InLikeFlynn

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On a small enough scale would a magnetic stirrer suffice?
 

UWe9o12jkied91d

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InLikeFlynn

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What would happen if one used sodium cyanoborohydride in place of sodium borobydride?
 

mithyl2

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what type of adapter should be used for the stir rod of the overhead stirrer? you need there to be a tight seal to make sure no hydrogen gas escapes, but because of the h2 gas evolving you shouldn't have something that will cause friction or any static discharge, so what would be the best solution for this?
 

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what type of adapter should be used for the stir rod of the overhead stirrer? you need there to be a tight seal to make sure no hydrogen gas escapes, but because of the h2 gas evolving you shouldn't have something that will cause friction or any static discharge, so what would be the best solution for this?
mithyl2You can use a stirrer bearing if you can ensure that your stirrer rod can be lead into the joint straight.
As propper stirrer bearings for larger RBFs can be quite cost you can also use a piece of rubber or something flexible that will prevent the stirrer rod from bumping against the joint
 
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You can use a stirrer bearing if you can ensure that your stirrer rod can be lead into the joint straight.
As propper stirrer bearings for larger RBFs can be quite cost you can also use a piece of rubber or something flexible that will prevent the stirrer rod from bumping against the joint
Gordon Ramsayi have a thermometer joint that the rod can fit through, but am not sure what to use to make it a sealed fit. i was thinking a piece of tape in the top of the thermometer joint with a small hole that makes a snug fit for the stir rod.
 

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i have a thermometer joint that the rod can fit through, but am not sure what to use to make it a sealed fit. i was thinking a piece of tape in the top of the thermometer joint with a small hole that makes a snug fit for the stir rod.
mithyl2Maybe a piece of kitchen foil might help when it's not winding up in the rod.
Otherwise using a silicone adapter could work too if the joint size fits

TnCibf5gG3
 

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Maybe a piece of kitchen foil might help when it's not winding up in the rod.
Otherwise using a silicone adapter could work too if the joint size fits

View attachment 16483
Gordon Ramsaytried that but the friction even after a couple of minutes is too much :(

i also tried putting over some clingfilm with a hole in it, but that didn't work because the hole would tear and get bigger with the stirring.

none of my thermometer probe joints will work either because the rubber ring is much to tight for the stir rod to fit through.

and i don't have an extraction fan or a fume hood to direct the fumes out of like in the video.

are there any suggestions on what i can do? what have other people done to get a seal for the stir rod that doesn't cause friction or break?
 

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tried that but the friction even after a couple of minutes is too much :(

i also tried putting over some clingfilm with a hole in it, but that didn't work because the hole would tear and get bigger with the stirring.

none of my thermometer probe joints will work either because the rubber ring is much to tight for the stir rod to fit through.

and i don't have an extraction fan or a fume hood to direct the fumes out of like in the video.

are there any suggestions on what i can do? what have other people done to get a seal for the stir rod that doesn't cause friction or break?
mithyl2Are you using a propper mask?
Please do not execute reactions without propper ventilation or the possibility to extract fumes directly from the source.
If you do, please at least use a propper mask lile the Drager X-Plore 4.500. 250$ for a mask can seem like a lot but it is less than the cost of your life

Maybe ask one of the experts to help you with your other issues.
 

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Are you using a propper mask?
Please do not execute reactions without propper ventilation or the possibility to extract fumes directly from the source.
If you do, please at least use a propper mask lile the Drager X-Plore 4.500. 250$ for a mask can seem like a lot but it is less than the cost of your life

Maybe ask one of the experts to help you with your other issues.
Gordon Ramsayyes, i have a good mask. i was going to lead the h2 through a hose out of a large window and for extra measure have a fan blowing behind it.

i'm only doing up to 10g synths for now, so the amount of h2 shouldn't be too much, but my setup still isn't perfect.

do you have an inline filter you recommend as part of an extraction setup for fumes?
 

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yes, i have a good mask. i was going to lead the h2 through a hose out of a large window and for extra measure have a fan blowing behind it.

i'm only doing up to 10g synths for now, so the amount of h2 shouldn't be too much, but my setup still isn't perfect.

do you have an inline filter you recommend as part of an extraction setup for fumes?
mithyl2Good :)

I do have an inline coarse filter for solid components, my activated carbon filter is not an inline due to environmental reasons. If that wouldn't be a factor I would always prefer an open tube at the end
 

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Good :)

I do have an inline coarse filter for solid components, my activated carbon filter is not an inline due to environmental reasons. If that wouldn't be a factor I would always prefer an open tube at the end
Gordon Ramsayi've looked around for them and they're so expensive. is there a cheaper alternative?
 

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what type of adapter should be used for the stir rod of the overhead stirrer? you need there to be a tight seal to make sure no hydrogen gas escapes, but because of the h2 gas evolving you shouldn't have something that will cause friction or any static discharge, so what would be the best solution for this?
mithyl2PTFE plug is like 20-30 E on aliexpress, made expressly for this purpouse, with o-ring and locking mechanism.PTFE paddle can also be had for cheap there.
As far as shaking and instability a somewhat flexible connection can be made with reinforced tubing from the hardware store, this connects your stirrer's drive rod to the paddle allowing for just enough flex to not shake everything to shit.Same effect can be replicated with 2 interlocking rings connecting the drive rod to the paddle.
 
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PTFE plug is like 20-30 E on aliexpress, made expressly for this purpouse, with o-ring and locking mechanism.PTFE paddle can also be had for cheap there.
As far as shaking and instability a somewhat flexible connection can be made with reinforced tubing from the hardware store, this connects your stirrer's drive rod to the paddle allowing for just enough flex to not shake everything to shit.Same effect can be replicated with 2 interlocking rings connecting the drive rod to the paddle.
UWe9o12jkied91di actually have some of those but refrained from using them because they can expand and get stuck in and even break the glass of the rbf. (happened to me once).

but it seems i'll have to use it. the temps being used for the synth aren't very high though, so with any luck there shouldn't be much risk in it getting stuck.

i'm going to put some cling film around it before putting it into the flask neck in the hope that it will help with easing it out.

i should also say i'm going to try the synth that i posted about several months ago that i got from dread which is almost the same as the one this thread is about.

my main concern was the build-up of h2
 

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i actually have some of those but refrained from using them because they can expand and get stuck in and even break the glass of the rbf. (happened to me once).

but it seems i'll have to use it. the temps being used for the synth aren't very high though, so with any luck there shouldn't be much risk in it getting stuck.

i'm going to put some cling film around it before putting it into the flask neck in the hope that it will help with easing it out.

i should also say i'm going to try the synth that i posted about several months ago that i got from dread which is almost the same as the one this thread is about.

my main concern was the build-up of h2
mithyl2There is models with sort of rings like the ones on condenser in/out, these are prone to what u are describing.One of them broke like 5 6000ml sulphonation flasks before it was switched with one that works like a normal stopper.
Naturally one should let the entire thing cool down to RT before even attempting to remove it.And watch for overtightening, its a real killer.
Why not use vacuum grease and a kek clamp while you are at it?
 

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There is models with sort of rings like the ones on condenser in/out, these are prone to what u are describing.One of them broke like 5 6000ml sulphonation flasks before it was switched with one that works like a normal stopper.
Naturally one should let the entire thing cool down to RT before even attempting to remove it.And watch for overtightening, its a real killer.
Why not use vacuum grease and a kek clamp while you are at it?
UWe9o12jkied91di'll need to get some grease. i've been using vaseline if i need any joint lube which is probably a no-no. or i don't use any at all to avoid contamination of whatever synth i'm doing altogether.

can you elaborate on the models with rings that you referred to in your first sentence?
 

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i'll need to get some grease. i've been using vaseline if i need any joint lube which is probably a no-no. or i don't use any at all to avoid contamination of whatever synth i'm doing altogether.

can you elaborate on the models with rings that you referred to in your first sentence?
mithyl2it's a yes-yes, as long as you apply reasonable amounts contamination should be minimal.A little goes a long way, but probably not a bad idea to get some Corning's, it will last almost forever and it's top class, well worth the price.
I was talking about these knurlings, it looks like the below picture but reverse and obviously made for that purpose, I can't find for the life of me the kind we had.
9KoLlEhd25
 

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Do you need to add acetone to salt it at the end? Is it not possible to salt it right from the IPA?
 
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