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Author Topic: KARPEN PILE  (Read 230963 times)

profitis

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Re: KARPEN PILE
« Reply #120 on: July 08, 2014, 06:42:17 PM »
You may proceed with the platinized Pt foil from the conductivity cell meantime and the treated Ag mr pomodoro.it will not fail you.leakage is the only concern and if H2 is piped through periodicly we can eliminate that completely.you can seal when the behaviour is as expected.we want the maximum power from overpotential differences that's all.

pomodoro

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Re: KARPEN PILE
« Reply #121 on: July 09, 2014, 05:39:08 AM »
Good news. I have small amounts of ammonium tetrachloropalladate, potassium hexachloropalladate,PdCl2 and 1.5 cm of PD wire about 1mm diameter. I also have some ammoniumtetrachloroplatinate,chloroplatinic acid and gold chloride. So think carefully of the best cell we can possibly have first up!

pomodoro

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Re: KARPEN PILE
« Reply #122 on: July 09, 2014, 07:09:50 AM »
Here is what I plan to build. It should keep the h2 in permanently don't you think? Others reading don't be shy and make any comments.
« Last Edit: July 09, 2014, 12:09:33 PM by pomodoro »

profitis

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Re: KARPEN PILE
« Reply #123 on: July 09, 2014, 12:19:14 PM »
Here's the ideal for keeping out air mr pomodoro.this ensures continuous dilution and purging of traces of air.the electrolyte on the bottom,away from wire leads,hydrogen gas pumped through the tubes once or twice/day and clamped shut(clamp in this pic),the one pipe remaining attatched to H2 supply cylinder..you cannot use candle-type wax for sealing its very weak and breaks if a vaccuum is formed and it reacts with NaOH making soap which will poison our catalysts.hardcore silicone is best.I  melt the rims of this plastic pill container with a cigarette lighter to seal totaly.I melt around the wires enough to seal. What metal are your lead wires made of pomodoro??

profitis

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Re: KARPEN PILE
« Reply #124 on: July 09, 2014, 12:35:09 PM »
Your setup will work for a few days but it won't be a permanent seal.oxygen in the air will be sucked in through the electrolyte via diffusion and it does this with quite a lot of force.is your flask-neck rough glass or smooth? What is that large metal disk in your pic?

pomodoro

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Re: KARPEN PILE
« Reply #125 on: July 09, 2014, 01:38:52 PM »
OK, I will listen and do an initial test first, with H2 slowly passed on top of the solution after an initial saturation   If it works I will find a glass blower to melt Pt wire to glass as leads with a top section that can be melted later to seal permanently.
Problem would be joining the Pt lead to the Ag wire. Will solder last for years?

The large disk is pure silver.  I thought of cutting it to shape, with a skinny section as wire.  I could solder it to Pt wire but again, I'm not sure about the solder...
I also have kilos of triple distilled Hg. Would this not be better than Ag? It can sit at the bottom of the cell with the tip of a  Pt wire encased in glass touching it- I havent checked if it amalgamates so that could be a problem too.. Doesn't it have a much higher overpotential?

I don't have all that many hours to work on this so would like to get something going that's pretty good.

profitis

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Re: KARPEN PILE
« Reply #126 on: July 09, 2014, 02:48:26 PM »
Do my setup above for now as a preliminary yes pomodoro.seal around the pipe entrances with harcore silicone. You must have minimum exposure of silver wire to the electrolyte on the anode side otherwise slow self discharge will take place there and reduce voltage.use smooth silver wire leads.you don't have to solder just twist properly(many twists) onto the anode Pt wire,no corrosion will take place as it is actually the Pt wire which is anodic.do not cut silver from the disk to use as wire use proper wire.gold wire is also fine.you can use the below v-setup using a single bent glass tube or polyethylene tube.I'm using a drinking straw in the pic just to illustrate.the v-setup allows to easily melt both ends shut one at a time.electrolyte is inserted via syringe when Pt side is melted shut then electrolysis gives H2 there and oxygen generated on the other open end with Pt wire prong and ejected.a tiny bit of air will be trapped when you seal cathode side but not enough to recombine all the H2.a slight vaccuum will form after sealing.the tube can also be wider on the Pt side for more space for H2.

profitis

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Re: KARPEN PILE
« Reply #127 on: July 09, 2014, 02:56:38 PM »
Don't use mercury now as it has small surface area as you know.cathode surface area is equally important as anode area for power current.we will have to amalgamate with silver later on and then anodize-cathodize same treatment as for the silver for area.your platinized foil looks well worn I see a lot of its black has fallen off but it should do fine.clean it in nitric,rinse thoroughly.

profitis

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Re: KARPEN PILE
« Reply #128 on: July 09, 2014, 03:04:12 PM »
You can use bare copper wire for the initial test but it must be far above the electrolyte.copper wire won't leak H2 out the device but it will corrode if wetted at the interwire connections.

pomodoro

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Re: KARPEN PILE
« Reply #129 on: July 09, 2014, 03:12:43 PM »
Thanks for all the ideas, you have given me plenty of info. Now its my turn to get something done. Next post will have some results, keep checking folks. Oh that pt is not platinized. I will try the palladizing treatment first.

profitis

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Re: KARPEN PILE
« Reply #130 on: July 09, 2014, 05:56:01 PM »
Please try electrolytic palladium deposition by the book first to be on the safe side pomodoro.I think its done much the same way as platinum deposition.swirl a few drops HCl in with the potassium chloropalladate solution and add a tiny bit lead acetate or chloride and deposit with small current.use graphite as your anode.etch your foil prior to deposition.palladium swells slightly when it takes in H2 so it must be adherent.google deposition methods to find out more.heat for a few mins in dil.HNO3 afterward to clean out any deposited Pb(lead)

profitis

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Re: KARPEN PILE
« Reply #131 on: July 09, 2014, 06:16:42 PM »
If you can smash that conductivity cell and retrieve that platinized foil I would feel less nervous @pomodoro.the first test that we show here must be good.

profitis

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Re: KARPEN PILE
« Reply #132 on: July 09, 2014, 06:30:50 PM »
Use tiktak presstick around H2 pipe entrances into the device instead of silicone pomodoro.if silicone peels from movement there will be problems.use lab clamp-stands to prevent movement of pipe inlets.test the device container for leaks under washbasin water before assembly,syringe in some conc NaOH and aluminum pieces INSIDE the shell through inlet holes to generate gas and press your fingers over the two gas entry/exit-holes..gas must only escape under your fingers NOT at the rims or through the wires.you will spot a leak under water.we want robustness. Syringe out or siphon out the waste and rinse

pomodoro

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Re: KARPEN PILE
« Reply #133 on: July 11, 2014, 01:30:23 PM »
Been busy last few days but managed to prepare the palladium sponge. The photos show the Pt electrode in aqua regia (it was still shiny after the 3 minutes), plating of Pd (followed a method from journal with no lead acetate), and the cathodic electrolysis of 1M NaOH over weekend at 60mA to test adhesion. I've made some AgCN in order to plate the other similar Pt electrode with Ag for the test. I don't have silver wire and it will be easy to check the plate during the oxidizing step.