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Saerynide
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OMG, What the f--- Please I need help!!!
Ok, I know this really should go into the Electrochemistry section, but I really would like replys ASAP, so I thought I would get more attention if I
post it here. Real sorry guys.
Here's what happened:
I had my catholyte from my new attempt to make H2SO4 (i trashed the iron contaminated one). Anyways, I found pure graphite anodes this time, so my
anolyte stayed clear, but the catholyte had turned bright orange.... It didnt look like iron, cause iron is kind of rusty orange. This was BRIGHT
orange  It mustve been crap on the cathodes  So I filtered out all the orange precipitate (i still cant figure out what it is).
I continued to filter a few more times, but using 3 filters at a time. All the yucky crap was gone and i was left with a clear, light green solution
(like the color of Cl2)!! The first thing that hit me was... could this be nickel??!? This is where I desperately need help.
So I took the catholyte (which contained MgSO4 and the contaminant(s)) and electrolyzed it far away from the house, incase it was some nickel
compound. AFter I turned on the power, the reaction became very violent in a matter of seconds. Bubbles were spewing like mad from the electrodes
and the solution was so hot it hurt to touch the glass jar. The carbon electrodes began to disintegrate VERY rapidly into dust. So there I was
wondering if it could be iron (II) or nickel. Suddenly, it starts smelling like H2S. Thats when I was like OMFG!!! and I ran for my life. I turned
the thing off at the extension cord outlet at the house and waited for the H2S to disapate. I was quite terrified by then.
I went back to catch a glimpse at the contents of the jar, and there was a few drops of what looked like oil floating on top of the solution. Im not
sure if I was imagining it, but i caught a small whiff of soemthing that resembled Cl2, but more musty. If I could put a smell into a color, a dark
rusty brown would come to mind. Unfortunately, I cant tell what color the solution is anymore cause the carbon dust turned it dark green/black. It was
still transparent though.
The formation of H2S from SO4 2- and other ions doesnt sound logical/possible...
Please some one help me, Im dead terrified that it could be a nickel compound. Its still sitting out in my yard cause I dare not go near it. I need
to find a way to get rid of it soon as poss if it is nickel.
I sound like a total whimp now, dont I? 
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Tacho
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Sorry, but I don't get it.
What is so terrible about nickel compounds? Maybe you mean chromium?
Nickel compounds, as far as I know, are not particularly dangerous. There is nickel plated stuff everywhere! Even in your kitchen, in contact with
your drinking water.
Did I miss something about your reaction?
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Saerynide
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Nickel salts are carcinogenic. And I dont deal with carcinogenic stuff 
Well, I guess the possibility of it being a nickel salt solution isnt so bad, cause its out in my yard but, Im really puzzled about the H2S (or
whatever it was that really smelled like it), the oily floating liquid, and that other strange smell.
Edit: Are there orange and green chromium salts? I know chromium sulphate is green... but what would the bright orange precipitate be?
[Edited on 13-1-2004 by Saerynide]
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Tacho
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I'm on vacations and don't have any books here, but I really think nickel salts are not even as bad as copper salts. I'm pretty sure
none of them is carcinogenic enough to panic.
Chromium salts, on the other hand, can be mean. The orange salts, Cr(III), are not bad, but the green ones, Cr(VI), are very carcinogenic.
Could there be chromium in your reaction?
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Theoretic
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The oil on top...
Well, the only thing I can think of is chromyl chloride, the formula is CrO2Cl2, and it's a dark-red liquid. The problem is that it's dense,
is your solution concentrated? The fact that it looks like oil (i.e., light yellow or colourless)... That could be linseed oil if you used a carbon
cathode (linseed oil is sometimes used to counter erosion).
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I am a fish
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| Quote: | | Are there orange and green chromium salts? |
There are also other colours. For example sodium chromate is yellow and chrome alum [potassium chromium(III) sulphate dodecahydrate] is purple.
| Quote: | | The orange salts, Cr(III), are not bad, but the green ones, Cr(VI), are very carcinogenic. |
You have the colours the wrong way round. Chromium(III) salts are generally green, whilst chromium(VI) salts are generally orange.
1f `/0u (4|\\| |234d 7|-|15, `/0u |234||`/ |\\|33d 70 937 0u7 /\\/\\0|23.
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Saerynide
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Oh dear god....
And my solution was bright orange!! You should've seen how much orange precipitate was in there!! Crap... I now have a jar of super
carcinogenic shit out in my yard thats worse than nickel salts....
Thank god I didnt touch any of it, I hope
Should I just knock it over into the grass?? The lawn can get cancer for all I care
Since I used a knife, it probably had chromium plating on it. But it was the cathode, why would it oxidize to make chromium salts? That makes no sense.
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chemoleo
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Lol you are funny 
Could you answer a few questions pls.. so it is easier to understand whats going on!
What electrode material did you use, for both cathode and anode? Graphite only? Where did you get it from? Often such electrodes contain clay
materials, oils, and god knows what.
What did your solution contain? H2O (destilled or tap) with MgSO4? Where did you get the MgSO4 from? Fertilisers, or a pure product?
Was there any electrode separation, i.e. by a diaphragm or salt bridge?
What voltage/amperage did you use? As you describe spewing etc, it sounds to me you overdid it with the power imput. I hope it was DC current by the
way 
What was the electrolysis vessel made of? Plastic, glas, metal, ceramics?
Was it a closed container, or could gases vent off easily?
By the way, take it easy with your 'supercarcinogenic shit' lol. I bet it's just a solution of iron III sulphate or something. or even
iron hydroxide, which also forms a precipitate that is orange brownish. Even if it was nickel or chromium, it's not going to do ANYTHING to you
unless you evaporate the water and make sure you INGEST it. Else, just wear gloves and flush it down the toilet (they have ways of filtering out such
metals), and NOT onto the soil (ts ts ts, these Americans ) - as you may poison
drinking water and nearby streams, and kill all the fish in the lakes, plus fishermen who may eat the fish. 
Nickelsalts are more toxic than copper salts by the way.
Anyway, chill, what you are doing is harmless
[Edited on 13-1-2004 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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guaguanco
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| Quote: | Originally posted by Theoretic
The oil on top...
Well, the only thing I can think of is chromyl chloride, the formula is CrO2Cl2, and it's a dark-red liquid. The problem is that it's dense,
is your solution concentrated? The fact that it looks like oil (i.e., light yellow or colourless)... That could be linseed oil if you used a carbon
cathode (linseed oil is sometimes used to counter erosion). |
You did *not* produce chromyl chloride! Not in an aqueous solution.
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Saerynide
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You guys are having fun teasing me.. so cruel
I used graphite anode. I bundled a bunch of thick pencil leads together. I scraped them all clean of glue and junk with a knife before using em.
For the cathode, I used a stainless steel knife.
I used distilled water and MgSO4 7H2O from the drug store.
I used a paper towel strip to separate the 2 jars. This was for when I was still making H2SO4. I stuck both electrodes in to the catholyte jar cause
I was trying to plate out the metal contaminant.
I was running it on 5 volts at 14 amps, and yes, it was DC It came from a
computer power supply.
I used glass jars and no, I didnt cap them.. I think it wouldve made a nice pipe bomb if I did, considering how hot the solution was and how much gas
was being released 
I really dont think it's iron sulphate.. It doesnt look anything like it. I mean its BRIGHT orange
BTW, I still dont understand why so much H2S was given off. Is that even possible? Or is there another gas that resembles it's smell that
couldve been produced?
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guaguanco
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| Quote: | Originally posted by chemoleo
Lol you are funny
Could you answer a few questions pls.. so it is easier to understand whats going on!
[Edited on 13-1-2004 by chemoleo] |
Like he says. Settle down! Chemistry and panic do not mix!
You should try a test run, using your cathode and anode and nothing but distilled water. Observe what happens. Once you can run cleanly, producing
nothing but H2 and O2, then and only then are you ready to try some other reactions.
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guaguanco
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| Quote: | Originally posted by Saerynide
You guys are having fun teasing me.. so cruel
I used graphite anode. I bundled a bunch of thick pencil leads together. I scraped them all clean of glue and junk with a knife before using em.
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Problem number one. Pencil leads have all kinds of stuff in them, they are far from pure graphite. Not suitable.
This thread should be moved to Electrochemistry.
[Edited on 13-1-2004 by guaguanco]
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Al Koholic
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Agreed.
Chill out, and before you dump this into your yard which I wouldn't do anyway, make sure you don't get your water from a well...
To be honest, if you smelled H2S and all outside, there is no reason to run for the hills. Without containment and with such a small source you are
in no danger.
Also, as chemleo stated, I believe the problem is with your power supply. I as well do hope you are using DC and believe you are. Although, how are
you getting this DC current? Have you done any measurements of current, voltage, resistance, while actually running the cell? From the sound of your
description IE: the cell getting very very hot in a very short time, I think you are using a HUGE current and a HUGE overvoltage hence you are driving
other reactions. To do this right, you really should be measuring these parameters. An multimeter only costs like 20 bucks at radio shack.
Holy shit. It took me 6 or 7 minutes to write that, and 4 posts came up in between!!!!
[Edited on 13-1-2004 by Al Koholic]
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chemoleo
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Yepp, I remember back in my heyday, I once electrolysed 1 l of saturated NaCl with 220 V (!!!) DC. Wow, that was fun! The solution heated up to
boiling within seconds, and I got heaps of NaOH etc.
Anyway, thats what I suspected... lead pencils... it's a very bad idea. They do contain clay materials, plus oils (which for sure is the oil u
noticed at the surface of the solution). Anyway, you are introducing all sorts of materials that way. How about you go to your local hardware store
and get yourself some decent welding carbon electrodes? They work much better. You can use them for electric arcs too, and make some CaC2 that way...
Now, the knife you use for the cathode..... what did it look like after you did your electrolysis? I bet it went from shiny to a dull colour - which
would indicate that the Fe got dissolved. Indeed, in this case, this would explain nicely why your solution turned orange. FeIII+ is orange/red/brown.
With closed container I meant to find out whether any evolving gases could back -react with the solution - just as with NaCl, where the Cl2 reacts
with the NaOH. Obviously you wouldnt close it completely (doh ), you would have
to have some kind of overpressure valve, or a venting hole at the top of your vessel.
Anyway... I would do what guaguanco suggested: Start simple. Use water, no salts, nothing else, and acidify slightly. Then run your electrolysis. Turn
down your power. The solution shouldnt get more than 40 deg C hot. If it works without producing H2S, chromium, nickel, cyanide, war gas etc, only
then you are ready to test it with MgSO4!!
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Theoretic
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"BRIGHT orange"
I have once hydrolysed some Fe(lll) salt in very hot water, in hope of making a ruby-red colloidal solution (a few drops of FeCl3 in boiling water, my
chemistry book stated). And I did only use a few drops. It didn't work... ...kind of. I got a very bright orange opaque solution, which in a few minutes settled to a voluminous, BRIGHT orange precipitate. So Fe(OH)3 pretty
much fits your description.
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vulture
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Don't let the media get all this supercarcinogenic crap in you.
Everyone's screaming about PAH in the air, gsm radiation poisoning the kids, but how many smokers out there are voluntarily inhalating CO, HCN
and VERY carcinogenic nitrosamines? How many people pump their tanks full of gasoline, but scream bloody murder if there's 1ppm of benzene in the
air?
[Edited on 13-1-2004 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Saerynide
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| Quote: | Originally posted by guaguanco
You should try a test run, using your cathode and anode and nothing but distilled water. Observe what happens. Once you can run cleanly, producing
nothing but H2 and O2, then and only then are you ready to try some other reactions. |
I used the knife many times before, and it didnt contaminate my solutions... It must have been that it got used too much and wear and tear is finally
taking its toll on it. Either that, or its some stuff that was plated on it from use in previous experiments. The second one is probably the case,
cause the knife didnt show show signs of corrosion.
However, as much as I would like to believe my solution is only iron salt, I think I know why its not. After electrolyzing the solution to try to
plate out the metal ions, I washed and left the knife out on the porch. The last time I did this with a with an kinfe plated with an iron solution,
it was black with rust the next day. Its been about 2 days and its still out there. It shows no signs of rusting, so it cant be iron.
| Quote: | Originally posted by Al Koholic
To be honest, if you smelled H2S and all outside, there is no reason to run for the hills. Without containment and with such a small source you are in
no danger. |
Well, my yard isnt exactly the biggest yard, and I have a very high fence. The area was starting to stink up pretty fast cause I did it by the fence.
"Far away from the house" means about 15 m or so... I guess I shouldnt have used "far" in my sentence
I know I sound like some over-paranoid freak about carcinogens, but I have lost a few family members to cancer. I do not want increase the risk of
having to lose anymore (or myself) by exposing them to more carcinogens than they need.
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Al Koholic
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I also forgot to mention this....
When using a stainless steel cathode, be sure to place the electrode to the same depths in each experiment if you are using the same knife over and
over. Ideally it would be best to make sure the whole electrode is under the surface of the solution and to keep the part above covered with plastic
or wax. I noticed when electrolysing brine before that the Cl2 attacks the portion of metal above the solution and forms salts that contaminate the
batch. You may have had something like this going on too I don't know...
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Saerynide
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Hmm....Maybe its the H+ from the anode?
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unionised
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I wonder if you managed to produce graphitic oxide. That could explain how itcarried on being violent, even after you shut off the power.
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Al Koholic
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I somewhat doubt he got graphitic oxide after reading a small bit about it just now. Apparently, the most cost effective and easiest way of making it
is by treating graphite with a strongly oxidizing solution. 100% H2SO4 with proportions of dissolved NaNO3 and KMnO4 is used to produce the graphitic
oxide which is supposedly a nice brown powder that I think would be useful for someone trying to make a metal oxide catalyst....
Anyway, thats a bit off topic but I seriously doubt your mix had the oxidizing power of the solution that would result from mixing H2SO4, KMnO4, and
NaNO3...
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Saerynide
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I agree, otherwise, I would be worried.. Who knows what else could've gotten in there
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Tacho
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Quote:
"You have the colours the wrong way round. Chromium(III) salts are generally green, whilst chromium(VI) salts are generally orange."
Sorry, you are right.
So, I gess the orange salts are the bad ones.
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unionised
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Al Koholic
I see you have read a little bit about it; if you read a little bit more about it you will find that another way of producing it is the electrolytic
oxidation of graphite.
I'm far from certain that he made the stuff but I wouldn't write the idea off just because it an be made differently.
Anyone got any other ideas about how it got violent after the power was shut off?
O, by the way, if I want to oxidise things like, for example, fluoride to fluorine, I might very well try to do it electrolyticaly. I wouldnt set up
the conditions he had, after all the water would bugger it up. OTOH I wouldn't try using a mixture of H2SO4, KMnO4 and NaNO3 because it's
not as oxidising as a properly made electrolytic cell.
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Saerynide
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What is the electrolytic method you have read about producing graphic oxide?
I think you misunderstood, the reaction just stayed violent for a short while after the power was cut, it didnt become anymore violent.
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