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Author Topic: KARPEN PILE  (Read 219683 times)

Offline profitis

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Re: KARPEN PILE
« Reply #105 on: July 07, 2014, 04:06:20 PM »
We can take this from a strictly overpotential difference point of view without causing too much of a stir mr pomodoro.I'm going to refrain from blowing the anti-2lot horn from now on and be strictly going by the textbook.

Offline pomodoro

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Re: KARPEN PILE
« Reply #106 on: July 08, 2014, 02:25:09 AM »
Guess I'll have to try Hg as well then?

Offline profitis

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Re: KARPEN PILE
« Reply #107 on: July 08, 2014, 09:03:09 AM »
You know it (-: ...try Hg/Ag amalg

Offline profitis

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Re: KARPEN PILE
« Reply #108 on: July 08, 2014, 09:15:12 AM »
@sarkeizen.gona make your dreams come true,by the textbook.

Offline pomodoro

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Re: KARPEN PILE
« Reply #109 on: July 08, 2014, 02:12:37 PM »
Ok, started to dig around to see what I've got.  So far I have a few shiny Pt electrodes,( platenized Pt electrodes I had are misplaced but if I cant find them  in a day or two I can break a specially constructed conductivity cell  to get new ones), pure silver electrode, new glassy carbon electrode, plenty of Hg, Gold ~200mg  which I precicipated from a weak cyanide solution with dithionite.  I'm hoping to make it into a plating solution, otherwise will need to buy some 24k gold and make an electrode out of it.  I've got some palladium chloride but in solution.  I've got UHP hydrogen, Ar and oxygen. 
Since the gold will take a while to sort out, I'll probably start on the Pt/Ag.  He are a few questions to save me some work and prove your concept quicky  mr profitus.

Note, electrodes are flat, about 1cmx1cm , water is milliQ quality, deoxygenated. Room temp approx 25C. Ag will be pre treated as you described, Pt trated in strong Hcl,  then both will be made cathodes in a separate alkaline solution to reduce any surface oxides

1.What conc. KOH or NaOH is preferable.
2.What distance between electrodes?
3.If I use the shiny Pt, will it work and what pre-treatment is  needed.
4.Any stirring or keep static.
5.If I saturate liquid with H2 , leave just a few mL of H2 gas above surface and seal it then connect it to a galvanometer , do you expect it to provide a constant current? 
6.How long would the current last?
7.Do you expect any dissolution of the silver?
8. Do you expect any silver oxide?
9.Do you expect the hydrogen to be consumed?




Offline profitis

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Re: KARPEN PILE
« Reply #110 on: July 08, 2014, 03:43:38 PM »
The way to judge a success in this instance will be to short-circuit the device for a few hours,disconnect,let re-equilibrate for an hour or so then measure if voltage climbed back up.a resting voltage that falls down to 0.1 with little or no current in its burst-discharge curve or less is a fail and has either a leak or is insufficiently saturated in H2. 1) KOH or NaOH will do fine in 1M conc. 2) put electrodes close-ish for max current,a cm or two apart.3) shiny Pt anodes are useless,you must use use black Pt.smash that conductivity cell carefully(I did,no regrets) 4) DO NOT STIR ANYTHING) 5) a few ml space for H2 is fine.we want to rid the device of as much air as possible.if you can pipe in H2 through the device periodicly or continuously slowly it is best.6) currents are in bursts,depending how much is drawn,you can leak a small steady current at the same or less rate than recharge rate.it depends on how much surface area you crammed into electrodes. 7) not in KOH or in NaOH under H2 no ways. 8) cathodize the Ag and Pt seperately in the device itself if you can using a Pt wire prong with nice big current through it.remove the wire and immediately begin piping H2 through.I used to just dump Al foil into the device to generate H2 and push air out but you must then use fairly con NaOH otherwise it takes too long.if you attatch Al foil to the electrodes its even better for reduction of oxides plus saturation of Pt.

Offline profitis

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Re: KARPEN PILE
« Reply #111 on: July 08, 2014, 03:57:28 PM »
I forgot your question number 9 mr pomodoro: this is impossible unless 1)the device is leaking(air will be sucked in).2) too much air was trapped in the device when sealed,creates a vaccuum and may pop a hole in the weakest part of the device container.3) Ag was insufficiently reduced to Ag metal prior to experiment.piping H2 through the device slowly,periodicly and out a small rubber or plastic valve is best option for those who have H2 lying around in cylinders.be sure to leak it out outside or the next time you light a cigarette will be your last.

Offline profitis

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Re: KARPEN PILE
« Reply #112 on: July 08, 2014, 04:16:02 PM »
At its very best.for a highly blackened Pt anode and Ag cathode and totaly leak-proof system you can expect up to 6milliamps or more/cm2 in bursts of a few seconds inbetween mr pomodoro.

Offline pomodoro

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Re: KARPEN PILE
« Reply #113 on: July 08, 2014, 04:18:16 PM »
I prefer not to have aluminate in solution. Now, I think the cell may work as follows. Pt black absorbs H2 and concentrates it. A concentration cell is formed, causing Ag to produce H2. As H2 builds up, voltage and current drop. When disconnected, H2 from Ag floats back up and voltage rises again, ready to repeat cycle. I can't see any need for catalytic   spillover!

Offline profitis

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Re: KARPEN PILE
« Reply #114 on: July 08, 2014, 04:32:13 PM »
Lol but thats also catalytic spillover.its repeatable.carbon is the usual substrate for spillover.

Offline profitis

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Re: KARPEN PILE
« Reply #115 on: July 08, 2014, 04:40:36 PM »
Aluminate is totaly inert much like silicate but it can give problems if it happens to crystallize out of solution on the electrodes impeding gas access.if the NaOH sol volume is large enough and at right concentration it won't crystallize.

Offline profitis

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Re: KARPEN PILE
« Reply #116 on: July 08, 2014, 04:44:11 PM »
And your PdCl2 solution can be very handy later on mr pomodoro (-: you can also leach Pd out of 10% Pd/C using aqua-reg.

Offline pomodoro

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Re: KARPEN PILE
« Reply #117 on: July 08, 2014, 05:26:31 PM »
If I have some time I'll send photos of the proposed setup. Once we agree on a foolproof cell I will proceed. I was thinking of bonding the Pd on C to a pt electrode with silver loaded epoxy if these initial experiments go well.

Offline profitis

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Re: KARPEN PILE
« Reply #118 on: July 08, 2014, 05:40:19 PM »
I was going to ask you about photos,that would add some spice to this thread for sure.don't bother epoxying anything mr pomodoro its going to have to be a tight adhering electroplate of Pd black.I used to burn conc PtCl2 syrup directly ontop Pt foil and it would decompose into the most beautiful grey sponge coat.I'm not sure if we can do this with PdCI2 but we can definitely do it with ammonium palladium chloride (this is how they prepare industrial catalysts) I just have to google quick to double-check on the decomposition products of PdCI2

Offline profitis

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Re: KARPEN PILE
« Reply #119 on: July 08, 2014, 06:07:52 PM »
PdCI2 decomposes to Pd sponge and Cl2 gas at 650 degrees C so a bunsen flame should be able to do it.ammonium chloropalladate precipitated from PdCI2 soln and a few drops ammonia soln melts then decomposes directly to sponge at low temp,300degrees