Sciencemadness Discussion Board

KCLO3 by way of H2O + KCL

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The_Davster - 4-1-2008 at 01:08

I came across a store that sells the single MMO electrodes, for those who have bought pool chlorinator electrodes, how do they compare in cost?
http://www.jumpinjackflashpyrosupplies.com/servlet/the-20/MM...

chloric1 - 4-1-2008 at 03:08

Thats why I want to sell if we get the coating just right. I mean that is like $5 worth of titanium.

Xenoid - 4-1-2008 at 05:26

Quote:
Originally posted by The_Davster
I came across a store that sells the single MMO electrodes, for those who have bought pool chlorinator electrodes, how do they compare in cost?


I think many people these days are buying MMO and platinised Ti electrodes for chlorate and perchlorate. Certainly those who are seriously into pyroechnics are, just check out the pyrotechnics sites.
As I pointed out in the ?perchlorate thread my platinised Ti anode has made over 3Kg of KClO4 so far and cost about $50.
My MMO chlorinator electrodes are performing extremely well and they cost...... nothing...:D
In Australia, chlorinator assemblies cost about A$200 - 300 new, for that you would get 5 - 7 electrodes, each with a surface area several times that quoted for the MMO anode you have found. I did come across somewhere that was selling individual electrodes, but I can't find it now, I think they were about A$80

http://www.directpoolsupplies.com.au/category9_1.htm

Click on the blue subcategories to see the variation in range!

I think commercially available anodes will become more common, whenever there is a niche market, someone will step in to fill it.

Of course this doesn't preclude one making one's own, I find it a challenge and an enjoyable pastime. Certainly if a coating can be found it will likely only cost a few cents, and the Ti will probably last a lifetime.

My current anode (Hubert) is doing very well at making KClO3 and the coating must have cost all of 10 cents... :o

Just like any field of human endeavour there will always be a range of options available to suit the individual, from buying chlorate and perchlorate directly or making the simplest and cheapest of anodes themselves.

jpsmith123 - 4-1-2008 at 05:40

Did you see the rest of their catalog here? I was wondering how long before somebody starts selling complete cells...now I know.

BTW, Xenoid, are you running your platinized titanium anode perchlorate cell in a "batch" type process (i.e., you go from high to low ClO3 concentration) or are you using a more-or-less "continuous" process?

[Edited on by jpsmith123]

tentacles - 4-1-2008 at 06:23

There is a legal problem with selling products made using techniques covered by patents. Much as I would like to see someone selling good perch anodes for a reasonable price, it does set a bad example. Noone is likely to complain, though, and at least some of these patents are past their expiry date.

[Edited on 4-1-2008 by tentacles]
edit: that said, I would probably still buy one if reasonably priced.

[Edited on 4-1-2008 by tentacles]

Aqua_Fortis_100% - 4-1-2008 at 07:44

Thanks Xenoid..
And is funny because before I tried , I was suspicious that this resistance method , as simple as I've pretended never will work.. I tried and this was pure true.. :(

But this is past and even if I was able to get a proper resistor, probably I would not be capable of get smooth current and therefore not be able to do proper calculations regarding current/mols of NaClO3 produced.

Quote:
Originally posted by Xenoid :
Yes, for you, the best thing is to solder directly to the remaining copper! You'll need a fairly heavy duty soldering iron. A lightweight electronic iron doesn't develop enough heat, well mine doesn't anyway. Put silicone grease on your connections, make sure no electrolyte gets on them...


Can I seal electrodes/lid joints with hot melt glue and after this put some silicone grease ? And can I replace silicone grease by hot-melt glue to seal wire/electrodes connections?

Thanks!

Xenoid - 4-1-2008 at 10:00

Quote:
Originally posted by Aqua_Fortis_100%
Can I seal electrodes/lid joints with hot melt glue and after this put some silicone grease ? And can I replace silicone grease by hot-melt glue to seal wire/electrodes connections?


Yes, seal everything with hot glue if you want...... but it will still corrode..... :(

Do you have a vent tube attached, for gasses and fumes. You'll need to be able to add water every few days.

@ jpsmith123

I ran the perchlorate in simple batch mode, I just did a rough calculation and ran it about 50% longer.

BTW when you get that chlorinator cell running, use KCl, you'll be able to watch KClO3 building up, and up, in the bottom of that big jar. I should have used a taller cell for Hubert because pretty soon I'm going to have to stop it and remove the KClO3.

@ tentacles

Why would there be any legal problems! The company has most probably got one of the Indian or Chinese anode manufacturers to make a batch of anodes to their own specification.

tentacles - 4-1-2008 at 12:01

xenoid: I mean if forum members are producing anodes for sale. That company may have had a batch made, but they don't look like anything used in industry, and the shape (tubes) makes me think they are made from some Ti scrap. It's still possible, though. But if he did go to the trouble of ordering a bunch of anodes from india (or whereever), why didn't he order some of those fabled long lasting industry LD anodes? Certainly the companies that make platinized and MMO anodes nearly always also make LD versions as well. (especially considering that MMO interface layers seem needed for Ti substrate LD)

[Edited on 4-1-2008 by tentacles]

Xenoid - 4-1-2008 at 12:31

@ tentacles

Sorry, I misunderstood what you were getting at!
I would imagine LDO anodes are just around the corner.

One problem with this widespread availability of cheap anodes, is that perhaps the "operation of a cell to manufacture hazardous oxidisers" will become illegal.... :o

There is not much point banning the sale of chlorates and perchlorates, if people can make their own at home, even cheaper.

Where will it end, a ban on the sale of NaCl and KCl .... :D

chloric1 - 4-1-2008 at 15:01

Quote:
Originally posted by Xenoid

Where will it end, a ban on the sale of NaCl and KCl .... :D


Yeh right! If they go that far then they would be better to rule themselves intrusive and fiscally inefficient! Refering to DHS, DEA or some other alphabet soup collection of pencil pushing bureumonkies.:D:D

10 litre chlorate cell

Xenoid - 26-3-2008 at 22:06

As a follow-up to my post a few months ago, earlier in this thread (see page 7), on the construction of a 10 litre NaClO3 cell using gouging rods, I offer this footnote. It's been sitting on my computer for months so I thought I better post it, in case someone is buiding a cell based on this design.

The calculated run-tme for my 10 litre "Big Bertha" chlorate cell (see earlier post) was about 21 days (at about 3.2 - 3.5 volts and 24 - 25 amps). However, I was planning on letting the cell run for several more days until the gouging rod anodes were fully consumed. However, on the 22nd day the cell died. The cell was remarkably trouble free, only requiring a top up with water every few days. The cell was completely odourless and gas tight, and only slight corrosion occurred over the three weeks of running (Image 1.). A little green corrosion product developed on the copper plate, just above the cable gland on several electrodes, this did not effect the electrical characteristics at all.

When the electrode assembly was removed, there was no evidence of cathode corrosion (Image 2.). The new "L" shaped cathode connection rods can be seen. These are made from threaded rod, and covered with black heat-shrink tubing (this is now grey due to the bleaching effect of the cell).

The cable glands on the underside of the lid (Image 3.) were quite badly bleached. These are described as "UL Approved NYLON 94V-2", however a flakey, bleached layer had formed. The glands should, however, be good for several more runs, as the effect is shallow.

When the cell liquor was poured off, the reason for the shortened run-time became obvious. At the bottom of the container, remnant lengths of all 12 anodes were found (Image 4.). All the rods had worn through at a point level with the top of the annular SS cathode, clearly this was a region of extra high current density. A rough estimate is that 25% of the rods were not consumed. This had happened on some of my smaller cells, and I had modified the annular cathodes into a slightly conical shape, with good effect. I did not however, feel it was necessary on this larger cell because the cathode was quite low slung and I assumed the anodes would erode from the bottom up.

I plan to refurbish "Big Bertha", fit new gouging rods and get it up and running again. The only real modification to the design will be to cut some slots in the SS cathode, so it can be bent closer to the bottom of the anodes, this should result in the anodes (gouging rods) corroding from the bottom up, and thus lasting longer.

After pressure filtering to remove the black carbon detritus, about 3.2 Kg of moist NaClO3 crystals were obtained fairly easily, using a series of concentration, precipitated NaCl removal, and crystallisation steps.

[Edited on 26-3-2008 by Xenoid]

BigBertha.jpg - 86kB

dann2 - 27-3-2008 at 16:28

Hello,

Looking at the picture it would appear that the anodes have wore, and broke, at the top of the liquid as opposed to level with the top of the Cathode?

Dann2

Xenoid - 27-3-2008 at 17:02

Hi Dann2

No, they wore through at the level of the top of the cathode. The remaining stubs which would have been about 7-8 cm long, continued to wear up to the liquid level, leaving the 1-2 cm stubs visible in the image. The longest of the broken-off rods exactly match the height of the cathode. Bit of a bugger, really, as the cell would have produced about 4 Kg of chlorate if it had run for, say, 28 days.

It was a real pleasure to run this cell, no trouble at all. I think I'll tweak the design and run it again, just for the hell of it. Not that I need another 4 Kg of chlorate.... :D

Xenoid - 27-3-2008 at 17:48

Here's a bit more "guff" I put together a while back, on the running of the cell .....

One advantage of running a large chlorate cell, is the ease with which large amounts of NaClO3 can be obtained. This may seem obvious, but really, for a little more work than is required for, say, a 1 litre cell, a 10 litre cell can be processed. With a 1litre cell only 1 or 2 crystallisation steps are worth performing, since the "law of diminishing returns" comes into play, but with a larger cell several hundred grams are recovered with each step. Three or four concentration, and crystallisation steps can be profitably carried out!

The 10 litre cell ran for a total of 12672 Amp hours, and the overall efficiency, based on say 3.2 Kg of NaClO3 produced, was 38.2%.

The consumable cost was about $4.50 for gouging rods, $1.80 for salt, about $7.50 for electricity and $3.50 for gas used during the "boiling down" and concentration phases. So about $5.80 per Kg.

Oh! I forgot my labour, say 10 hours at $50 per hour, that's $500 so really more like $173 per Kg.
No, really it was a "labour of love" so I don't include that!

The attached image shows a pyrex bowl (30 cm diameter) containing 3.22 Kg of moist, crude NaClO3 from the 10 litre "Big Bertha" cell, the jar on the left contains, precipitated salt, ready for recycling, and the jar on the right is the remaining "mother liquor" (about 1.2 litres) still saturated with NaCl and NaClO3

ChlorateBB.jpg - 17kB

dann2 - 27-3-2008 at 19:12

Hello,

Is guff = waffle??? :D

Here's some more Whoredom (as suggested in 'forum matters') :cool:

Graphite is inclined to get a bit of a bashing from the BYCM* (or indeed the FYCM) when it comes to making Chlorate. It is a good way to go. Perhaps a lot of the bashing stems from using it in cells with far too low Chloride conc => lots of erosion.
The more I think about it, the more I think it would be worth the bother of pH controlling a (big, as you suggest) Graphite cell.
The amount of Graphite that gets worn in industry for a quantity of Chlorate is small.
8 to 30 grams per kg Chlorate made, I have read.
I wild-ass-guessed the Graphite in your cell is 255 cubic cm. Subtract 10% to allow for bits at top etc gives 230cm cubed. Thats approx. 230 x 2 = 460 grams Graphite. (assum G density 2g/cm cubed). That lot should make (or would make in industry) 460/30= 15 kg Chlorate in pH controlled cell. Less mess per kg Chlorate to clean up too.
I am assuming pH control will give less erosion.
Froggots page goes into Graphite erosion.
http://www.frogfot.com/synthesis/chlorateel.html#anodes
quote;
Graphite anode corrosion rate also increases with decreased concentration of NaCl in the electrolyte. As example, at NaCl concentration of 200 g/l the corrosion is 2 times lower than at 120 g/l. It is therefore advised to never run cell to completion, in the end of electrolysis the electrolyte should contain at least 10 %-w/v NaCl.
end quote

If pH control is realizable with a bag/drip it would be worth the bother IMHO. Syringe pumps are great for experimenting with but probably too much cash outlay for the average Chlorate maker, especially if a bag/drip yoke will do the job.

Dann2



*Back Yard Chlorate Maker

Xenoid - 27-3-2008 at 20:33

Hi Dann2

Hmmm.. perhaps I shouldn't have used "guff", I just looked it up in the dictionary; "empty or foolish talk; humbug; nonsense"

Dann2, I don't think you can compare graphite and gouging rod erosion rates.

When I first started making chlorate cells, I used genuine graphite anodes "electrode quality". They were 12" x 1/2" rods. One of my first cells used 4 x 6" lengths of these. I ran the cell at about 8 amps for about 2 - 3 weeks, when the cell failed. When I dismantled it, I found it had been running on only one of the four rods for virtually all the time, because a non-conducting layer had formed underneath the electrical "clamp" connections of the other rods. So, really, the high quality graphite performed very well! These rods were only a few US$ each from the "graphite shop", I have never ordered anymore because the freight charges quadrupled the cost. Tim's (12AX7) graphite chlorate cell seemed to run for a long time as well.

Gouging rods are just rubbish in comparison, they are coarse grained and mine even have longitudinal cracks in them!

If the 10 litre cell had used the "genuine" graphite rods, I think they would only have been about 25% eroded at the end of a month.

If the 12 gouging rods only cost about $5 and I can get them to last a month, I don't think it's even worth messing with pH control of any type. I didn't even add any "additives" like dichromate etc.

chloric1 - 28-3-2008 at 03:12

At $50 per hour you are expensive Xenoid:D:P. Yeh not using dichromate does seem like a good idea. Not having to add barium chloride and worry about barium ions in your final product. It did seem to remember that after filtering the chlorate liquor after adding BaCl2 the excess Ba++ deposited when boiling down before the NaCl dropped.

dann2 - 7-4-2008 at 13:28

Hello,


@Markgollom: I just wanted to ask what type of MMO/DSA anodes have you got. What was there original application etc.

About high temperatures in Chlorate cells, it is my opinion that there is no advantage in having warm/hot cells (75C say) in the non pH controlled cell as there is not going to be any reactions going on in the bulk of the solution. This is were Chlorate is made in Industrial set up's. In our non pH controlled cells it all happens at the anode surface.
If you cells go to that temperature on their own I suppose it is not going to do any actual harm, with DSA anyways.
It is a challange to seals etc though, as you stated.
DSA may get damaged in hot cells when the pH is allowed to go up to 9 or 10 (wild assed guess/speculation BTW)
Perhaps you plan to pH controll, in that case it is a big advantage to run hot. Lots (most) of Chlorate formed in the bulk of the cell.

Dann2

Aqua_Fortis_100% - 7-4-2008 at 14:39

Hello Xenoid, nice pics and results!


My small cell (~1,9 L) was running a very long time (~ 605 h... ~ 1938,4 Ah ) , with dichromate added and large excess of chloride (I started with 590g NaCl and then added during the whole procedure more 130g) and even so the gouging rods not survived! .. The rods are very similair to your ones, but still more physically damaged! Most of it breaked during the electrolyses. I recognized damage to rods due to the almost abrupt decreasing current measured by multimeter..

I'm thinking that this result was because my anodes were not surrounded by any cathode.. Just the opposite , nickel cathodes on centre and anodes sorrounding it (I did this since at the construction the only thing I have at hand to cathodes were some Ni rods).
A lesson was learned , in the worst way :(

If my math in running formula is correct I'm inclined to think that the most affecting parameters in amateur cell (using gouging rods anodes and non controled pH setup) are not only (most) chloride ions and temperature, but also cell geometry(anodes positions and spacing,etc) and another details in cell construction..

It was a pain in the butt to filtrate the cell liquor, since was full of very small graphite particles.. But I've done it and have a yellow/orange liquor..

The next step will be add KCl and try to see how much was converted..

Sciocrat - 11-4-2008 at 09:56

I'm having a problem with my cells. I made two chlorate cells, almost exactly as described here. I am running them on 9 volts and 3 amperes, the cells are connected in series as this picture shows. The problem is that the reaction occurs only in one of my cells (intensive gas formation), while there is no noticeable reaction in the second cell. I would appreciate any advice or ideas you have regarding this problem.

ps. I noticed later, that the electrolyte in the cell where there was no gas formation, turned dark green, and there are dark particles floating in the liquid.

Here is a pic of my cells


[Edited on 11-4-2008 by Sciocrat]

cells.jpg - 42kB

Sciocrat - 11-4-2008 at 11:28

This is the result after a few minutes...

cells2.jpg - 41kB

Xenoid - 11-4-2008 at 12:43

Nice work Sciocrat ...

I would say the problem is due to slight differences in the electrode geometry of the two cells. The one on the left (greenish, no bubbles) may have short circuited or be of such low resistance that it requires less than about 2.5 - 3 volts for the 3 amps to flow.

What is the voltage across each cell, if they are being supplied from a 9 volt source, you should have 4.5 across each cell.

Can you check each cell separately, with say, a 3.5 volt source and see what happens!

markgollum - 11-4-2008 at 16:08

@ dann2
In reply to your question, I don't know for certain what the MMO anode I have is specifically designed for,
I strongly suspect that it was purpose-made for chlorate production. I bought it from the fellow that runs the online store at the top of the page (Jumping Jack).
As for temperature, it seems to me that the rate of chlorine loss drops off at the higher temperatures.
But the main reason that the temp gets hot is that I am running 14-18 A at 3.8-3.9 volts through a 4.3L cell.
I don't think that the erosion rates of MMO anodes will increase much at very high pH since some of the literature I have read mentions MMO anodes used in the chlor-alkali industry. (They use a divided cell but I am under the impression that, in practice, the anolyte gets quite basic)
On that note I am thinking about making a chlorine cell, this could be a convenient way to generate a constant stream of cheap chlorine over a prolonged period (for the slower photochemical chlorinations).

Edit:

To Sciocrat
I am certain that you have a short in the non-bubbling cell.
The voltage drop across a conducting electrochemical cell is irrelevant as far as weather or not there is an electrochemical reaction going on.

[Edited on by markgollum]

dann2 - 11-4-2008 at 17:46

Hello Sciocrat,


As other have said, I would be inclined to blame a short circuit. What are the lids made from (metal)?. Have you used O rings to insulate the anodes and cathodes from the lids. Short circuit may be there.

Dann2

Aqua_Fortis_100% - 11-4-2008 at 19:44

@ Sciocrat ,

Very good job you did.. Next times which you make new cells you can follow Xenoid's advise (in this thread, IIRC) for keeping at least some of the original copper layer on gouging rods to make the connections, this will reduce the electrical resistance across the connection points. I also agree with the (per)chlorate guys ; short circuit is what you have in your cell.. This ocurred with my cell some time ago, while I tried to put a aluminium foil around the exposed parts of the graphite anodes ; some of the foil touched the cathode and the cell did not worked.. This is easily perceptible since in the short circuit area a good amount of heat will be generated by joule effect.

This is why I would prefer clean and transparent cell bodies than PVC pipes or such, since you can look instantaneously if some problem is ocurring, like the eletrodes not generating gases.

@ Dann2,

I did what you've said.. I extracted the KClO3 from the liquor using KCl solution rather than solid KCl in boiling liquor.

I'm now recrystallising the KClO3.. A very nice and pleasant thing.. Nice snow like crystals being obtained :D:D:D

My yield based on crude KClO3 from the liquor was more than 56%.. More since I didnt boiled the residual liquor and cooled to get more chlorate. I was using Na2Cr2O7 additive..

Also, honestly , besides agreeing which pH control really appear to help greatly retarding the corrosion of the graphite anodes, I dont think pH control really worth.. Gouging rods are cheap and one will loose quickly the patience bothering with pH control all day .. Well, maybe may worth, if you have time and patience to experiment.. At least 2-3 times adding HCl to the liquor and computing Cl- , H+ ions...
It would be great if this could be automatized in amateur setup.. Lots of time and patience saved..



[Edited on 12-4-2008 by Aqua_Fortis_100%]

Xenoid - 11-4-2008 at 20:52

Incidently - I'm not sure if I've mentioned this before, but a good way of mounting gouging rods in thin metal or plastic lids is to use rubber grommets. I used these on a lot of my early cells, before using the screw together cable glands. They last quite well, seal well (with a little silicone grease) and support the rod as well as electrically insulating it from a metal lid.

They come in a range of sizes (make sure they are a really tight, stretchy fit on the rod. The hole in the lid should be about 2mm larger than the diameter of the rod. Fit them in the hole first and then force the rod through with a little silicone grease.

They are available from electronic parts suppliers, automotive shops and engineering suppliers. They are normally used where electrical wires are passed through thin sheet metal, to protect the wires from cutting on the edge of the hole.

Grommets.jpg - 9kB

Sciocrat - 12-4-2008 at 14:03

Tnx for your fast replies. You were right, there was a short circuit. The lid is made of metal, and it wasn't properly insulated from the screws that connect to the cathode. I applied some electrical rubber tape on the part of the screw that was in contact with the lid, and now it works just fine. The cells have been working for 4 hours and so far, everything is fine. I hope it will remain that way untill the reaction is finished :)

Pulverulescent - 13-4-2008 at 12:24

Sciocrat, metal lids and spacers will corrode fairly quickly under operating conditions.
This corrosion will badly contaminate your electrolyte, making isolation of the product (NaCl03) very difficult.

If you replace them with plastic or rubber components electrolysis will proceed smoothly apart from some disintgration of graphite anodes.
NaCl is the preferred salt for chlorate production; potassium chlorate is obtained by metathesis.

If you use KCl, chlorate will precipitate after some hours of electrolysis once the solution cools; KCl03 is far less soluble than NaCl03 but the sodium salt works slightly better and causes less damage to carbon anodes.

The downside is---you'll have to wait longer for NaCl03 to precipitate, because of NaCl03's high solubility.

P

dann2 - 13-4-2008 at 15:07

Hello,

A big down side to K salt when using Graphite anodes is that the Graphite sludge is difficult to remove from K salt. You usually end up filtering hot solutions to keep K Chlorate in solution. Use Na and you can filter cold. Using DSA, MnO2 this is not a problem as you can take solid K Chlorate and use directly as no cleaning up necessary.
Perhaps it is OK to use black K Chlorate (Graphite contamination) in Pyro stuff anyways?

Dann2

12AX7 - 13-4-2008 at 19:30

Quote:
Originally posted by Pulverulescent
NaCl03


Subtle error: it's not spelled with a zero.

Tim

Pulverulescent - 14-4-2008 at 02:53

What difference does it make? It's still a cyclo-form!

P

Aqua_Fortis_100% - 15-4-2008 at 17:13

Hello guys,

Dried my chlorate today... The results were much worse I'd imagined.. Probably the water content of the crude product blinded me :(

After two recrystalisations and drying, the weight was around 360g which is a crap yield (about 25%.. Considering the chlorate dissolved in all liquors it would rise only to about 35-36%, at best), this liquor using Na2Cr2O7 :mad:

Why people claim that 50% efficience is easy to get? I dont remember seeing a person that reached that with gouging rod and no controled pH setup.
Even Tim website states crap yield for Na/K chlorate..

Well.. Anyway I'm happy, since is my first chlorate bath..

Hope better yields in next batches..

Pyrotechnics world, I'm here!!!!

[Edited on 15-4-2008 by Aqua_Fortis_100%]

12AX7 - 15-4-2008 at 20:32

How large a cathode did you use?

Aqua_Fortis_100% - 16-4-2008 at 05:48

Very small infact...

I've used 7 small Ni rods, since was the only good material I'd at the time...
Now I see that was a great mistake (anodes around cathodes!) and IMHO certainly this was the most relevant thing to my anodes anodes premature death :( Uneven distribution of current on surface of graphite rods..

Next time I will use better things as cathode..

thanks

Sciocrat - 10-5-2008 at 04:43

One question - On a few sites I noticed that scientists/engineers(?) named Foerster and Mueller described the conversion of chloride to chlorate by eletrolysis, but I can't find any more useful information about them. I would be thankful if someone mentioned something related to them, or recommended sites where the info could be found. I'm writing a paper about potassium chlorate synthesis, and have been told to provide more info about these individuals...

Tnx in advance...

Foerster and Mueller

phlogiston - 10-5-2008 at 06:38

They published their observations in the first decades of the last century, say 1900-1930.

Use google. For instance, using 'Foerster Mueller chlorate' as the search string, this yields some relevant literature, for instance this link:

http://www.rsc.org/publishing/journals/article.asp?doi=ca900...

Click on 'pdf' to get the free full-text article, which contains a bit of literature, from the year 1900, by Foerster and Muller themselves about chlorate formation.

The very first hit using Google is:

Landolt D et al, Anodic chlorate formation on platinized titanium, J. Applied Electrochem (1971) 2:201-210

which is more recent and elaborates quite a bit about certain details/hypothesis of Foerster and Muller.

Other relevant references:

Z. Elektrochemie (1903) 9:195
Z. Elektrochemie (1902) 8:515

However, you will need access to a pretty good university library to access them due to their age, and (as a lot of chemistry literature from that era), they are written in German.

dann2 - 19-6-2008 at 10:59

Hello,

Has anyone here ever purchased one of these (or one like it) for making (Per)Chlorate.

http://www.pyrosecrets.com/chloratecellplans.html

Do they make the Perchlorate my heating the Chlorate?
What's the story with the DSA Anode instructions?

Perhaps I could try the references section...........:P

Dann2

Armistice19 - 7-5-2009 at 12:27

Don't waste your time with that stuff, there is plenty of information in this forum, all over the internet, and at your local library about preparation of chlorate and perchlorate. Just do some hearty reading and make sure to double check all your sources.

Xenoid - 7-5-2009 at 12:48

Quote: Originally posted by Armistice19  
Don't waste your time with that stuff, there is plenty of information in this forum, all over the internet, and at your local library about preparation of chlorate and perchlorate. Just do some hearty reading and make sure to double check all your sources.


LOL... Good one, Armistice19. Are you aware that Dann2 is responsible for most of the infomation on amateur chlorate and perchlorate production both on this forum and also the internet..... :)

Formatik - 7-5-2009 at 12:58

Speaking of which, Geocities is killing all of their webpages later this year: http://help.yahoo.com/l/us/yahoo/geocities/geocities-05.html So enjoy dann2's website while you can.

dann2 - 10-5-2009 at 18:03

Quote: Originally posted by Formatik  
Speaking of which, Geocities is killing all of their webpages later this year: http://help.yahoo.com/l/us/yahoo/geocities/geocities-05.html So enjoy dann2's website while you can.


Yes indeed the peep show is coming to a close.
Ladies and Gentlemen, time please, time please, order you last drinks and get you final peeps and finish up............

I would not mind getting a peep at those 'instructions' for Chlorate and Perchlorate making.
@Armistice19 Did you actually get your eyeballs onto the instructions or are you assuming they are just a repeat of alot of the stuff that is already known?
Cheers,
Dann2

uchiacon - 3-7-2009 at 21:32

Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense :mad: ), and there was this great thread on chlorate production which had loads of details. Now its lost to the net I must relocate to a alternative thread.

Ok, so I think I'm going to be making mainly chlorate(I dont see myself making proper fireworks anytime soon using perchlorate, but it'd be nice to have)
and I have two options.
Platium plated niobium mesh(Pt coating of 2.54microns thick and $5USD per square inch). Suitable for perchlorate, but if misused will lose Pt coating, and Pt has a high resistance to current.
OR
MMO coated Titanium anodes. Cheaper than Pt but unable to be used for perchlorate and has less resistance to current than Pt. Heres all the details www.anometproducts.com//App_Themes/anometproducts/PtCladNb_M...

So what do you guys think? Which one would be better for a person slightly less experienced in chlorate production?
Cheers
Oh, and if anyone has the pyrosecrets instruction manual on the chlorate production I'd love to download it!

[Edited on 04-07-09 by uchiacon]

[Edited on 04-07-09 by uchiacon]

hissingnoise - 4-7-2009 at 06:51

Quote: Originally posted by uchiacon  
Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense :mad: ),

The DoD?---Yeah, right!
Mega's probably sorting out RS's problem right now and the site'll be back anytime now. . .
Everything anyone needs to know about chlorates and perchlorates is contained in threads like this one---all you have to do is read a few posts!

JohnWW - 4-7-2009 at 08:49

Quote: Originally posted by uchiacon  
Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense), and there was this great thread on chlorate production which had loads of details. Now its lost to the net I must relocate to a alternative thread.
Have you actually heard from Megalomania personally? What is his email address now? Did he tell you that the U$ DOD removed roguesci.org, and WHY did they do it? Does he have an up-to-date backup of it, and does he plan to move it to a hosting server outside the U$A?

uchiacon - 4-7-2009 at 15:12

Well guys, the fact remains the roguesci is down, and Idefense(a US internet censorship agency working for US DoD) has closed them down before. If you google "what happened to roguesci" you should come across the email sent to users in 2004 when it last went down.

Anyway, can I get some opinions here about what I should buy?
Pt plated niobium mesh or MMO mesh? Details are in my post further up.

And no, the information I need is regarding Pt mesh and MMO mesh for use as anodes, how indestructable they are, what is the max current and voltage they can take and what levels does chloride have to get down to before they start to erode.

[Edited on 04-07-09 by uchiacon]

hissingnoise - 5-7-2009 at 04:08

I'd go for lead dioxide anodes if I wanted perchlorates and graphite gouging rods for chlorates, but I found long ago that not all gouging rods are equal. . .
Producing perfect LDAs is by all accounts an art but they're now used commercially for perchlorates.
They can go from chloide to perchlorate in one go and this makes them convenient.
As for RS, a suspension implies reinstatement at some point, so I expect to see the site back sometime. . .not that I had a great interest in it at any time.

uchiacon - 6-7-2009 at 00:13

Choices are for Pt anode
www.anometproducts.com//App_Themes/anometproducts/PtCladNb_M... @ $5USD a square inch.
Or
MMO pool chlorinator - www.directpoolsupplies.com.au/prod733.htm

So I might be making a small amount of perchlorate in the futute, it'd be nice to have that option open. But is Pt still as good as MMO in a chlorate cell?
I'm still unsure on this, can somebody just point me in the right direction?(scroll up for original post.)

Cheers

uchiacon - 7-7-2009 at 19:00

Oh, yeah and I was just wondering if I have the process running correctly... should the electrolyte be black with graphite? I switched from art pencils(pretty shit at conducting the current, and they blister quickly) to hard graphite electrodes from a 6v battery. So the electrolyte had a faint yellowish tinge to it from the day or so that the art pencil was in. Want a better anode guys, give me some opinions!

And the second picture is after about 2-3 days on 5v, 30a current. Very, very racially sensitive.
Considering all that though, at the amount of graphite in the water would you suspect that perchlorate is starting to be made? There is so much of it, and I have no way to test if chloride levels are low lol, and I haven't bought my KCl yet. Which I will have soon.

[Edited on 04-07-09 by uchiacon]

[Edited on 04-07-09 by uchiacon]
For some reason cant post pictures...just imagine a very very well tanned picture of a very dark electrolyte. Graphite dark.

[Edited on 04-07-09 by uchiacon]

12AX7 - 8-7-2009 at 04:06

Graphite never makes perchlorate. Graphite should come off, but not as much as you are evidently seeing. Try 5A on that anode.

Tim

hissingnoise - 8-7-2009 at 06:11

Tim, using chloride-free NaClO3, graphite *will* make perchlorate, but anodic erosion will be runaway and the rate of perchlorate production will be tiny. . .
And using compressed carbon sticks from batteries seems a waste of time, since they're usually made from compressed amorphous carbon.

uchiacon - 8-7-2009 at 15:36

So, should I just get the Pt anode for chlorate and perchlorate?
Can't find a MMO anode that isn't too small or too expensive...

hissingnoise - 9-7-2009 at 11:32

That's a question you'll have to answer yourself, IMO, but try to get *all* the facts first. . .
To start with, you could check out prior threads on perchlorates and the various anodes used by others!
IIRC, there's an old, good long thread on PbO2 anodes that might help; UTFSE!

uchiacon - 9-7-2009 at 16:22

Except for the fact I don't have the chemicals to make a lead dioxide anode and dont want to have to deal with lead compounds. They are nasty. I got about 20 pages(for about 2 hours) through that thread before it went on a tangent of shit that didn't concern me.

Don't try and tell me to UTFSE, the info(Pt vs MMO) isn't there. UTFBrain nextime.

hissingnoise - 10-7-2009 at 06:01

Uchiacon, the "F" in UTFSE stands for forum, not fucking---you can unknot your knickers. . .
No route to perchlorate is hassle-free but lead dioxide is a cheap and effective method which requires reagents, thought and effort.
Failing that, you *can* buy NH4ClO4. . .

uchiacon - 10-7-2009 at 13:48

You are completely missing what I'm wanting to do here...
I just want an opinion of whether I should buy Pt or MMO(and try to make PbO2 anodes for chlorate) for moderate chlorate and light perchlorate production lol.

hissingnoise - 10-7-2009 at 14:05

I'd go for Pt/Ir alloy; expensive wire but virtually trouble-free---Pt-plate has a habit of eroding in amateur cells and the rest disintegrate to varying degrees over time.
The last time I wanted perchlorate I ordered NaClO4 from a local pharmacist; I had it in three days but it wasn't exactly cheap. . .
It probably depends on your level of commitment!

watson.fawkes - 10-7-2009 at 14:31

Quote: Originally posted by hissingnoise  
the "F" in UTFSE stands for forum, not fucking
News to me. No, really. And the way it seems to be intoned (albeit in text form), it seems to practically mean the latter almost always.

uchiacon - 11-7-2009 at 00:15

So just get an MMO/Ti setup for chlorate off ebay and some Pt/Ir wire for perchlorate ?

Something like http://cgi.ebay.com/Platinum-Iridium-20-002-wire-x-5-Five-Fe...

and just coil it around a cathode for perchlorate?

hissingnoise - 11-7-2009 at 04:56

That wire is verrry thin uchiacon--- .002" is about .05mm. . .
The electrical conductivity of Pt/Ir is only moderate and a strand of this wire would be subject to unacceptable resistive heating at even low-amperage currents.
The minimum "convenient" thickness, I'd say, would be around .5mm.
If you were to purchase this wire, you would need to form your anode as a ribbon, comprising many strands, each of which would need a secure electrical connection.
It's doable but fiddly---if you were adventurous you could perhaps weave the wire into the form of a mat, effecting a connection by thick copper or brass strips holding the anode in a vise-type arrangement. . .
Do not use *ferrous metals* in the connections as iron can quite easily contaminate platinum surfaces.
It's also well to remember that along with adding corrosion resistance, iridium hardens platinum, making it somewhat brittle. . .


[Edited on 11-7-2009 by hissingnoise]

chloric1 - 11-7-2009 at 10:08

Some areas, ammonium perchlorate is still available. An equal mix of nitric and hydrochloric acid will convert this to perchloric acid on evaporation. Heating AP with alkali and alkaline carbonated furnished ANHYDROUS perchlorates!

Believe it or not, the chlorine in the acid mix is not responsible for the destruction of ammonium, its the nitrous acid! That is why you use equal portions of HNO3 and HCl instead of the normal aqua regia methods.

uchiacon - 11-7-2009 at 16:00

This is the Pt mesh I'll be buying for chlorate and perchlorate synthesis. I cant be fucked buying different anodes. The Pt plating is 2.54 microns thick, and I'm getting 20 square inches of it for $100USD. There'll be 2 seperate Pt anodes for chlorate and perchlorate.
www.anometproducts.com//App_Themes/anometproducts/PtCladNb_M...

Comments?

[Edited on 04-07-09 by uchiacon]

hissingnoise - 12-7-2009 at 04:17

It probably comes down to personal preferences, but I'd stick with graphite for chlorate. . .
In my day, I used gouging rods but found that there were two grades of gouging rod.
One type disintegrated quickly producing a black electrolyte which when allowed to settle left a foggy white viscous solution---I assumed the anode had been made from graphitic powder compressed with some kind of water-soluble polymer.
The other type eroded slowly even at high temperature and on settling left a clear solution.
Chlorate was isolated by decantation and evaporation; I used two cells with the one anode/cathode arrangement.

I'd use the platinised anode only where it's essential. . .


[Edited on 12-7-2009 by hissingnoise]

appetsbud - 21-7-2009 at 09:44

just a quick question that im sure has been answered before but is long since buried in the sciencemadness vaults, as im sure someone will be able to answer this painlessly.

im just wondering what the safety issues are with the electricity. i plan on doing the electrolysis with a 4amp power supply (old laptop charger) with something like 10V .

obviously im not planning on touching the naked wires whilst running, but i was just interested about the potential danger... death? wikipedia tells me that 100mA can kill, which is substantially less than my 4A, making it seem pretty clear.

i just wanted to get a heads up from others who have done this in the past and precautions, if any regarding the power, that are needed to be taken. just a simple 'stay well back when running and turn off the power supply with a broomstick before approaching', or more?

just before anyone thinks to concern themselves with enlightening me to the chemical dangers im fairly confident in that area, practical electro-chemistry is a little new to me.

hissingnoise - 21-7-2009 at 11:59

Quote: Originally posted by appetsbud  
Im just wondering what the safety issues are with the electricity. i plan on doing the electrolysis with a 4amp power supply (old laptop charger) with something like 10V .obviously im not planning on touching the naked wires whilst running, but i was just interested about the potential danger... death? wikipedia tells me that 100mA can kill, which is substantially less than my 4A, making it seem pretty clear.
just a simple 'stay well back when running and turn off the power supply with a broomstick before approaching', or more?

OK, I've got my composure back!
Thanks appetsbud; I think I can say without the slightest fear of contradiction that 4A @ 10V won't kill you!
With DC you can grasp both bare wires tightly and not know they're actually carrying current.
The voltage would need to be quite a bit higher to cause noticable shock.
How much higher is a good question but below 30V there's little to worry about.
Mains voltage here is 220V and that voltage can be dangerous.
The combination of high current and voltage is very dangerous.
It's probably better not to touch any bare wires anyway but the real voltage will be in the primary windings if they're mains-fed.
(It was the broomstick bit that caused me to pepper my keyboard and screen with explosively expelled hamburger). . .
Now for the cleanup!

[Edited on 21-7-2009 by hissingnoise]

appetsbud - 22-7-2009 at 02:00

luckily for me you managed to edit your post before i could witness the horrific flaming (i presume) that mine instigated ...

yeah, sorry about the broomstick thing, it was meant to be a bit tongue in cheek. i was trying to exemplify my lack of knowledge about electrical safety by alluding back to the videos you (or at least i) got shown in lower school years about the 'horrors of electricity' or whatever... im sure you'll appreciate my over cautious approach was probably the most fitting given my lack of knowledge on the subject, and the veil of mystique that seems to enshroud the subject somewhat.

thanks for clearing that up, i dont really have many people i can ask directly, and the only ones that seemed to have answers were people who knew as little as me but weren't afraid to relentlessly advocate their presumptions.

just managed to get some beautiful bubbles sprouting from my electrodes this morning after a little tinkering with my spatterings of physics knowhow, just have to get a vent hole with tube and drop a flea in and i should be good to go.

hissingnoise - 22-7-2009 at 03:10

Quote: Originally posted by appetsbud  
luckily for me you managed to edit your post before i could witness the horrific flaming (i presume) that mine instigated ...

Indeed appetsbud, the unfortunate members who did witness it are now receiving counselling and will bear the scars. . .etc..
Trying to be serious---the broomstick bit conjured a slapstick image which hit the funny-bone, with laughter being the spice of life.
BTW, your electrolyte won't need stirring if the cathode reaches close to the bottom of the cell---hydrogen evolution will provide enough circulation by itself. . .

densest - 26-9-2009 at 18:25

I hate to deflate the levity here.... but.... there's a reason that ground fault circuit interrupters trigger (depending on the local laws) at 5 mA or so: 50 mA through the heart region can kill. Once past the insulating skin, the interior resistance of the human body ranges from 10 to 1000 ohms. In the unfortunate event that one has a cut or one's hands are wet with a salt solution, it doesn't take a high voltage to kill if the current passes across the chest (head to feet, hand to feet if you're unlucky, hand to hand). Anything over about 12 volts can be bad if you're really unlucky. AC at 50 Hz is especially bad because it's close to the ideal frequency to disrupt the pacemaker centers in the heart to cause fibrillation which is often fatal.

So - many of us have survived shocks from the mains or high powered electrical or electronic apparatus. That doesn't mean that one should be careless if one has water and electricity in the same place. Insulating (rubber, plastic, etc) shoes (a 1Meg grounding conductor to prevent sparks is not a hazard), and keep one hand in your pocket while fiddling with any electrodes which are supplied from a non-current-limited source. Insulating gloves (not leather, plastic or rubber instead) can help, but if they have holes (sharp wires etc.) they are not effective.

In dry conditions without wounds you can get away with touching many high powered things. Chemistry often involves salt solutions which are highly conductive and which will render your skin conductive. Pure water (11 Megohm, for instance) can be used as an insulator... but that's no fun :)
Under 12V it takes an incredible run of bad luck and ignorance to hurt yourself. Under 24V it's quite difficult but possible. SELV (safety extremely low voltage) stops at 48VAC and current limiting is required to qualify as "safe". So anything involving a computer PSU, wall wart power supplies, etc. is usually safe if you keep your hands dry.

I do know of an incident with 5VDC in which someone wore a gold wedding ring while working on live equipment. It shorted power to ground (250 A or more) and got red hot. Very bad burns! So current limiting on any experimental supply is a good idea.

New safety regulations in the US require protection against molten metal splatter from accidental shorts while working on mains feeds capable of serious high currents (1000 A or more at a guess).

I witnessed an incident in which a very experienced technician dropped a screw inside a high power (KW+) computer power supply. A transistor melted with sufficient violence that a molten metal ball shot through the transistor case, through the computer case, and buried itself halfway through a 1/2 inch plate glass window. There were about 6 people in the same room - we were all lucky not to be in the trajectory!

Anyway, power limited supplies are the norm for easily available apparatus (except for microwave oven transformers) and are quite useful for a lot of work.




[Edited on 27-9-2009 by densest]

UnintentionalChaos - 26-9-2009 at 18:49

Quote: Originally posted by densest  
I hate to deflate the levity here.... but.... there's a reason that ground fault circuit interrupters trigger (depending on the local laws) at 5 mA or so: 50 mA through the heart region can kill. Once past the insulating skin, the interior resistance of the human body ranges from 10 to 1000 ohms. In the unfortunate event that one has a cut or one's hands are wet with a salt solution, it doesn't take a high voltage to kill if the current passes across the chest (head to feet, hand to feet if you're unlucky, hand to hand). Anything over about 12 volts can be bad if you're really unlucky. AC at 50 Hz is especially bad because it's close to the ideal frequency to disrupt the pacemaker centers in the heart to cause fibrillation which is often fatal.

So - many of us have survived shocks from the mains or high powered electrical or electronic apparatus. That doesn't mean that one should be careless if one has water and electricity in the same place. Insulating (rubber, plastic, etc) shoes (a 1Meg grounding conductor to prevent sparks is not a hazard, and keep one hand in your pocket while fiddling with any electrodes which are supplied from a non-current-limited source. Insulating gloves (not leather, plastic or rubber instead) can help, but if they have holes (sharp wires etc.) they are not effective.

In dry conditions without wounds you can get away with touching many high powered things. Chemistry often involves salt solutions which are highly conductive and which will render your skin conductive. Pure water (11 Megohm, for instance) can be used as an insulator... but that's no fun :-)


Where are you getting your pure water? It's more like 18Megaohm in our labs ;)

densest - 26-9-2009 at 18:58

Quote: Originally posted by UnintentionalChaos  

Where are you getting your pure water? It's more like 18Megaohm in our labs ;)


I can only afford second-hand water from surplus dealers and luck on labx and ebay! :( Someday, if one of my inventions works & sells, maybe I can afford a deionizer to go after my reverse osmosis unit :D

VladimirLem - 1-7-2011 at 20:53

nevermind...

[Edited on 2-7-2011 by VladimirLem]

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