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making potassium (per) chlorate


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#4641 WSM

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Posted 14 March 2017 - 06:57 AM

I've been super busy at work (12 hour days, six days a week) and haven't been able to do much else, lately.
 
I did fill the experimental cell with water and, unfortunately, there's a slight leak amongst the bottom fittings. I'll check it more closely when I can manage to get home during the daylight hours. I'm sure it's just that I didn't tighten some of the fittings enough when I assembled the bottom plate.

The Viton gasket is holding fine though, so that's not the problem.  
 
I think things will ease up at work soon, and I'll be able to adjust the fittings and find out if the cell will seal properly and work the way I planned it to.

We'll see...
 
WSM B)

Edited by WSM, 15 March 2017 - 06:18 PM.


#4642 WSM

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Posted 16 March 2017 - 07:01 AM

I think things will ease up at work soon, and I'll be able to adjust the fittings and find out if the cell will seal properly and work the way I planned it to.

 

It's starting to look like I'll have this weekend free (Yay!), so we'll see how the cell looks after I tighten the fittings and try the water test again.

 

Once everything is tight and secure, it's time to set up a trial run and try to determine how much time it'll take to reduce the fluid level to approximately 50% of its starting point (which is when the harvesting cycle begins).

 

I'm excited to see the difference between the way things went last year and how this new cell works. If it runs as well as expected, this might be a real game changer for amateur perchlorate production  :D.

 

WSM B)



#4643 Nitrotitanite

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Posted 16 March 2017 - 01:59 PM

When everything is completed it would be nice to have a full tutorial that summarizes all 233 pages of this long post, very heavy to understand to be honest.

#4644 Mumbles

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Posted 16 March 2017 - 02:22 PM

I don't know if it will ever truly be complete.  If you want write ups you may want to check WSM's blogs.  There have also been some articles written in the PGI bulletin on chlorate and perchlorate cells.


Just so you guys quit asking, here is the link to the old forum. http://www.xsorbit2....forum/index.cgi

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#4645 WSM

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Posted 18 March 2017 - 09:15 AM

I don't know if it will ever truly be complete.  If you want write ups you may want to check WSM's blogs.  There have also been some articles written in the PGI bulletin on chlorate and perchlorate cells.

 

Hi Nitrotitanite,

 

If you do read my blog postings and have questions about anything there, feel free to ask here or by PM (your choice) and I'll do my best to answer.

 

This is true for everyone here. If we don't ask, we don't learn.

 

WSM B)



#4646 Nitrotitanite

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Posted 18 March 2017 - 10:34 AM

Ok thanks for your time😃

#4647 greenlight

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Posted 19 March 2017 - 02:41 AM

Sorry for the massive delay bit I have been busy with work.
I only just got around to wiring up the whole system today.. Another reason for the delay is I decided I wanted the whole thing mounted on a wooden table that is dodgily made from a wooden pallet and sheets of thin plywood.
There is also a dividing section that the ammeter sits in to seperate the electronics from the cell a little bit.
Here is a pic from the electronics side. It is half wired together.

Attached Files


Edited by greenlight, 19 March 2017 - 02:47 AM.


#4648 WSM

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Posted 20 March 2017 - 03:16 PM

Sorry for the massive delay bit I have been busy with work.
I only just got around to wiring up the whole system today.. Another reason for the delay is I decided I wanted the whole thing mounted on a wooden table that is dodgily made from a wooden pallet and sheets of thin plywood.
There is also a dividing section that the ammeter sits in to seperate the electronics from the cell a little bit.
Here is a pic from the electronics side. It is half wired together.

 

It looks like it's coming together. I think it'll work fine. Let us know how it goes.

 

WSM B)



#4649 WSM

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Posted 20 March 2017 - 03:18 PM

Happy Vernal Equinox (unless you're in the Southern hemisphere, in which case; Happy Autumnal Equinox;)  :D !!!

 

WSM B)


Edited by WSM, 20 March 2017 - 03:19 PM.


#4650 Kevin

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Posted 21 March 2017 - 08:56 PM

Hi, I'm going to be adding a temperature display to my chlorate cell for its next run (May at the earliest). I bought an Inkbird ITC-100VH temperature controller/ display and a PT100 teflon insulated sensor online. I have 1/4" compression fittings, but the temperature sensor is too narrow to make a tight seal where it will enter the lid. The best solution I've come up with (Somewhat based on WSM's blog post I recall reading a while back) is to use a (roughly) 1/4" plastic plug with a hole drilled through the center for the sensor and then I'll use heat shrink tubing over them both to seal it. I have some NTE electronics brand clear, thin-walled heat shrink tubing on hand, but all it says is that it's polyolefin which, to the best of my knowledge, could be any of a number of different types of plastic. I tried contacting them to find out specifically which type it is, but, unsurprisingly, they didn't respond. Any idea if I can use this for my cell? I'm figuring I'll give it a try and if it doesn't hold up I'll purchase some better heat shrink tubing. 

 

Kevin



#4651 WSM

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Posted 21 March 2017 - 09:22 PM

Hi, I'm going to be adding a temperature display to my chlorate cell for its next run (May at the earliest). I bought an Inkbird ITC-100VH temperature controller/ display and a PT100 teflon insulated sensor online. I have 1/4" compression fittings, but the temperature sensor is too narrow to make a tight seal where it will enter the lid. The best solution I've come up with (Somewhat based on WSM's blog post I recall reading a while back) is to use a (roughly) 1/4" plastic plug with a hole drilled through the center for the sensor and then I'll use heat shrink tubing over them both to seal it. I have some NTE electronics brand clear, thin-walled heat shrink tubing on hand, but all it says is that it's polyolefin which, to the best of my knowledge, could be any of a number of different types of plastic. I tried contacting them to find out specifically which type it is, but, unsurprisingly, they didn't respond. Any idea if I can use this for my cell? I'm figuring I'll give it a try and if it doesn't hold up I'll purchase some better heat shrink tubing. 

Kevin

 

Hi Kevin,

 

What I did with the first sodium chlorate cell (last Summer), was to use a 1/4" PVDF compression fitting and filled the gaps with a slit piece of silicone tubing. When I tightened the ferrule, the silicone squeezed tight around the leads and sealed them. Say what you will but it worked.

 

If you need to use shrink tube, use either PTFE or PVDF shrink tube, especially if it needs to come in contact with the electrolyte. It's available on eBay from China for a "reasonable" (some more than others) cost. It does require higher heat to shrink it, which may cause problems with lower melting point insulation on the sensor leads.

 

With the PTFE coated PT100 sensors, I don't see a problem, but the split silicone tubing trick might be all you need to do to seal it in the compression fitting.

 

One question though, are you using the temperature controller just as a temperature display or are you using it to control the temperature of your cell?

 

Good luck and please share your experiences.

 

WSM B)


Edited by WSM, 21 March 2017 - 09:30 PM.


#4652 PTFE

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Posted 22 March 2017 - 09:18 AM

hey guys!

For a Cell with a thin Cell material, you can use your sensor mounted at the outside, when you ensure its well insulated.

Another good way is, to take a 10x8mm PTFE Tube and a 8x6mm Boro. Glass tube.

A 5mm sensor will fit in well and with thermal sealing you can seal one side of your glass tube and putting it into the PTFE tube to make a thightly seal.

Unfortunately i've only got one picture of it, since the small boro tube has broken when i disassembled the cell the last time.

Between the right Cathode and the Anode you can see the small diffusor-tube for the HCL and in the front the Tube for the Temperatur sensor.

Attached Files


Edited by PTFE, 22 March 2017 - 09:26 AM.


#4653 Kevin

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Posted Today, 08:53 PM

 

Hi Kevin,

 

What I did with the first sodium chlorate cell (last Summer), was to use a 1/4" PVDF compression fitting and filled the gaps with a slit piece of silicone tubing. When I tightened the ferrule, the silicone squeezed tight around the leads and sealed them. Say what you will but it worked.

 

If you need to use shrink tube, use either PTFE or PVDF shrink tube, especially if it needs to come in contact with the electrolyte. It's available on eBay from China for a "reasonable" (some more than others) cost. It does require higher heat to shrink it, which may cause problems with lower melting point insulation on the sensor leads.

 

With the PTFE coated PT100 sensors, I don't see a problem, but the split silicone tubing trick might be all you need to do to seal it in the compression fitting.

 

One question though, are you using the temperature controller just as a temperature display or are you using it to control the temperature of your cell?

 

Good luck and please share your experiences.

 

WSM B)

 

I like that, it's really simple but would work quite nicely! Your idea also has me thinking.. To seal my lid I made my own silicone o-rings that fit into a groove in my lid like this: 

IMG 0387
 
I made my o-ring by cutting a groove in HDPE plastic and filling it with silicone. Silicone doesn't bond to HDPE, so with some care I was able to remove it intact. I wonder if I could make a much smaller one and if it would work to seal my temperature sensor... 

 

I'll more than likely be using it just as a display initially and adjust things manually if I want to regulate the temperature. I did also purchased a solid-state relay that I may use to power a heating element if it's not running hot enough. However, these cells seem to run quite warm even without insulation, so if I decide to run it warmer I think I'd start with insulation. I may need to cool my cell rather than heat it so I might end up using my controller to operate a fan or small pump- though I'm not overly familiar with solid-state relays, so I'll have to read up on them first regarding their ability to operate inductive loads. 

 

I'm still fairly interested to know how well my heat shrink tubing will hold up to the conditions of the cell so I may involve some somewhere (even just around an electrode) to test it. 

 

hey guys!

For a Cell with a thin Cell material, you can use your sensor mounted at the outside, when you ensure its well insulated.

Another good way is, to take a 10x8mm PTFE Tube and a 8x6mm Boro. Glass tube.

A 5mm sensor will fit in well and with thermal sealing you can seal one side of your glass tube and putting it into the PTFE tube to make a thightly seal.

Unfortunately i've only got one picture of it, since the small boro tube has broken when i disassembled the cell the last time.

Between the right Cathode and the Anode you can see the small diffusor-tube for the HCL and in the front the Tube for the Temperatur sensor.

 

I placed a temperature sensor on the outside of my cell the last time I ran it. I didn't insulate it though, and once I thought of it I didn't want to because I figured it would render my initial temperature readings irrelevant. I may do it in the future though in case I want to know the temperature in multiple locations to see if the temperature is uniform.

 

Did you get any salt creep coming through in between the boro. glass and the PTFE tubing? 

 

Thanks for the suggestions, WSM and PTFE, I'll be sure to post how things go!

 

Kevin






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