BetaTest
Harmless
Posts: 10
Registered: 18-6-2011
Member Is Offline
Mood: No Mood
|
|
Hydrogen peroxide concentration by freezing I need to make 12% h2o2 from 3%
Hi everyone!
I'm trying to make an at home tooth whitening gel that needs a final concentration of 6% hydrogen peroxide, when means I need a stock of 12%(1:2
dilution). My local drug store only sells 3% hydrogen peroxide. Now I know that I can buy 30-35% online very easily but the problem for me is it costs
a lot. So I was reading another topic on this forum about people getting h2o2 to like 90% (not sure why) but they mentioned that you can get h2o2 to
62% by freezing. My question is how can I get 12-20% by freezing? I don't want it to get all the way up to 60% and I'm also not clear on the method
(just place it in the freezer and take out the ice cubes?). Also after I'm done with the freezing concentration, how do I estimate the final
concentration?
thanks to everyone who read this, any advice would be appreciated!
|
|
|
m1tanker78
National Hazard
Posts: 685
Registered: 5-1-2011
Member Is Offline
Mood: No Mood
|
|
15% H2O2 is 'typical' for me by the freezing method but 20% is doable. Example, 2 large bottles of 3% peroxide:
Open and drain half the contents of each bottle into 2 other STERILE and clean bottles of similar capacity. If possible, just use 2 empty peroxide
bottles. Stick the 4 half-filled bottles in the freezer and leave for at least 12-24 hours. After the contents are COMPLETELY frozen solid, turn them
upside down (in the freezer). Make sure they're capped well and don't let them warm up (leaving the freezer door open too long, etc.).
Have a clean, sterile plastic or glass bottle handy with a small funnel. Every hour or so, quickly remove one bottle at a time from the freezer but
keep them upside down. Carefully uncap and pour the contents of the cap into your container. You'll typically only get a few drops at a time.
Read up on hydrogen peroxide safety! WEAR GLOVES AND GOGGLES. Make sure everyone in your house knows what you're up to. That way, the Mrs. or kids
don't knock the containers over or get 'stung'. DO NOT PLACE THE FULL BOTTLES IN THE FREEZER.
Tank
|
|
|
ScienceHideout
Hazard to Others
Posts: 391
Registered: 12-3-2011
Location: In the Source
Member Is Offline
Mood: High Spin
|
|
You can get 12% from any beauty or makeup store. Ask for 40 volume peroxide. I've found 'clairoxide' brand 40vol is 12%. If you don't wanna go in
there, ask your mom!
BTW: It is quite pure, too!
[Edited on 19-6-2011 by ScienceHideout]
hey, if you are reading this, I can't U2U, but you are always welcome to send me an email!
|
|
|
BetaTest
Harmless
Posts: 10
Registered: 18-6-2011
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by m1tanker78  | 15% H2O2 is 'typical' for me by the freezing method but 20% is doable. Example, 2 large bottles of 3% peroxide:
Open and drain half the contents of each bottle into 2 other STERILE and clean bottles of similar capacity. If possible, just use 2 empty peroxide
bottles. Stick the 4 half-filled bottles in the freezer and leave for at least 12-24 hours. After the contents are COMPLETELY frozen solid, turn them
upside down (in the freezer). Make sure they're capped well and don't let them warm up (leaving the freezer door open too long, etc.).
Have a clean, sterile plastic or glass bottle handy with a small funnel. Every hour or so, quickly remove one bottle at a time from the freezer but
keep them upside down. Carefully uncap and pour the contents of the cap into your container. You'll typically only get a few drops at a time.
Read up on hydrogen peroxide safety! WEAR GLOVES AND GOGGLES. Make sure everyone in your house knows what you're up to. That way, the Mrs. or kids
don't knock the containers over or get 'stung'. DO NOT PLACE THE FULL BOTTLES IN THE FREEZER.
Tank |
So once the h2o2 is completely frozen and still in the freezer inverted, what causes the more concentrated h2o2 to thaw and drip down? Also how
concentrated would you expect it to be (the 15% you mentioned)?
Thanks!
|
|
|
BetaTest
Harmless
Posts: 10
Registered: 18-6-2011
Member Is Offline
Mood: No Mood
|
|
So I took 16 oz of 3% h2o2 then froze and inverted. I ended up with about 8 mls of fluid. How do I estimate the concentration of the liquid I
collected? Also how much should I expect to collect by this method?
Any advice would be most appreciated!
|
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
Why not just buy ebay 35% H<sub>2</sub>O<sub>2</sub> and dilute it accordingly?
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
| Quote: Originally posted by BetaTest | So I took 16 oz of 3% h2o2 then froze and inverted. I ended up with about 8 mls of fluid. How do I estimate the concentration of the liquid I
collected? Also how much should I expect to collect by this method?
Any advice would be most appreciated! |
Decompose fully the H<sub>2</sub>O<sub>2</sub> with a MnO<sub>2</sub> or other proper catalyst and measure the
volume of evolved O<sub>2</sub> with an inverted graduated cylinder and quantify.
[Edited on 1-7-2011 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
not_important
International Hazard
Posts: 3873
Registered: 21-7-2006
Member Is Offline
Mood: No Mood
|
|
You start with 3%, you hope to get 30% - ten times as concentrated, should be about 1/10 the volume of liquid.
As for the MnO2 decomposition for testing the strength, to determine how much solution to test remember that a 3% solution of H2O2 will generated 10
times its volume of O2, a 6% solution 20 times the O2, and so on with 30% generating 100 times its own volume of O2.
|
|
|
497
National Hazard
Posts: 778
Registered: 6-10-2007
Member Is Offline
Mood: HSbF6
|
|
35% is available in nursery stores and greenhouses for use in hydroponics... It's kinda expensive, at least where I am, but I bet it would still end
up cheaper than freezing 3%.. Also search for "bacquacil"
.
|
|
|
cyanureeves
National Hazard
Posts: 744
Registered: 29-8-2010
Location: Mars
Member Is Offline
Mood: No Mood
|
|
there is another thread that deals with h2o2 right here. i used their method by pouring the contents into a glass and waiting until 50% was frozen
then i quickly filtered the ice with a coffee filter and kept the liquid. by the time i was done with two bottles my finger tips were bleached white.
that stuff itches at first but then starts to burn non stop for about 30 sec. i dont know how concentrated it is but one drop will burn the palm of my
hand until it leaves a white chalky blotch. i also used a burner at about 200 deg. and evaporated 2/3 of the liquid and got the same strength as
freezing. i also left it out in the west texas sun inside a pickle jar and let it evaporate 2/3 and got mostly water. i guess it has to be evaporated
quickly and just under boiling but i noticed that it could take more heat without bubbling after 2/3 was evaporated on the burner.it surprised me that
the remaing 1/3 would hardly steam the side of the glass while heated.
[Edited on 2-7-2011 by cyanureeves]
[Edited on 2-7-2011 by cyanureeves]
|
|
|
#maverick#
Hazard to Others
Posts: 209
Registered: 7-4-2011
Member Is Offline
Mood: hybridised
|
|
I believe zhmapper has a vid on u tub of him concentrating h2o2 by heating it gently so it doesn't decompose. I'm on my phone otherwise I woulda
posted a link
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Check out this thread. http://www.sciencemadness.org/talk/viewthread.php?tid=15881
Me and tank went back and forth on the topic of freezing vs evaporation. While I never did the tests I mentioned, I still use the slow evaporation
with a dry air stream/aspiration method.
[Edited on 2-7-2011 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
BetaTest
Harmless
Posts: 10
Registered: 18-6-2011
Member Is Offline
Mood: No Mood
|
|
wow guys thanks to all for taking the time to reply. I'm going to try some version of the heat/evaporation when I get some time. For the moment what
really has me thinking is the use of a catalyst and measurement of the evolved gas. It was mentioned earlier, that this could be done with an inverted
cylinder... does anyone have a link or more information on how to properly setup such an apparatus?
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I seem to remember a similar topic being posted years ago in the E+W forum.
Apparently, solutions of H2O2 can be concentrated up to 62% (?) by freezing out the water, but after the solution reaches that concentration the H2O2
will begin freezing out; I do not remember the exact percentage, but I am sure it was somewhere between 60-80%. This was just a post I remember,
cannot find any information about it now. I also cannot remember whether the poster said the H2O2 begins to freeze out with the water, or whether it
begins to freeze out separately. I think it might have been separately, in which case it would be possible to obtain 85% + concentrations, but one
would have to know the exact percentage at which the H2O2 would begin to freeze out, and have some way of measurement, to know when to discard all the
water-ice crystals that had formed so that any additional solid that freezes out would be 85%+ H2O2.
[Edited on 4-7-2011 by AndersHoveland]
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
|
|
|
cyanureeves
National Hazard
Posts: 744
Registered: 29-8-2010
Location: Mars
Member Is Offline
Mood: No Mood
|
|
this forum also talks about % on the other h2o2 thread but it is too much work for me. they said it is only a 1 deg. difference freezing point between
water and h2o2. i had to make about 3 or 4 extractions because when the solution freezes to half it quickly thaws to 1/4 of ice and the just below
boiling actually takes about 6 to 7 hrs. letting the sun do it took about 6 days and it was very weak.
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Don't use the sun, I would think the UV would increase decomposition. 4-5 hours to bring 500ml to <100ml with gentle heating (surface temp
<=170F) isn't a raw deal. Using a little blower or aspirator speeds things up a good bit. Even using non-dried air from a fish tank blower knocks
about an hour off.
Anders, I would think it would be very hard to get anything approaching high-test with freezing due to the diminishing variance in freezing points.
Heating/evaporating also cant give you much higher than 25%-35% because as the solution becomes more concentrated, more heat is required to drive of
the water. More heat = more decomposition.
All in all the best bet is to just buy 30% food grade. It is readily available in most places. If higher concentrations is needed, just pull a little
vacuum on it and boil off the water. Be careful though. anything over 70% is very wicked I would imagine, and I bet anything approaching 90% could
undergo explosive decomposition with the slightest provocation. (ex. dust or crud in the glass, etc, etc.)
[Edited on 4-7-2011 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
I also had the idea of adding acetone peroxide (diluted in pure acetone for safety) to water. After several days in the dark, the acetone peroxide
should hydrolyze into acetone and hydrogen peroxide.
The hydrolysis is catalyzed by dilute acid- but too acidic and the equilibrium does not favor any change.
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
| Quote: Originally posted by BetaTest | wow guys thanks to all for taking the time to reply. I'm going to try some version of the heat/evaporation when I get some time. For the moment what
really has me thinking is the use of a catalyst and measurement of the evolved gas. It was mentioned earlier, that this could be done with an inverted
cylinder... does anyone have a link or more information on how to properly setup such an apparatus?
|
Decompose the peroxide and lead the gas into the inverted cylinder filled with water. Measure the volume of gas that displaced the water.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
m1tanker78
National Hazard
Posts: 685
Registered: 5-1-2011
Member Is Offline
Mood: No Mood
|
|
Botonist's drawing sums it up; I'll just add a few points:
If you don't have a graduated cylinder, use any type of clear container of known and uniform inner diameter. Run a piece of electrical tape
from top to bottom (lengthwise). Use a sharpie to mark the initial water level then make another mark after the decomp. Measure between the 2 marks
and calculate the volume of water displaced.
My decomp container allowed me to load the MnO2 into a bent plastic "J" tube (attached to the lid) so that I could seal the container before
contacting with the peroxide. You could probably get away with pouring the peroxide and then dropping a smaller tube containing the catalyst in the
chamber. Once sealed, tilt or shake a little to release the catalyst.
Dilute the peroxide in such a way that it won't decompose so fast as to warm the mixture (give false results). On the other hand, you don't want it to
be so diluted that it takes a long time to complete the test. It should take no longer than 3 minutes.
After the initial stream of bubbles dies down, swirl the decomp container but make sure you don't squeeze the bottle (if it's
plastic). Again, this will give false results.
It may take a few trial and error runs before you get it dialed in. Be sure to rinse all of the MnO2 out after each test.
+++++++++++++++++
| Quote: | | So once the h2o2 is completely frozen and still in the freezer inverted, what causes the more concentrated h2o2 to thaw and drip down? Also how
concentrated would you expect it to be (the 15% you mentioned)? |
It doesn't really freeze at all. It gets trapped within the ice crystals and slowly makes its way down through the ice. Cold, concentrated peroxide
sticks to surfaces better than water (you may have noticed that when emptying the peroxide bottle caps) so it takes time and never completely drains.
You might be tempted to tap or bang the bottles before you uncap them. Doing so will knock small chunks of ice into the cap, diluting the harvest.
My minimum has consistently been 12% while my maximum concentration is usually 18%. I've been rewarded with 2 or 3 20% harvests by being very careful
but it isn't worth all the trouble to squeeze out an extra 2%. I almost always dilute down to 12% anyway so it works out.
Tank
[Edited on 7-6-2011 by m1tanker78]
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
Good idea with the "bent plastic "J" tube" attachment.
About the raise in temperature, I also worried about that. I guess adding the catalyst slowly to allow time for heat dissipation would help keep
things STP. I thought of adding the H<sub>2</sub>O<sub>2</sub> drop-wise into a catalyst bed, but that may
even get hot enough to steam. I wonder if a simple way could be devised to add the MnO<sub>2</sub> a little at a time, while keeping a
sealed chamber. Maybe some variation on the "J" attachment.
Maybe a large, room-temperature water bath would work?
I need to stop armchair experimenting and do some trials I guess...
[Edited on 6-7-2011 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
m1tanker78
National Hazard
Posts: 685
Registered: 5-1-2011
Member Is Offline
Mood: No Mood
|
|
| Quote: | | I thought of adding the H2O2 drop-wise into a catalyst bed, but that may even get hot enough to steam. |
If your decomp gets too hot and/or proceeds too quickly then adjust the quantity of your unknown peroxide as well as how much water it's diluted in.
For example, if 10mL of unknown peroxide + 30 mL water is giving you a run for your money, half the peroxide or double the water. Make sure you take
note of the unknown peroxide quantity - the added water only slows the decomp but produces exactly the same quantity of gas at the end.
Don't use an excessive amount of catalyst. This generates unwanted heat as well. I may have already mentioned this: Don't forget to swirl (but not
squeeze) the decomp chamber!
Tank
|
|
|
aliced25
Hazard to Others
Posts: 262
Registered: 31-7-2010
Member Is Offline
Mood: No Mood
|
|
Found some decent articles on increasing the molarity of H2O2 in solution.
Now can anyone think of a way to improve the sulphuric acid/vacuum pump model? Does H2O2 react with other absorbents, like H3PO4, MgSO4(anhydrous),
CaCl2(anhydrous), etc? Then removal of the water from the mixture in the gas phase might be feasible, especially under vacuum, where the boiling point
of the mixture would presumably be lowered appreciably.
Attachment: Maas.Herzberg.The.Properties.of.Pure.Hydrogen.Peroxide.II.pdf (152kB)
This file has been downloaded 852 times
Attachment: Maas.Hatcher.The.Properties.of.Pure.Hydrogen.Peroxide.III.pdf (536kB)
This file has been downloaded 862 times
Attachment: Maas.Sulfuric.Acid.Concentrator.and.Vacuum.Pump.pdf (320kB)
This file has been downloaded 1108 times
Attachment: Mass.Hatcher.The.Properties.of.Pure.Hydrogen.Peroxide.I.pdf (1.6MB)
This file has been downloaded 1180 times
[Edited on 28-4-2013 by aliced25]
Attachment: Sulaymon.etal.Concentration.of.H2O2.by.Batch.Distillation.Column.pdf (1.2MB)
This file has been downloaded 1074 times
From a Knight of the Realm: "Animated movies are not just for kids, they're also for adults who do a lot of drugs." Sir Paul McCartney
|
|
|
zed
International Hazard
Posts: 2283
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
Or, you could just put some 3% on a dinner plate and allow it to evaporate.
|
|
|
Bot0nist
International Hazard
Posts: 1559
Registered: 15-2-2011
Location: Right behind you.
Member Is Offline
Mood: Streching my cotyledons.
|
|
unless you live in a hot, dry climate, this takes days and days, even weeks, if ever, to get to >25%. After reading about the guy in Arizona, I
tried it, (in Ga). No luck at all. Its was in a clean place with minimal dust too. After 5 day, only a very slight reduction of volume was observed.
The evaperative proccess must be sped up with gentle heating and a dry, clean air flow over the surface. Mag stirring help to keep the heating even,
and as long as the surface temp doesnt exceed ~180f, decomp is minimal.
Pouring a liter of 3% peroxide in a clean glass cassarole dish, and putting it in your oven, set to 170f does work though. After 8-12 hours the volume
is reduced to around 50-80ml, and what remians is very close to 30% H2O2, so be carefull...
[Edited on 3-5-2013 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
|
|
|
Pyro
International Hazard
Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline
Mood: No Mood
|
|
since we are talking about it. is 130vol. H2O2 35 or 40%? in our cleaning cupboard I found a bottle with 1l 130vol that had cost 7eur. It was, however
very old and nearly empty and I used to clean out my fish tank (After I removed the filters, heaters, fish and plants.
Is this conc. worth buying?
all above information is intellectual property of Pyro.  |
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
