gilbert pinkston

"While we are on the Ammonium topic, has anyone out there tried manufacturing their own Ammonium perchlorate from homemade Sodium perchlorate? And if so, what method did you use to destroy decisively any chlorate contamination? "

yes from sodium perchlorate and ammonium nitrate
the ammonium perchlorate will drop out
the chlorate should all be removed BEFORE adding the ammonium salt indigo carmine is the indicator used to make sure all chlorate is removed (although im convinced there are other less exotic dyes that would work and be just as sensitive)
i run a cell until the perchlorate crystalizes out this is vacuum filtered so it contains little chlorate then disolved in a little boiling water acidified and i add "iron out" (sodium-sulphite,hydrosulphite,metabisulphite) which is used to get the iron out of wash water a few drops of indicator is added from time to time to make sure the solution will hold a blue color
this method is much better than HCl alone purification (my old method) for obvious reasons
of course this solution must be brought to pH7 after all chlorate is destroyed
any (which is significant) perchlorate left in solution can be dropped out by adding KCL
the ammonia MUST be removed from this and nessler reagent is really nice to have as an indicator

"load you cell, leave it go, top it up with saturated kcl ( no need even to remove sodium at the end of the run) and stir it untill it is perchlorate"

hummmm?

i guess im not getting it

since perchlorate is formed when chloride is less than 10% but this condition is not good for Pt annodes so clorides must be added to keep the concentration above 10% when does the pechlorate form?

of course it could be done in two steps by removing less soluable KClO3 from KCl solution and KClO4 from KClO3 solution

gilbert here
someone once wrote

"carbon rods are not worth the trouble, they disolve too rapidly don`t bother with carbon/graphite"

glad i diddnt know that before i converted 3 40# bags of NaCl to NaClO3 with (real) graphite not welding rods
in a properly run cell (as i have said many times but nobody wants to believe) one pound of graphite erroded will produce hundreds of pounds of chlorate
i used NaCl because i quicky recognized the disadvantages of starting with the potassium salt... for one the immensly more soluable NaClO3 produced allows for the graphite to settle out eliminating the need for filtering
then there is the soluability problem with KClO3 to KClO4 not to mention that for proper purification all products of the cell must be in solution and KClO4 is not very soluable meaning a huge amount of water must be used in the process compared to what is needed when working with sodium compounds

"then tried the auto ox , but still no purple (perchlorate)"
what can i say it worked for me but not the most efficient path to perchlorate

"for a small outlay its much easier to do it all in one with no mess using pt .............. continuous for about 2 weeks + or untill ptt turns from a abrasive crystal to a creamy smooth iceing sugar crystal"

if this is what you are saying all the literature says because of excessive corrosion Pt should not be used in a contiuous operation

in my unregarded opinion the best way to perchlorate is chloride to chlorate using graphite then chlorate to perchlorate using leade dioxide unless you have money to burn

"One member here has a perc cell definitely making perchlorate producing kilos per day"
come on man give
whats his name here?
i would like to read all about it

ok MDA i acknowledge your accolade
and i will bless you now
have you read the archives?
they contain an abbreviated account of my endeavors ( i only type with one finger )
PS:
i like your style