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Author: Subject: Hg(CNO)2 synth question
quantumchromodynamics
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[*] posted on 16-12-2013 at 21:47
Hg(CNO)2 synth question


(reaction performed outside at 45 degrees F yesterday)

1st beaker is 5g Hg dripped into 40ml 70% HNO3
beautiful reaction, some NO2 gas evolution

i went running for an hour, upon return
rich dark blue green layer on bottom, clear layer on top

2nd beaker with 55ml CH3CH2OH was prepared
dripped first beaker into ethanol beaker with swirling

...nothing happened...

a few minutes of gentle heating and tiny bubbles started
this developed into a huge plume of white stinky vapor
this part frightened me
several hours later reaction was over
temperature down to about 35 degrees outside
poured contents onto wet filter paper
wash with water, then ethanol, then water again

drying filtrate over night yields slightly clumpy slightly off white material.
1) under magnifying glass I can see no distinct crystals.
2) under different lights I do see tiny glints of reflection.
3) the pics on powerlabs seem to show tiny crystals
4) the pics on image search seem to show tiny little crystals

about five sand size particles of this product detonates with hardly any provocation

please,

1) did the cold outside mess me up?
2) are there suppose to be visible crystals?
3) does the product seem correct?
4) have i synthesized some random nitrate slop?
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[*] posted on 17-12-2013 at 01:50


Sounds like a success to me.that white cloud with the smell similar to freshly cut apples is a good indication that things are going as they should be. The product i get is a beige colour crystalline substance. you should try looking at it under a microscope as this will reveal the crystalline features much more clearly.



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[*] posted on 17-12-2013 at 10:19


If you want large crystals- (And that might NOT be a good idea!)

Dissolve the fulminate in strong ammonia, filter the solution and while gently and continuously stirring, SLOWLY neutralize the ammonia with a drip of glacial acetic acid. You'll see crystals growing in the liquid as the ammonia is taken up by reacting with the acid. The slower the addition, the larger the crystals you'll get. When you've added nearly enough acid to neutralize all the ammonia, drop a ph cube or test paper into the beaker and slowly continue just until it indicates neutral. Filter the crystals out and wash with distilled water several times, then do a final wash with alcohol.

Store the crystals under water- NOT dry. And know that even wet fulminate can be detonated by dry fulminate.




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[*] posted on 17-12-2013 at 13:58


Umm if it detonate easily then it should be correct since mercury fulminate is famous for that, and as for neon pulse, smelling the detonation product, the smoke, to decide whether if it is mercury fulminate might not be a good idea.
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[*] posted on 18-12-2013 at 01:53


Quote: Originally posted by DubaiAmateurRocketry  
Umm if it detonate easily then it should be correct since mercury fulminate is famous for that, and as for neon pulse, smelling the detonation product, the smoke, to decide whether if it is mercury fulminate might not be a good idea.


Geez, give me some credit! i think i have been misunderstood there.i don't mean to directly sniff the fumes of the detonation- those fumes are pretty toxic. i meant the smell that lingers during the fuming off period of the synthesis, kind of smells like a fruity smell similar to cut apples. Also not a good idea to intentionally inhale but you certainly can smell it in the air.




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[*] posted on 18-12-2013 at 02:20


The fruitiness is acetaldehyde ─ oxidation of ethanol . . .



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quantumchromodynamics
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[*] posted on 18-12-2013 at 10:37
recrystallize!!


I should have thought of that.
Sam Barrows recrystallized too.

Yes, vary the crystal size... Interesting...

Is acetaldehyde the prominent white vapor that occurs during the second mix?

I am so slow with learning about compounds. It took me about two months to satisfy myself with copper sulfate. This compound is going have me experimenting for a very long time.
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[*] posted on 18-12-2013 at 10:54


Quote: Originally posted by quantumchromodynamics  
This compound is going have me experimenting for a very long time.
I sincerely doubt it.

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