Author Topic: Concentrating 35% Peroxide  (Read 2559 times)

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noj

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Concentrating 35% Peroxide
« on: December 17, 2001, 02:34:00 PM »
What would the concentration of peroxide be if I were to vacuum distill off 50% of a 35% solution?

Ex: 100mL of 35% peroxide reduced to half the volume under vacuum.

A theory is a tool - not a creed. -J. J. Thomson

hest

  • Guest
Re: Concentrating 35% Peroxide
« Reply #1 on: December 17, 2001, 04:23:00 PM »
C'mon take a wild guess

uemura

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Re: Concentrating 35% Peroxide
« Reply #2 on: December 18, 2001, 12:19:00 AM »
Use the calculator (easy, no aceotrop between H2O2 and H2O), see for more details (it's on Rhod's site):

http://webhome.idirect.com/~earlcp/FAQs/FAQ.html



BTW: SWIM has some 35% H2O2 in the freezer, according to the above reference he may get a 62% concentration (under optimal conditions).


Carpe Diem

noj

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Re: Concentrating 35% Peroxide
« Reply #3 on: December 18, 2001, 03:16:00 AM »
My problem was from reading a ref stating that a 10% peroxide solution would have 1% peroxide at the distillate. So at the beginning of distillation of 35%, I would believe that 3.5% of the distillate is peroxide. I am really not that great in algebra to come up with a formula to figure this out.

A theory is a tool - not a creed. -J. J. Thomson

uemura

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Re: Concentrating 35% Peroxide
« Reply #4 on: December 18, 2001, 09:24:00 PM »
noj,

what uemura read so far is that with increasing percentage of the h2o2-h2o indeed more h2o2 destilles over which isn't something special since the bps of h2o and h2o2 differ by just 50 DegC.

In addition, some of the h2o2 gets decomposed (hopefully not kinda explosive  :) ) so in the end he would determine the percentage of the concentrated h2o2 either as proposed by lugh using the density OR by decomposing 1ml of the h2o2 by MnO2 and measure the oxygen coming out. Uemura plans to do so with his freeing concentrate and will post how this is to be done.

Cape Diem

uemura

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Re: Concentrating 35% Peroxide
« Reply #5 on: December 18, 2001, 10:02:00 PM »
It's uemura again...
He found the write-up for the calculation of the percentage of a h2o2 solution. This extract comes from a paper on growing shrooms with the help of peroxide which allows a kind of 'sloppy' technique instead of working in a clean and sterile environment. :)
Here it is:

Here is my method for getting a rough measurement of peroxide:

Get a clean test tube (preferably one with a lip or screw cap), a small birthday-party type balloon, and a slice, small enough to fit into your test tube, of the stalk of any mushroom you have handy (for best results, use a young, rapidly growing mushroom and take a piece of stalk, trimming off the natural skin to expose plenty of broken cells). If you don’t have any mushrooms, a piece of banana or other skinned vegetable should do just as well) MnO2 works as well! . You will also need your peroxide solution, a rubber band, a pasteurized measuring pipette, a 100 ml graduated cylinder, and a pot of water.

1) With the pasteurized measuring pipette, withdraw 5 ml of the peroxide solution from the bottle and transfer it into the test tube.
2) Place the slice of mushroom in the upper part of the tube (don't let it slip into the peroxide yet).
3) Make sure the balloon is empty of air and stretch the mouth of the balloon over the mouth of the tube (tilt the tube to keep the slice of mushroom from slipping into the solution until the balloon is in place.
4) Put a rubber band around the mouth of the balloon on the tube, to keep gas from escaping as the pressure builds (I have found it most effective to use a broken rubber band that can be wound tightly around the threads of the tube, over the mouth of the balloon).
5) Once the balloon is sealed in place, let the mushroom slice slip down into the peroxide solution. The solution should begin bubbling oxygen immediately.
6) Agitate the tube. The peroxide solution should be largely decomposed in five to ten minutes, depending on the amount of catalase/peroxidase in your mushroom slice.
7) When decomposition is almost complete, you'll see that the bubbling will have slowed and the bubbles will have become quite small. Meanwhile, the balloon should have become taut as it began to fill with released oxygen.

Now, my college chemistry training tells me that 5 mls of a 3% solution of hydrogen peroxide should generate about 49 mls of oxygen when the peroxide decomposes completely at room temperature and one atmosphere pressure. To measure the oxygen released from your peroxide solution:

1) Fill a graduated cylinder with water and turn it upside down in a pot of water, making sure all bubbles are out.
2) Twist the balloon on your test tube to trap the released oxygen, remove the balloon from the tube holding the twist tightly, and put the balloon under the water in your pot.
3) Carefully release the gas from the balloon up into the inverted graduated cylinder, displacing the water inside it.
4) Keeping the open end of the cylinder under water, read the volume of oxygen off the graduated cylinder.

The first time I did this, I got 52 mls of gas inside my graduated cylinder from 5 mls of peroxide solution. Given that there may well have been about 3 mls of air in the flat balloon before I started, the peroxide solution probably generated pretty close to the theoretical amount of oxygen for 5 mls of 3% solution.

Here’s how to calculate the amount of peroxide solution you will need, if you solution tests higher or lower than 3%:

1) Divide the volume of oxygen expected for 5 mls of 3% solution (49 mls if the balloon is completely empty to begin with, or 52 mls in the above example, counting the few milliliters of air initially trapped in the balloon) by the volume of oxygen you actually got.
2) Multiply the previous number by the volume of peroxide solution you would add to your medium or substrate if it were really a 3% solution (this volume is given in appropriate section of this manual, for instance, in the section on agar culture, you will find that you would need to add 6 mls of 3% peroxide for 1 liter of pressure-cooked agar medium).


Carpe Diem

uemura

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Re: Concentrating 35% Peroxide
« Reply #6 on: December 20, 2001, 04:55:00 PM »
Side note: Refrigeration of a 30-35% H2O2 solution did not give any H2O cristallisation after 48 hours in fridge at -20DegC The above reference asks for -55DegC freeezing. Lession learned: Concentration via freezing isn't possible 'on the fly'

abc123

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Re: Concentrating 35% Peroxide
« Reply #7 on: December 22, 2001, 04:18:00 PM »
uemara if the performic is the reason for the concentration of peroxide...find some 98% HCOOH then with 30 % H2O2..allilte water would then have to be added to get correct concentrations

even with say 70 or 80% HCOOH and 35% peroxide the ratio would be off but swim would guess would work OK because the peroxide is more important than the acid to have the correct concentration of....swim thinks so

abc123

Johny's in the basement mixing up the medicine...I'm on the pavement

noj

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Re: Concentrating 35% Peroxide
« Reply #8 on: December 22, 2001, 06:22:00 PM »
I found that in the freezer a 7% (according to 30 Volume) H2O2 froze into a slush with almost no liquid available. After finding another source I just tossed it.

A theory is a tool - not a creed. -J. J. Thomson

uemura

  • Guest
Re: Concentrating 35% Peroxide
« Reply #9 on: December 22, 2001, 11:52:00 PM »
abc123,
the reason uemura wants to concentrated h2o2 is to reduce the amount of water in the MeOH/MeCN epoxidation. Ritter provided a reference in which yield have been boosted by reducing the water in the rxn mix.
noj,
if your 7% h2o2 froze more or less completely perhaps uemura should start with a less concentrated solution in the hope that everything non-frozen is 62% h2o2?

Merry XMas to the Bees