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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
 2003-11-14, 08:25
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I had no choice but to FLOOD it....now what??
Switrd had purchased a flask at a garage sale here a while back. I t looked as though it was going to be a good one. WRONG!! 2 or 3 minutes into the beginning of his rxn, he heard that awfull spine chilling sound....cccrraaAAKKK!! So, he immediately flooded the rxn with dh2o and salvaged most of the ingredients into another flask. Now he used quite a bit of dh2o as the rxn was quite livid. Now should he continue by boiling away most of the excess dh2o and then attempt to kick start it back up? Or would he be better off saving the reactants, then adding them to a future rxn? Any help would be appreciated. Thanks.
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#2
 2003-11-14, 10:20
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kirby 
Regular
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Re: I had no choice but to FLOOD it....now what??
to boil off the water isnt a good plan..
light heat
say 45c
and when the water content gets right..
rekick the reduction off
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#3
 2003-11-14, 11:01
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Re: I had no choice but to FLOOD it....now what??
Ok then. Thanks for you input kirby.
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#4
 2003-11-14, 12:03
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Str8_Shooter! 
Regular
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Re: I had no choice but to FLOOD it....now what??
I don't know if this is "the right thing to do"- but I would (with condenser/p/p/balloon etc.) in place, do what you would do under normal circumstances, but much longer, until the tell-tale signs of completion are there. And after sometime, if I didn't like the way it was progressing, I would increase the heat- gradually- and if progress continued to be unsatisfactory- I'd push the threshhold of what you consider too hot. I really don't know though, that's just what I would do in that situation.
(I wouldn't have added any water though...I would have transferred the flask to a bowl or pot or something, and only being a couple of minutes into the rxn, I probably would have tried to funnel it into the "substitute vessel"...I don't know if that'd be "the right thing" to do, or if I could pull it off...taping serran wrap over the top of the bowl it was transferred to (because it probably isn't heat proof) and letting it "cold react" for about 3 days would probably be the safest and best thing to do- espeacially if it was "gettin' with it" like you said...some people swear by doing it that way...I'd rather risk fucking the whole thing up and do it my way though!
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#5
 2003-11-14, 12:41
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kirby 
Regular
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Re: I had no choice but to FLOOD it....now what??
you make me smile tex
im sure he really wants to know you wouldnt do what he did
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#6
 2003-11-14, 12:48
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Str8_Shooter! 
Regular
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Re: I had no choice but to FLOOD it....now what??
...Future reference...another possible scenario to consider or not have to consider 'cause you already did. Well roundedness ok with you?....OK, you're right!LOL
[This message has been edited by Str8_Shooter! (edited 11-14-2003).]
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#7
 2003-11-14, 12:51
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stillbill 
Regular
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Re: I had no choice but to FLOOD it....now what??
Tired, you know better than to buy plain glass at a garage sale! Whoopeee, Tired got a deal! Let's play "The Price is Right" or
"Let's Make a Deal". Way to much time cleanin
precursors to risk such a catastrophe. Bill thought he saw Tired hangin around a dumpster
gettin ready to dive....just kiddin dude!
Wish I could help, but your situation is a tough call. Shooter sounds reasonable to salvage the goods. Good Luck! BTW, this Sat.,
my neighbor's havin a garage sale, wanna go?
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#8
 2003-11-14, 15:03
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Str8_Shooter! 
Regular
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Re: I had no choice but to FLOOD it....now what??
Bill, you are familiar with the fine sport of dumpster diving too I see. I hear that it can be quite lucrative, for those elite few that posess the coveted knowledge: Where...When...
But its not all fortune and glamor, of course. Just the other day, there was a tragic, 3-way territorial dispute for the bitterly sought-after U-Stor-It dumpster and its inherent riches...Its such a shame that 2 people had to die over a box of "kitchen stuff", a bag full of assorted women's shoes and a laptop from 1985.
[This message has been edited by Str8_Shooter! (edited 11-14-2003).]
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#9
 2003-11-14, 15:38
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Str8_Shooter! 
Regular
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Re: I had no choice but to FLOOD it....now what??
I must risk being- how do you ammedicans say "flamed" by my more catch-phrase enlightened and acronym-slang empowered peers...But, what does BTW stand for? I'm sure when you tell me I'll be like -"duh"-
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#10
 2003-11-14, 16:58
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stillbill 
Regular
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Re: I had no choice but to FLOOD it....now what??
Damn right, Shooter! Bill has a route of dumpsters he checks regular and riches abound
from these metal-clad behemoths.  The other
day, bill found a Hammond organ and a violin
BTW stands for "by the way". Hey Shooter, since I've noticed you back on again, have you checked out WR's hcl generator for gassin your goods? Using a gator-ade bottle and damp-rid, muriatic acid, aquarium tubing
and pump. Excellent info! Later on
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#11
 2003-11-14, 17:32
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Re: I had no choice but to FLOOD it....now what??
*quietly jumps back out of the dumpster*
Ahem.......oh yeah...the uhh rxn. hahaaahaaha
Ok well Switrd hasn't done anything to it yet. It's sitting in a flask with about 14oz of dh2o, and a blob sitting at the bottom. (blob = reactants) Switrd's telling me to see if I can find some more info before taking any "all or nothing" type of risks. Thank you for your insight.
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#12
 2003-11-14, 20:01
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madchemist 
Regular
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Re: I had no choice but to FLOOD it....now what??
Go ahead and basify the rxn contents. If you can steam distill thats even better. Extract all your goods like you would at the end of the rxn (normal workup). The final product will of course be pseudo/iodoephed, but you can just scrape it up and start a new rxn using it as the precursor. Thats you best bet, cuase now concentrations of HI and so forth are all out of whack. So it's best to extract half converted and unconverted product, and start all over.
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#13
 2003-11-14, 20:56
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Re: I had no choice but to FLOOD it....now what??
amalgum...thank you

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#14
 2003-11-14, 21:52
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stillbill 
Regular
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Re: I had no choice but to FLOOD it....now what??
The Madscientist is sharp, huh Tired. Glad
he was surfin around Totse today. Let this be a lesson to you, Tired. No more garage sales! Dumpster divin rules!  ahahahah
Later on
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#15
 2003-11-14, 23:01
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buckrogers 
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Re: I had no choice but to FLOOD it....now what??
Swim was telling me a similar story, but the flood was an accident, he said it kicked off and then all of a sudden he heard this god awful deafening sound, he said for those who have heard it will never forget it  , water sucked in from the muffler jar, he said he was fucking pissed. He was telling me what he did was boil off most of the water, (and we're talking a quart, took 5+ hours), after it returned to about where he started he said he added a little more R&I, then he added about 50-60 ml of dh2o hooked it all to a ballon and let it "simmer" for like 6 more hours. He said he thought with the long cook to remove the water, additional ingrediants and a slow cook after this would still yield something, SWIM said it sure as hell did and he also said you can bet your ass or arse he will never use that damn muffler thingy again.
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#16
 2003-11-15, 01:50
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Re: I had no choice but to FLOOD it....now what??
No more freakin garage sales for Switrd! Phew. After some searching through some old archives, Switrd came across a remedy kind of like what buck was talking about. Switrd did a modified version of that. He has a dish sitting in front of him with what looks to be like a 35% return. That's an optimistic guess. And he will weigh it when it completely dries. He is greatful for even having a return, considering the circumstances.
Thanks again to all who helped and those who just threw in their two cents. The humor was much relief at a tense moment. Hey, if you are just now reading this thread...please go ahead and post your ideas anyway. I'd like some more input if possible.
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#17
 2003-11-16, 04:06
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the meth god 
Regular
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Re: I had no choice but to FLOOD it....now what??
quote:Originally posted by LwaysTired:
Switrd had purchased a flask at a garage sale here a while back. I t looked as though it was going to be a good one. WRONG!! 2 or 3 minutes into the beginning of his rxn, he heard that awfull spine chilling sound....cccrraaAAKKK!! So, he immediately flooded the rxn with dh2o and salvaged most of the ingredients into another flask. Now he used quite a bit of dh2o as the rxn was quite livid. Now should he continue by boiling away most of the excess dh2o and then attempt to kick start it back up? Or would he be better off saving the reactants, then adding them to a future rxn? Any help would be appreciated. Thanks.
Swims flask fell off the hot plate and broke he flooded his chili in order to get it off the broken glass a slow 24 hour light boil worked great(went back to normal temp after that).if one had enuff feed and red and i2 too add this should work ok too also and then resume normal cooking temp.
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#18
 2003-11-16, 15:06
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amine_assimilator 
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Re: I had no choice but to FLOOD it....now what??
a simple aluminum foil mantle/crucible can help when the glassware shatters by catching everything. good, cheap insureance. speaking of aluminum, swim has heard, that if added to the mix (beer can pull tabs), that it can help "even out" a reaction. anyone try this? what's the mechanism behind it?
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#19
 2003-11-17, 10:24
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Str8_Shooter! 
Regular
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Re: I had no choice but to FLOOD it....now what??
Bill, (If you happen to catch this)
I don't pay much attention to threads etc. related to gassing...I've always went with titration. Therefore,(stupid human instincts) I feel like there's 2 camps: Us, and them, and naturally (with no basis on fact or experience) I think my way's better and the other way sucks.
Actually I'm not sure of the pros and cons of each, except bits and pieces, I'd like for someone to lay them out for me, or maybe even give me an argument on why gassing is better.
Bill...Those self storage Ironclads are the lick! When people fail to make that payment...
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#20
 2003-11-17, 11:45
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kirby 
Regular
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Re: I had no choice but to FLOOD it....now what??
hi str8
BTW means,,,,,, by the way
i think
and gassing is better cause i say it is
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#21
 2003-11-18, 07:41
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Re: I had no choice but to FLOOD it....now what??
One other thing. The day Switrd gassed his nano...(as a test) He got some return, not near what was expected. Then he took that same np and proceeded to add dh2o and drops of acid, then evap....and got what he thought he had been missing.(or close to it) Is that uncommon? Or perhaps he gave up on it too soon? And why does gassing not work well with smaller batches?
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#22
 2003-11-18, 08:04
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Wicked_Rain 
Regular
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Re: I had no choice but to FLOOD it....now what??
gassing works fine for SWIM on smaller batchs. once you perfect the art tired you will see, dont give up. when you didnt get the return you were seeking after you gassed your NP you titerated and got the difference back correct? well SWIM woulda simply gassed the NP again and the same result would have been achieved. see what i mean? SWIM always gasses lightly so as not to overgas. you can gas, filter, gas again filter, gas untill you get all the goods out. when the goods are all out the gassing will simply produce no results and your NP will remain clear with no coudy/snow activity.
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#23
 2003-11-18, 09:29
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Re: I had no choice but to FLOOD it....now what??
Ok....I'll tell 'em not to give up. I can probably think of a thing or two that may be causing his less than satisfactory results. Thank you rainman
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#24
 2003-11-19, 07:42
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the meth god 
Regular
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Re: I had no choice but to FLOOD it....now what??
quote:Originally posted by Wicked_Rain:
gassing works fine for SWIM on smaller batchs. once you perfect the art tired you will see, dont give up. when you didnt get the return you were seeking after you gassed your NP you titerated and got the difference back correct? well SWIM woulda simply gassed the NP again and the same result would have been achieved. see what i mean? SWIM always gasses lightly so as not to overgas. you can gas, filter, gas again filter, gas untill you get all the goods out. when the goods are all out the gassing will simply produce no results and your NP will remain clear with no coudy/snow activity.
There is a fine line when gassing nanos swim has overgassed them plenty of times.the problem with the gas and filter and gas and filter is whenever you dont get it all gassed out is you still have meth oil (oh my precious meth oil)in your np.So when your filtering your salt your gogo has oil still on it plus your filter is traping some oil in it also.So lets say your using colemans as your np after filtering your salt pour some fresh colemans over to wash any left over oil back into your np.That way we dont loose any of our precious oil.Then put your filter over a seperate container and give your normal tone rinse or mek(i prefer mek but to each his own or whats available in your neck of the hoods).Peace out
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#25
 2003-11-19, 09:40
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Wicked_Rain 
Regular
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Re: I had no choice but to FLOOD it....now what??
exactly- SWIM has it down to where there is never nothing left in NP on the 3rd gassing.excellent advice tho for the new gasser to think on.SWIM also had the advantage of being shown 1st hand. SWIM shudders when he thinks how it must be to learn gassing from reading text. SWIM is sure the only thing he would get gassed is himself if he had to learn this way lol.
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#26
 2003-11-19, 12:10
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Re: I had no choice but to FLOOD it....now what??
"to learn gassing from reading text. SWIM is sure the only thing he would get gassed is himself if he had to learn this way lol."
Switrd says "been there, done that" hahahaha
Excellent information guys....this is a copy 'n paste moment.
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