making potassium (per) chlorate

[WSM]

Good stuff WSM I will need that blog soon especially for the processing of the electrolyte. Well hopefully soon.

I installed the 200 amp shunt today after finally receiving it. Instead of 297 amps which the last one was reading, it now reads 111 amps which is still wrong considering the power supply is only 20 amp.

It is wired correctly too and I have no idea what the problem is.

Thanks. As soon as I figure out what's wrong and correct it, I'll post Part Fourteen.

 

The high read on your meter is strange. I wonder if using the wrong shunt might have damaged it somehow?

 

WSM

[greenlight]

You could be right, I will see if I can find any information on it.

I can order another meter as they are not expensive.

[WSM]

I was hoping to repair my high temperature sodium chlorate experiment and get it running by now. Unfortunately, we're running understaffed at work and so we've got a lot of overtime and heavy schedules lately, leaving little time at home to pursue hobbies.

 

I'll see if I can find some time to continue my research and get the cell up and running. The potential to step up production of sodium chlorate for an ample supply of feedstock for my perchlorate research, is exciting.

 

WSM

[greenlight]

Well done on the blog WSM, I was just reading it.

A 27 litre cell will surely make you an ample amount of sodium chlorate for recreational needs.

[WSM]

Well done on the blog WSM, I was just reading it.

A 27 litre cell will surely make you an ample amount of sodium chlorate for recreational needs.

 

It was an experiment and an aid in learning how to make sodium chlorate. It ran for six weeks before the run was completed and the yield of NaClO3 crystals was about 5 kilos (there's a lot of dissolved chlorate left in the "depleted" electrolyte, but I plan to recharge it with more NaCl and run it again).

 

I'm setting up a second experiment which will hopefully be a game changer and speed the production, plus simplify the process. If it works out, I'll be able to make more usable chlorate faster, and have a good supply of feedstock for my perchlorate experiments.

 

The electrolyte for the perchlorate cells uses lots of sodium chlorate (>5 lbs/gallon), so the more I have ready, the sooner I can try the perchlorate cell again. This project is a fun challenge.

 

WSM

[eb666]

Chlorate site

 

https://geocitieschloratesite.000webhostapp.com/

 

 

 

 

[WSM]

I was hoping to repair my high temperature sodium chlorate experiment and get it running by now. Unfortunately, we're running understaffed at work and so we've got a lot of overtime and heavy schedules lately, leaving little time at home to pursue hobbies.

I'll see if I can find some time to continue my research and get the cell up and running. The potential to step up production of sodium chlorate for an ample supply of feedstock for my perchlorate research, is exciting.

WSM

Well, work has slowed enough to have us back on a normal schedule; so I repaired and reassembled the electrodes into the bottom plate of the high temperature cell.

 

Soon, I plan to reassemble the cell and test it to assure it's water tight.

 

When it's well sealed I'll give it a trial run and see how it works.

 

WSM

Edited June 2, 2017 by WSM

[WSM]

Well, work has slowed enough to have us back on a normal schedule; so I repaired and reassembled the electrodes into the bottom plate of the high temperature cell.

Soon, I plan to reassemble the cell and test it to assure it's water tight.

When it's well sealed I'll give it a trial run and see how it works.

WSM

 

I reassembled the cell and filled it with water but realized it still leaks a little. I need to put it on a raised platform to give it a closer look and determine exactly where the leak is coming from. I suspect it's the anode tube, but need to be sure and attempt to seal it permanently.

 

In this configuration, the head pressure of the tall cell design may make getting a good seal difficult but I'm sure it's possible. If not, I can always replace the tubular leads with solid CP titanium leads, with the electrode end milled flat (for spot welding the electrodes on) and the other end drilled and tapped to accept the power leads. If I do that I have to test it and see if heating will be an issue.

 

Titanium is only about 3% as conductive as the copper core in my tubular titanium leads, and heating may be an issue in higher current setups. Heating won't be a problem for the cell, but the polymer compression fittings can be adversely affected by high temperatures and may fail. I don't think leaking hot electrolyte would be trivial .

 

I'll see what I can do to make this experiment work and report it here...

 

WSM

Edited June 7, 2017 by WSM

[WSM]

As Summer approaches, I'm putting my research on hold. My Wife and I are traveling cross country to visit family and I'll be gone for many weeks. I'll still check in using my smart phone from time to time, but the research will have to wait till I get back. I'll still be able to answer questions or post, but my responses may be slow.

 

WSM

[WSM]

A week or so ago I was thinking about my high temperature sodium chlorate cell experiments and had a flash of inspiration.

 

While I'm working out the problems of sealing the PVDF cell, I can try a smaller version by setting up a 4 liter beaker with a thick acrylic lid, fitted with the necessary fittings and attachments to hold the electrodes, sensors and other accessories.

 

A side benefit is that I have a heating mantle and controller fitted for the beaker. I can use the heating in case the electrodes don't heat the electrolyte enough.

 

I believe this setup would work as an excellent "proof of concept" cell.

 

Any thoughts?

 

WSM

[greenlight]

How many volts and amps is you power supply again WSM?

5 volt 55 amp?

 

I think you will need some sort of external heating to get all 27 litres up to a good temperature (70C or so).

Mine is 5 volt 20 amp and needed a water bath after an hour or two for the short time I did run it but yours is a lot larger in volume even though you have a lot more amps.

 

P.s ammeter never came. Reordered free of charge.

[WSM]

How many volts and amps is you power supply again WSM?

5 volt 55 amp?

I think you will need some sort of external heating to get all 27 litres up to a good temperature (70C or so).

Mine is 5 volt 20 amp and needed a water bath after an hour or two for the short time I did run it but yours is a lot larger in volume even though you have a lot more amps.

P.s ammeter never came. Reordered free of charge.

I have several power supplies available to use (I've been studying this subject for years). The premier supply in my arsenal is a high end unit with a range of 0-7.5 V and 0-140 A. It has constant current (CC) capability and can auto-sync with a second similar supply if needed. The downside is it's very expensive ($500-$600 range in the surplus equipment market). I also have several smaller units to choose from.

 

The cell I'm talking about is smaller and the current demand is determined by the working surface area of the anode (plus the ratio of anode to cathode surface areas).

 

In my high temperature sodium chlorate experiment, the target temperature of operation is about 110^oC, which is why I have the thought of using a heating mantle with a controller, if needed, for a smaller cell using a four liter beaker.

 

At these higher temperatures the cell will boil off excess water, thus naturally concentrating the chlorate levels to where crystalline sodium chlorate can be harvested at room temperature.

 

The depleted electrolyte can then be recharged with purified brine and run more.

 

I think (hope) the whole system can produce much more sodium chlorate in far less time. We'll see...

 

WSM

Edited July 21, 2017 by WSM

[WSM]

I've been eyeballing (watching) an expensive piece of glassware on eBay and finally took the plunge and bought it. I have one similar and feel it will be useful in my research. This is a 5000 ml Pyrex observation beaker:

 

http://i.ebayimg.com/images/g/xoYAAOSwhvFZBYJx/s-l1600.jpg

 

Part of my willingness to spend so much is an $18 credit due to me (which was about to expire), which I applied to the purchase, so my total expenditure was less than the asking price.

 

Look for it in future postings as I use it in my studies.

 

WSM

Edited July 27, 2017 by WSM

[Kevin]

Couple quick questions:

 

A have a chlorate cell currently running with 1" x 5" MMO/ titanium electrodes, which have been used once previously. I'm using a computer power supply modified to operate at constant current and it's been operating under 20 amps. The cell body is a 1 gallon jar. After beginning this run the cell temperature reached around 77C and after a day I added a fan, cooling it to around 55C. I noticed a gray sediment at the bottom of the jar. Could this be from the electrodes? When I removed them I couldn't discern any significant corrosion. The pH was also not controlled at this point.

 

On day 6 I started my pH control. My system is gravity fed and consists of a timer controlling a solenoid valve, and a needle valve to add 20% Hydrochloric acid (I would have diluted farther but I was worried about adding too much water). I initially manually added extra acid to try to bring the pH closer to an ideal 6.8 but I believe it ended up lower (close to 6). I decreased my dosing rate before ultimately stopping the pH control in an effort to get the pH to increase. I'm using pH papers to test and after a little over a day I believe the pH is still around 6. Shouldn't the pH have increased by now? I'm using a 1/4" outside diameter polyethylene tube with holes in the lower portion deep in my cell, near yet not between my electrodes. I'm wondering if bubbles have been forming in/ entering into the tubing, displacing more acid into the cell. Hopefully these pictures will help:

 

I'm not sure if this has much significance, but my cell liquor also had a faint yellowish color to it but that disappeared after dropping the pH and now has a clear/ white color.

 

Any help is appreciated as this is my first time dealing with pH control!

[WSM]

Couple quick questions:

A have a chlorate cell currently running with 1" x 5" MMO/ titanium electrodes, which have been used once previously. I'm using a computer power supply modified to operate at constant current and it's been operating under 20 amps. The cell body is a 1 gallon jar. After beginning this run the cell temperature reached around 77C and after a day I added a fan, cooling it to around 55C. I noticed a gray sediment at the bottom of the jar. Could this be from the electrodes? When I removed them I couldn't discern any significant corrosion. The pH was also not controlled at this point.

On day 6 I started my pH control. My system is gravity fed and consists of a timer controlling a solenoid valve, and a needle valve to add 20% Hydrochloric acid (I would have diluted farther but I was worried about adding too much water). I initially manually added extra acid to try to bring the pH closer to an ideal 6.8 but I believe it ended up lower (close to 6). I decreased my dosing rate before ultimately stopping the pH control in an effort to get the pH to increase. I'm using pH papers to test and after a little over a day I believe the pH is still around 6. Shouldn't the pH have increased by now? I'm using a 1/4" outside diameter polyethylene tube with holes in the lower portion deep in my cell, near yet not between my electrodes. I'm wondering if bubbles have been forming in/ entering into the tubing, displacing more acid into the cell. Hopefully these pictures will help:

I'm not sure if this has much significance, but my cell liquor also had a faint yellowish color to it but that disappeared after dropping the pH and now has a clear/ white color.

Any help is appreciated as this is my first time dealing with pH control!

 

Hi Kevin, Let's see if I can answer these concerns.

 

The grey sediment on the bottom of the cell can be from the electrodes. Most people first suspect the anode is being attacked, but for some reason I find the cathodes are more likely the source of the sediment. I haven't figured why this is the case, but there are several possible causes (to be determined later).

 

I'll write more later about the other observations...

 

WSM

 

Edit, As far as the high concentration of HCl, water is consumed by the process so replacing it with more diluted acid is okay in my opinion.

The hypochlorite, et cetera, formed as the cell runs accounts for the faint yellow color (I've seen the same thing in my cells). The color clarifying is another matter. It's quite likely you've over-shot the desired levels by using higher concentrations of additives, tus changing the chemistry to where it's not making what we want.

 

Try diluting the acid to 8% or 10% (and go light with the amounts added) and see if you can more accurately track the changes. Good luck.

 

WSM

Edited August 10, 2017 by WSM

[PeteyPyro]

I found that this Perchloric acid/Perchlorate article is interesting reading with some concepts that are commercially used in manufacturing.

 

It touches upon some information that we've already known to those pursuing chlorate/perchlorate cells, and some info that is new (at least to me).

[PeteyPyro]

Thanks. As soon as I figure out what's wrong and correct it, I'll post Part Fourteen.

The high read on your meter is strange. I wonder if using the wrong shunt might have damaged it somehow?

WSM

When I've needed an ammeter for reading a current (greater than the 0-10amp setting on one of my ammeters), I'd take 10, 0.1 ohm resistors and connect them all in parallel, then connect the assembly in series with the circuit to be measured, and then connect my 0-10 amp ammeter in series with one of the 0.1 ohm resistors. I would then multiply the reading on my 0-10 amp ammeter by 10, to get the true current total. The 10 resistors, assuming that they are identical, would divide the current into 10 equal paths of 1/10th of the current. By multiplying the measured current, through just one of them, by 10, I'd arrive at a true reading.... i.e. an 18 amp current into the cell would be divided equally among the 10 resistors, with 1/10th (1.8 easily measured amps) of the total current flowing through each resistor. Even my cheapie ($4) Harbour Freight multimeter can measure 1.8 amps (in this example). The value of the resistors doesn't matter too much as long as all 10 can handle the power... [power (in watts) = current (in amps) x current (in amps) x resistance (in ohms)]. The total resistance must also be low enough that it doesn't significantly affect the current (that's why I chose such a low resistance level of 0.1 ohms as the complete resistor array would only introduce 0.01 ohms of total resistance). If I needed to measure, let's say 50 amps for a bigger cell, I could use 25 of them, for example, and multiply the measured current in one resistor, by 25.... i.e. 2.0 amps, measured flowing through one of the 25 identical resistors, would indicate a true cell current of 2.0 x 25 or 50 amps total. Again, be sure that the resistance is low enough to ensure that current isn't adversely affected, and that the power rating of the resistor isn't exceeded. P=i*i*R. Or power (dissipated by the resistor) = i (the current flowing through the resistor) x i (current flowing through the resistor) x R (the resistance of the resistor in ohms). A 0.1 ohm resistor, with 2 amps flowing through it would be dissipating 0.4 watts of heat, so that a 1/2 watt rated resistor would do nicely. That value of resistor would also only drop the voltage, applied to the cell, by 0.2 volts. (e=i*r or voltage drop = current through the resistor x resistance in ohms)

[Arthur]

Yellow colour in the solution may possibly be (among other things!) chrome salts from stainless steel.

[WSM]

I found that this Perchloric acid/Perchlorate article is interesting reading with some concepts that are commercially used in manufacturing.

kirkperc.pdf

It touches upon some information that we've already known to those pursuing chlorate/perchlorate cells, and some info that is new (at least to me).

The Kirk-Othmer articles are excellent. I have copies of various editions and find them useful (mostly for reference purposes).

 

WSM

[WSM]

When I've needed an ammeter for reading a current (greater than the 0-10amp setting on one of my ammeters), I'd take 10, 0.1 ohm resistors and connect them all in parallel, then connect the assembly in series with the circuit to be measured, and then connect my 0-10 amp ammeter in series with one of the 0.1 ohm resistors. I would then multiply the reading on my 0-10 amp ammeter by 10, to get the true current total. The 10 resistors, assuming that they are identical, would divide the current into 10 equal paths of 1/10th of the current. By multiplying the measured current, through just one of them, by 10, I'd arrive at a true reading.... i.e. an 18 amp current into the cell would be divided equally among the 10 resistors, with 1/10th (1.8 easily measured amps) of the total current flowing through each resistor. Even my cheapie ($4) Harbour Freight multimeter can measure 1.8 amps (in this example). The value of the resistors doesn't matter too much as long as all 10 can handle the power... [power (in watts) = current (in amps) x current (in amps) x resistance (in ohms)]. The total resistance must also be low enough that it doesn't significantly affect the current (that's why I chose such a low resistance level of 0.1 ohms as the complete resistor array would only introduce 0.01 ohms of total resistance). If I needed to measure, let's say 50 amps for a bigger cell, I could use 25 of them, for example, and multiply the measured current in one resistor, by 25.... i.e. 2.0 amps, measured flowing through one of the 25 identical resistors, would indicate a true cell current of 2.0 x 25 or 50 amps total. Again, be sure that the resistance is low enough to ensure that current isn't adversely affected, and that the power rating of the resistor isn't exceeded. P=i*i*R. Or power (dissipated by the resistor) = i (the current flowing through the resistor) x i (current flowing through the resistor) x R (the resistance of the resistor in ohms). A 0.1 ohm resistor, with 2 amps flowing through it would be dissipating 0.4 watts of heat, so that a 1/2 watt rated resistor would do nicely. That value of resistor would also only drop the voltage, applied to the cell, by 0.2 volts. (e=i*r or voltage drop = current through the resistor x resistance in ohms)

Thanks for the suggestion of paralleling

high accuracy resisters for creating a shunt. I hadn't considered doing that but the reasoning seems sound.

 

WSM

[WSM]

Yellow colour in the solution may possibly be (among other things!) chrome salts from stainless steel.

Possibly, but usually chrome salts make strongly colored compounds. I suspect he's referring to the faint (clear) yellow color of hypochlorites, et cetera; often seen when a cell has run for a period of time.

 

WSM

Edited August 14, 2017 by WSM

[Mumbles]

There's a lot of things involved in a chlorate cell that can turn the solution sort of yellow. Any iron that might be dissolved will probably appear slightly yellow as well. In any case, it's really only a problem if it's interfering with the cell, or makes it into the final product. Chlorate cells aren't going to be pretty.

[taiwanluthiers]

Is this a sodium chlorate cell?

 

I find sodium chlorate cell liquor has a yellow-green color as it forms. Like bleach.

 

Potassium chlorate cells have this as well. I think hypochlorite just has that color.

 

I never bothered with ph control because I was just lazy and I ended up with more chlorate than I can use anyways (had to destroy them all when I moved to the US).

[eb666]

Lots of reading to be had here

 

https://geocitieschloratesite.000webhostapp.com/chlorate/further/bedtime.html

 

 

I am going to attempt to make an anode from a piece of Ti physically attached to a piece of Platinum. This method of attaching Pt and Ti have been shown to work by PDFBDQ (a poster here) quite some time ago. It will be held against the Ti using a bolt and the joint MUST be below the water line for to allow the current to jump the joint.

The piece of Pt will be a one gram 'bar' and can be purchases for around the price of Pt and not some inflated price like you have to pay for Pt wire etc. Only perk will be made as it is more sensible to make all chlorate using MMO or graphite imo.

The anode will be good for around 5 amps approx. A modest anode no doubt.

 

EB

[WSM]

Lots of reading to be had here

https://geocitieschloratesite.000webhostapp.com/chlorate/further/bedtime.html

I am going to attempt to make an anode from a piece of Ti physically attached to a piece of Platinum. This method of attaching Pt and Ti have been shown to work by PDFBDQ (a poster here) quite some time ago. It will be held against the Ti using a bolt and the joint MUST be below the water line for to allow the current to jump the joint.

The piece of Pt will be a one gram 'bar' and can be purchases for around the price of Pt and not some inflated price like you have to pay for Pt wire etc. Only perk will be made as it is more sensible to make all chlorate using MMO or graphite imo.

The anode will be good for around 5 amps approx. A modest anode no doubt.

EB

 

Excellent.

 

Are you working with sodium or potassium salts?

 

Let us know how it goes.

 

WSM

Edited August 15, 2017 by WSM