Author Topic: Old HgCl2?  (Read 1842 times)

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dave1234

  • Guest
Old HgCl2?
« on: September 11, 2004, 09:39:00 AM »
Swim has just discovered his HgCl2 is 14 years old and now stopped reacting.  Swim uses it as catalyst in MM amalgamation.  The HgCl2 has … evidently it’s now past its expiry date.  Swim thought that the Mercury would still be fine. So a good option would be to extract the mercury back out of the HgCl2 and proceed in converting it back to new HgCl2..is this practical?   

Swim last night attempted to make HgCl2 from a small amount of mercury out of a couple of thermometers… it hasn’t been tested yet, but it’s looking good.

Swim would still like to use the mercury out of the old HgCl2, What would be the best way of extracting the mercury back out of the HgCl2?
Cheers

Nicodem

  • Guest
Swim would still like to use the mercury out...
« Reply #1 on: September 11, 2004, 10:11:00 AM »
Swim would still like to use the mercury out of the old HgCl2, What would be the best way of extracting the mercury back out of the HgCl2?

What do you mean by "extracting the mercury"? If there is no change in color of your HgCl2 than it is just fine. 14 years is nothing to it if it was well stoppered to prevent sublimation.


stratosphere

  • Guest
i assume you have a aqueous solution of HgCl2?
« Reply #2 on: September 11, 2004, 04:26:00 PM »
i assume you have a aqueous solution of HgCl2?
while i have no idea why it isn't reacting , if you want to recover your mercury the 2 ways i can think of are to precipitate it as a sulfide by adding Na2S for instance, HgS is very insoluable.
the other way to recover the mercury would be as a metal by reducing it, for instance Hg(+2)+ 2Fe(+2)--> Hg + 2Fe(+3)

dave1234

  • Guest
there is no change in color.
« Reply #3 on: September 13, 2004, 06:41:00 AM »
There is no change in color. The HgCl2 is a fine white powder and kept in the original glass bottle with parafilm wrapped around it. It now doesn't seem to (but did once upon a time) react with the foil and methanol.
Should I just make new HgCl2 and throw the old away?
Thanks

abolt

  • Guest
i assume you have a aqueous solution of HgCl2?
« Reply #4 on: September 13, 2004, 09:22:00 AM »
  i assume you have a aqueous solution of HgCl2?

AFAIK, It is impossible to have an "aqueous" solution of HgCl2, hence it's name "corrosive sublimate". It doesn't exist as a liquid.

There is no change in color. The HgCl2 is a fine white powder and kept in the original glass bottle with parafilm wrapped around it. It now doesn't seem to (but did once upon a time) react with the foil and methanol.

Then it is still HgCl2, the powder is not your problem. Add a small amount of water to your MeOH/Foil to assist in  your amalgumation. Storing your HgCl2 in a couple of air tight containers in a freezer(not the one with your food in it) is probably a good idea.


RogarThedodger

  • Guest
Abolt: i reaad you have done a 100g MDp2p- MM...
« Reply #5 on: September 14, 2004, 06:38:00 AM »
Abolt: I read you have done a 100g MDp2p- MM  Nitro, AlHg reduction in a 3lt RBF. 
Did you just proportionately scale up your reagents as according to MM method?
What sort of yields have you been receiving?
Does scaling up decrease you yield?
Do you think the swim could perform a 200g reduction in a 5lt RBF...and still achieve good yields? Sorry about all the quesstions. Thanks

Swim is planing to use .06mm thick Al.  If anyone else has past experience with scaling up this method it would be great to hear from you.
25g is just too much 'thorough' work for such a small outcome...
Thanks

abolt

  • Guest
Did you just proportionately scale up your...
« Reply #6 on: September 14, 2004, 07:43:00 AM »
Did you just proportionately scale up your reagents as according to MM method?

100 grams 0.3 mm Al flashing (1x1 cm pieces)
100 grams MeNO2
100 grams ketone
1500 + 100 mls MeOH
80 mls DH2O
200 - 300 mg HgCl2

What sort of yields have you been receiving?

75% plus molar yield ketone to hydrochloride salt.(90% plus w/w)

Does scaling up decrease you yield?

Not when it is done properly.

Do you think the swim could perform a 200g reduction in a 5lt RBF...and still achieve good yields?

Yes, although, if you are a newbee, I would strongly advise you to start a lot smaller.

A write up on this technique is coming soon.


stratosphere

  • Guest
AFAIK, It is impossible to have an ...
« Reply #7 on: September 14, 2004, 08:40:00 AM »
AFAIK, It is impossible to have an "aqueous" solution of HgCl2, hence it's name "corrosive sublimate". It doesn't exist as a liquid.

HgCl2 is in fact water soluable, so it is possible to have  an aqueous solution of it.
that is indeed how swim stores HgCl2 he has made.
notice i said aqueous HgCl2, not liquid HgCl2.

i would also agree that the problem more likely lies with your amalgamation procedure then with your HgCl2.

abolt

  • Guest
HgCl2 is in fact water soluable, so it is...
« Reply #8 on: September 14, 2004, 09:51:00 AM »
HgCl2 is in fact water soluable, so it is possible to have  an aqueous solution of it.

Yes stratosphere, "solution" is probably poor terminology.
 
What I meant to say was that HgCl2 does not have a liquid phase.


RogarThedodger

  • Guest
Abolt: thanks. What type of stirring do you...
« Reply #9 on: September 16, 2004, 08:54:00 AM »
Abolt: thanks.
What type of stirring do you use? i.e 3" egg shaped stir bar.  Also do you prepare the flushing in any way...i.e NaOH to remove any silicon or other elements? Swim uses .06 Al thick pie tins,  all the Al seems to break down during the reaction.
Swim thinks he should bite the bullet and spend the time in making an overhead stirrer...
Cheers again

abolt

  • Guest
What type of stirring do you use?
« Reply #10 on: September 16, 2004, 08:38:00 PM »
What type of stirring do you use?

Only overhead stirring will work.

Also do you prepare the flushing in any way...i.e NaOH to remove any silicon or other elements?

No, use regular hardware store flashing.

Swim uses .06 Al thick pie tins,  all the Al seems to break down during the reaction.

Use thicker Al when doing larger reactions. Hardware store flashing is 0.3 or 300 microns thick.

Swim thinks he should bite the bullet and spend the time in making an overhead stirrer...

Absolutely. Do it.