making potassium (per) chlorate

[frank]

The strips of Ti (used llike rivets) is a great 'get away'. Bolts (Ti bolts) would of course be better but if this lasts long enough then it's perfect.

 

I presume that the part with the homemade rivets is actually submerged below the level of the electrolyte? (ie. all of the MMO is in the salt solution).

Just to bore you all, when bare Ti is used as a Cathode the non conducting Ti Oxide layer is still on the surface of the Ti. It does not magically dissappear.

It becomed totally conductive by hydrogen being produced at the cathode surface (as happens at the cathode).

This hydrogen dopes the non conducting Ti Oxide and it magically becomes a conductor.

If the same piece of bare Ti is then used as an anode the H does not get produced and the Ti Oxide reverts back to being non conductive and the

current stops flowing. If you put a high enough Voltage of say 15 volts to the anode, the oxide layer breaks down and the Ti gets eaten away.

 

I imagine that when you rivit the bare Ti to the MMO there must be a small amount of Hydrogen produced at the interface of the MMO and bare Ti

which keeps the Oxide layer on the bare Ti doped and conductive. Since electrons are going out of the MMO surface at the interface (as they do in a cathode)

some H is being produced which keeps the (bare Ti) Oxide conductive. (I think!!!!!!!!)

 

How many hours running has the joint done and is there any sign of the voltage rising accross the joint (or accros the cell because of the joint)?

 

Frank

[WSM]

I'm only 16, it's mostly just a science project, and I have a tight budget

 

Hi Tesla,

 

Good for you. Your answer is your best introduction to the weld shop owner. Maybe they'll take pity on you and do it for free. All you can do is ask. The worst they can say is no.

 

Good luck.

 

WSM

[oldmanbeefjerky]

frank, i think theres something wrong with your logic.

how does the hydrogen form when the titanium dioxide is non conductive, and the hydrogen is required to start electrolysis to make hydrogen to allow the titanium to become conductive to make hydrogen.EE

 

its a parradox. i just think the titanium dioxide is a semi conductor in this situation and thats it. it wont allow a reaction that further oxidizes the titanium dioxide, but will allow reduction reaction, which occures at the cathode.

not all the water will touch all the surface of the titanium, such as that touching the anode mesh, and it will take a long time before water gets between it and wrecks it, so long as its done up real tight.

 

tesla,three words

 

MOT , Copper electrodes

Edited August 6, 2011 by oldmanbeefjerky

[Tesla]

Now that I think about it, I have a friend whose dad is big into welding...hmmm

[frank]

Why Titanium (and other valve metals) will not conduct when used as an Anode (oxide layer not conductive) and why the oxide layer becomes conductive

when they are used as a Cathode is explained in a hell of a lot more detail than my explanation.

 

http://downloads.hindawi.com/journals/apec/1974/398185.pdf

Hydrogen doping it is!!

If you dont believe Mr. C. K. DYER all the way from the Department of Metallurgy and Materials Science, University ofNottingham, Nottingham, U.K. ON JULY 6 1974 (WOULD YOU BELIEVE)

then I give up.

The joint that is created by the homemade rivets in not a sealed joint. The solution will be able to get in between the Ti and the MMO yet it works.

It's time someone had got around to actually trying and doing it.

I am not condemming the rivited joint. If fact the complete opposite. Its a marvelous idea. A winner.

Since it has not failed during the first few runs it will last forever IMO.

It would be great if it could be pulled apart just to see what the MMO and Ti actually looks like at the contact points. (want a job pdfbq)!

Frank

Edited August 6, 2011 by frank

[patsroom]

http://nastyprisms.com/temp/cache/www.geocities.com/CapeCanaveral/Campus/5361/basechem.html

[pdfbq]

I imagine that when you rivit the bare Ti to the MMO there must be a small amount of Hydrogen produced at the interface of the MMO and bare Ti

which keeps the Oxide layer on the bare Ti doped and conductive.

Nice!! I just made my small post to show my working solution but got a fun and interesting reply!

Hope to not disappoint you all by telling that its not a MMO but a Pt anode but I guess this won't change much to the H2 doping idea.

When I would try the same trick on an MMO I would first remove the MMO layer. I did not do that with this Pt anode because the Pt is so conductive.

How many hours running has the joint done and is there any sign of the voltage rising across the joint (or across the cell because of the joint)?

About 30 days all together, six runs or so. But I can not tell you much about the voltage because I did not measure that. I only measured the Amps and that is still hard to tell because, as you can see the Pt starts to wear and I lost one rivet .

It went down to as I recall 16 Amps at startup for the last run.

It would be great if it could be pulled apart just to see what the MMO and Ti actually looks like at the contact points. (want a job pdfbq)!

The problem here is that my Pt anode is fragile (and a bit expensive ) but I am curious too.

Edited August 7, 2011 by pdfbq

[oldmanbeefjerky]

i cant imagine why anyone would remove the MMO layer off an anode, unless they were filthy rich or crazy , or had a fried anode.

 

 

well, i care little for the discussion that went ahead prior...

 

im gonna build a permanent cell, and my first run ( since i have no ammeter and thus no means of safely running the cell without risking wrecking the anode), im going to use a steel anode, but not the iPod, just yet. im sure the low voltage of 3.3V will be nicer to stainless steel than 5v.

 

steel wont somehow ruin CP titanium cathode will it? i plan to reuse it in the forseeable future

[WSM]

i cant imagine why anyone would remove the MMO layer off an anode, unless they were filthy rich or crazy , or had a fried anode.

well, i care little for the discussion that went ahead prior...

im gonna build a permanent cell, and my first run ( since i have no ammeter and thus no means of safely running the cell without risking wrecking the anode), im going to use a steel anode, but not the iPod, just yet. im sure the low voltage of 3.3V will be nicer to stainless steel than 5v.

steel wont somehow ruin CP titanium cathode will it? i plan to reuse it in the forseeable future

 

Hi OMBJ,

 

I imagine the stainless steel anode will break down (start to dissolve) and will fill any product with traces of nickel and chromium, plus probably iron. I don't believe the cathode will be affected (cathodic protection).

 

I used to remove a small patch of the MMO just where the strap was spot welded (believing the MMO would interfere with the weld; not so). I tried spot welding without MMO removal and it worked just fine, so I don't bother anymore. MMO is more conductive than the titanium, I think.

 

WSM

[pyrojig]

I used to remove a small patch of the MMO just where the strap was spot welded (believing the MMO would interfere with the weld; not so). I tried spot welding without MMO removal and it worked just fine, so I don't bother anymore. MMO is more conductive than the titanium, I think.

 

WSM

 

This is interesting.... , I scraped the MMO off very carefully in the welding areas as well. I just assumed that the weld would have less contaminated crap in it. Although the spot weld is a fast weld, I want to expose myself to as little MMO smoke as possible.

Edited August 7, 2011 by pyrojig

[hillbillyreefer]

Here is my situation. Cell was running for about 48 hrs, solution had a bit of a yellow tinge to it, otherwise it was clean. Sometime between 48 and 56 hours the power supply was interrupted. Never trust your 3 month old rottie to look after business. Anyway, my mmo anode looks fine, but my 316 stainless cathode looks rusted, and my liquor has a black tinge to it. The cell is back on line and working like it was before the power interruption. Should I carry on and finish the run or should I discard this batch, put together another cathode and start over?

 

My thoughts are to filter and recrystalize in much the same way as the people running graphite do. Then start with fresh cathodes for the next batch.

[patsroom]

i cant imagine why anyone would remove the MMO layer off an anode, unless they were filthy rich or crazy , or had a fried anode.

 

 

well, i care little for the discussion that went ahead prior...

 

im gonna build a permanent cell, and my first run ( since i have no ammeter and thus no means of safely running the cell without risking wrecking the anode), im going to use a steel anode, but not the iPod, just yet. im sure the low voltage of 3.3V will be nicer to stainless steel than 5v.

 

steel wont somehow ruin CP titanium cathode will it? i plan to reuse it in the forseeable future

 

 

The anode is the positive connection and the negative is referred to as the cathode. Both of the electrodes will bubble when working so it is important to insure that your anode is connected to the positive side of the electrolytic cell power supply. It is not enough to connect anodes of miscellaneous material to the positive connection, it must be one that has been proven to work. The same is true for the cathode, if not then the electrolytic cell will not work properly and you end product may not suit your needs. So it is best to stay with known elecrtodes, or you may be just wasting your time and chemicals. After finding about the kind of electrodes that fits your needs best. You have the choice to make them or to buy them.

 

Anodes: Graphite, PbO2 Lead Dioxide, MMO Titanium Mesh, Platinum

 

Cathode: Graphite, Stainless Steel, CP Titanium

 

I am not saying that you can not experiment with other anodes and the likes but to produce a chlorate or even a (per)chlorate it is best to use the known materials that will make the proper end product.

Edited August 7, 2011 by patsroom

[patsroom]

Here is my situation. Cell was running for about 48 hrs, solution had a bit of a yellow tinge to it, otherwise it was clean. Sometime between 48 and 56 hours the power supply was interrupted. Never trust your 3 month old rottie to look after business. Anyway, my mmo anode looks fine, but my 316 stainless cathode looks rusted, and my liquor has a black tinge to it. The cell is back on line and working like it was before the power interruption. Should I carry on and finish the run or should I discard this batch, put together another cathode and start over?

 

My thoughts are to filter and recrystalize in much the same way as the people running graphite do. Then start with fresh cathodes for the next batch.

 

 

IIRC (if I remember correctly):

Stainless steel will make a yellow tint to the solution. And it is not good to leave a stainless steel in the salt solution without power or it will corrode.

Replace the stainless steel with a new one. Filter the solution, put it back in and it should put it in working order again.

Edited August 8, 2011 by patsroom

[oldmanbeefjerky]

The anode is the positive connection and the negative is referred to as the cathode. Both of the electrodes will bubble when working so it is important to insure that your anode is connected to the positive side of the electrolytic cell power supply. It is not enough to connect anodes of miscellaneous material to the positive connection, it must be one that has been proven to work. The same is true for the cathode, if not then the electrolytic cell will not work properly and you end product may not suit your needs. So it is best to stay with known elecrtodes, or you may be just wasting your time and chemicals. After finding about the kind of electrodes that fits your needs best. You have the choice to make them or to buy them.

 

Anodes: Graphite, PbO2 Lead Dioxide, MMO Titanium Mesh, Platinum

 

Cathode: Graphite, Stainless Steel, CP Titanium

 

I am not saying that you can not experiment with other anodes and the likes but to produce a chlorate or even a (per)chlorate it is best to use the known materials that will make the proper end product.

 

 

 

actually i am experimenting with different anode materials, within reason of course. i wont use an anode that becomes soluble when it erodes.

 

there is allot of data out there in tests and such run on these "known" types of anodes, but little to non on corrodeable ones. usually it just says it wont work, and thats it. not how long it works, or if its contaminants can be easily removed, or any such thing.

 

anyway, like i said, until i have a proper cathode for my cell, i wont go and wreck my iPod chrome/steel anode, just quite yet.

[WSM]

IIRC (if I remember correctly):

Stainless steel will make a yellow tint to the solution. And it is not good to leave a stainless steel in the salt solution without power or it will corrode.

Replace the stainless steel with a new one. Filter the solution, put it back in and it should put it in working order again.

 

Actually, the first step to making chlorate is the water breaking down and forming hypochlorite plus free hydrogen. Hypochlorite has a greenish-yellow tint to it, and of course smells like bleach because that's what it is . Stainless steel is fundamentally iron, nickel and chromium; and the iron can react with hydrochloric acid and form iron chloride, a soluble brown substance.

 

WSM

[pdfbq]

Here is my situation. Cell was running for about 48 hrs, solution had a bit of a yellow tinge to it, otherwise it was clean. Sometime between 48 and 56 hours the power supply was interrupted. Never trust your 3 month old rottie to look after business. Anyway, my mmo anode looks fine, but my 316 stainless cathode looks rusted, and my liquor has a black tinge to it. The cell is back on line and working like it was before the power interruption. Should I carry on and finish the run or should I discard this batch, put together another cathode and start over?

 

My thoughts are to filter and recrystalize in much the same way as the people running graphite do. Then start with fresh cathodes for the next batch.

Took me a while to respond because I knew I red something about your type of contamination somewhere.

 

Now I think I remembered where. On the WF visser page (http://www.wfvisser....nl/indexEN.html) which is gone for two years now but here is kinda mirror:

http://www.scribd.co...y-Wouter-Visser

 

Anyway it said as i recall that you will not be able to filter the iron oxide off as is.

You need a chemical trick to bind the iron oxide first so you'll get bigger particles that you can filter.

[oldmanbeefjerky]

so i wont get any iron chloride as long as i dont use ph control.

goody!

[pdfbq]

so i wont get any iron chloride as long as i dont use ph control.

goody!

Dream on......... or buy yourself a $5 dollar multimeter and start using your MMO.

[oldmanbeefjerky]

$5 multimeter only reads up to 10A max before it overloads and burns out. $30 multimeter, same deal 10A max but with a built in fuse to protect the internal shunt.

 

in some things, i follow the saying, if you cant do it right dont do it at all, and this applies now. besides, i now find that i have no cell, since PETE is unsuitable. ill have to hunt for some PVC, and this means that any holes i make must be permanent, so ide best wait for my Titanium mesh to come in or for me to find some good FLAT stainless i can eventually replace with the same size titanium plates currently in use for my anode.

 

ill do what i can, and at the moment, its experimenting with other anodes!

[pdfbq]

You can measure easy big amps with a $5,- multimeter with a trick.

 

Get a 1 ohm 10W resistor when you buy your multimeter.

Attach one side of the resitor to the + of your powersupply, te other to your -.

 

Now the law of OHM (U = I x R) wil tell you you'll have about 5.2 amps (5.2 = I x 1) running.

 

Remove two times some insulation on your + cable, say 5cm apart.

 

Put your multimeter on uAmps and stick the two probes in the two bare copper places.

You will get a value, say 1.6. You now can calculate a factor, your factor (in this example 5.2/1.6 = 3.25).

Your $5 dollar 100 amp multimeter has been calibrated.

 

When using in a cell, say you read 7.3 uAmp, you do 7.3 x 3.25 = 23.725 which will tell you you are running about 23 amps.

 

This is by the way exactly how big amp meters work, there is no massive currenr running through a spool, it is done by a bridge, exactly as desribed above.

Edited August 8, 2011 by pdfbq

[pyrojig]

Your ah smart cookie !!!! Thanks for the tip... I have a 20A meter that my cell has gone beyond that capacity to measure and this is a awesome idea!!! You ROCK!!!

I recently purchased a inline digital amp meter+shunt that reads up to 50A for $11 off ebay.. It is worth browsing and finding one.

 

You can measure easy big amps with a $5,- multimeter with a trick.

 

Get a 1 ohm 10W resistor when you buy your multimeter.

Attach one side of the resitor to the + of your powersupply, te other to your -.

 

Now the law of OHM (U = I x R) wil tell you you'll have about 5.2 amps (5.2 = I x 1) running.

 

Remove two times some insulation on your + cable, say 5cm apart.

 

Put your multimeter on uAmps and stick the two probes in the two bare copper places.

You will get a value, say 1.6. You now can calculate a factor, your factor (in this example 5.2/1.6 = 3.25).

Your $5 dollar 100 amp multimeter has been calibrated.

 

When using in a cell, say you read 7.3 uAmp, you do 7.3 x 3.25 = 23.725 which will tell you you are running about 23 amps.

 

This is by the way exactly how big amp meters work, there is no massive currenr running through a spool, it is done by a bridge, exactly as desribed above.

[Bonny]

 

there is allot of data out there in tests and such run on these "known" types of anodes, but little to non on corrodeable ones. usually it just says it wont work, and thats it. not how long it works, or if its contaminants can be easily removed, or any such thing.

 

 

I think the logic for little to no data on them is: why bother using ANY corrodeable electrodes?? They might work, but WHY contaminate the cell when you don't need to? It just creates more work cleaning up the product.

 

 

 

in some things, i follow the saying, if you cant do it right dont do it at all, and this applies now. besides, i now find that i have no cell, since PETE is unsuitable. ill have to hunt for some PVC, and this means that any holes i make must be permanent, so ide best wait for my Titanium mesh to come in or for me to find some good FLAT stainless i can eventually replace with the same size titanium plates currently in use for my anode.

 

ill do what i can, and at the moment, its experimenting with other anodes!

 

What is PETE? If you are referring to HDPE (high density polyethylene [PE]), it will work just fine for a cell. I don't care what anyone says, I've made kilos of chlorate and then perchlorate using HDPE buckets and they work just fine.

 

Stop being so scared about damaging your MMO. Load up the cell, fire it up and stop when the amperage noticeably drops. (in my case my cell ran 20-25A, I stopped when it would drop to about 15A).

[oldmanbeefjerky]

well it looks like im gonna have to take a trip down to jaycar then...

 

also i was talking about PETE polyurethanaterphthalate , the clear kind. my HDPE pharmacy jar wont fit my anodes. also mumbles says it will degrade.

It's just that i have a lobg history of destroying brand new expensive things which i buy, or damaging them , like my new carbon fiber fishing rod, my telescopic fishing rod, my nitro-rc car, my first soldering iron, my first pocket flame torch, my first atx, my tv the list goes on

[Mumbles]

PETE is polyethylene terephthalate***. It's the clear plastic that soft drink and condiment bottles are made from. In this case he asked a while ago about using an old pill bottle, but was too lazy to look up what it was made from. The opaque ones are made from HDPE, and the clear ones tend to be made from PETE. I mentioned to him last night that PETE may not stand up to the cell conditions, as it is somewhat susceptible to hydrolysis.

 

 

*** - I mean seriously Oldmanbeefjerky, did you even bother looking up the acronym?

[oldmanbeefjerky]

i did actually, i must have misspelled it

 

anyway, i found some PVC which has a cap on one end which i can use for my cell. now i just need a screw lid from the hardware store and my ammeter and my permanent cell is complete!

Edited August 9, 2011 by oldmanbeefjerky