Sciencemadness Discussion Board - HClO3

HClO3

Fantasma4500 - 13-5-2013 at 07:06

well yes you guessed it.. the new k3wl on SM really did it..
before you starts yelling its a deadly compound at your screen please read following:

it was done first with 37% 1.27 mole H2SO4 as in tiny grains of KClO3 (around 0.01g) on THICK glass that would if it would happen be capable of sustaining the shock without turning into projectile / fragments / shrapnel / younameit

it didnt show anything at all

thereafter was several drops of concentrated H2SO4 added to a similar amount on a dry surface

a brown substance / liquid with consistense of conc. H2SO4 was formed, it was probably due to excess H2SO4

anyhow it was coloured lightly brown.. already at this point i knew this was not something safe to do, but again keep in mind were speaking several DROPS (~0.12 mL)

at first i tried holding a storm lighter to the liquid and heard tiny crackling, decided to put some gloves on before proceeding and keeping in mind even such small amounts would be able to give off quite a bang if it would go off

i then used a pipette to take a tiny amount onto another thick glass piece, but it showed no interesting things whatsoever when heated

aside from this i saw smoketrails coming from the HClO3, pretty much like with 99% HNO3, i didnt blow at it as i wanted to keep a thoughtful distance in case it would go bang and pour tiny droplets of concentrated H2SO4 into the air

i filmed it aswell.. see for yourself if you ever wondered how this infamous substance looks..

http://youtu.be/Ahc1YikGeJE

im quite sure you would have seen something different if you would have used more of this, perhaps more KClO3 in H2SO4.. anyhow this was pretty nerve wrecking for even these amounts

Bot0nist - 13-5-2013 at 08:03

Cool. Dip the corner of a peicer of paper into the drop, and it should burst into flames

I made a contribution to the "make fire" video that HKParker made. I ignited cotton, NSAIDs, 91% IPA, sugar, etc. The IPA kind of detonated though. Very small amount only!

[Edited on 13-5-2013 by Bot0nist]

Dornier 335A - 13-5-2013 at 10:04

I would also like to see reaction with combustible materials. You could you try small amounts of magnesium powder or red phosphorus.

Chloric Acid Video

chemcam - 13-5-2013 at 10:46

I performed this experiment today and recorded it, the video link will be at the end of my post. I made the chloric acid by adding three small drops of lab grade 98% sulfuric acid to a small pile of lab grade potassium chlorate. It bubbled and fumed quite a bit, I added a small piece of paper and it exploded, no flames just splattering the mix with a BANG, luckily I planned for this and used a container which would catch the spray.

Chloric Acid Preparation w/ Paper Explosion

Bot0nist - 13-5-2013 at 11:18

Nice. Try rubbing some dry KCLO3 onto the corner of a napkin ir cotton ball, and then add a drop of conc H2SO4. this will ignite it. When I did the IPA, I made a suspension of KCLO3 in a couple drops of IPA and then added the drop of acid. This poped anbd then ignited with a blue flame.

Fantasma4500 - 14-5-2013 at 04:46

wow.. brilliant.. didnt know you guys were willing to do this (:

considering this can be handled somewhat the same way as Mn2O7 its quite interesting, and with much higher explosive potential, something i still dont like about it is the spray of H2SO4 that plausibly will be formed.. depending on its power i could try and put a cup over this thing to catch it..? perhaps just a high density plastic bag?

thinking about ether or NM destillation isnt something i prefer to do by any means.. but wasnt HClO3 discovered when a scientist attempted to distill this stuff?
also.. it is seen that this acid is stable enough at tiny amounts, but would this be stable enough to be mixed with something to go into HClO4??
low concentrations would perhaps be preferred for this if it would be dealt with..

but red phosphorus i might try, already wetmixed armstrongs mix gets on my nerves more than anything literally anything does

Bot0nist - 14-5-2013 at 05:10

Perchloric acid can be had wusing KClO4 instead of KClO3, IIRC.

There is a thread on urea perchlorate or something, in which members distill highly dilute chloric and perchloric acids. A search may reveal this thread. I believe the acids were once used in electroplating, until vats started exploding... I think Wizard is In posted some nice snippets on this.

Fantasma4500 - 15-5-2013 at 01:07

Quote: Originally posted by Bot0nist

Perchloric acid can be had wusing KClO4 instead of KClO3, IIRC.

There is a thread on urea perchlorate or something, in which members distill highly dilute chloric and perchloric acids. A search may reveal this thread. I believe the acids were once used in electroplating, until vats started exploding... I think Wizard is In posted some nice snippets on this.

interesting.. sounds nerve wrecking to attempt tho.. but about KClO4 yes thats true, but if you can skip needing a proper anode in order to make KClO4, and basically make HClO3 into HClO4 it could be a pretty neat shortcut.. i know that its possible to do as in decomposition of KClO3 to KClO4 but you need really good heat control if its attempted, KClO4 is more interesting as it can be used to make NH4ClO4 also.. (:

woelen - 15-5-2013 at 03:27

If you add concentrated H2SO4 to solid KClO3 then you only have HClO3 as intermediate. HClO3 is unstable at more than 35% concentration. Highly concentrated HClO3 disproportionates to HClO4, ClO2 and water. The ClO2 gives the orange color. If you do the experiment in a small glass beaker (e.g. 25 ml beaker with two or three drops of H2SO4 on a small pile of KClO3), then you can see the yellow color of gaseous ClO2 in the beaker.

The explosive properties come from the anhydrous HClO4 and the ClO2. Both are notoriously dangerous and hence you should not work on a larger scale than a few drops of acid and a few tens of mg of KClO3.

Fantasma4500 - 15-5-2013 at 06:31

Quote: Originally posted by woelen

If you add concentrated H2SO4 to solid KClO3 then you only have HClO3 as intermediate. HClO3 is unstable at more than 35% concentration. Highly concentrated HClO3 disproportionates to HClO4, ClO2 and water. The ClO2 gives the orange color. If you do the experiment in a small glass beaker (e.g. 25 ml beaker with two or three drops of H2SO4 on a small pile of KClO3), then you can see the yellow color of gaseous ClO2 in the beaker.

The explosive properties come from the anhydrous HClO4 and the ClO2. Both are notoriously dangerous and hence you should not work on a larger scale than a few drops of acid and a few tens of mg of KClO3.

wow.
i think i might try this a few more times, perhaps say 5 drops of h2so4 as the limit, then i just hope that i wont get the HClO4 to go off when diluting it as im gonna try to react it with K2CO3

it would be brilliant if i would be able to figure out how to make 50% HClO3, which would then become ClO2 and HClO4, but im sure that would become very advanced calculating on, i might use my 70% H2SO4 instead for this, or wait perhaps not, it contains ultrafine carbon
ill report back in with results later on i hope to (;

but about the 35% HClO3 limit, is there any info on how long time it takes to go into ClO2 and HClO4 or is it known to be instantly?

woelen - 15-5-2013 at 06:38

This method hardly is useful for isolating perchlorates, but you could give it a try. I would take 5 drops of H2SO4 (assume this is 0.25 ml) and use an equimolar amount of very finely powdered KClO3. Add the H2SO4 to the KClO3 and allow to stand for a while. Then AT ONCE add a few ml of water. Next, boil the liquid (no need to add a potassium salt, you already have potassium ions from the KClO3) until all material has dissolved. Then allow to cool down and see if you get crystals. These crystals could be KClO4.

This, however, is not a decent method of synthesizing much KClO4. It is way too dangerous and yields are poor, due to losses as ClO2.

Fantasma4500 - 16-5-2013 at 11:23

Quote: Originally posted by woelen

This method hardly is useful for isolating perchlorates, but you could give it a try. I would take 5 drops of H2SO4 (assume this is 0.25 ml) and use an equimolar amount of very finely powdered KClO3. Add the H2SO4 to the KClO3 and allow to stand for a while. Then AT ONCE add a few ml of water. Next, boil the liquid (no need to add a potassium salt, you already have potassium ions from the KClO3) until all material has dissolved. Then allow to cool down and see if you get crystals. These crystals could be KClO4.

This, however, is not a decent method of synthesizing much KClO4. It is way too dangerous and yields are poor, due to losses as ClO2.

oh yes theres already K ions in it.. hm..
perhaps this could be done more dilute, but ofcourse as they had some pretty loud accidents with HClO3 back in time it might not be the thing you wanna mess around with.. at all..
one thing is broken glassware with acids in

another completely new scenario is superfine metaborosilicate glass fragments PLUS boiling acid / acid gasses

i was actually considering to try the whole HClO3 thing on concrete as it contains CaCO3 already, so it might be able to produce Ca(ClO4)2 in an instant, but as theres already K in it it would be of no real use..

about the drop thing, i believe we did measure how many drops 1 mL was consisting of and the result was pretty much 16 drops per mL