10-27-03 05:42
No 466997
Morning Bee's,hope alls well.
while dreaming of a long wet reflux(12+hrs)for the first time.About 5-6 hrs. into it lots of HI crystals were noticed to have formed on the upper neck of the flask and even in the ballon.
Swic's first instinct was to open it up and wash the HI down w/little dh2o to get it back into the soloution/reaction.
Is it important to yeild/reaction completion to do this?
Swic's dream baloon is suffering from structural integrity damage and Swic's afraid if he takes it off it's not going to go back on w/out breaking.Any advice is appreciated bee's,will bee standing by in dreamlimbo......Peace,ChambeRed.
Bee's Don't Die,Only Multiply....
(Of Counsel)
10-27-03 07:35
No 467017
You probably are running the reaction a little drier than you should, in my opinion, or you have holes in the balloon that have allowed moisture to escape from the reaction over the six hours you have cooked it.
If you were using an condenser I would expect to see these crystals in the condenser rather than the flask neck. I assume you are doing a reaction with a balloon on the flask, or a balloon on a hose attached to the flask.
The crystals in the flask neck are most likely PI3 crystals. Add water to them and you get HI. Why are they there? I think its because you do not have enough water in the reaction. You have phosphorous and Iodine escaping the reaction as PI3. The iodine is not being recycled to HI, even though there is phosphorous present. The PI3 does not harm the reaction, but it doesn't help it either. It removes iodine and phosphorous from the reaction. You have that much less HI in the soup. HI in the reaction will help drive it completion. You want to return it to the reaction.
So wash the PI3 crystals down back into the flask with a little water.
Let the reaction cool down as you go buy another balloon. With a syringe or something equivalent add enough water to wash the PI3 back into the flask. Cap immediately with a new balloon, return to heat. I would suggest how much water to add, but have no idea how much you started with or how much you have now.
You describe this as a long wet reflux and if you started with "enough" water and it has not escaped, you may be cooking at a higher temperature than the reaction needs. I suspect, however, that you are leaking moisture from the reaction and it is getting drier as it progresses.
Your reaction has been active, you have reduced most of the pseudo to meth, but still probably have some intermediates present. You are at the point of the rection where you cross the line between good dope and great dope. The effort and time it takes to get a new balloon and let this reaction continue will be well worth it. The formation of the PI3 crystals shows the I2 is still present and the phosphorous is active, which indicates your pseudo was clean enough not to contain inactives that coated your phosphorous and took it out of the mix. Get that phosphourous and I2 back into the soup and let it make HI and get a complete reduction. That is the beauty of the long wet reflux. Just let it simmer to full reduction. Use a little more water. It really helps.
ICMOI I
(Hive Addict)
10-27-03 07:37
No 467018
Edit: Follow geez's advice its better than mine. Sorry geez i think we must have posted at the same time and you beat me to the punch
Just replace the balloon with a new one or better yet a condenser. You can knock those crystals into the flask or throw them out along with the balloon either way it won't effect the finished product or yeild.
It wasn't Me!
(Stranger)
10-27-03 08:04
No 467023
Does the formation of the crystals when using a condenser mean the same?
(Hive Addict)
10-27-03 08:18
No 467026
I get those with almost every rxn and i use 50% hypo. I never considered adding more water but maybee it would be worth a try. Geez?
It wasn't Me!
(Of Counsel)
10-27-03 09:12
No 467035
I've had these crystals in the condenser so thick that they clogged the condenser. I dropped some water on top of them, but had not taken the flask out of the oil bath. The water would not dissolve all of the crystals...and I started to tamp them down with a thermometer and fortunately realized the flask had to be building pressure inside it. I removed it from the heat and let it cool and thus narrowly escaped blowing HI all over the cieling and myself.
The reactions where I had this happen were all on the low end range of the amount of water in the reaction. I don't seem to see the phenomenon when I use at least 0.8ml H2O per gram of pseudo (which is really saying 0.8 ml H2O to 1.2 gm of I2. I was testing the envelope at the time trying to establish some personal ratio for water to use in the PIE reaction. (I settled on 1.0 to 1.1 ml per 1.2 gm I2 and a thirty six hour reflux, because of personal preferences on temperature and time of reflux.)
I noted the formation of the crystals and their relationship to the moisture content of the reaction long before I started doing long wet refluxes. I noted them when the reaction "cooked down" to a thick state in my early days. Back then, I would add more water and cook it down to a thick state a couple of times before believing it was magically "done." I considered the crystals forming as a sign of success. It is, but only incidentally. Most of my failures at the time were red P related, and caused by less than clean pseudo, so the formation of those crystals did at least indicate my P was still clean enough to react.
I also note that PI3 formation seems to be more prominent when there is an excess of P and I2 available for the pseudo to be reduced. The water used was low for the amount of P and I2, but not for the pseudo. Tying the water amount to the I2 rather than pseudo would prevent this, and still give the same concentration of HI as the more common ratios would.
I once wondered if the formation of PI3 might be incidentally related to the progress of the reduction of pseudo to meth, reasoning that as there was less pseudo to be reduced, no more HI was produced. The problem with this is that it assumes that the I2 and P know what is going on and plan accordingly. I rather doubt that is involved.
Shorty: I used to get the PI3 crystals in the neck of the flask doing hypo reactions using concentrated hypo. When using it straight from the container without concentrating it, and refluxing for a longer time, I never got the PI3 crystals, but I never cooked for more than about five or six hours even with the 50% hypo. The difference? Might be the ratio of phosphorous to H20 in the reaction. More phosphorous for the same amount of water might result in some phosphorous tying up some I2 and taking it out of the reaction as PI3. I think just adding a little water to rinse down the PI3 crystals would be all I would add to a hypo cook, but you do more of these than I do, since I haven't been doing them at all of late.
ICMOI I
(Stranger)
10-27-03 09:41
No 467043
In the relatively miniscule number of reactions swig's done, (all PIE) he's been fairly certain that there was, if anything, an excess of water. Having only a post-Long Reflux Surprise Geezmeister and Osmium (any time period) as primary influences insured a healthy fear of anything that's hot, dry, or over in less than a day.
This is why I am interested, swib tells me he does have them form in his condenser and I'd be happy to tell him to add water.
thanks
(Stranger)
10-27-03 17:37
No 467164
Well its been about 24 hrs. now.Bubbles in the flask have been alot larger than at the reactions start but it seems to fluctuate beetween bubbling small and big bubbles.
Yes geez despite all eforts Swic's vessel did have a small leak somewhere,not enough to keep the ballon from blowing up though.Swic didn't bother taking the balloon off and going to the store for another so he just used electrical tape to tape off a small square on the baloon.Pierced that with a syringe and sprayed in enough dh2o to wash down those crystals(very quick violent exothermic rxn took place)carefully removed the syringe with another square of tape ready to cover the small hole.
Ratio's were 4-4.5g. pfed/8.0g. I(from tinc)/5.5-6g.rp(from matchbooks but as pristine as that gets)/about 13-15 drops out of an eye dropper.
Swic was think after he did it that that was probably excess water for those amounts?,while moisture was lost over 24hrs from the leak the reaction has stayed very liquidy throughout and as stated earlier in this post a little more h20 was added to wash those xtals down at about the 12hr. mark.
Swic is thinking he's probably good to go and should pull it from reflux and let it cool for a few hrs.
But Swic don't know jack and he seems to think if he did add too much h2o then its gonna require extra cook time(36-48hrs.)is this so?
Swic's gut tells him its a go but advice would bee very welcome.Peace bee's,ChambeRed.
The balloon finally went bust about 2hrs. ago so now its just a tube running into cold water/sand slurry for odor control.
Bee's don't die,just multiply!!!.....
(Stranger)
10-27-03 17:50
No 467167
In case it takes a while for someone more qualified to answer, I'll give you my two cents worth. I think you may have actually run a very dry reaction. As I understand it, 4-5 ml of water would have been wettish, and I think it takes ~20 drops to make 1 ml
I could be confused though
(Stranger)
10-27-03 18:10
No 467173
Hm,just put 15 drops in a cup to see what it looked like,not even close to what swic put in.Swic's now guessing more like 3 full eyedoppers,about 45 drops.Sure wish i had a 10ml. graduated.
(Of Counsel)
10-27-03 18:12
No 467174
For a long wet reflux of 4.5 gm of pseudo, I would use 5.4 gm I2, 3 gm red phos, and 4 to 5 ml of water. Your ratios were heavy on I2 and red phos, you had an excess of I2 and P for the water available, which was way too little for a wet reflux. Hence the PI3 crystals. Remember. Water is essential to this reaction. You did not really use enough water in my opinion for a wet reflux.
More I2 is not necessarily better. The additional I2 will cost you in yield over what you could have had if you had added about five and a half grams of I2. More water, less I2, less red phos. Longer time. The results will pleasantly surprise you.
ICMOI I
(Stranger)
10-27-03 18:47
No 467180
Thanks for your responses geez.
Swic will definately do it the way suggested by bolth u and wareami next time.
But as for this run...add a couple mls h2o and cook for another 12-24hrs.?,call it good enough,experienced gained and move on to the post-rxn workup?
Thx geez.Peace,ChambeRed.
(Hive Addict)
10-27-03 22:33
No 467219
Water without a trap or you could end up adding alot more water than you want to should suckback occur.
It wasn't Me!
(Stranger)
10-28-03 01:51
No 467243
Must bee Swic's lucky day.
Found about 100ml. pre-dried acetone in an unlabeled(gotta quit doin that)container.
Product was acetone flashed at near dryness and followed by another acetone rinse.Rinses were saved for reduction/cooling.
No recrystalization was done on sampled portion but it appears pristine anyway.(everything but sample will bee recrystalized tomarrow)
As far as comparing it to swic's previous runs,it can't bee done.There is no comparison!.Now many bee's claim a comparable product can bee obtained from a shorter/dryer reflux and swic beelieves them.However someone as inexperienced as swic w/the rp/i reduction of eph beeing able to turn out professional grade dope using a long/wetter reflux(mostly geez,scotty,and wareami's posts for info)tells me something anyway.
Swic says he likes it too
.Thank you so much guys/hive swic hasn't experienced a high this pleasant since his first or second time trying ME,
and swic only took 2 tokes because he's hopin to sleep!, a liitle anyway
.Good luck and sweet dreams bee's.
try this out sometime when you got a stash and aren't too impaitent,you'll bee glad you did.
Peace,ChambeRed.
[blue]Edit:
Swic just had the opportunaty to share some with a friend and he claims not to remember when the last time a hit from the glass made him feel like that.
Nice to have your opinion seconded(esspecially when you don't have enough ex. with the substance to judge it properley).Doesn't look like sleep is forthcoming as i'd hoped so i guess swic should start that next run instead....36-48hrs. can bee a loooong time...
Bee's Don't Die,Just Multiply........