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mackolol
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Quote: Originally posted by Sulaiman  | Apply vacuum first then heat,
if you heat first, when you apply vacuum there is a good chance of violent boiling. |
But is there any other disadvantage beside too violent boiling? (maybe glassware damage)
Ah, right
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Sulaiman
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Has anyone checked the 'accuracy' of cheap Chinese pH papers ?
CAUTION : Hobby Chemist, not Professional or even Amateur
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mackolol
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I'm using ones and they work quite well for my purposes, but the scale isn't very precise..
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karlos³
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The chemoluminescence reaction with NaBH4 and KMnO4 is known I would guess?
I would like to try it soon, but the reaction also calls for sodium hexametaphosphate which I don't have.
But why is that stuff involved?
I don't understand it, because actually, it is not really involved:
NaBH4 + Mn(III, IV or VIII)/H+→ products + Mn(II)*→ Mn(II) + light (~690nm)
What does this salt do in there? Is it needed?
Can it be replaced, if so, what can I use as replacement?
I read up on that, and besides it seems that it can be substituted with sodium orthophosphate, and that it is only in there because it affects the
wavelength.
What would be a good replacement? I have no phosphorus acid, neither its salts.
chemplayer uses phosphoric acid, instead of the sulfuric, is it just for acidification used, or does it affect the wavelenght as well?
Only P-containing substance I can offer would be some sodium hypophosphite.
Can someone help? I would really love to try it, but I'm just not sure if it is even worthwhile under these circumstances.
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wg48temp9
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| Quote: Originally posted by karlos³ | The chemoluminescence reaction with NaBH4 and KMnO4 is known I would guess?
I would like to try it soon, but the reaction also calls for sodium hexametaphosphate which I don't have.
But why is that stuff involved?
I don't understand it, because actually, it is not really involved:
NaBH4 + Mn(III, IV or VIII)/H+→ products + Mn(II)*→ Mn(II) + light (~690nm)
What does this salt do in there? Is it needed?
Can it be replaced, if so, what can I use as replacement?
I read up on that, and besides it seems that it can be substituted with sodium orthophosphate, and that it is only in there because it affects the
wavelength.
What would be a good replacement? I have no phosphorus acid, neither its salts.
chemplayer uses phosphoric acid, instead of the sulfuric, is it just for acidification used, or does it affect the wavelenght as well?
Only P-containing substance I can offer would be some sodium hypophosphite.
Can someone help? I would really love to try it, but I'm just not sure if it is even worthwhile under these circumstances. |
You should read the following paper:
Attachment: Mechanism-Permanganate-Chemiluminescence-hindson2010.pdf (436kB)
This file has been downloaded 471 times
Apparently polyphosphate ions complex Mn3+ which increases the chemoluminescence 50 fold. The correct ph is also required.
Interestingly phenols and ascorbic acid can be used in place of the NaBH4.
I am wg48 but not on my usual pc hence the temp handle.
Thank goodness for Fleming and the fungi.
Old codger' lives matters, wear a mask and help save them.
Be aware of demagoguery, keep your frontal lobes fully engaged.
I don't know who invented mRNA vaccines but they should get a fancy medal and I hope they made a shed load of money from it.
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mayko
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You might be interested in this too (same first author)
Hindson, C. M., Smith, Z. M., Barnett, N. W., Hanson, G. R., Lim, K. F., & Francis, P. S. (2013). Autocatalytic Chemiluminescence Sheds New Light
on the Classic Permanganate–Oxalate Reaction. The Journal of Physical Chemistry A, 117(19), 3918–3924. https://doi.org/10.1021/jp312603m
Attachment: Hindson et al. - 2013 - Autocatalytic chemiluminescence sheds new light on the classic permanganate-oxalate reaction.pdf (1.6MB)
This file has been downloaded 486 times
al-khemie is not a terrorist organization
"Chemicals, chemicals... I need chemicals!" - George Hayduke
"Wubbalubba dub-dub!" - Rick Sanchez
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karlos³
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Thank you both very much! 
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karlos³
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I need some dimethylamine freebase, and I have DMF, can I hydrolyse it with base simply at RT?0
That would be very practical for me, giving me a solution I can use directly as it is for the reductive amination I intend to use it for.
If not, I guess I have to go via the HCl hydrolysis instead.
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stoichiometric_steve
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| Quote: Originally posted by karlos³ | I need some dimethylamine freebase, and I have DMF, can I hydrolyse it with base simply at RT?0
That would be very practical for me, giving me a solution I can use directly as it is for the reductive amination I intend to use it for.
If not, I guess I have to go via the HCl hydrolysis instead. |
Why not hydrolyze with NaOH with heating, driving off the Dimethylamine through a drying column and collecting it in chilled MeOH until saturated?
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karlos³
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Because the smell lingers 
Well guess I rather go via the HCl hydrolysis.
Its better and easier stored this way.
My ketone is a hydroxyketone as you well know, and so it will form an imine very readily and a stable one even.
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stoichiometric_steve
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| Quote: Originally posted by karlos³ | Because the smell lingers
Well guess I rather go via the HCl hydrolysis.
Its better and easier stored this way.
My ketone is a hydroxyketone as you well know, and so it will form an imine very readily and a stable one even. |
You have a point there, but i think a solution in MeOH would be way more versatile, and if set up correctly, you won't even have to deal with any
fumes whatsoever.
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Belowzero
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After the whole corona thing dies down I expect the market to be flooded by used cheap plexiglass , perhaps even free.
While looking for fumehood designs I stumbled across designs that are made entirely out of plexiglass , although not the most important feat. it looks
really slick.
Relatively easy material to work with and not too heavy.
Now I wonder if this material is resistant enough to withstand at least a few years of abuse?
I could coat the parts exposed to the highest airflow volume with say epoxy/paint to make it more resilliant.
[Edited on 3-7-2020 by Belowzero]
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Σldritch
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How much space do i need for GAMESS, macmolplt and avogadro? I want to look at orbitals of up to maybe 30 atom clusters and only have 30Gb. Do i even
have enough space for all the programs?
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karlos³
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How reliable is this patent regarding the reductive amination of napthylglyoxyl hydrate?
Can aldehyde hydrates be reductively aminated like this? Never saw another example of it so far.
The patent is United States Patent Office 3,463,808, like look at example 13.
Or, United States Patent Office 3,312,733, example 9.
What do you guys think? I'm trying to run a reductive amination of 2-naphthylglyoxyl hydrate right now, but I am not so confident it will work.
Still in the process of aldimine formation.
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karlos³
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Sadly, it didn't seem to work so far.
I still have to work it up properly, but after an acidic quench way too much oil fell out, indicating my substrate hasn't reacted to an amine as
intended.
Can someone shoot an opinion about these doubtful patents please?
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LuckyWinner
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i dried my calcium chloride dehydrate inside an old iron pan with some minor rust on the stove.
my CaCl appears dry but it now has a slight reddish , (iron oxide?) tint.
will this cause any trouble when drying diethyl ether for example or other solvents?
how can I clean my CaCl from the rust contamination?
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Sulaiman
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I want to make chloroform via the haloform reaction but I am presently unable to cool the bleach so
can I add acetone to RT bleach a little at a time over an extended period?
E. G. 5L 6% sodium hypochlorite plus acetone in 10ml portions over several hours to allow cooling.
and
acetone bp=56C, how high can I allow the temperature of the mixture to get without significant losses?
CAUTION : Hobby Chemist, not Professional or even Amateur
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j_sum1
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| Quote: Originally posted by Sulaiman | I want to make chloroform via the haloform reaction but I am presently unable to cool the bleach so
can I add acetone to RT bleach a little at a time over an extended period?
E. G. 5L 6% sodium hypochlorite plus acetone in 10ml portions over several hours to allow cooling.
and
acetone bp=56C, how high can I allow the temperature of the mixture to get without significant losses? |
No expert. I have only done it a few times.
I have always heard that you need to keep temp brlow 20C during the reaction and that NaOH byproduct causes chloroform to decompose. Both of these
would suggest problems with what you propose.
Can't you buy a bag of ice?
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S.C. Wack
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The only time anyone does it (edit: should do it) cold is when they are trying to do it without glassware.
[Edited on 21-8-2020 by S.C. Wack]
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Sulaiman
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I tried 5L of 5.5% NaOCl with 200ml acetone at RT (c30oC)
here is a view of the crude product :
A yield of 3.7% 
____________________________________________________
I am fairly confident that the bulk of the remaining available chloroform (estimate >60ml) is dissolved in the 5L of water.
I may try distilling the 5L solution sometime later to see what I can recover.
_____________________________________________________
Judging by smell (which is not quantitive) there was significant evaporation of chloroform during the experiment.
... 200ml of chloroform lost to the 5L solution and the environment
______________________________________________________
Do not waste effort trying this at home
===============================================
next: playing with tcca per this thread and links http://www.sciencemadness.org/talk/viewthread.php?tid=5686
CAUTION : Hobby Chemist, not Professional or even Amateur
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Jimmymajesty
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Is there an easy way to convert N'N'diethyl hydroxylamine back to hydroxylamine? Thanks for your help!
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solo
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What is this piece used for....some type of trap .?......solo
It's better to die on your feet, than live on your knees....Emiliano Zapata.
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RogueRose
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| Quote: Originally posted by Sulaiman | I tried 5L of 5.5% NaOCl with 200ml acetone at RT (c30oC)
here is a view of the crude product :
A yield of 3.7%
____________________________________________________
I am fairly confident that the bulk of the remaining available chloroform (estimate >60ml) is dissolved in the 5L of water.
I may try distilling the 5L solution sometime later to see what I can recover.
_____________________________________________________
Judging by smell (which is not quantitive) there was significant evaporation of chloroform during the experiment.
... 200ml of chloroform lost to the 5L solution and the environment
______________________________________________________
Do not waste effort trying this at home
===============================================
next: playing with tcca per this thread and links http://www.sciencemadness.org/talk/viewthread.php?tid=5686 |
Was your bleach new? I've heard of low yields from using old NaOCl. Did you chill the bleach and the acetone before mixing the two?
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RogueRose
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Well you kind of cut off the bottom of the picture, is it just sealed glass at the bottom? Also, does the tube from the top & middle section seal
to the bottom tube, or is it open at the bottom?
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solo
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sealed at the bottom with a small hole on the upper side...and open on top ....solo
[Edited on 9-9-2020 by solo]
[Edited on 9-9-2020 by solo]
     
It's better to die on your feet, than live on your knees....Emiliano Zapata.
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