Sciencemadness Discussion Board - Hydrogen Peroxide purification

Hydrogen Peroxide purification

APO - 29-12-2012 at 13:40

Well, you can purify it buy fractional crystallation(freezing the water away) which will give 62% concentration, fractional distallation is highly dangerous with H2O2 so that's out of question. But is there a way of seperating the H2O2 into two layers?

[Edited on 29-12-2012 by APO]

[Edited on 30-12-2012 by APO]

neptunium - 29-12-2012 at 15:05

in short no. they are both missible in one another in all proportion

APO - 29-12-2012 at 17:24

What are the most efficient methods of purification?

Ephesian - 29-12-2012 at 17:35

I have 500 mL of 30% H2O2 fisher scientific if you need some, ill put it up on ebay for you at a reasonable price.

plante1999 - 29-12-2012 at 18:09

I think the best way is passing air trough 3% hydrogen peroxide at a temperature of 60-70 degree Celsius. Water evaporate before the hydrogen peroxide, effectively concentrating the peroxide. I already concentrated it too much at 50%, so I think it could go all the way to 90%. Do not concentrate it more than 30% for safety!

http://hclo3chem.weebly.com/concentrate-hydrogen-peroxide.ht...

elementcollector1 - 29-12-2012 at 19:14

I agree with plante, but freezing only gives somewhere around 15-30% before it stops working.

APO - 29-12-2012 at 19:24

Thanks plante1999! Sounds like a pretty good method, I'll have to try it sometime.

shannon dove - 30-12-2012 at 10:06

Wow, plante, I didn't know concentrating hydrogen peroxide was that simple.
How much is lost along with the water? (How efficient is it?)

plante1999 - 30-12-2012 at 10:20

The efficiency is very high, I had made a test with 1 L of 3% H2O2 and got 100ml of about 88.5-90 volume hydrogen peroxide, or about 29-30% more than 95% yield is obtained if one troughly clean the labware and equipment.

kristofvagyok - 30-12-2012 at 10:29

Quote: Originally posted by plante1999

The efficiency is very high, I had made a test with 1 L of 3% H2O2 and got 100ml of about 88.5-90 volume hydrogen peroxide, or about 29-30% more than 95% yield is obtained if one troughly clean the labware and equipment.

Khm, 1l of 3% solution contains 30g of pure H2O2, so if you've got 100cm3 at the end and we're saying that you had a 100% yield than your end product is circa 26% pure.

plante1999 - 30-12-2012 at 10:36

If one ml of 3% produce 10 volume of O2 when decomposed, and 6% is 20 volumes, Wouldn't 90 volume be 30%?

I'm sure one ml of the peroxide produced 90 ml of gas. As for the volume of the starting peroxide and finishing volume my glassware are +-10% (Beaker) since I don't have a large enough measuring cylinder.

shannon dove - 30-12-2012 at 10:47

Why was fractional distillation and freezing methods developed if it is that easy to concentrate? Am I missing something here? It's not April fools day.

plante1999 - 30-12-2012 at 10:51

I don't know why air evaporation method is not used, I decided to use it because the low temperature protect peroxide from decomposing, the process is also easy. But a fish air pump is probably obligatory as fish pump troughly filtrate the air (at least mine do).

kristofvagyok - 30-12-2012 at 10:59

Quote: Originally posted by plante1999

If one ml of 3% produce 10 volume of O2 when decomposed, and 6% is 20 volumes, Wouldn't 90 volume be 30%?

Gas volumetric titrations are not the best, they have a high percent failure rate. Titrate it with KMnO4.

You've said that you can go up with this method to 50-90% H2O2 content, you also wrote that you have started from 3% H2O2 and got 100cm3 of +90% H2O2 what is everything but not true.
So what did you get from what? If you have ended up with 30% H2O2, than it's aint special, anyone can buy it and also everyone can make it.

shannon dove - 30-12-2012 at 10:59

I have a dream that one day I will go to the nitric acid thread and there will be a just as easy method of of concentrateing nitric acid, then I will go to the elemental phosphorus thread .......

plante1999 - 30-12-2012 at 11:05

Quote: Originally posted by kristofvagyok

Quote: Originally posted by plante1999

If one ml of 3% produce 10 volume of O2 when decomposed, and 6% is 20 volumes, Wouldn't 90 volume be 30%?

I will try to do something for titration, as permanganate is regulated here, and as you may know, not everybody here have the mean and the resource of a commercial lab as you do.

I NEVER SAID that I got 90% peroxide. I said that I already concentrated too much accidentally to 50% and as such I do think that 90% concentration is possible. I would greatly want a quote for this affirmation.
I never said that I made 90%, if I did it was by a typo or a misunderstanding..

@shannon dove
If you don't believe in my procedure then you are not obligated to try it. It is not the first time I publish procedure never one saw/used. You can look in the mercury from cinnabar, as I told a process for neptunium.

Not everyone is obligated to trust a 16 year old guy tough.

[Edited on 30-12-2012 by plante1999]

shannon dove - 30-12-2012 at 11:13

I do believe you plante, and I very much appreciate your research.
I would buy you a beer if I could.

APO - 30-12-2012 at 13:04

Would the evaporation method work better in a descicant chamber?

platedish29 - 31-12-2012 at 08:48

Quote: Originally posted by APO

Would the evaporation method work better in a descicant chamber?

Guess it works significantly for V > 30% by putting anhydrous silica in it thus easily reaching 70% concentration considering how big silica gel grows

Poppy - 31-12-2012 at 09:39

How about merging both air evaporation and chemical dessication?
H2O2 + 7 H2O + CaCl2 -> H2O2 + CaCl2.7H2O dessicates
wherein H2O stands for removable water
H2O2 + 3CaCl2 + 2K3PO4 --> H2O2 + 3/2Ca2PO43(ppt) + 6KCl(some ppt)
wherein additional salts were dissolved in the own peroxide but in a different vessel
H2O2 + 2KCl + Fe(ClO3)3--> H2O2 + KClO3(ppt) + FeCl3
H2O2 + FeCl3 + 3NH3 --> H2O2 + Fe(OH)3 + 3NH4Cl Extra dessication occurs by the formation of hydroxides and ammonium ion
H2O2 + 2NH4Cl + PbCO3 --> H2O2 + PbCl2 + CO2 + 2NH3 + H2O
virtually removing ions from the solution

Might that go for 90%?

ScienceSquirrel - 31-12-2012 at 10:04

It is almost inevitable that your dessicants will contain traces of metal ions like copper that will be concentrated in your peroxide.
This is extremely dangerous as highly concentrated hydrogen peroxide is explosively unstable in the presence of dust, some metal ions, finely divided metals, etc.
Even 35% hdrogen peroxide will cause rapid and painful burns if the cold solution touches the skin.
I use it on a routine scale in litre quantities for cleaning and sterilising brewing equipment and I treat it with respect.

Poppy - 31-12-2012 at 14:06

On account for the need for a centrifuge this route could also be used to prepare the loudest bang after pulling the whole machine into tears!!
Honestly, I don't think there will be any contaminants after the process is done am I wrong?

elementcollector1 - 31-12-2012 at 22:33

This is slightly off-topic, but does anyone know what the concentration of hydrogen peroxide is in glow sticks? If it's anywhere higher than 12 or so, this could be a useful and viable source (esp. from camping stores, Halloween season, etc.).

APO - 31-12-2012 at 23:01

Happy new year!!!

ScienceSquirrel - 1-1-2013 at 05:14

Quote: Originally posted by Poppy

On account for the need for a centrifuge this route could also be used to prepare the loudest bang after pulling the whole machine into tears!!
Honestly, I don't think there will be any contaminants after the process is done am I wrong?

You do not want any contaminants at all in hdrogen peroxide as it becomes very concentrated.
Hydrogen peroxide of over 70% concentration should be treated as a strongly corrosive, oxidisng agent and sensitive explosive.
Above this concentration contact with a suitable catalyst will cause instantaneous decomposition into oxygen and steam.
http://en.wikipedia.org/wiki/High-test_peroxide

DerAlte - 1-1-2013 at 09:14

Déjà vu all over again

It is perhaps inevitable in a long running forum like SM that the same old topic gets repeated time and time again, ad nauseam and to the nth degree. This is one of them. UTSE

Concentration by freezing is covered in
http://www.sciencemadness.org/talk/viewthread.php?tid=15881#...
(this will get you to 25-30% in a domestic refrigerator, and maybe 45% using a dry ice refrigerant. Past that you’ll get the eutectic).

For considerable info re H2O2 see
http://www.h2o2.com/technical-library/default.aspx?pid=9&...
The method suggested by Planté also works. However, it is rather tedious and takes a long time. The partial vapor pressure of H2O2 is considerably less than water. See the reference above.

I would emphasize the warning given by Science Squirrel about over concentration. And don’t mess about with organics either. Scrupulous avoidance of any heavy metal ions is essential for the stability of H2O2 solutions. Remember that on concentration by the above methods you also concentrate whatever stabilizer the manufacturer has added..

Der Alte

Glucose Oxidase - 1-1-2013 at 10:36

APO if you want a high concentration hydrogen peroxide try to produce BaO2 and then treat it with sulfuric acid it should give a yield close to 90% percent
PS: i never tried this myself so dont ask me about details i just digged it up from the internet.
PS2:BaO2 can be produced (as far as i remember) by heating BaO to 700C or something good luck.

plante1999 - 1-1-2013 at 10:41

Quote: Originally posted by Glucose Oxidase

PS2:BaO2 can be produced (as far as i remember) by heating BaO to 700C or something good luck.

It is 500 to 600. You can only make 3-6% peroxide with barium peroxide by my work. You don't have tried it, it is evident.

platedish29 - 1-1-2013 at 14:33

SS from your link to wikie's:
"High-concentration hydrogen peroxide was formerly available in 70, 90, and 98% concentrations in sizes of 1-gallon, 30-gallon, and bulk-tanker truck volumes, but is now no longer available to the public in the United States due to action by the Department of Homeland Security."

How?

shannon dove - 1-1-2013 at 14:50

Quote: Originally posted by platedish29

SS from your link to wikie's:
"High-concentration hydrogen peroxide was formerly available in 70, 90, and 98% concentrations in sizes of 1-gallon, 30-gallon, and bulk-tanker truck volumes, but is now no longer available to the public in the United States due to action by the Department of Homeland Security."

How?

I don't think I would like to be riding next to a tanker truck full of 98% hydrogen peroxide.
Would that be a yellow and an orange placard?

Poppy - 1-1-2013 at 19:12

Haven't witnessed H2O2 in high concentrations b4, but cmon, if vapors are scary then you need some fans..
Gasoline is sickly scary even when like 50cc are poured around, and even NG wont explode on shock that easily mostly in water.
so that 2% water should be ok to save your life?
Don't think so.
But after wathing youtube's video on Cl2O I feel something bad about all this.

mayko - 30-1-2013 at 08:19

Quote: Originally posted by plante1999

Quote: Originally posted by kristofvagyok

Quote: Originally posted by plante1999

If one ml of 3% produce 10 volume of O2 when decomposed, and 6% is 20 volumes, Wouldn't 90 volume be 30%?

I will try to do something for titration, as permanganate is regulated here, and as you may know, not everybody here have the mean and the resource of a commercial lab as you do.

I've seen a number of guides to concentrating peroxide, but analyzing it has generally been treated qualitatively. I have generally done this by determining the density of the solution, and working backwards from that. This has the advantage that it only requires tools for accurately measuring mass and volume, which would hopefully be available even to a DIY lab. Here's a walkthrough:

http://topologicoceans.wordpress.com/2013/01/30/lablulz-densitometry-of-hydrogen-purr-oxide/

I've since gotten a bunch of syringes donated and I've started using them for controlled additions. Less derpy.

Valentine - 31-1-2013 at 00:21

Yesterday I did some experiments on concentrating hydrogen peroxide with a rotatory evaporator. My first try gave me a 53,6 % H₂O₂ solution. Next time I measured almost everything. I started with 98 g 30,1 % H₂O₂ solution and I could concentate it on 75 °C and 50 mbar to 33 g 67,0 % solution. It means only ~25 % of the H₂O₂ had decomposed during the procedure. These concentrations are based on double-checked permanganometric titrations. I used the cleanest flask I had for my first attemption, and for the second I used one with some spots of selenium or some orange dye. It's interesting that the 53,6 % solution constantly bubbling (not vigorously, just very slowly) and the 67 % H₂O₂ in the "dirtier" flask was "in quiet" during the day, I haven't seen a bubble yet. Probably there was some very little amount of metal salt in the first flask.

[Edited on 31-1-2013 by Valentine]

APO - 5-2-2013 at 19:22

Is hydrogen peroxide miscible with salt water?

elementcollector1 - 5-2-2013 at 20:34

Yes.

Highfields - 8-2-2013 at 12:16

I think it is the case that the worst dangers of hydrogen peroxide lie mostly with what happens in the vapour rather than the liquid. Highly concentrated peroxide was made (by Laporte) and trucked (fairly casually) around the UK back in the 1960's leading up to its use on the launch vehicle the British used to get their one and only independent satellite in orbit. Subsequently, the whole project was abandoned and manufacture of peroxide ceased.

Although I do not recommend this to anyone, I did once (just once!) concentrate a quantity of 30% electronics grade peroxide up to around about 90% by reduced pressure (nitrogen atmosphere) distillation. All of the glassware had been thoroughly cleaned and pre-conditioned before use.

[Edited on 8-2-2013 by Highfields]

APO - 8-2-2013 at 17:19

Hey I found this which is similiar to salting out, but I'm skeptical if it will work, haven't tried it yet.
http://www.instructables.com/id/Distill-Hydrogen-Peroxide/

elementcollector1 - 8-2-2013 at 18:19

Quote: Originally posted by APO

Hey I found this which is similiar to salting out, but I'm skeptical if it will work, haven't tried it yet.
http://www.instructables.com/id/Distill-Hydrogen-Peroxide/

I call ALL the shenanigans. Hydrogen peroxide should by no means separate from a solution of any salt in water.

APO - 8-2-2013 at 18:24

Sounds right.

Sedit - 8-2-2013 at 21:00

I have yet to use this method that has been running through my mind for sometime now ( I get 35% rather cheep and its more then I need) but if the opening of a bottle was stuffed with cotton to keep dust out and it was placed in a desiccating bag with a large amount of MgSO4 I would think that the concentration should in theory get rather high over time. It should be a simple set and forget means of concentration as long as dust from this desiccating agent was not allowed to come into contact with the H2O2.

Can anyone test this or provide a valid argument as to why this would not work.

APO - 8-2-2013 at 21:11

No doubts here! I will do it and post my results!

elementcollector1 - 8-2-2013 at 21:17

Hydrogen peroxide does decompose on its own, though slowly. I imagine that this would only affect the concentration a little bit at a time, but it may be worth mentioning.
Alternatively, what of a stronger dessicant such as NaOH or H2SO4?

DerAlte - 8-2-2013 at 22:07

Quote: Originally posted by APO

Hey I found this which is similiar to salting out, but I'm skeptical if it will work, haven't tried it yet.
http://www.instructables.com/id/Distill-Hydrogen-Peroxide/

Sounds like BS. H2O2 has a dielectric constant very similar to H2O,~80, and should be an equally effective solvent for ionic substance. The reason is the ability to form hydrogen bonds, which it shares with HF, HCN and liquid NH3 as a consequence of forming highly polar molecules. The high dielectic constant allows the dissociation into ions to occurs with greater ease. Very little data is available as to the measured solubility of ionic substances in H2O2 probably due to its reactivity. I managed to find the following from a quick web seach via Google:
http://www.springerimages.com/Images/Physics/1-10.1007_s1166...
Phase diagram for the system sodium chloride-hydrogen peroxide-water at 283.15 K. SA, solubility of NaCl in water at 283.15 K; w, mass fraction
This suggests that the solubility of NaCl in a solution of H2O2 and H20 (Miscible in all proportions) differs very little from than in pure H2O. It is highly dubious that any layer separation could occur due to differential solubility.
Der Alte

kt5000 - 6-11-2013 at 10:45

Quote: Originally posted by shannon dove

I don't think I would like to be riding next to a tanker truck full of 98% hydrogen peroxide.
Would that be a yellow and an orange placard?

I'm more concerned about the UPS guy tossing around the box with the 1-gal 98% H2O2

[Edited on 6-11-2013 by kt5000]