • Guest
temp
« Reply #2 on: December 20, 2003, 04:27:00 PM »
The internal temperature will be lower (~10-20°C) if you have liquid refluxing, if you have not, then the temperature will be rather similar (~5-10°C lower).


bbob

  • Guest
Swim has a reaction (E,I,RP) that is at the 24
« Reply #3 on: December 20, 2003, 10:11:00 PM »
Swim has a reaction (E,I,RP) that is at the 24 hour mark under reflux, and he just realized the temperature has been slightly lower than the 100'C that he thought it was.  Is there anything other than correcting the temp that he should do to compensate?

It is 9g, 12.5, 9g (E, I, MBRP) w/ 9cc's dH20

thanks


SHORTY

  • Guest
I would let it go longer
« Reply #4 on: December 21, 2003, 01:00:00 AM »
I would turn up the temp a little and let it cook for another 12 hours if possible.


kris_1108

  • Guest
Ah Huh!
« Reply #5 on: December 21, 2003, 01:20:00 AM »
I had a dream and in that dream i said....

"Boitechdude & Rhodium; thanks guys.
Rh yep I think itll be fairly liquid in there, all up probably 6gE, 6gmbRP, & 7.2g lgI2. With about 0.8mL of h20 per g of E, all up about 5mLs.
Biotechdude that makes perfect sense ill just put about an equal amount of h20 in there and note the oil temp when she starts bubbling like mad (taking the temp as soon as it comes to a FULL BOIL and no sooner or later than that).

One other thing, the hotplate doesnt have an infinitely variable temp control, instead its got about 15 different temp settings, i was thinking if it will only settle at 95'c and the next click makes 105'c, well i could just add or subtract the oil volume which once i get it right will sit around 100'c.
anyway thanks again.
Now im searching for a post that details a LWR rxn, like the slow adding of the i2 etc. If anyone can point me to a good LWR rxn post thatd be good too.
ok seeyas"

bbob

  • Guest
Shorty- I'm sure that can be arranged.
« Reply #6 on: December 21, 2003, 04:21:00 AM »
Shorty- I'm sure that can be arranged. 

Do you happen to know if letting it cook for even longer is safe? 
I think someone posted something recently that I took to mean that it would be...   I'll look for the post though

thanks again

see signature


wareami

  • Guest
Temperature for a Wetdream (LWR)
« Reply #7 on: December 21, 2003, 08:03:00 AM »
Many have argued or disagreed in the past over matters of personal preference since the LWR won much acclaim and acceptance in the colony.
Much of those preferences surrounded trying to combine p/p hot/dry/fast adjustments with the easier, longer wetdream to suit personal tastes in order to avoid what are considered unpleasantries or incoveniences.
Those unpleasantries are the neccessary ingredients that make the reaction what it is.
It's understandable that most will want to shave time off the overall cooking time!
And basically it's easy to do but you won't end up with the same quality product.
Examples:
¤The cook temps are one way to adjust cooktime. High Temps lower cooktime
¤Intitial dh2o amounts added to the precursors when mixed is another. Little to no dh2o lower cooktime.
¤Ratio of initial precursors is another. This will make or break the rxn in regards to HI concentration.

Ibee's cooktimes for a fully reduced product range between 30hr minimum and 48hr max. That range may seem wide but it's influenced by the other two determining factors mentioned above.
The earliest cooktime can be lowered to 24hr but at a price.
Either unreacted product is present if the initial dh2o added is skimped on in order to lower the cooktime...
or spacedope is made if temps exceed 120°-140°C.
Bees will also find that an abundance of I2(above the norm) from the ghetgo will also enhance a cooktime making it shorter. This isn't a good practice because of the excess impurities/iodosides present in the end result.
First off, the extra suggested time limits have been arrived at using standard ratios that eliminate impurities in the suggested timeframe. Any attempt to shave time off is defeating the purpose and isn't considered a wetdream(LWR)
This directly effects the health aspects from what the Kidz have been told and learned.
Using a 5g example:(NEWBEES TAKE NOTE of the two cooktime examples and what makes them so.)
Ibee's suggested cooktimes fall in the range of
30hrs(example1=.5ml-dh20 per every 1gE) or
48hrs(example2=1ml-dh2o per every 1gE)for a
5g-E:7.5-I2:3.75g-MBRP or decrease to 2.5g LGRP
Yeah Yeah Yeah...some will argue that when using LGabgrade RP that a ratio of a third RP to E is sufficient to create enough HI to fully reduce the E but Ibee says that in todays cooks it's best to side with caution in regards to inhibitors designed to weaken RP or tarnish it so to speak.
Concerns that surrounded the 1E:.33LGRP earlier were to avoid flask fire or burning the E.
Today that seems to be rare and Ibee can say that because he's experienced flask fire in the past as a result of excess RP.

Cooktemps by Ibee's circle are always given in relation to bath temps not internal flask temps.
He never exceeds 120°C and always recommends bath temp be set between 95°-120°C.
As Rhodium's internal/external conversion shows, if you follow Ibee's suggestion, the internal temp never reaches a critical spacedope producing temp. An internal boiling point of water.
As we know, dh2o is a main constituent of the HI/RP rxn and Ibee's always used that relationship in temp regulation.
Bees can trace back every post from Ibee's corner and they'll find that consistant warning to not exceed 120°C when opting for the LWR wetdream.
These are just some of the main variables regarding the HI/RP LWR that make the this method what it is.
That's Ibee's take on the deal and he's stickin to it! ;D


SHORTY

  • Guest
Bbob
« Reply #8 on: December 21, 2003, 12:27:00 PM »
Do you happen to know if letting it cook for even longer is safe? 

It depends on what type of "safe" your concerned about.
If you mean will the product bee safe to use then the answer is it will most likely bee safer if cooked for 36 hours rather than 24 as you will have reduced more of the intermediates to meth.

If you are worried that you might get unexpected company and your setup is not hidden then it might not bee as safe.

The longer and cooler you cook a lwr the safer your meth will bee in my opinion.

As far as cooking it too long, wareami has done a few rxns which lasted for several days and i beleive he ended up with pseudo in some of them and that was after having made meth first and then the meth going back to pseudo.

I don't have enough patience to perform these types of experiments.  My typical rxn is a 12 hour lwr.  With hypo instead of rp.


kris_1108

  • Guest
GoodRead
« Reply #9 on: December 21, 2003, 12:34:00 PM »
I had a dream and in that dream I said...

"wareami
Thankyou Sir that was a great read. Man I've been doing some reading over the last few weeks! And I learn more every time that I come here.
However there is one thing that I am not sure of; wareami will use .5mL h2o for every gm of E in a 30hr redxn, whereas geez will use .8mL/g in a 24hr reduction. I imagine ware would reflux for ~40hrs using .8mL/g, and geez might reflux for ~16hrs using .5mL/g. Please dont think I am trying to say that one of you guys must me wrong or anything; its just an observation. Maybee I could start of using about 0.5mL/g and increase if necessary.
Anyway thanks again,
Seeyas
Kris"

bbob

  • Guest
Shorty I was worried about overreducing or...
« Reply #10 on: December 21, 2003, 12:45:00 PM »
Shorty

I was worried about overreducing or ending up with psuedo, and I completely forgot about Wareami's week-long marathons.   My patience would have, and swim's did run out at about hour 39...  oh well

thanks for the input


wareami

  • Guest
Another consideration...
« Reply #11 on: December 21, 2003, 03:17:00 PM »
As it's easy to see...the list of variables are infinate based on each adjustment and preferences that come into play....so let me clarify that not all the preferences are incorrect or attempts to cut corners.
Now after rereading...let's clear that UP for the record!

Back after geez's first report on success with a longer cook, think it was 18hr, but don't quote that, Ibee replied, "Wait til SWIG gets a load out of a 36hr run."
It wasn't long after that SWIG's corner reported "As good as it gets" product.
In so many words...or something like that.
Ibee also recalls that Geez's confimation was the happiest day in The Kidz lives as a bees because Ibee was running the LWR for months and couldn't convince bees of the selling points!
Shows ya why Ibee's not made a successful career as a salesbee ;D  or quit his day job ;)
Come to think about it....Ibee stayed looped back then as a direct result of the end-result being irresistable...
Hey? Ya think that might bee a good excuse for the invention of "Wareamiese" and Ibee's writing style?
Okay...we'll use that excuse! ;)
Well staying looped only succeeded in not researching the answers for a while which were here all along in the search engine from elder bees such as Osmium and Rhodium.
Once Ibee came out of the loop(As if :) ....hehehehe), he did search for posts that detailed controlled rxn's.
Only then did two and two make four!
Ibee only reports on his preferred method and his experience with fully reduced product.
Other bees may be using freebase which changes the playing field considerably and the reports and write-ups shoud be followed closely. If reading and following Geez, you won't be disappointed if the instruction is followed as written just as if your reading Jacked's suggestions as written. And the list GO's on for all the trustworthy bees and their contributions.
As we all know....everybees methods are tailored to suit their tastes and experience.
Ibee is far from an expert and only reports what he's been successful at and the above standards are the ones Ibee follows. They are as such with explanations why they're that way. At least the way Ibee perceives them.

The seven day cooks were back to back exactly duplicated but on the third day were combined with new precursors added and cooked for a total of seven excrutiatingly long daze and upon workup was ~30% meth and ~70% pfed.
If a reverse rxn took place we'll never know for sure but every attempt was made at bringing the product to full reduction to no avail...Keep in mind that Ibee had to take samples at various intervals and replaced precursors in guesstimates and that likely influenced what Ibee considered a reconversion.
The runs were slated to replace thankgiving dinner that were started 7 daze before turkeyday and suffice it to say, Ibee spent less time in the kitchen than he spent in the dining room! Well not really cause he was the chef that hosted the dinner and it would have been nice to have a quick pickmeUP for the Before and after KP.
Hope this helps...
Oh....Ibee likes cooking at 95°C and the bare minimum cooktime that produced fully reduced, consecutively was 30hrs with .5ml dh2o added per 1g E.
Ibee bets that others may prefer higher temps (within the ranges above) with the addition of more dh2o as suggested by geez and that would bring the cooktime down to 24 but Ibee just sets his mindset based on HIS preference and seldom deviates from that until necessity dictates otherwise.
Always take note of the writers suggestions regarding their reported successes and the Temp...Cooktime...Ratio for a LWR....they will vary but if they report "As good as it gets" achievements, it won't bee by much from the standard guidelines outlined here.
Way back when, Ibee promised gaurantees to bees that perform the LWR and he's still here since those promises were made so that should speak volumes to any bee that may have any doubts.
Ibee didn't invent the longwetreflux...he stumbled on it by way of a fluke accident and because his yields and quality seemed to differ from others reports he set on a UTFSE joyride and whatta know...The elders have been preaching this very thing for longer than Ibee was a bee.
Had Ibee read more and posted less he'd have had the foresight and salestips to offer sooner than he did!
So it just goes to show ya...following suggestions and reading things that might be considered over yer head might deserve more attention than we place on them at any given time. Not just at the time we GO in search of answers for oue fuck-UPs.


HolyCrap...Did Ware write all that?
Oh well...add another 4000 word assay to the anals of the ARKHIVES!

Sorry Os! ;)
The only thing worse than possibly pissing Os off is the Hour it takes to proofread and edit the damn thing! :P


geezmeister

  • Guest
the envelope of success
« Reply #12 on: December 22, 2003, 02:56:00 PM »
The wet reflux has a pretty big envelope of success. The range of variation of water and temperature and time has a good sized "sweet spot" that will give you good success, where the drier and hotter reactions have a much small sweet spot and much better chance of poor results.

Ware, of course, doesn't use enough water. I mean, if he did, you could probably understand what he writes.  ;D
He is as stubborn as I am, and will never admit he needs to add water and will always say I should use less, which I refuse to believe, because, after all, I'm right...

Actually we both probably are. We are both in the success envelope for this reaction. I have done a number of refluxes to test the volume of water in the reaction and to test the time against the volume of water. There is an obvious correlation between more water and longer times, or shorter times and less water. I noted that when the volume of water in mls was more than the mass of I2 in grams, the peak point in the success envelope had been passed. You can exceed that 1:1 ratio and have success, but you can also stall the reaction by having the HI too dilute. The 0.8 ml water to 1.2 gm iodine gives a more concentrated HI and I posted the 24 hour figure hoping more people who would not reflux at all would break down and do one for just a day. Once I convince you to go a day, 36 hours gets easy. Then 48 seems like a piece of cake. And suddenly you realize how simple this reaction really is.

Or you can skimp on the water like Ware. He says its enough, but I always wonder how much of his language skills are water related!  ;D  He wonders why mine seem to be related to tequila. I suspect that if you use at least a 0.5 ml water to 1.2 gm I2 ratio you are on the dry end of success, and if you use no more than 1.2 ml water to 1.2 gm I2 you are on the wet end. No guarantees outside that range, although success can be had above and below those levels by adjusting temperature, ratios of rP to I2, and increasing cooking time. At some point you sail outside the success envelope.

Ware amy be aware of where that is and I just couldn't understand the way he said it.  ;)

Actually we are both right on the ratios. I'm just a little righter. IMHO.  ;D


biotechdude

  • Guest
Daa Da Da Daaah!!
« Reply #13 on: December 22, 2003, 06:31:00 PM »
Tonight on FOX sports..

Ware -vs- Geez - The Battle for the Envelope

Ahh, i love the envelope discussions...


wareami

  • Guest
He who drinks the most tequila wins...
« Reply #14 on: December 22, 2003, 07:12:00 PM »
;D
Okay...okay...I quit!
I could try the osmium approach....
"Just put the shit in the flask with dh2o and set it @ 100°C and forget it for 36hr!"

Now that would work :)
And he's right!
And my ears are ringing now too! ;)

Anybee that has encountered the frustration of going 30-40hrs and ending UP with 30-50% meth 50-70% unreacted will know the importance of finding the right combination that works and sticking with it.

This thread started out as a request about bath temp and bees wound UP getting more than they bargained for which is cool by me.
The main point beeing...Bees following either suggestion from Geez or Ibee will come UP!
Why?
Because the one thing that Geez and Ware do agree on is standing behind the Gaurantees they make to bees.
It really is that simple.
No tequila needed for that.

Their lab practices and experiences may differ, but putting bees in the ballpark of success makes for the winning combination, IMHO

Anvil-lope Please? ;D



kris_1108

  • Guest
Thanks
« Reply #15 on: December 22, 2003, 09:47:00 PM »
Hi guys
Thanks especially to Geez and Ware for those posts.
Ok so I reckon Ill settle on 6gmsE, 6gmsRP, 7.2gmsI2 and 4.8mLs dH2O, reflux for 24hrs, with internal flask temp at ~100'C.

As for adding the ingredients well how about add the E and the RP and all of the dH2O, swirl it a bit and add the I2 in a few 1.5gms portions. When the initial rxn has subsided, the flask will bee moved to the oil bath (at about 60'c), then the heat will bee increased to make the internal flask temp 100'c.
Maybee give the flask a swirl every 5hrs...???.

The condenser is just a tube but it will have a fan blowing on it and there will be a WASHED OUT balloon on the top of the condenser for the first couple of hours of reflux. This will be removed (as long as the HI gas wont come up out of the 500mm tube!).
Followed UP by a steam distill.
Thanks again

geezmeister

  • Guest
more, less, longer
« Reply #16 on: December 23, 2003, 12:50:00 PM »
I would add a little more water, a little less rP, and cook it longer. I suggest you go thirty six hours rather than twenty four. Those were all suggestions it took forever for me to take. I wished I had taken them much earlier.

Your ratios are in the envelope the LWR provides. The excess red phos can give you a faster reaction making HI, which you really do not want here, but the slow addition of the I2 should prevent this problem.

You shouldn't need to swirl it at all after you get it mixed to start with. Leave the balloon on the condenser. There is no reason to take it off,  and it does serve as a second line of fume control.  The glass tube with the fan blowing on it should work just fine.


wareami

  • Guest
And don't forget...
« Reply #17 on: December 23, 2003, 01:09:00 PM »
The stopwatch doesn't start until the HI is made and recycling.
Ibee does his different but that's just him. And he always takes a ribbin from the bees that suggest making HI first then adding pfed. He takes the ribbin because he's hardheaded too....it's a prerequisite it seems ;)
Mixing the I with E first then adding dh2o and mixing til liquid, then adding RP, mixing, capping off and on the heat it GO's, works just fine and seems to get things underway sooner stopwatch-wise.
It is, after all, "A Set it! Forget it!" rxn.