oxone

Soap · Thu May 12, 2005 8:17 am

well swim has another problem. hes been to pool stores, to hardware stores, to electronics stores, just about every store he can think of in search of oxone. the highest % of potassium peroxymonosulfate he can find is 42.8% the rest is all "inert". his guess is taht this inert substance(s) is (are) either magnesium carbonate or (and) sodium (bi) carbonate. the worst part is he can not find a msds on the product. is there a way to purify this product? hes read something about mixing the oxone product with dh2o and methanol and filtering. should this help clean up the product? what method would he use to determine the oxone purity afterwards? also listed on the product is 4.3% active oxygen
He has made it this far he cant stop now!!!

Soap · Thu May 12, 2005 10:02 am

well bees, swim went ahead and did a little experimenting (very little lol). he added about 2 oz of the oxone product to 250ml dh20. after it disolved (except for a very small amount) he added meoh. instantly a white precipitate formed. what the hell is this stuff? he can only hope its all the buffer or all the oxone... any ideas? why cant he find much info on this subject?

Soap · Thu May 12, 2005 11:09 am

well a friend of swim sent him this old post from the hive... now hes confused!

hCiLdOdUeDn
(Hive Bee)
10-11-02 14:18
No 367429
Oh yeah and also a side note: 100% oxone is 42.

Oh yeah and also a side note:

100% oxone is 42.8% potassium peroxymonosulfate(potassium monopersulfate) with 4.5% active oxygen.

Do not confuse 85% oxone as being 85% potassium monopersulfate.

can someone please explain this? things just got real confusing for him...

bio · Working Bee

You didn't try looking very hard now did you! Tsk, Tsk
Try GOOGLE you might like it or any other FSE.

Work the numbers from the empirical formula to arrive at your answer. Wink

The composition of the oxidizing agent Oxone® is 2KHSO5.KHSO4.K2SO4. The active component potassium monopersulfate (KHSO5, potassium peroxomonosulfate) is a salt from the Caro´s acid H2SO5.

Potassium monopersulfate triple salt, active oxygen ca 4.7%
1kg $31.90

CAS Number: 37222-66-5
Formula: H3K5O18S4
Formula Weight: 614.76
UN Number: UN3084

“Oxone” [Du Pont].

TM for an acidic, white, granular, free-flowing solid containing the active ingredient potassium peroxymonosulfate; readily soluble in water; 1% solution has pH of 2–3; minimum active oxygen content 4.5%; strong oxidizing agent.
Hazard: Fire risk in contact with organic materials.
Use: Manufacture of dry laundry bleaches, detergent-bleach washing compound, scouring powders, plastic dishware cleaners, and metal cleaners; hair-wave neutralizers, pharmaceuticals; general oxidizing reactions.

Soap · Fri May 13, 2005 7:19 am

swim thanks you fro the info. he got a hold of the msds (finally) here are the contents: Potassium peroxymonosulfate 43 % potassium bisulfate 23% potassium sulfate 29% potassium peroxydisulfate 3% magnesium carbonate 2 % well this pretty much awnsers swims question about the 42% peroxy... being actualy 100% oxone... (right?) so should swim go ahead and add this to his iso plus the amount of bicarbonate used with 98% oxone? he would love to make some ketone tonight, help is greatly appreciated!

brixtonj · Fri May 13, 2005 5:05 pm

Hi Soap !! It seems we are running at the same pace !!!

I am also with the same Oxone-related doubts !!! Smile

In thy olde Europe .. there's no Oxone , or at least no-one has ever heard of (even in Chem-supply shops )

However , there's something which is called "Active Oxygen" , for chlorine-free swimming pools which says "Pottasium monopersulphate" and PH-Buffer , and goes around 15 Euros/Kg which I thinkg It will be the same.

I am not worried about the concentration . What' worries me .. is that -if only 50% is PotasiumMonopersulphate - What the fuck is the other 50 ? Wouldnty it screw up the reaction ?

Also .. What happens if I put much more Oxone (as there seems to be a big confussion about the concentration of oxone Itself, dunnow if that 80% is the percentage of 2KHSO5 amonth the other 2 salts , or just the total of 3 salts amonth the ph-buffer ) . So ..Its ok to put in a lot- ?????? or should I adhere to the exact proportions ?

Any help is mostly appreciated .. as I am gonna run the reaction today... I must see /smell some ketone this weekend !

Cheers.

Soap · Sun May 15, 2005 11:44 am

well swim has not been around the lab lately. but he has been researching. could some one at least remind him how to set up the formuals to figure out how much of the active he needs to use? we are using a large excess of it right? thanks!
hers some great oxone info swim found:
http://www.organic-chemistry.org/frames.htm?http://www.organic-chemistry.org/chemicals/oxidations/oxone-potassiumperoxomonosulfate.shtm

Soap · Mon May 16, 2005 8:00 am

well swims getting everyones drift. hes asking for to much, he needs to do some research for himself! heres what he thinks should be done:
Oxone product should be disolved in dh20. the magnesium carbonate in the product is water insoluble so it should remain a white powder on the bottom of the dh20/oxone mixture. running the mixture through a filter and slowly heating the water to evaporate it will result in 100% oxone powder.

(taken from chromics oxone procedure) 1991 ref said 1g Dupont Oxone contains 2.75mmol KHSO5, although 1985 ref said 0.2mol is 61.5g Oxone (ie 1g contains 3.25mmol KHSO5). I went with the info from the 1991 ref... who really cares anyway, as the reagent is used in excess.

Now swim is going to go ahead and try this. hes a littel confuzed about the %peroxymonosulphate. hes starting with 42.8% but there is 2% magnesium carbonate. When he removes the carbonate then there should be a higher % amount of peroxy. now he realizes this % is proably not taht important but he cant help to wonder what product the magnesium carbonate was replacing. since oxone is suppose to be 100% when the peroxy percent is at 42.8%

MargaretThatcher · Mon May 16, 2005 6:15 pm

brixtonj: Oxone is marketed as "Chlorine-Free Oxygen Shock".

loki · guinea pig

i don't think it's going to work to boil that oxone down. heat usually drives the oxygen away IIRC. if not, in any case, it's dangerous to heat oxidisers willy nilly unless you know what you are doing.

from the list of ingredients you listed, the first is the oxone, the second is a buffer, the third is a potassium peroxyDIsulphate and the magnesium carbonate is probably not very soluble anyway (the hydroxide of magnesium certainly isn't). At a guess, I'd say that if you are wanting it to have nothing but oxidising goodness, make sure that the magnesium carbonate all falls out. The rest that dissolves will be mono- and di- peroxy-sulphates and buffers.

If there is a problem in the reaction scheme stipulating only peroxy-MONO-sulphate, you need to look for somwhere you can get that by itself, or maybe look at the solubilities of the chems in your solution and see if you can precipitate stuff you don't want simply by dumping more of the salts into the water than can dissolve, and stirring it up to make it so the liquid is saturated solution of what you want. warming it up a bit while mixing will ensure that all the desired more soluble parts end up in the solution, and the undesired insolubles re-precipitate. you can just give it time, and it will do it, heat just speeds up the dissolution/precipitation thing.

It could be the other way around... Only way to know is to get the proper solubility numbers for the chemicals and the highest solubility one, by adding an amount of water equal to the amount of the desired chemical can dissolve into, one only gets the most soluble chemical dissolving. (again, heat and mixing, and then cooling to the temperature of known solubility will ensure that the dissolved concentrated solution will be what you want).

brixtonj · Tue May 17, 2005 12:52 am

Hi !!!!
Well ,I may got it .

Oxone is apparently sold in two "flavours" PH-Buffered and PH-UnBuffered.

PH-Buffered 's got around 15 % of some other salts Mg ,etc.. to keep PH within range . That's the Oxone found in "Clhorine-free swimming pools treatment" Its got its own Magnesium PH controls , to reduce the hassle of PH control for the swimming pool operator.

However ... Unbuffered Oxone (that is 100% Oxone with 45% of KHSO5) is the one sold in "dual-packet" pool treatments (one packet for the Oxone , and the other for the Magnesium Salt) .

That explains that -while some people experiences undissolved salts on their solutions.. , other dont's . I don't get any undissolved salt , for example.

I have just dissolved -right now , indeed- 1gram of pure-unbuffered Oxone in 100 mL of water and the Ph is exactly 2.3 , exactly as the Dupont -reference sheet indicates and got cristaline water with absolutely no precipitates.

and That could be the reason that some-write-ups specify the addition of 25 grams of NaCO3 and other writeups dont'

Therefore .. if your Oxone-Water solution is grossly accidic , and without precipitates ,.. then you got pure-unbuffered oxone. and need to add , either baking soda , or Magnesium salts ,etc.. to correct the PH.

However if you see white precipitates .. then you are probbably using PH-Buffered Oxone.. and that' precipitate is indeed NEEDED to keep PH within control..

Anyway .. tomorrow I will give it again a go ... with my last Isosafrole... I will post the results..(or lack of )

Cheers.

brixtonj · Fri May 20, 2005 3:53 pm

Success !!!!!! I got my first Ketone. !!! and what's more .. the first confirmation that I am indeed performing chemical-reactions and not just moving safrole from flask to flask .

-I mean-

Until now ,as Sassafras , Safrole , IsoSafrole , Epoxide smells quite the same , I didnt knew if I was indeed performing reactions .. or just nothing at all. Surely some of you also had the same feeling .

but when -for my first time- a NEON YELLOW distillate appear on the receiving flask (instead of the white/clear Iso , Sass ,Safrole , Epoxide) .. that was confirmation that -up to this point I am doing it correctly .

Well , I fuck'd up the yields by doing 3 really stupid things.. such ass

mistake 1 :

15 % H2SO4 is by WEIGHT not by volume (H2SO4 is nearly twice as dense as water! ).... I wrongly mixed 15cc of acid with 100 cc of water ... WRONG !

mistake 2:

when hydrolising the epoxide .. IT should be done with a water bath.....It shouldnt heat up over 80 C !. Indeed I burned up a whole batch by heating it up in the mantle ...It exploted !! or something like that . Most of my glass went bust !.

mistake3 :

triying to distill ketone ... I didnt use a buffer oil .. therefore by the time first ketone was starting to drip .. it was getting dark .. and burnt in the 1st flask. Of course I tried to distill up to the last drop of ketone .. so I really burn the contents on the flask .. and fuck it up at least 10 ccs of quite promissing ketone.

anyway .. I got 12 grams of Ketone (out of a total of 60 grams Isossafrole , including mistakes and accidents ) so Its not that bad .

I have even taked pictures to that fluorish-yellowish nectar.

2spun · The Resistor

brixtonj,

thats great frist Ketone. swiy knows the feel'n.
swiy was read'n in " mistake3 " swim states that he use'd a buffer oil?
was that mean'n that swim put a heaver oil in his flask? with his goodies? that can cause swim problems. like contaminate your ketone or even make ones yelds suffer. from all swiys understand'n buffer oil is a fallacy .
edited
my bad Brixtonj i reread you did not use a buffer oil. sorry . i wouldn't use one.

what was the size of your flask? maybe going to a smaller one would help with ones distill'n of the ketone.

"You will maximise yield by utilising the correct size glassware, and vacuum."

this was told to swiy and he follow'd and it work'd for him.

swiy would love to see swims pic he took as well !!!