Author Topic: Preparation of mercury salts from Hg metal  (Read 670 times)

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Re: Preparation of mercury salts from Hg metal
« Reply #20 on: April 15, 2009, 04:44:34 AM »
Has to be short wave. The electrons in mercurys shell absorb higher frequency UV. Thats one of the reasons that when its excited it will emit that wavelength also. To do this one should probably get a HP Hg quartz lamp and a floresent background.
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Vesp

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Re: Preparation of mercury salts from Hg metal
« Reply #21 on: April 15, 2009, 04:49:19 AM »
Oh I missed that part, well that is not really worth it at all.
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timecube

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Re: Preparation of mercury salts from Hg metal
« Reply #22 on: April 15, 2009, 05:06:39 AM »
This guy seems alright.  8)

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Re: Preparation of mercury salts from Hg metal
« Reply #23 on: April 15, 2009, 05:11:04 AM »
Sure it is,
You could probably get away with removal of the white coating on (flouresent lights with out breaking it). and letting the UV shine though that. I know I know how the fuck to do that without breaking it... I use electricity. HV supply.

I got a few tesla coils laying around that make sure work of it but if one terminal of a HV supply is hooked up to the end of the light and the other is waved over it the powder flys off and leaves you with a pale blue Highend UV source. Probably to much work for most but Im use to it and have all the shit I need to strip one down in about 5 minutes. Yeh so Im a fucking mad scientist whats it to ya ;D... of course I also built a TEA nitrogen laser so I got 337nm wavelengths bright as hell on command.

Shaking the shit out of one with a blown filamint to scratch the powder off may do the same thing but give you carpletunnel syndrom in the process. Imagine your stroking it for hours on end to kill the time while the powder slowly wares away :o
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Vesp

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Re: Preparation of mercury salts from Hg metal
« Reply #24 on: April 15, 2009, 05:16:19 AM »
Very interesting! I guess if you have all that go for it, but I was thinking since it didn't seem to have any practical use it just wasn't worth it.

Quote
of course I also built a TEA nitrogen laser so I got 337nm wavelengths bright as hell on command.

I almost built one of these! I have multiple transformers; flybacks and NST's. Does a TEA laser have any application when it comes to radical chlorination or similiar reactions? I've heard if you use a CO2 atmosphere it produces infrared light, so that might be of interest to you.

Timecube, I've been looking for that picture for a while! I think there is even a video of him, but I haven't been able to find that either. Thanks for the post :P
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Re: Preparation of mercury salts from Hg metal
« Reply #25 on: April 15, 2009, 05:38:03 AM »
Iv thought about the chlorination also But these fuckers are just a bitch to deal with, I was pumping mine with a 10kv 24ma OBIT and it ran like a CW laser and the pulse wasnt notices. Problem is local overheating and the dielectric blows out to fucking much thats why I dont mess with it much. A low pressure N2 laser would be way better IMO. I want a Cu vapor laser now. They make a CO2 look like a toy and they produce a green and yellow beam with no mirrors to adjust. Cut a hole thru a fucking brick man in no time.
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poisoninthestain

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Re: Preparation of mercury salts from Hg metal
« Reply #26 on: April 15, 2009, 04:28:39 PM »
Impressive observations, seeing the shadow to me makes a lot more sense then seeing mercury vapor fluoresce in a blacklight. If anyone tries this and has luck let us know.

Poison, any luck with getting to be able to try the CuSO4 reduction on some nitrostyrenes?

Probably next month. I'm crammed with work right now.

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Re: Preparation of mercury salts from Hg metal
« Reply #27 on: April 24, 2009, 12:38:16 AM »
Few Questions:
HgSO4 When dissolved in water preciptated nothing.
When NaOH was added yellow/orange precipitate appears and dissapears until reaching the point where it stayed. Question is the precipitate looked more along the lines of the pictures of yellow precipitate and not the Deep orange/red color that HgO appears most of the time.

Also the Yellow precipitate Was mixed with HCl and the solution took on a grey appearence with  a small amount gray precipitate. Is that normal because given HgCl2 solubility I dont think it should drop out the way it did.
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poisoninthestain

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Re: Preparation of mercury salts from Hg metal
« Reply #28 on: April 24, 2009, 06:53:27 AM »
Hmm, I'm wondering. Based on what you said I'd say you either had mercurous sulfate or mercuric sulfate which eventually led to an impure mercurous or mercuric chloride. The (I) and (II) forms both have to do with heating issues when forming the sulfate, that sorta thing.

The HgO has a variety of color forms based on the the size of the crystals, which if they are under a certain microgram size they will vary between yellow/orange/red. It all has to do with what alkali your basifying with. You used NaOH and got yellow. I used sodium carbonate and got orange. Both are chemically identical more or less with the exception at the rate they crystalize. I have a feeling you just basified too quickly or something along those lines and trapped some impurities in your HgCl2 which resulted in a grey color for the chloride in the end. Worst case scenario you formed the mercurous chloride instead of the mercuric.

My chloride was always white but then again I always used sodium carbonate instead of bicarbonate or NaOH.

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Re: Preparation of mercury salts from Hg metal
« Reply #29 on: April 24, 2009, 03:16:00 PM »
Its working or the amalgum so no matter. I did add a little to much HCl and thats comming thru with the crystals as a yellow collor so im going to recrystalize it but other then that its fine.
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Re: Preparation of mercury salts from Hg metal
« Reply #30 on: April 24, 2009, 05:20:50 PM »
OK,

I just found out something that I thought everyone should know because to me its kind of important. I evaportated the HgCl2 solution down very slowly on a hot water bath. As it evaporated I decided to see if any one the HgCl2 was subliming off by putting a clean piece of glass over it and letting the condensate dry. Well this morning it was dry and there was a small amount of fine white powder in its place. This is evidence that as you condense the solution to crystals there is some HgCl2 being carryed over either in the form of condensed steam or sublimination Im not certine yet but seeing as how it was a very low heat Im leaning to sublimination. Moral of the story is BE CAREFUL.

After giving it much thought I dont see the need to create HgCl2. Wouldnt it be more practical from a safty stand point to make the HgCl2 insitu from HCl and HgO. This would eliminate the need of handling the very toxic HgX compounds. Anythoughts on that?
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poisoninthestain

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Re: Preparation of mercury salts from Hg metal
« Reply #31 on: April 24, 2009, 06:32:05 PM »
Ha, I had the HgCl2/water solution boiling for a LONG time to drive the water off a few times and I lost A LOT of HgCl2 for those runs. I'm glad someone else confirmed this.

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Re: Preparation of mercury salts from Hg metal
« Reply #32 on: April 24, 2009, 06:44:59 PM »
I think this means that when evaporating the solution the vapors should be run into a NaOH wash bottle which im going to do next time and weight the resulting HgO to determine how much is comming out.
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Re: Preparation of mercury salts from Hg metal
« Reply #33 on: April 24, 2009, 10:34:07 PM »
If it is small HgCl2 particles being kicked up out of the solution from the bubbles, you could boil the solution in a RBF attached to a reflux condenser with out water running through it. This will help prevent the small particles from getting into the air.
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Re: Preparation of mercury salts from Hg metal
« Reply #34 on: April 24, 2009, 11:27:22 PM »
There where no bubbles just a real low heat was used. The evaporation dish was placed over a popperie burner filled with water.  There is the occasional mist that comes from it but no splattering from bubbles.
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Re: Preparation of mercury salts from Hg metal
« Reply #35 on: April 25, 2009, 07:48:53 PM »
Oh I see so it is most likely ALL sublimation. That really surprises me it sublimates enough to be detectable using that method. Are you sure the glass wasn't dirty to begin with? the water could have dissolved that gunk and only made it appear like it was the HgCl2.
I wonder what the distillates of a flask with water and mercury metal would be? it would make sense that maybe tiny droplets of Hg metal would form in the receiving flask.
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Re: Preparation of mercury salts from Hg metal
« Reply #36 on: May 28, 2009, 06:10:27 PM »
Ha, I had the HgCl2/water solution boiling for a LONG time to drive the water off a few times and I lost A LOT of HgCl2 for those runs. I'm glad someone else confirmed this.

swim had a dream where he evaporated the water on heat to yield the hgcl2 and it was taking forever to evap all the water so swim left and did something else, temp was probably around 80C.  when he came back it appeared as though all the water had evaporated and the hgcl2 in the middle was slightly molten and bubbling very slowly, needless to say he killed the heat immediately.  what he was left with were long shardy hgcl2 crystals around the sides and in the middle was hard, compacted, caked hgcl2 where it got too much heat.  he tested a little bit using this hgcl2 from the center where it was subliming and the al foil amalgamated but it wouldn't dissolve in water very well.  had to add alcohol to get it to dissolve then the amalgam took right off.
« Last Edit: May 28, 2009, 06:12:04 PM by time2poop »

Vesp

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Re: Preparation of mercury salts from Hg metal
« Reply #37 on: May 29, 2009, 04:48:26 AM »
Ha, I had the HgCl2/water solution boiling for a LONG time to drive the water off a few times and I lost A LOT of HgCl2 for those runs. I'm glad someone else confirmed this.

swim had a dream where he evaporated the water on heat to yield the hgcl2 and it was taking forever to evap all the water so swim left and did something else, temp was probably around 80C.  when he came back it appeared as though all the water had evaporated and the hgcl2 in the middle was slightly molten and bubbling very slowly, needless to say he killed the heat immediately.  what he was left with were long shardy hgcl2 crystals around the sides and in the middle was hard, compacted, caked hgcl2 where it got too much heat.  he tested a little bit using this hgcl2 from the center where it was subliming and the al foil amalgamated but it wouldn't dissolve in water very well.  had to add alcohol to get it to dissolve then the amalgam took right off.

Hopefully this was done outside, or somewhere besides where you live?
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time2poop

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Re: Preparation of mercury salts from Hg metal
« Reply #38 on: May 29, 2009, 12:57:52 PM »
Hopefully this was done outside, or somewhere besides where you live?

in the dream it was done outside, at what temp does hgcl2 decompose versus sublimation?
« Last Edit: May 29, 2009, 01:03:03 PM by time2poop »

Douchermann

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Re: Preparation of mercury salts from Hg metal
« Reply #39 on: May 29, 2009, 05:07:51 PM »
That's actually freakin scary.  If I had known it sublimates so easily, perhaps I would have evaporated it outside as opposed to in my garage (at leas the door was open).  Fortunately for me, I have about 5g, which is more than I'll ever need in my life time hahaha.