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guy
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Copper(II) Sulfate
*NOTICE*
I know this is a very cheap and non-interesting compound that many take for granted but I remember when I couldn't get this and I was pretty happy
when I figured out how to make it. So maybe this could be useful to someone, or not. Also I posted this before, but I just wanted to "officially"
put it here.
-------------------------------------------------------------------------
<b>Copper(II) Sulfate</b>
CuSO4*5H2O
<b>Materials:</b>
Copper metal
Ammonia
Ammonium sulfate
Ethanol
Air bubbler/Aquatic pump
Bucket w/ cap
Filter paper
Heat source
<b>2Cu + O2 + 2NH3 + (NH4)2SO4 ----> [Cu(NH3)4]SO4 + 2H2O
[Cu(NH3)4]SO4 ----heat----> CuSO4 + 4NH3
CuSO4 + 5H2O -----> CuSO4*5H2O</b>
This method uses very cheap and common materials so it is good for larger scale productions.
Set up the bucket with air stones at the bottom and connect it to an air pump. Pour 187 g of 10% NH3 solution into the bucket. Add 73g of (NH4)2SO4
to water to make a saturated solution, and pour that into the bucket also. Place 70g of Cu on top of the air stones. Turn on the pump. Cover the
bucket to lessen ammonia evaporating. After about 24 hours, most of the Cu should have dissolved leaving a dark blue solution.
After...
Add denatured alcohol to the solution until all the [Cu(NH3)4]SO4 precipitates. Filter the precipitate and add a little more alcohol to make it as
free of water as possible. Water will cause the formation of copper(II) oxide when this is heated.
Heat the precipitate until all ammonia has evaporated, leaving the white, anhydrous copper sulfate.
To make the hydrate, add water and recrystallize.
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Darkblade48
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Just wanted to add that an alternative method to make copper sulfate is to make the hydroxide (electrolysis of copper metal in an MgSO4 bath) followed
by addition of sulfuric acid.
Same end result, different starting reagents 
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guy
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Yeah, but that would be the easy way! Haha, really, when I wanted to make this, I had no access to any of those reagents. So this is like a poorman's
version.
And Ive done the electrolysis method before with poor results. So I seeked a better way of doing this.
[Edited on 11/23/2006 by guy]
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chromium
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Good prep!
I have heard of people saying that this section should be only for trully advanced works. In my opinion this is not the case. Any finished and
tested designs or synths ( no matter simple or complex ) that could be usefull for others should be placed here as otherwise these might well remain
unnoticed in other forums that contain mostly discussions, ideas, propositions, references to scientific works most of which can probably never be
used in home, etc.
Edited to make my thoughts intelligible.
[Edited on 23-11-2006 by chromium]
When all think alike, then no one is thinking. - Walter Lippmann
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woelen
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| Quote: | Originally posted by chromium
In my opinion this is not too easy for Prepublications. |
Isn't this tested? Guy provides a mechanism and provides pictures of the result. I think most people can reproduce this and the required chems and
equipment are easy to obtain in almost every part of the world. Whether this is the most efficient, easy or optimal method is another discussion, but
I think it does work and can be interesting.
Thanks for sharing this guy!
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Baphomet
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Nice one guy. I like your use of an (aquarium?) air pump which is something I too like to use for that little extra entropy.
Any technique that can help the amateur chemist acquire the raw materials for practise of their art is all good in my book.
By the way, some hardware shops sell CuSO4 as 'bluestone' for use as a fertilizer on citrus trees.
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chromium
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| Quote: | Originally posted by woelen
| Quote: | Originally posted by chromium
In my opinion this is not too easy for Prepublications. |
Isn't this tested? Guy provides a mechanism and provides pictures of the result. I think most people can reproduce this and the required chems and
equipment are easy to obtain in almost every part of the world. Whether this is the most efficient, easy or optimal method is another discussion, but
I think it does work and can be interesting.
Thanks for sharing this guy! |
Well, it seems that i did not express myself clearly. I think like you that this is good preparation and it's very well that guy put it up here.
I have always wonderd why so few members dare to write anything for prepublications while almost anyone of us has at least something to put up here.
My post was in fact about that matter.
When all think alike, then no one is thinking. - Walter Lippmann
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woelen
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Sorry chromium, now I read your sentence correctly . I first interpreted as if
you wanted to tell that this synthesis is not easy enough for prepublication and that still a lot of issues have to be addressed before it is easy
enough.
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Mr. Wizard
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| Quote: | Originally posted by Baphomet
Nice one guy....snip....
By the way, some hardware shops sell CuSO4 as 'bluestone' for use as a fertilizer on citrus trees. |
Most hardware store around here sell the CuSO4 'bluestone' KILL tree roots that invade sewer piping. Now I've learned it's also used to treat the
soil for trace mineral deficiencies and to prevent many fungal diseases both in plants and animals.
This has been a very good thread for me.
The procedure is actually a net generator of Ammonia too, so the step that liberates the Ammonia could be used to reclaim the initial Ammonia and
more.
I'm curious if it will work on US 5 cent coins "Nickels" which are 75% Cu and 25% Ni.
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guy
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Thanks everyone for your compliments!
| Quote: | Originally posted by Mr. Wizard
| Quote: | Originally posted by Baphomet
Nice one guy....snip....
By the way, some hardware shops sell CuSO4 as 'bluestone' for use as a fertilizer on citrus trees. |
Most hardware store around here sell the CuSO4 'bluestone' KILL tree roots that invade sewer piping. Now I've learned it's also used to treat the
soil for trace mineral deficiencies and to prevent many fungal diseases both in plants and animals.
This has been a very good thread for me.
The procedure is actually a net generator of Ammonia too, so the step that liberates the Ammonia could be used to reclaim the initial Ammonia and
more.
I'm curious if it will work on US 5 cent coins "Nickels" which are 75% Cu and 25% Ni. |
Yes it will work since I also have done it before to try and get nickel salts.
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12AX7
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Ammonium sulfate is even easier to get than ammonia (well, I'm not sure of anywhere that doesn't sell janitorial (10%) strength ammonia, but maybe in
terms of quantity or price or concentration it's true...*shrug*), you think it'd work that way too?
Let's see... 2(NH4)2SO4 + Cu + O = Cu(NH3)4(2+) + 2SO4(2-) + H2O... hmm needs excess base to proceed in that manner.
How about urea, another common source of nitrogen? (Heck, does urea complex with copper at any pH?) If nothing else, you can leave out a solution
and it'll get some nitrogen-hungry things in it that'll (at least partially) turn it into ammonium carbonate, which should serve just as well for the
above reaction.
Tim
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guy
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Yeah this uses a combination of ammonia and ammonium sulfate. The ammonia can be regenerated and reused so its a good deal.
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12AX7
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Durr, blind me 
How about urea?
Tim
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guy
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| Quote: | Originally posted by guy
*NOTICE*
I know this is a very cheap and non-interesting compound that many take for granted but I remember when I couldn't get this and I was pretty happy
when I figured out how to make it. So maybe this could be useful to someone, or not. Also I posted this before, but I just wanted to "officially"
put it here.
-------------------------------------------------------------------------
<b>Copper(II) Sulfate</b>
CuSO4*5H2O
<b>Materials:</b>
Copper metal
Ammonia
Ammonium sulfate
Ethanol
Air bubbler/Aquatic pump
Bucket w/ cap
Filter paper
Heat source
<b>2Cu + O2 + 4NH3 + 2(NH4)2SO4 ----> 2[Cu(NH3)4]SO4 + 2H2O
[Cu(NH3)4]SO4 ----heat----> CuSO4 + 4NH3
CuSO4 + 5H2O -----> CuSO4*5H2O</b>
This method uses very cheap and common materials so it is good for larger scale productions.
Set up the bucket with air stones at the bottom and connect it to an air pump. Pour 187 g of 10% NH3 solution into the bucket. Add 73g of (NH4)2SO4
to water to make a saturated solution, and pour that into the bucket also. Place 70g of Cu on top of the air stones. Turn on the pump. Cover the
bucket to lessen ammonia evaporating. After about 24 hours, most of the Cu should have dissolved leaving a dark blue solution.
After...
Add denatured alcohol to the solution until all the [Cu(NH3)4]SO4 precipitates. Filter the precipitate and add a little more alcohol to make it as
free of water as possible. Water will cause the formation of copper(II) oxide when this is heated.
Heat the precipitate until all ammonia has evaporated, leaving the white, anhydrous copper sulfate.
To make the hydrate, add water and recrystallize.
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12AX7
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| Quote: | Originally posted by guy
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Why did you quote yourself, plus the pictures, to add...nothing?
Tim
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guy
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oops! I meant to edit something! haha
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UnintentionalChaos
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Would an excess of ammonia have any negative affect on this reaction? I have some ammonia that was unlabeled as to it's concentration, but a quick
calculation of density (even including huge error assumptions for the fairly innacurate postal scale) leads me to believe that it is only 2.5%, maybe
as low as 2%  I'll re-mass the stuff, but the first check left me with a density of
988 kg/m^3, just 3kg/m^3 less than 2% solution and 5 kg/m^3 more than 3%) I'm just wondering if assuming 2% for safety and adding extra ammonia will
do anything to the final product. My gut instinct is that it will not, but I'd appreciate another opinion.
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guy
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No, an excess of ammonia would be even better.
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UnintentionalChaos
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Very confused...
I am getting some very weird results from this synth. I now have very well drained and washed tetraamminecopper sulfate (hopefully). When I heat it,
it definetly lets off ammonia, but does not become white, off white, or even light green. Instead, it turns a medium green. When I add this to water,
it turns blue, but refuses to dissolve to any visible concentration. I tried boiling it to make it dissolve and I get a color change to light "mint"
green. No black CuO is formed. Anyone have any ideas/tests I could do to see what's going on?
PS: When I boil the un-heated material in water, it definetly turns to CuO (as expected).
[Edited on 25-12-2006 by UnintentionalChaos]
[Edited on 26-12-2006 by UnintentionalChaos]
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guy
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You didnt heat it long enough the tetramminecopper sulfate.
It turns from blue --> green --> white.
Try heating it longer until it turns white.
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UnintentionalChaos
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Roughly what temperature should I be at? It's definetly temperature, not time that seems to be my problem. I don't have the luxury of a hotplate,
unfortunately. I've been using a homemade alcohol burner, which uses up my waste alcohol, since I'm still working on a still. It;s at least 420 C in
the open flame because i can melt zinc chips, no problem. With a setup made of old cans and flower pot pieces, I can simulate a ringstand (though one
is coming in the mail soon), but the temperature is probably significantly lower. That is enough to get it to green, but clearly not hot enough for
white. Clearly, I can't exceed 650 C....Hmm...I may have to put this one on hold until I get a hotplate because I don't have much temperature control
beyond hot and really hot...that is, the difference between alcohol stove and gas stove...and I've managed to burn copper sulfate in the gas stove all
the way to CuO.
Thanks for your help guy!
[Edited on 27-12-2006 by UnintentionalChaos]
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Aqua_Fortis_100%
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| Quote: | originally posted by UnintentionalChaos :
Would an excess of ammonia have any negative affect on this reaction? I have some ammonia that was unlabeled as to it's concentration, but a quick
calculation of density (even including huge error assumptions for the fairly innacurate postal scale) leads me to believe that it is only 2.5%, maybe
as low as 2% I'll re-mass the stuff, but the first check left me with a density of 988 kg/m^3, just 3kg/m^3 less than 2% solution and 5 kg/m^3 more
than 3%) I'm just wondering if assuming 2% for safety and adding extra ammonia will do anything to the final product. My gut instinct is that it will
not, but I'd appreciate another opinion. |
I also have the less concentrated amonia.. but i even not determine the conc since i haven't the right equipment for measure the density... and also
have only a homemade alcohol burner.. 
30 min ago , i tried to dissolve a small amount of my CuO(made last night! But as posted by other members can also be bought in some pottery and
ceramics stores and supplies) in NH4OH/(NH4)2SO4 solution for make tetraamminecopper sulfate, but after the colour of solution stays clear with black
suspension of unreacted CuO.. i still don't warm this.. maybe wait a little more can result in anything...
UnintentionalChaos,about the CuO , you give me a probably great idea!!!! THANKS!!THANKS!!!
Obviously the CuO is a basic substance.. if reacted with an acid gives a salt.. how about dilute H2SO4?!?
the method is easy and cheap... simple to you get your CuSO4 from you CuO: react it in dilute H2SO4...
my H2SO4 from old batteries is pratically *FREE*..simple go in any auto store and to order the (most) probably free and useless (for they)acid liquid
from used batteries... filter the liquid (containig PbSO4 and other nasty stuffs), and ready!
actually, my only source of H2SO4 is this..
i also tried:
measured 30ml of this filtrated acid battery solution and pour in a small cup.. add two pinches of CuO and wait..the CuO starts to give small
bubbles and then stired the solution ..after 1 or 2 minutes the clear solution becomes blue!!!!
just:
H2SO4 + CuO ---> CuSO4 + H2O (heat helps the speed of reaction...)
the advantages of this method,i think, are several:
*not required any other chemicals or equipments further the heat source, CuO(or other Cu II H2SO4 reactive compound) and the free dilute H2SO4...
*if CuO is used, not generates nasty fumes or vapour as the guy's method (NH3) or SO2 from standard method (conc H2SO4 and heat:
2H2SO4 + Cu ---> CuSO4 + 2H2O + SO2^
*cheap and easy!
the only problems, i think, maybe be:
*obtain a more impure CuSO4*5H2O (because of some of the lead salts which can stay in H2SO4 solution even after the filtration);
*the energy spent to evapore the water from solution;
*and the yield difficulty be 100% because is need a small excess of CuO to consume the H2SO4... and then filter this CuO..(however can be used in
other batches!)...
(and sorry since i still not evapore this solution, because my stove for experiments stay in yard and is a homemade wood-charcoal stove, and now it's
raining here.. )
the funny part of my experimet it's which the my CuO was made from proper CuSO4*5H2O!!! hahaha because have some kilos of this in my home which i
bought in a garden store as fertilizer.. cost about R$ 7,00 the Kg( ~ US$ 2,50)
i interested in synthesising my own and tried this.. but my original purpose with CuO was made thermite which worked almost perfectly (not all pile
consumed.. )
probably it's also a good method of home manufacture if one has some copper (II) salts or CuO ..
the Guy's method is also very interesting and has great merits because one don't need any copper salt, simple just the metallic Cu which is much more
easy to find..
Thanks Guy, and nice picks!
one question about your method: how much faster the copper react if cutting or even grinding (to make a coarse Cu powder) the Cu things ???
again thanks .. i need try this one day...
[sorry about my very poor english..]
[Editado em 27-12-2006 por Aqua_Fortis_100%]
"The secret of freedom lies in educating people, whereas the secret of tyranny is in keeping them ignorant."
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guy
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| Quote: | Originally posted by UnintentionalChaos
Roughly what temperature should I be at? It's definetly temperature, not time that seems to be my problem. I don't have the luxury of a hotplate,
unfortunately. I've been using a homemade alcohol burner, which uses up my waste alcohol, since I'm still working on a still. It;s at least 420 C in
the open flame because i can melt zinc chips, no problem. With a setup made of old cans and flower pot pieces, I can simulate a ringstand (though one
is coming in the mail soon), but the temperature is probably significantly lower. That is enough to get it to green, but clearly not hot enough for
white. Clearly, I can't exceed 650 C....Hmm...I may have to put this one on hold until I get a hotplate because I don't have much temperature control
beyond hot and really hot...that is, the difference between alcohol stove and gas stove...and I've managed to burn copper sulfate in the gas stove all
the way to CuO.
Thanks for your help guy!
[Edited on 27-12-2006 by UnintentionalChaos] |
It doesnt need to get that hot, its just a matter of time since you need to remove 4 NH3 groups. Try heating a small amount until it turns white.
Trust me it will!
| Quote: | Aqua_Fortis_100%
30 min ago , i tried to dissolve a small amount of my CuO(made last night! But as posted by other members can also be bought in some pottery and
ceramics stores and supplies) in NH4OH/(NH4)2SO4 solution for make tetraamminecopper sulfate, but after the colour of solution stays clear with black
suspension of unreacted CuO.. i still don't warm this.. maybe wait a little more can result in anything... |
CuO is very slow to react with ammonia or water. It has a more favorable structure where it is stabilized by the O2-. This is why CuO reacts very
slowly with water.
Here's how I tested my method before I made it a large scale.
I took Cu wire, sodium percarbonate (realeases O2 in water) and (NH4)2SO4 and NH3. Immediatly a dark blue solution is obtained.
| Quote: |
one question about your method: how much faster the copper react if cutting or even grinding (to make a coarse Cu powder) the Cu things ???
|
Im sure it would definetly.
As for the H2SO4 method...Im quite aware of it but H2SO4 is hard for me to get because of parents....and I would probably not use it for large scale
methods like this.
As you can see, my method is a "copycat" of the Gold leaching process with cyanide and its pretty efficent on large scale.
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Aqua_Fortis_100%
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| Quote: | originally posted by guy :
CuO is very slow to react with ammonia or water. It has a more favorable structure where it is stabilized by the O2-. This is why CuO reacts very
slowly with water.
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Oh! Right!!! you are 100% sure!
about the CuO reacting with ammonia/(NH4)2SO4 , i wait two hours and the solution becomes blue ,but separed by two layers: the layer on top has a
pale blue colour and most volume and the down thin layer has a dark blue colour... after some more hours it's totally dark blue... are there a
catalist for this reaction? heat isn't good, i think, because of generation of NH3 gas...
| Quote: | originally posted by guy :
Here's how I tested my method before I made it a large scale.
I took Cu wire, sodium percarbonate (realeases O2 in water) and (NH4)2SO4 and NH3. Immediatly a dark blue solution is obtained.
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Wow, another great idea! thanks! i really need try this...
how about using others compounds to provide O2 (like perborate, etc)???
[Editado em 28-12-2006 por Aqua_Fortis_100%]
"The secret of freedom lies in educating people, whereas the secret of tyranny is in keeping them ignorant."
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UnintentionalChaos
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"I also have the less concentrated amonia.. but i even not determine the conc since i haven't the right equipment for measure the density"
Are you sure you dont? I did the calculation using the given volume of a container, a couple of cut off soda bottles, and a low capacity postal scale.
Since I couldn't mass the whole gallon at once, i poured it off into the bottles on the scale and took down the individual weights. This site is
amazing for conversion help..it does everything (this is the link for volume but they have mass/weight, and just about anything else you could need.)
http://www.convert-me.com/en/convert/volume
After the conversions, it is a simple mass/volume. To minimize error (since the postal scale isnt too accurate) I massed the whole gallon, where a few
grams either way does nothing to the density calculation. Then just use google and search for density of ammonia solution or some similar wording and
something will turn up. Use that to calculate concentration from density.
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