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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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 #1 
Old 2003-12-11, 19:57
amine_assimilator amine_assimilator is offline
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Default please, help this sorry SWIM

SWIM just tried his first synth. it was a disaster! SWIMS story:

ing.:

4.5 gm. pseudo freebase

6.5 gm. MBRP

8.5 gm. I2 (from 7% tinc.)

SWIM had the pseudo and rp mixed and cooling in the freezer (250ml erl flask)

SWIM removed the flask from freezer and added the I2, two marbles (big mistake), and an aluminum beer can pop tab (possible mistake). at this point SWIM should have added a 2ml dH2O ice cube, but added no dH2O at all (stupid SWIM), right? in addition, SWIM had a solid stopper on the flask (stupid SWIM, should have had the condenser on) bcause SWIM was waiting to see if it fired bfore adding the dH2O (stupid SWIM)

SWIM began swirling it and after a while noticed some liquifing.

in between SWIM's swirling SWIM began dipping the flask in a bowl of cool dH2O. should have been ice dH2O, right? (stupid SWIM).

at this point SWIM noticed an RP fire in the flask! SWIM began swirling it forcefully, nothing, SWIM ran to the sink and got some cool faucet water and added this to the bowl the flask was sitting in and began swirling again, too late! solid stopper popped out, was replaced. SWIM began swirling it again at which point SWIM's fucking marbles cracked the flask (concussion plus high pressure from solid stopper, fucking SWIM!)!

bottom line:

SWIM has a reaction flooded w/ 250ml water (SWIM lost 30 or 40mls of it)

CAN IT BE SAVED?!?

SWIM only has 20 hr.s to do something w/ it, otherwise has to wait untill tue. to do anything w/ it. how can it b stored?

it can b boiled down and reacted again, right? do more reactants need to b added, if so how much and at what point?

how much should it b cooked down? should it b cooked down w/o the condenser? should SWIM just forget it and chalk it up to newbieitis, and start over?

SWIM knows he's an idiot, but could anyone tell SWIM where he went wrong and what to do next time? (what a waste of obviously very reactive precursors though, fuck!)
 #2 
Old 2003-12-11, 20:19
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

can't SWIM just boil till the cows come home (condenser on or off?)?
 #3 
Old 2003-12-11, 20:43
kman kman is offline
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Default Re: please, help this sorry SWIM

What the hell did you put an aluminum beer tab in there for? Even if aluminum works(I don't know if it does), I think you'd need to put tiny pieces of aluminum foil, not a friggin' beer tab! Hope you have better luck next time.
 #4 
Old 2003-12-11, 21:01
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

yeah, SWIM knows, but can it b saved?
 #5 
Old 2003-12-11, 22:48
RNX57 RNX57 is offline
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Default Re: please, help this sorry SWIM

sure it can be saved, pour into a jar first n remove the tab n marbles, put in a flask and boil at bout 250 for while, ur lookin to get back to a thicker lookin mix, u could add a gram or so of suse to it also to help lose the dh2o, 250ml is alot of dh2o and it will be a while boiling.. if u can swim would start over, this time use a 1 part rp to 3 parts suse and io,,, add half the weight of suse in dh2o ( 3 g's suse = 1 1/2 g's dh2o) to be safe throw a tad more rp in, but keep suse and io at close to same or a TAD more io, add nothing else to the mix.... just rp/suse/io and dh20.

go with what u read on basic rxn with rp/io, dont add or inprove on it till u got an idea of how it workzzz.

hope u have better luck on next dream, stick to basic's on it n u will dream fine...

rnx57
 #6 
Old 2003-12-11, 23:11
DarkSky DarkSky is offline
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Default Re: please, help this sorry SWIM

My friend, at this point you should just forget it and write it off to experience. You've put enough H2O into it for 20 rxn's. Your just going to waste your time trying to save it at this point

Next time forget the marbles and forget the aluminum, you just don't need it! Also, NEVER seal the flask, you risking having the flask explode and embedding galss in everything in the room, including you! Not only that but HI acid would be sprayed everywhere. SEALED FALSKS ARE A NO NO!

Your I2 seems a little high in your mixture, I would suggest for a 4.5gE rxn I would suggest 4.5gE/6gI2/5gRp and 4ml DH2O at 100°C for 8 to 12 hours using a condenser.

Don't feel too bad, almost everyone fails on their first few attempts. Just don't give up and you will succeed
 #7 
Old 2003-12-11, 23:16
RNX57 RNX57 is offline
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Default Re: please, help this sorry SWIM

glad u said that dark, swim plum forgot to say...... put a ballon on the top, or a condencer,,,, never SEAL a RXN

broken flask = 20 bucks

lost regents = 50 bucks

good advice = priceless

RNX57
 #8 
Old 2003-12-11, 23:17
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

thanx, RNX,

so, you're saying to boil it at 250F? isn't that a little high? should this b w/ the condenser attached? it's an awful lot of water (250ml), any idea how long it will take?

this was SWIM's first attempt at a synth and after all the prep time to see that flask crack, well, let's just say it was a let down!
 #9 
Old 2003-12-11, 23:21
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

yeah, fellas,

i'm just gonna say fluck it and go buy some more pseudo. thanx for the help.
 #10 
Old 2003-12-11, 23:55
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Default Re: please, help this sorry SWIM

What?! Sure he's got enough for 20 Rxns, but a simple boiling-off the extra water with no top on and adding a tad-bit more of I2 is all you'd need to get this bad-boy back in the saddle!!



Hell if anything, salvage the R.P. man! If not the whole damn Rxn. It's just water and its easily easy to overcome if it becomes a roadblock in ones reaction/reduction.
 #11 
Old 2003-12-12, 00:00
RNX57 RNX57 is offline
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Default Re: please, help this sorry SWIM

jams got it, swims run 250degrees to disperce dh2o, and it is recoupable, add a bit of suse n io, tad rp if ya got it,,, and star heatin,,, if u was cookin say 6 hrs,,, might take 12 now with extra dh2o. depends on alot of things fur real... not to long in swims eyes though

and yes with condencer, ballon, open even for couple hrs, no harm will come of it, u should smell it becomeing a rxn more than just boiling dh2o at 250, just dont cook till dry, when it gets a little thick slow down temp a bit,, and swims cooked at 150 gaining to 290 then back down a bit,,, swim plays alot,,,, or useto anyway,,, things on hold round here!!!!

play with it, u will learn from it.

RNX57

[This message has been edited by RNX57 (edited 12-12-2003).]
 #12 
Old 2003-12-12, 00:03
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

Jam, my hero, so at what point should SWIM attach the condenser? there is about 250ml of H2o now. SWIM knows about salvaging RP but is happy to hear he can save the whole RXN, thanx Jam.

oh yeah, SWIM has to wait 'till tue. to start boiling it, can it b stored in flask w/ cond. attached at room temp. untill then?
 #13 
Old 2003-12-12, 00:05
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Default Re: please, help this sorry SWIM

Absolutely.
 #14 
Old 2003-12-12, 00:06
RNX57 RNX57 is offline
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Default Re: please, help this sorry SWIM

id cap it off and store in fridge if poss, if not find a cool place in darkness with a ballon on top,,,,, it will hold till them.
 #15 
Old 2003-12-12, 00:13
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

how much of SWIM's pseudo freebase does anyone think was eaten up by the RP fire SWIM had in the flask?
 #16 
Old 2003-12-12, 00:28
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

main things SWIM has learned from his mishap:

1. add dH2O ice and water bfore the last ing. (I2)

2. have a bowl of ice dH2O for flask cooling

3. cool flask in freezer before mixing last ing. (I2)

4. no fucking marbles or aluminum

5. condenser on immediately

6. constant swirling/shaking at the begining

if anyone could tell SWIM the observational cues of the initial reaction and how to respond to them it would b very helpful.
 #17 
Old 2003-12-12, 01:50
kman kman is offline
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Default Re: please, help this sorry SWIM

Amine, there's some nice pictures in the multimedia part of the chem section of the rhodium.ws site.
 #18 
Old 2003-12-13, 04:57
RNX57 RNX57 is offline
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Default Re: please, help this sorry SWIM

add dH2O ice and water bfore the last ing. (I2) ,,, yep swim dreams 70 cent dh2o from any store..rp/suse/dh2o/io, in order.

have a bowl of ice dH2O for flask cooling ,,,yep, keep it to cool rxn during cook time to kick it off more.

cool flask in freezer before mixing last ing. (I2) ,,, swim hasent had to do this one.

no fucking marbles or aluminum ,,, righto, lol.

condenser on immediately,,,,,, yep, could shoot out so its safer with quick condencer applied.

constant swirling/shaking at the begining,,, yep sounds good, swim mixes rp/suse/dh2o, mixes that, then adds io to mix. easyer mixin that way swim believes.

RNX57
 #19 
Old 2003-12-13, 07:51
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California
Default Re: please, help this sorry SWIM

Keep your head on straight, save it til Tues. and then get back whatever you can. Switrd had an experience recently with a cracked flask, also had to flood it. Hey, here's the thread's name...-->

I had no choice but to FLOOD it....now what??

Type my name in the space where it says user...in the search engine, search in labtips, and you'll see it.

[This message has been edited by LwaysTired (edited 12-13-2003).]
 #20 
Old 2003-12-13, 16:13
amine_assimilator amine_assimilator is offline
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Default Re: please, help this sorry SWIM

more things learned from mishap:

7. respect that pseudo freebase is more reactive than Hcl

8. respect the upper limits for flask size (SWIM was at the top, never again)

9. b careful of excessive amounts of I2 (SWIM used a bit too much)

now that SWIM sees the errors of his ways, next time is almost sure to b a triumph, can't wait! thanx to all for the help.
 
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