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YT2095
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sad.gif posted on 27-1-2008 at 08:15
Embarrassing mistake


ok, I`v Goofed.

I`ve been growing a copper sulphate crystal(s) for nearly 6 months now in a Gas jar, now I have a perfectly round crystal in the bottom of it and I can`t get it out :(
it`s well and truly stuck in the bottom of the jar.

currently I have the jar inverted with a small 22W Halogen light over it about 10cms away, it`s been there for half an hour and it`s still not even starting to slide with gas pressure :(

anyone have any ideas How I can get this out?

I don`t want to re-dissolve it again and waste all those months.




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vulture
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[*] posted on 27-1-2008 at 08:24


Can you sacrifice the jar?



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YT2095
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[*] posted on 27-1-2008 at 08:25


I can, but I`d really rather not, I only have 2 of them.



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YT2095
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[*] posted on 27-1-2008 at 09:25


Forget it, it`s a moot point now :(

my last Brainfart of putting it in a pan of water and slowly heating it up, resulted in the breaking of the gas jar before the water even hit 50c :(


and then there was one... :(




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Ozone
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[*] posted on 27-1-2008 at 09:38


You got your crystal out before the vessel flooded, right?!:o

O3

[Edited on 27-1-2008 by Ozone]

Well, a moment of silence for your jar...

And hooray for your big-fat crystal!

pics?

[Edited on 28-1-2008 by Ozone]




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YT2095
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[*] posted on 28-1-2008 at 09:07


yes, it eventually came out perfectly, I gently knocked the glass away with small rock hammer, to leave my crystal, it`s sad to see that gas jar go however, it`s roughly the same age as me.



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[*] posted on 28-1-2008 at 16:06


Next time use a tiny glass bead suspended on a thread as a nucleous. But you said your crystal is "perfectly round?" I hope not! A geologist friend made a 90# CuSO4 crystal in her bathtub. She was frequently scraping dislocations off of it as it grew.



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YT2095
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[*] posted on 31-1-2008 at 08:02


here`s the "Strange" round crystal(s):



and from the side:



I think NOW I know why all the large crystals grown in the lab at high school when I was a kid were all done in 2l ice cream tubs!
much easier to get out.

although beyond the breakage of my gas jar, I`m not unhappy with the result, it`s now Much more pure copper sulphate than the 1250g tub of the Technical grade that I bought, with all it`s strange impurities and such.

[Edited on 31-1-2008 by YT2095]




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[*] posted on 31-1-2008 at 08:32


Quote:
Originally posted by YT2095
...

although beyond the breakage of my gas jar, I`m not unhappy with the result, it`s now Much more pure copper sulphate than the 1250g tub of the Technical grade that I bought, with all it`s strange impurities and such.


This is only true if the impurities are not other 2+ D-block metals or similar, FeSO4 forms solid solutions with CuSO4 for example.

A common way of eliminating iron and manganese was to and nitric acid or a bit of sulfuric acid and H2O2 to the sulfate solution, bring the solution to near boiling, then add enough Cu(OH)2 or "copper carbonate" to swing the pH slightly alkaline. This resulted in the precipitation of Fe(III) and manganese hydrated oxides onto the excess of the basic copper compound. After stirring for awhile the solution is allowed to stand and then filtered off from the precipitate.
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[*] posted on 31-1-2008 at 09:21


absolutely, and that`s more or less exactly what I did (I used the Sulphuric acid route rather than the nitric in case of group 2 contamination).
there was even little black bits in it like Rocks or something!

but I reckon I`v taken it from the 99.5% purity to something Much higher now, and for that I`m pleased, my Daughter certainly likes looking at it :D




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[*] posted on 31-1-2008 at 19:54


That is a very beautiful crystal, it would appear as if all your hard work has paid off. Would you mind sharing the procedure and ratios you used? I tried the H2SO4/CuO route and just got hot black sludge could you please give a detailed description of your process and steps taken, if its not too much to ask that is.



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[*] posted on 31-1-2008 at 20:00


Have a look here for a lot more info
https://sciencemadness.org/talk/viewthread.php?tid=5529&...




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[*] posted on 1-2-2008 at 01:32


you`ll find that H2SO4 and CuO won`t readily form CuSO4 unless you heat it for a while and stir well.
if it`s cold it will take ages to do anything remotely noticable.

as for My particular crystal it really pretty straight forward, as I started with 99.5% copper sulphate in the first place, it really was just a matter of filtering initially.

then I used a little excess sulphuric and H2O2, then after heating I neutralised it with copper carbonate and stir well.
then it`s filtered again and poured into a gas jar (I don`t advise doing that now), a layer of vaseline is spread around the rim (it prevents crystal creep) cover with cheese cloth and leave it alone and undisturbed in the corner of a room for about 6 months.

when the liquid level is about to drop below the crystal then a good stir is needed (there will be light blue carbonate bits in it) and the quickly pour that liquid off to leave your crystal.

If you`re luckier than myself you`ll be able to get your crystal out, then give a Very quick rinse in ice water and leave it to dry on a sheet of glass.

there are other ways to do it also, some better than mine, I would seriously consider using a large plastic container to grow them in, Ice cream tub or a large margarine tub or the likes...

there`s quite a few crystal growing tutorials all over the net as well, Google images will help.




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[*] posted on 1-2-2008 at 13:00


Wll I just gave it another go and it worked marvelously, I added 50ml conc. sulfuric acid to 50ml of water and got it hot almost boiling. Then I added small portions of CuO until most of the bubbling stoped. Then I filtered it, within 10 min it was crystalizing, within 12 hours there were large bright blue crystals at the botttom but now I have fell victim to the same problem as you, the crystals are firmly stuck to the bottom of my beaker. What should I do? The crystals aren't my focus i just want some copper sulphate pentahydrate without buying so I can make some copper benzoate. How can I get all the crystals out of solution and out of my beaker without breaking my beaker?



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[*] posted on 1-2-2008 at 13:33


Just jab at them with a wooden rod (large skewer, less likely to break the beaker) or stainless/copper rod The crystals are rather brittle and you should be able to break them up rather easily.



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[*] posted on 2-2-2008 at 01:11


Quote:
Originally posted by crazyboy
The crystals aren't my focus i just want some copper sulphate pentahydrate without buying so I can make some copper benzoate. How can I get all the crystals out of solution and out of my beaker without breaking my beaker?


in that case it`s easy, redissolve them again in plain water, you`re going to Have to do that at some point Anyway to make your copper benzoate ;)




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[*] posted on 3-2-2008 at 09:30


Thanks a lot I have my crystals but I believe they are slightly acidic from the sulfuric acid will this affect my copper benzoate? if so how can I fix this I don't want to use sodium bicarbonate because the sodium will contaminate the blue color.


Here are my crystals they are drying right now


[Edited on 3-2-2008 by crazyboy]




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[*] posted on 3-2-2008 at 09:56


I would a portion of them dissolved and then add a K2CO3 soln to them making copper carbonate (easily filtered out and dried), then re add that to the rest of your copper sulphate in soln.

don`t worry, you don`t lose ANY copper sulphate doing this, only the acid ;)

then follow your copper benzoate procedure from there, I gather you`re using Ammonium or Potassium benzoate to react it with yes?




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