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Author: Subject: Copper(II) Sulfate
Aqua_Fortis_100%
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[*] posted on 27-12-2006 at 20:58


Thanks for all, UnintentionalChaos.. (great link.. NOW put in my favourites )..
i searched some stuffs for made my own scale as Brainfever's page describes... about the table of density of NH4OH i just appreciate it...
there are a lot of things i still need make .. chemicals, equipments, etc....
thanks again.. tomorrow i start the plan.. :cool:
thanks again..




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[*] posted on 27-12-2006 at 21:12


Anything that provides oxygen can oxidize the Cu, aqua_fortis_100%

As I read from another post, it seems you made CuO from Cu(OH)2? If so, just use Cu(OH)2 because that will work MUCH faster.




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[*] posted on 27-12-2006 at 22:19


Wow, it's true..thanks...

Actually ,as i says, my CuO don't was made with the original purpose for make CuSO<sub>4</sub> (rather, my CuO comes from proper CuSO<sub>4</sub>...).... i tried the procedure only for experiment the theory...
in fact, you are 100% sure because hydroxides usually reacts faster than oxide... but thinking on this, almost gives in same, because the Cu(OH)2 has a lot of water in it and also using a dilute H<sub>2</sub>SO<sub>4</sub> will make which you must evaporate TONS of water in it...and (for me) is more easy handle the powdered CuO than provide space for enormous volume of Cu(OH)<sub>2</sub>..
how i cann't see it's before?!?!
i tried NOW your idea:
just spill Cu(OH)<sub>2</sub> in half of cup volume,about 100ml.. then i added 45ml of acid battery solution.. after about 4 seconds the black solution in my hand turns INSTANTLY clear green colour and this INSTANTLY converts to clear blue colour... some black particles of Cu(OH)<sub>2</sub> settle on bottom of the cup, but after some seconds it's just dissolved..
Thanks guy! tomorrow i re-edit my earlier post about H<sub>2</sub>SO<sub>4</sub> method..

[sorry about my poor english...i try to improve]

[Editado em 28-12-2006 por Aqua_Fortis_100%]




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[*] posted on 28-12-2006 at 20:49


Quote:
I took Cu wire, sodium percarbonate (realeases O2 in water) and (NH4)2SO4 and NH3. Immediatly a dark blue solution is obtained.


today i just tried your method, but with a slight modification: i replace the sodium perborate by H<sub>2</sub>O<sub>2</sub> ...
put some thick wires and 1 cents coins (as described by other member) in a 500ml PET bottle, then put some ammonium sulfate in it (unfortunately this is the impure farm grade...but very cheap).. then added 50ml of household ammonia...nothing happened.. but when added 100ml of 3% H<sub>2</sub>O<sub>2</sub> , the solution after 2 or 3 seconds starts to bubble, and the bubbles staying located in copper things..some fast seconds after this becomes to clear to deep blue!!!unfortunately the Cu things not was all eat (actually, small amounts in surface of these which in fact be are eated by solution) and the H<sub>2</sub>O<sub>2</sub> was consumed quickly(probably releases O<sub>2</sub> too fast because of the copper ion which catalyses the decomposition). About this, can you help me about how i can improve the O<sub>2</sub> generation (or how i can let the H<sub>2</sub>O<sub>2</sub> releasing the O<sub>2</sub> for more, much more time) H<sub>2</sub>O<sub>2</sub> or other oxodizing substance???


one idea about this: if one gets many (old) very thin wires, cut all in small pieces with a pair of scissors and put in a blender with water and turn this on (almost as Al foil method), and turn on , and off , with care (wait some minutes after each time turned on, to not overheating the motor), to make many VERY small pieces and/or even maybe a coarser Cu powder, and make the tetraamminecopper sulfate route H<sub>2</sub>O<sub>2</sub>/(NH<sub>4</sub>;)<sub>2</sub>SO<sub>4</sub>/NH<sub>4</sub>OH or by ...(because , as you in an earlier post said,about the small pieces "eat the copper MUCH faster" )... and after make the CuSO<sub>4</sub>*5H<sub>2</sub>O ..
using H<sub>2</sub>O<sub>2</sub> as a O2 source, has a advantage which the H<sub>2</sub>O<sub>2</sub> finish to decompose in water which help to keep the final product more pure .. but the disadvantage is which decomposes too fast what do the solution need more O<sub>2</sub>...one care is to use LOW concentrations of hydrogen peroxide, because higher conc. gives TOO VIOLENTS reactions ( i tried put 5 - 10ml of 50% hydrogen peroxide, and the reaction was just violent,with jets and clouds of hot NH3 given off almost instantly the H<sub>2</sub>O<sub>2</sub> was added and the PET bottle also turned very hot in my hands in 2 seconds...fortunately i was used goggles and to be in outside)...

But if a air bubbler or aquatic pump is used (as in your original idea),will be faster because of greater superficial area of small Cu things.. and the yield will be much better without hydrogen peroxide addition...and without hazards of H<sub>2</sub>O<sub>2</sub> or another thing...
(i have just mentioned the H<sub>2</sub>O<sub>2</sub> because is quite cheap here.. a liter of hazardous 50% cost R$ 6,00 (about US$ 2,50 ) in some cleaning stores..so one can dilute this in a very weak H<sub>2</sub>O<sub>2</sub> solution)


[sorry by not finish the experiment because, also of my parents (my mom today, give me a great told off because i was made some experiments which accidently releases a strange tear odor when i washed in the paper filter , just when she go in my direction...), i cann't filter and boil the solution at the moment... :(
but tomorrow i try boil it ...if my mom to calm..]

[sorry about my poor english and any fool thought]

[Editado em 29-12-2006 por Aqua_Fortis_100%]




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[*] posted on 28-12-2006 at 21:32


Hmm..Ive never used perborate. Does it release O2 on contact with water?

Percarbonate (Na2CO3*H2O2) also sold as Oxiclean realeases huge amounts of O2 in water.

Anyways. that was just a confirmation test to see if the theory checks out.

ANd dont worry about your english its pretty good.




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[*] posted on 28-12-2006 at 22:24


Farm grade ammonium sulfate....you mean browish junk from (probably) iron impurities? I've unfortunately got the same stuff. If you have some time on your hands, its not too hard to clean up somewhat. Dissolve in water (it is extremely soluble), run through some kind of filter (I used cheap paper towels quadrupled over) a few times until the paper stops turning brownish-gray. The solution should be tan now (Probbaly started out quite brown). Microwave or boil off about half the liquid (assuming you started with a saturated solution) and filter it. These crystals are fairly clean (this was what I used for the synth). A quick wash with alcohol or acetone might get a bit more iron stained solution off ( I didn't bother). Halve it again and repeat the above process. The rest is quite contaminated. If you have blueberry bushes or conifers, I should think they would enjoy the last bit of it. (If you're working with a larger batch, obviously continue to boil off water until only a small amount remains) Alternately, you might be able to let it crystallize with evaporation, but I would think it's hygroscopic nature might interfere. On second thought, you could probably booze the stuff out by adding alcohol to a saturated solution until the salt precipitates out. I'll have to try this now...

PS: Alcohol works like a charm. You just have to wring out the ppt very well and almost all of the iron goes with it. The only thought I had, though, is that due to ammonium sulfate's immense solubility, youd lose a huge amount of salt and a whole lot of alcohol if you tried this with the whole batch. I'd just use this method for what I called unsalvageable up a bit. I had saved that stuff and just cleaned it using this method a minute ago.

[Edited on 12-29-06 by UnintentionalChaos]
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[*] posted on 28-12-2006 at 22:37


The ammonium sulfate I have (I assume it isn't an alum or anything) seems to be rather easy to crystallize. Every time I dissolve and evaporate it, I can't help but get chunky, white to transparent (not necessarily well-formed) crystals from it.

Seems to me the brown crud should settle out quite easily, after maybe a week tops. pH up or down might help if it's a soluble thing, and recrystallization once or twice should be sufficient for the stingiest use.

Tim




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[*] posted on 28-12-2006 at 22:45


Oh, sorry guy!!! i almost always make troubles with the words perBORATE and perCARBONATE :( at the start of post i wanted said which "i replace the sodium percarbonate by H2O2 " , but i wrotes "i replace the sodium perborate by H2O2 "..i'm ashamed...
----------
about the perborate, even if you used this instead of percarbonate probably the same effect was obtained..(like the percarbonate, the perborate in contact with water undergoes hydrolisis giving (in these case) borate and H<sub>2</sub>O<sub>2</sub> ),i heard which is also used like "oxiclean" or in other laundry bleaches, etc , but i never find this here in supermarket, only the percarbonate which is quite expensive.... my only worry about using this percompounds is if the impurities generated by sodium carbonate or borate ...what about? more details on your procedure using perborate? thanks .

tomorrow, i (try) to go on city center to buy some percarbonate (because there is much more cheap..) and try all about...
---
[thanks again for to think which my english is regular...if my nice english teacher to think it's , i will be happy! haha actually mine is a primitive type "from dictionary" because i dont know too right how use the "would", "does" and others verbs...]

[Editado em 30-12-2006 por Aqua_Fortis_100%]




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[*] posted on 28-12-2006 at 22:47


Of course, that's if you're quite patient or plan well in advance. :P
You can do the heating/alcohol to get a much improved, if not perfect product in under an hour and in the microwave. Definetly not wise for mass production though...electricity drain + ethanol waste = $ouchmywallet$
For use in this synth though, a crudely filtered product should be fine (to keep large particles out of the filters at the end), because part of the process (At least the original post) is to ppt with alcohol anyway and the impurities will just be left in solution. :D

"I assume it isn't an alum or anything"
So test it by heating. Ammonium Aluminum Sulfate or ammonium alum, the stuff I assume you're referring to, as well as potassium alum both melt at temperatures below the boiling point of water. Ammonium sulfate requires high temperatures to decompose into a lovely plume of ammonia, SOx, and/or NOx. I realize just how close I was to doing that when drying the salts in the oven :o

[Edited on 12-29-06 by UnintentionalChaos]
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[*] posted on 29-12-2006 at 19:36


Quote:
originally posted by UnintentionalChaos :
Farm grade ammonium sulfate....you mean browish junk from (probably) iron impurities? I've unfortunately got the same stuff. If you have some time on your hands, its not too hard to clean up somewhat. Dissolve in water (it is extremely soluble), run through some kind of filter (I used cheap paper towels quadrupled over) a few times until the paper stops turning brownish-gray. The solution should be tan now (Probbaly started out quite brown). Microwave or boil off about half the liquid (assuming you started with a saturated solution) and filter it. These crystals are fairly clean (this was what I used for the synth). A quick wash with alcohol or acetone might get a bit more iron stained solution off ( I didn't bother). Halve it again and repeat the above process. The rest is quite contaminated. If you have blueberry bushes or conifers, I should think they would enjoy the last bit of it. (If you're working with a larger batch, obviously continue to boil off water until only a small amount remains) Alternately, you might be able to let it crystallize with evaporation, but I would think it's hygroscopic nature might interfere. On second thought, you could probably booze the stuff out by adding alcohol to a saturated solution until the salt precipitates out. I'll have to try this now...

PS: Alcohol works like a charm. You just have to wring out the ppt very well and almost all of the iron goes with it. The only thought I had, though, is that due to ammonium sulfate's immense solubility, youd lose a huge amount of salt and a whole lot of alcohol if you tried this with the whole batch. I'd just use this method for what I called unsalvageable up a bit. I had saved that stuff and just cleaned it using this method a minute ago.

[Edited on 12-29-06 by UnintentionalChaos]

yes, mine ammonium sulfate is same thing you has...
about the purification of (NH<sub> 4</sub> )<sub> 2</sub> SO<sub> 4</sub> , my stupidity has no limite :
one year ago i would rather to feel lazy for do clean up this compound...this almost resulted in serious accident: i needed at occasion , some HMTD and no have ammonia (for hexamine), when i followed one "alternative" synth from KIBC book: ammonium sulfate, formaldehyde and 3% hydrogen peroxide.. like i never have success with too weak H<sub>2</sub>O<sub>2</sub>,then i tried dissolve some ml of 50% H<sub>2</sub>O<sub>2</sub> in water and added in fitered brownish solution (this shit brown impure (NH<sub> 4</sub> )<sub> 2</sub> SO<sub> 4</sub> and some CH<sub>2</sub>O .. about this, i remember what when added the CH<sub>2</sub>O to ammonium sulfate this generate some heat and in one point formed some "chunks" of a gelatinous substance (paraformaldehyde? think which probably formalin was polymerized to paraformaldehyde due presence of formed H<sub>2</sub>SO<sub>4</sub> from sulfate ))..anycase the temperature was the normal..(25°C -30°C) and when i added the hydrogen peroxide instantly the solution turned cloudy white and warms a little.. then i put the bottle with the mixture stand in my room for get more yield..but some time after..(2 or 3 hours),when i stays in kitchen, i feel a nasty smell from my room.. quickly i run and can seen which the bottle was hot, boiling and giving off formalin vapours .. the hot solution destroyed fast the small cristals of presumed HMTD as same facility as formed...then discarded immediately the solution in a manual sink there outside... this give me a basic and important lesson about which ALL chemicals are treacherous (some more than others..) if not treated with respective respect... today i'm less insane,but still ignorant...
Thanks for all, UnintentionalChaos and Tim, i have about 10 Kg of this (NH<sub> 4</sub> )<sub> 2</sub> SO<sub> 4</sub> and plan to purify it after new year's eve ...

[sorry about any grammar error and bad english]

[Editado em 30-12-2006 por Aqua_Fortis_100%]




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[*] posted on 31-3-2007 at 21:37


I'm trying this method right now and it's working wonderfully. Thanks! One thing I noticed however is that the equation given initially is balanced incorrectly. It should be

2 Cu + O2 + 4 NH3 + 2 (NH4)2SO4 --> 2 Cu(NH3)4SO4 + 2 H2O

which means that 35g of Cu is only needed in the given recipe.

[Edited on 31-3-2007 by Cesium Fluoride]
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