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Soap

Joined: 26 Mar 2005
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Mon Apr 25, 2005 5:53 am
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Swim currently only has 2g of elemental mercury. it is possible for him to get more but he is hoping that he dosnt have to. will he get satasfactory results if he puts the 2g in a 50ml flask and gasses it with chlorine? hes looked into making the iodine salts but he rather use the more common route.
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IndoleAmine
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Mon Apr 25, 2005 7:02 am
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I doubt this will work. Better dissolve in excess HNO3 65%, and evap acid+water under vacuum to make the nitrate.

Easy process, check Rhodium's...


i_a
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Soap

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Mon Apr 25, 2005 7:32 am
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any reasons why it wont work? something about mercury nitrate dosnt appeal to swim. swim doe not know if its because he would have to go look buy stump remover for some kno3 or if its because it proably isnt the best salt to be mixing with flamables. i did some very quick research and it appears to be a oxidzer. is this true? thanks again
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Spacemonkey

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Mon Apr 25, 2005 7:37 am
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It will work, but it'd be better if you had a bit more to work with. Make sure you're able to shake the flask while gassing.

There was a document discussing the synthesis of Mercurous Chloride and it's use over Mercuric Chloride in an al/hg amalgalm. I'm not sure where, Rhodiums probably.
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Spacemonkey

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Mon Apr 25, 2005 7:40 am
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Found this on the ol' Hard disk:


Mercurous Chloride (Hg2Cl2)

by AtomicDog

Mercurous Chloride is a simple mercury salt with the form of Hg2Cl2. The reaction described herin was thought to produce Mercuric Chloride (HgCl2) instead, which is used for making amalgams. But it turns out that Mercurous chloride does a perfectly fine job for amalgams and is thus a good substitute. Hg2Cl2 is insoluble in alcohol and only slightly soluble in water but it still manages to coat aluminum in a sol'n of either solvent. It is suggested that Hg2Cl2 amalgams be made in mildly acidic water (pH 5-6) because it is at least somewhat soluble in water and acidity increases that solubility. Apparently even plain Hg in acidic water can work but Atomic feels that this is very difficult to measure out plain mercury and thus get the same results. This reaction is super easy and takes only a few hours at most.

On the plus side, Mercurous Chloride isn't quite as dangerous as HgCl2. That insolubility makes it difficult for your body to absorb, the Merck even says that if ingested, a saline laxative should be administered to prevent mercury poisoning, try that with HgCl2! (joking, don't try that). Hg2Cl2 is a white, odorless, tasteless powder. Protect it from sunlight or it will slowly degrade into HgCl2 and Hg. Hg2Cl2 sublimes at 400-500C without melting. Please note that any solution of mercury should be considered EXTREMELY dangerous and poisonous and be handled using vynal gloves with extreme care.

We'll be making Hg2Cl2 today by passing chlorine gas over elemental mercury at room temperature and pressure. You'll need elemental mercury from an old thermometer or thermostat, and muriatic acid (31.5% HCl), and sodium hypochlorite sol'n (Clorox bleach). Atomic has found that a 2:1 ratio of bleach to acid is about right or you could use liquid chlorine (stronger stuff) from the same pool store you got the acid at go 1:1. Chlorine gas is a nasty green gas that will drive you out of the lab in very small amounts and is so corrosive that in time it will turn steel into dust. You don't want any leaks in your setup for gas to escape! 200ml of acid and 400ml of bleach will give you 15-20 min of gas and that should do it for you. In an ideal setup, your Sodium Hypochorite sol'n drips from an addition funnel into a flask filled with your acid and is stirring away. If you don't have mag stirring then you'll have to swirl the flask occasionally to get everything to react. A tube leads the gas to another where it bubbles through water to clean the gas and then another filled with CaCl2 to dry it, and then to another where the mercury waits. Atomics experience is that the water and drying aren't really necessary because not much else will react with the Hg and since Hg2Cl2 isn't really H2O soluble or nightmarishly dangerous that drying the gas is no big either. But be warned! The best way to go is clean and dry. If you use water to clean the gas be aware that for a few minutes it will absorb your gas until it becomes saturated and lets it pass through, be patient. When the green gas does hit the mercury you'll se it right away: Your fast moving, T2 looking blob will turn a dull dark gray instantly and slow down or freeze up entirely. This is a hard layer of Hg2Cl2 forming on the outside of your mercury, protecting it from the gas all around it. You have too pick up the flask and shake that baby to break out the Hg inside and spread it all around the flask so it can react, expect to be doing a lot of this.

And try to use only as much Hg as you think will coat your flask or you'll have a hard time getting it all to react. At this point Atomic should point out how nice it is to use surgical tubing for this reaction instead of regular chem tubing. Surgical tubing is very flexible and allows you to really pick-up and shake that flask without pulling your setup apart. Once you have that stuff spread all around it will probably be dark grey with white at any tips. If you can see that the flask is full of green chlorine gas then you can stop the gas for now and wait. You need to wait for the mercury to react, you'll be done when it's almost completely white and even looks reacted from underneath. You'll probably never get it 100% reacted unless you take the flask out of the setup (hold your breath!) and use a spatula to 'scratch' around in there and break-up any remaining clumps and unreacted patches. This is especially true if you use too much Hg for the size flask you're using. Once finished you can use that spatula to scrap out all you can and put it in a suitable container. Then pour some water in the flask and swirl that baby to lift the remaining Hg2Cl2 off the flask walls and quickly pour it into a Pyrex dish. When the water evaporates you can scoop the rest of your Hg2Cl2 into your container.

There you have it, the new and improved doc, now go forth and bee fruitful!
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IndoleAmine
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Mon Apr 25, 2005 7:41 am
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Mercury nitrate is fine for Al/Hg.
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Soap

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Mon Apr 25, 2005 8:04 am
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whats the worst that can happen? swim will have to go buy some more mercury, oh well.. hes going to go ahead and try to make the salt with what he has now. he thanks you all for your help
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ApprenticeCook
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Mon Apr 25, 2005 11:16 am
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well gassing with chlorine isnt my favorite thing to do anyway...
If you want mercuric chloride use method on rhodium, ((Hg + H2SO4) + carbonate) + HCl. Nice and easy, not to mention safer than gassing with chlorine gas...

-AC
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capricorn

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Mon Apr 25, 2005 5:14 pm
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(Hg)2+ can be reduced to (Hg2)2+ by addition of Hg(l). So Mercurous Chloride can easily be produced from Mercuric Chloride just by addition of Mercury metal. But that still involves working with Mercuric Chloride, but at least one dont have to use it in the reductive amination procedure.
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IndoleAmine
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Mon Apr 25, 2005 9:12 pm
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Quote:
Hg)2+ can be reduced to (Hg2)2+ by addition of Hg(l).
Question

Maybe you confused the names and meant:

mercurous (1) chloride = Hg2Cl2

mercuric (2) chloride = HgCl2

mercuric chloride HgCl2 + Hg = mercurous chloride Hg2Cl2


You can indeed make mercurous chloride from mercuric chloride and elemental Hg..

But through chlorination of elemental Hg, you are just left with Hg2Cl2 (mercurous chloride), no mercuric chloride - hence no possibility to "employ further Hg atoms" like you described....

the Hg(2) salts are more toxic, so you have to work with the more toxic variant HgCl2 and elemental Hg to make the less toxic variant Hg2Cl2 - so far you were right about toxicity.

But:
The more toxic HgCl2 is better for Al/Hg reductions due to better solubility, the less toxic Hg2Cl2 can be used too, although its waaay less soluble (hint: add some NaCl to enhance dissociation into Hg(2)Cl2 and Hg(0)!).

Arrow no possibility to make anything else but Hg2Cl2 from Hg and chlorine.


i_a


Last edited by IndoleAmine on Tue Apr 26, 2005 3:07 pm; edited 1 time in total
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capricorn

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Tue Apr 26, 2005 12:09 am
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No confusion here, I meant exactly what I said.
HgCl2 is reduced to Hg2Cl2 by addition of elemental Mercury
Hg2+ + Hg(l) ---> 2(Hg2)2+ lgK = 1,94
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capricorn

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Tue Apr 26, 2005 12:31 am
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Quote:

Arrow no possibility to make anything else but Hg2Cl2 from Hg and chlorine.
i_a


That is not correct. Since Chlorine gas can oxidize (Hg2)2+ to Hg2+, bubbling chlorine through a Hg2Cl2 solution at ~pH 1 will oxidize it to HgCl2.
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ApprenticeCook
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Tue Apr 26, 2005 6:15 am
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can you stop saying (Hg2)2+ its just confusing, its Hg+1 for mercurous and Hg+2 for mercuirc.

-AC
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capricorn

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Tue Apr 26, 2005 10:43 am
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That seems like an exellent idea. Didn't think of that. Sorry if I confused by writing (Hg2)2+ for Hg1+
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IndoleAmine
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Tue Apr 26, 2005 3:16 pm
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You also confused elemental Hg as being Hg(1) - in fact it is Hg(0).

Quote:
No confusion here, I meant exactly what I said.
HgCl2 is reduced to Hg2Cl2 by addition of elemental Mercury
Hg2+ + Hg(l) ---> 2(Hg2)2+ lgK = 1,94


Quote:
Since Chlorine gas can oxidize (Hg2)2+ to Hg2+, bubbling chlorine through a Hg2Cl2 solution at ~pH 1 will oxidize it to HgCl2.


Rolling Eyes Confused Laughing

And whats the purpose of celebrating such a mercury mess?? You can straight gass Hg(0) (=elemental mercury!) with chlorine under dry conditions to get Hg2Cl2 directly - especially since you need a chlorine generator for your proposal anyway...
https://www.synthetikal.com/synthforum//viewtopic.php?t=842&postdays=0&postorder=asc&start=0#

Maybe you were factually right with all of your posts so far, but the whole picture makes just no sense to me, sorry. Convert back and forth - to get same result with more work and dangers involved? No thanks, not for me..

The only useful point I can make out in your preceeding posts is making the more useable HgCl2 from equimolar Hg2Cl2 and Hg(0), or by aequ./acidic chlorination (?) - but then again you suggested reverting it again due to toxicity converns, wich is a contradiction in itself.. Question

i_a


Last edited by IndoleAmine on Tue Apr 26, 2005 3:26 pm; edited 2 times in total
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