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how to make concentrated hydrogen peroxide?


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#1 chilled_fluorine

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Posted 26 August 2012 - 02:17 AM

On someone's blog about h2o2 that I found randomly (sounds stupid, right? I did find it interesting though), I read that you can make exceptionally strong h2o2 with sodium percarbonate. Does anyone know how I could do this, and get a 30-40% concentration? Dilution is allowed, but I don't like the idea of messing with test grade+ HP more than I have to... Anything above 40 just frightens me, it's nasty stuff. Apparently the other product is sodium carbonate, could I remove that with a coffee filter, or would it (the sodium carbonate) dissolve in the solution? Please try to stay on topic, not that you wouldn't. This is meant to be a practical exercise, cost effectiveness is the overriding concern.
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#2 chilled_fluorine

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Posted 26 August 2012 - 06:23 PM

On someone's blog about h2o2 that I found randomly (sounds stupid, right? I did find it interesting though), I read that you can make exceptionally strong h2o2 with sodium percarbonate. Does anyone know how I could do this, and get a 30-40% concentration? Dilution is allowed, but I don't like the idea of messing with test grade+ HP more than I have to... Anything above 40 just frightens me, it's nasty stuff. Apparently the other product is sodium carbonate, could I remove that with a coffee filter, or would it (the sodium carbonate) dissolve in the solution? Please try to stay on topic, not that you wouldn't. This is meant to be a practical exercise, cost effectiveness is the overriding concern.


Would someone mind going to this
http://www.sciencema...p?tid=17770Page and telling me what it is about? I can't view it on my browser
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#3 elementcollector1

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Posted 27 August 2012 - 05:29 PM

Topic died. I hear a better, more efficient way is to place some 3% on a hotplate and heat it to 99 C (just under boiling). After a few hours, it'll evaporate right down to a good concentration.
Source:
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#4 chilled_fluorine

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Posted 25 September 2012 - 12:24 AM

Topic died. I hear a better, more efficient way is to place some 3% on a hotplate and heat it to 99 C (just under boiling). After a few hours, it'll evaporate right down to a good concentration.
Source: http://www.youtube.c...h?v=pMLy5sVqX38


I'm afraid it will decomp. on me. Bad experience with 55% once... No one was hurt, lucky thing. I don't know why it took me so long to realize you had replied.
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#5 elementcollector1

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Posted 25 September 2012 - 05:39 AM

I've had my own experiences with heated H2O2... not fun.
However, that was at about 300 C on a stoveplate, and I had no clue about the dangers.
95-99 C wouldn't boil the water, it would basically evaporate it at an elevated rate. If you're worried, lower the temperature: This slows things down while being safer in terms of sudden decomposition.
I've had to wait for months for certain topics to get replied to... In fact I just received a reply email a few days ago, about a query I had sent over a year ago. Things like this happen... :D
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#6 chilled_fluorine

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Posted 25 September 2012 - 12:10 PM

I've had my own experiences with heated H2O2... not fun.
However, that was at about 300 C on a stoveplate, and I had no clue about the dangers.
95-99 C wouldn't boil the water, it would basically evaporate it at an elevated rate. If you're worried, lower the temperature: This slows things down while being safer in terms of sudden decomposition.
I've had to wait for months for certain topics to get replied to... In fact I just received a reply email a few days ago, about a query I had sent over a year ago. Things like this happen... :D


Again, sorry. I've noticed that at that temp, at least 50% of it decomps. in the time it takes to do any useful concentrating. I miss when 55% was EASILY available, before 9/11. Damn terrorists. Now I can hardly buy anything more dangerous than bleach, without being put on a watch list. Ironically enough, it is very easy to make explosives from bleach... Maybe it'll become the new ammonium nitrate, ridiculously regulated.
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#7 Ronald Hyde

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Posted 3 October 2012 - 08:13 PM

Very dangerous. Even just in ordinary handling. The least bit of contamination can set of fires and explosions.
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#8 chilled_fluorine

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Posted 3 October 2012 - 08:34 PM

Very dangerous. Even just in ordinary handling. The least bit of contamination can set of fires and explosions.


You're going to need to be more specific if you actually want a response. Is bleach dangerous? Is 55% h2o2 dangerous? Are explosives dangerous? I've never made explosives with bleach. If, in a purely hypothetical scenario, I were to make the same type, I would use very pure KClO3.
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#9 Ronald Hyde

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Posted 3 October 2012 - 09:01 PM

You're going to need to be more specific if you actually want a response. Is bleach dangerous? Is 55% h2o2 dangerous? Are explosives dangerous? I've never made explosives with bleach. If, in a purely hypothetical scenario, I were to make the same type, I would use very pure KClO3.


A friend of mine worked at a hotel, some German guests were staying. There was a little earthquake, they ran down
to front desk and said 'Was that an earthquake? We didn't get any warning.' No response was needed, it's more
like a heads-up for anyone doing this.
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#10 chilled_fluorine

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Posted 4 October 2012 - 03:01 AM

A friend of mine worked at a hotel, some German guests were staying. There was a little earthquake, they ran down
to front desk and said 'Was that an earthquake? We didn't get any warning.' No response was needed, it's more
like a heads-up for anyone doing this.


If there had been a real earthquake in my state in the last 500 years, yeah, I might worry. When I used to do this stuff, I would string them up high in a sturdy oak for safe storage. Nice copper wool wrapping, to stop those pesky squirrels. Stay away from my HMTD, stupid squirrels! I can only imagine what the neighbors think of me.
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#11 elementcollector1

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Posted 7 October 2012 - 06:34 PM

If there had been a real earthquake in my state in the last 500 years, yeah, I might worry. When I used to do this stuff, I would string them up high in a sturdy oak for safe storage. Nice copper wool wrapping, to stop those pesky squirrels. Stay away from my HMTD, stupid squirrels! I can only imagine what the neighbors think of me.


...
Yeah, I haven't had a 'real' earthquake in my lifetime. Lots of drills, though.
I did a quick search on Sciencemadness and found the following:

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.

I also ran across a few sources on the hundreds of forums about H2O2 that said heating gently under vacuum can get you to ~17%. I wish either of these methods got to 30%, but don't we all.
Also,
"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""
http://www.sciencema...d.php?tid=15881 is another good forum to read.
You can test the strength of the peroxide by measuring how much pain you feel when pouring it on your fingers! XP
But seriously, don't try that.

Edited by elementcollector1, 7 October 2012 - 06:36 PM.

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#12 chilled_fluorine

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Posted 13 October 2012 - 08:03 PM

...
Yeah, I haven't had a 'real' earthquake in my lifetime. Lots of drills, though.
I did a quick search on Sciencemadness and found the following:

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.

I also ran across a few sources on the hundreds of forums about H2O2 that said heating gently under vacuum can get you to ~17%. I wish either of these methods got to 30%, but don't we all.
Also,
"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""
http://www.sciencema...d.php?tid=15881 is another good forum to read.
You can test the strength of the peroxide by measuring how much pain you feel when pouring it on your fingers! XP
But seriously, don't try that.


I've heard of the freezing and heating methods before, but I can get VERY cheap percarbonate and would really like to try that method. Largely out of curiosity, but still. Concentrations that high are just too tempting... Once we made 85-ish percent with my highschool buds. I really wish I could remember how, as scary as it is. Do you have any info on the percarb method, ignoring wether or not there are better ways? I wasn't able to find anything. The bacquacil looked like very interesting stuff. A gallon of 27 for 15 dollars... Do you know anything else about it? Stabilizers, if any? Hazmat fees? What stores I could buy it at? Right now, it looks like my best option...
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#13 elementcollector1

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Posted 16 October 2012 - 05:22 PM

I've heard of the freezing and heating methods before, but I can get VERY cheap percarbonate and would really like to try that method. Largely out of curiosity, but still. Concentrations that high are just too tempting... Once we made 85-ish percent with my highschool buds. I really wish I could remember how, as scary as it is. Do you have any info on the percarb method, ignoring wether or not there are better ways? I wasn't able to find anything. The bacquacil looked like very interesting stuff. A gallon of 27 for 15 dollars... Do you know anything else about it? Stabilizers, if any? Hazmat fees? What stores I could buy it at? Right now, it looks like my best option...



My best guess would be to dissolve the percarbonate in lukewarm water, then chill overnight. Filter the insoluble contaminants, and you've got a slightly stronger, somewhat alkaline solution of H2O2.
Well, that's odd. Bacquacil is apparently Polymeric Biguanide Hydrochloride, which has nothing to do with H2O2. It's an oxidising agent nonetheless, but no mention of H2O2 anywhere in the MSDS.
MSDS: http://www.poolquip....ds/Baquacil.pdf
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#14 John Cuthber

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Posted 16 October 2012 - 08:56 PM

How do you think they make the percarbonate?
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#15 chilled_fluorine

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Posted 19 October 2012 - 01:18 AM

My best guess would be to dissolve the percarbonate in lukewarm water, then chill overnight. Filter the insoluble contaminants, and you've got a slightly stronger, somewhat alkaline solution of H2O2.
Well, that's odd. Bacquacil is apparently Polymeric Biguanide Hydrochloride, which has nothing to do with H2O2. It's an oxidising agent nonetheless, but no mention of H2O2 anywhere in the MSDS.
MSDS: http://www.poolquip....ds/Baquacil.pdf


I think I saw what you are talking about as well, but the bacquacil OXIDIZER is 27% h2o2, apparently with stabilizers. They also have algae removers and other pool chemicals, but I'm positive the oxidizer is h2o2. Said so right on the website. I'm sure there's another method to make the peroxide, they could never sell a product that would make peroxide that dangerous if someone accidentally dissolved it in water. Your method sounds like it could get <10%, but I'm looking for stronger. I thought it had something to do with a vacuum... Anyways, you have anything else about the bacquacil?

How do you think they make the percarbonate?


Ummm... H2O2 and sodium carbonate? Care to explain how that question is useful?
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#16 elementcollector1

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Posted 19 October 2012 - 03:31 AM

I think I saw what you are talking about as well, but the bacquacil OXIDIZER is 27% h2o2, apparently with stabilizers. They also have algae removers and other pool chemicals, but I'm positive the oxidizer is h2o2. Said so right on the website. I'm sure there's another method to make the peroxide, they could never sell a product that would make peroxide that dangerous if someone accidentally dissolved it in water. Your method sounds like it could get <10%, but I'm looking for stronger. I thought it had something to do with a vacuum... Anyways, you have anything else about the bacquacil?



Ummm... H2O2 and sodium carbonate? Care to explain how that question is useful?

Nope, not really...

What would you think about freezing regular 3% to get around 15% H2O2, and then vacuum distilling that? Could work, or could give you the 20% variety?
I can try freezing some regular H2O2, but I wouldn't know how to titrate (MnO2, calculate moles of oxygen released?)

Edited by elementcollector1, 19 October 2012 - 03:35 AM.

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#17 weiming1998

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Posted 19 October 2012 - 11:00 AM

Nope, not really...

What would you think about freezing regular 3% to get around 15% H2O2, and then vacuum distilling that? Could work, or could give you the 20% variety?
I can try freezing some regular H2O2, but I wouldn't know how to titrate (MnO2, calculate moles of oxygen released?)


Vacuum distillation of 15% H2O2 should give H2O2 of a high concentration, since H2O2 is much less volatile than water. If one distillation doesn't give a high quality product, then repeated distillation would eventually yield H2O2 with a high concentration. Fractional (vacuum) distillation would take less time, though, if you have the equipment.

As for titration, acidified KMnO4 should do, reducing the H2O2 to Mn2+. If your KMnO4 was acidified, no MnO2 should form and catalyse the decomposition of H2O2. Titration with a known hypochlorite solution also works, but finding an indicator for it would be difficult (I'd go with CuSO4 as the indicator, since Cu(ClO)2 is insoluble).
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#18 chilled_fluorine

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Posted 19 October 2012 - 05:17 PM

Vacuum distillation of 15% H2O2 should give H2O2 of a high concentration, since H2O2 is much less volatile than water. If one distillation doesn't give a high quality product, then repeated distillation would eventually yield H2O2 with a high concentration. Fractional (vacuum) distillation would take less time, though, if you have the equipment.

As for titration, acidified KMnO4 should do, reducing the H2O2 to Mn2+. If your KMnO4 was acidified, no MnO2 should form and catalyse the decomposition of H2O2. Titration with a known hypochlorite solution also works, but finding an indicator for it would be difficult (I'd go with CuSO4 as the indicator, since Cu(ClO)2 is insoluble).


I've always diluted to a safe concentration, added mno2, calculated how many times more gas than original h2o2, then compared it to a chart that relates % to gas count. I find it much easier than chemical titration.
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#19 elementcollector1

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Posted 21 October 2012 - 09:04 PM

Just put some 3% H2O2 in the freezer an hour ago, and already half the mass is frozen. It appears to freeze sooner than regular water. Could repeated freezing work?

EDIT: Ahaha, my flesh burned for a bit there. Anyway, results were right on target with ~30%, as I spilled some on myself and noticed immediate, short-term whitening of the skin and a very strong 'burning' feeling for a few seconds. It wasn't the icy temperature, it was too short (and my hands were still numb anyways).

Edited by elementcollector1, 22 October 2012 - 04:25 AM.

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#20 elementcollector1

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Posted 23 October 2012 - 01:18 AM

Just put some 3% H2O2 in the freezer an hour ago, and already half the mass is frozen. It appears to freeze sooner than regular water. Could repeated freezing work?

EDIT: Ahaha, my flesh burned for a bit there. Anyway, results were right on target with ~30%, as I spilled some on myself and noticed immediate, short-term whitening of the skin and a very strong 'burning' feeling for a few seconds. It wasn't the icy temperature, it was too short (and my hands were still numb anyways).


On another note, did a little research on ScienceMadness. Apparently, below a 35% H2O2 eutectic, the higher concentration of H2O2 freezes first, allowing for concentration. Above that, the mix freezes all at once, making separation by repeated freezings impossible.
^Don't know if I worded that quite right, but I hope you got the gist.
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