Author Topic: Failed reaction...  (Read 3573 times)

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snoozer

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Failed reaction...
« on: August 08, 2004, 08:47:00 AM »
Recently swim dreamed of a 35g reaction. As this was only swims 2nd dream he figured it a better chance of success to stay largish. Swim proceeded to add first H2O, then LG I2 and finally LG RP. Problem was swim couldn't place the condensor on in time, before a large cloud of yellow gas escaped out the top of the flask! then when he added the E 30 mins later any HI gas that was in there would well and truly have escaped before he got the condensor back on FUCK! :( Swim was convinced that the HI dropped below the required concentration because the E didn't liquify immediately as expected but rather after about 10 mins with swirling.
There was a very little smoke being generated but not as much as expected. By this stage swim felt the reaction was doomed but let it go for the full 48 hrs anyway with fingers crossed.
So after swim distilled the reaction fluid he had a nice thick clear layer sitting on top of the water. Swim wasn't getting his hopes up though as he realized it could just be unreduced Eph. When he recrystallised his heart sank as he saw needles form instead of the hoped-for plate-like meth crystals. However swim needed confirmation it was not gogo, so had a toke. It melted clean as, but was still the shitty Ephedrine buzz.
So swim has decided to go with adding the E along with the RP,I and H20. Better that than waiting 2 days to find out he got back nothing! To make matters worse his final yield was only 9g of E! (thats 25%). He can't afford to waste precious precursors...
So swim's question is: If swims using .8ml of H20 per g of E, when the E is added won't the water be soaked into the E rather than sitting as a puddle in the flask? or does this not matter if theres no free water as long as its in there its OK?
Back to the drawing board :-[

abominator

  • Guest
Sounds like you done everthing right, sans the
« Reply #1 on: August 08, 2004, 03:05:00 PM »
Sounds like you done everthing right, sans the condenser.  Get it on in time next time and you should have no problems.


So swim's question is: If swims using .8ml of H20 per g of E, when the E is added won't the water be soaked into the E rather than sitting as a puddle in the flask? or does this not matter if theres no free water as long as its in there its OK?
Back to the drawing board




I doesn't f*&King matter man, the whole point of a LWR is that one doesn't have to go by the signs like the push/pull guys do.  As Ware and Geez say "Set it and forget it."

These refluxes are very tame reaction

EDIT:Wizard X has always maintained to add the iodine and red phosphorous first to make the HI.  By doing this, the E will not be affected by any by-products produced by the HI being made.




p2e3r4f5e6c7t8

  • Guest
Crazzy man
« Reply #2 on: August 08, 2004, 03:23:00 PM »
Helloo snoozer dude :) , Just a question,?
If you have lag grade PH and lab grade I2, Why the hell would you want to fuck around making HI, When you could just do a push/pull reaction ::) , Not to mention that 2 days refluxing compared to a few hours just dosent make any sense ::) .
I know swip would rather get shit done in a few hours and have some product finished, rather than a a couple of days.
Not to mention having to have glassware and hot plates siting around for a few days, This is just swip's rambling's but it just dosent sound economical. ::)


snoozer

  • Guest
Yeah well swim was concerned about damaging...
« Reply #3 on: August 09, 2004, 04:08:00 AM »
Yeah well swim was concerned about damaging the E if it was added at the same time as the RP and I, so thought making the HI first would be safer.
A litmus test confirmed the pH was 1 so obviously some HI was made, probably just not enough to reduce the E.
There wouldn't be any reason not to use the same E again would there?

geezmeister

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You want the E to be wet at the start, in my...
« Reply #4 on: August 09, 2004, 04:32:00 AM »
You want the E to be wet at the start, in my opinion. If you will add the E and Water and red phos, and swirl until you have a homogenous mixture, your red phos will be spread out in the flask in the wet mix so you won't have that quick fuming smoking start. You don't want any smoke. If you add the I2 last, after stirring all the other ingredients well, you won't have a lot of red phos hitting the Iodine and making HI suddenly. The process will be slower, the I2 will dissolve slowly, and you can bring the whole thing up to heat over thirty to forty minutes. If you add the I2 and spread it out, then pour in the red phosphorous, no matter what you do you have an area with a concentration of red phosphorous that will react immediately with any I2 present.

That, anyway, is my rationale for adding the I2 last. Everyone has a reason for the way they add the ingredients. There isn't a right way, there's just the way you have figured out how to do it and have success.


CharlieBigpotato

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toss it all in at once
« Reply #5 on: August 09, 2004, 04:55:00 AM »
not only does it work, its way less confusing.
also, in the vein of "less confusing", never open the god-damned rxn after tossing it all in.
you'll only fuck it up.

why make this difficult?

try these numbers:
4 gms H20
5 gms. precursor
6 gms iodine (dry)
7 gms mbrp (dry)

rb flask in oil-bath; top temp 100c
cap with punch ball after allowing HI to generate; chasing out flask air. ignore (as best you can) for 24 hours. fuk 48 hrs. 24 is too many already.

expect absolutly nothing exciting.
ignore all smells; colors; pushing; pullings; phases #1 and # 2.


The_Animal

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Re: When he recrystallised his heart sank as...
« Reply #6 on: August 10, 2004, 03:10:00 AM »

When he recrystallised his heart sank as he saw needles form instead of the hoped-for plate-like meth crystals




Ephedrine or pseudoephedrine do not crystallise into needles a.f.a.i.k, swim seems to think pinwheels is their description.pinwheels are different from pins

 in fact I seem to remember chemfinder used to describe the pure crystalline material as pins, as did Fester I believe although  of course - I cant be arsed to back up any of these claims as chemfinder doesn't show this info anymore and I am easily discouraged




CharlieBigpotato

  • Guest
while i'm at it:
« Reply #7 on: August 10, 2004, 03:56:00 AM »
(gosh, animal. so cool to see you!) (cyber-see)

for a newbee, obsessing on particular chrystal formations is as distracting as focusing on colors and smells.
consider all the varying forms of H2O chrystals.
(jack frost, etc)

you may never see pinwheels.
fb fans my never see plates.
if you use way excess I2 or way too little rp, you post-rxn "honey" will look like purple shit; even if you had 100% reduction.

put your trust in the ingrediants; the rest is like baking a cake.