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toothpick93
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Leaching H2O2 out of Sodium Percarbonate
I done a little research with the forum search engine to see if people have tried to use a solvent to leach
H<sub>2</sub>O<sub>2</sub> out of Sodium percarbonate. it was mentioned a few times but those comments were ignored. What
solvent is able to leach out H<sub>2</sub>O<sub>2</sub> out of Sodium percarbonate leaving Sodium Carbonate behind?
The Wiki states:
"Sodium percarbonate can be used in organic synthesis as a convenient source of anhydrous H<sub>2</sub>O<sub>2</sub>, in
particular in solvents that cannot dissolve the carbonate but can leach the H<sub>2</sub>O<sub>2</sub>out of it."
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papaya
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I did it with 50% H2SO4 , temperature control is needed (ice water, etc.) and you must add solid to acid. Once I tried to get H2O2 out of washing
powder which stated to contain 30% percarbonate, interesting thing I noted if you calculate percarbonate contains about 1/3 H2O2 per mass, so 30% of
it must give me only about 9% peroxide, taking into account that I add also acid I had to end up with even lower H2O2 concentration. However I was
very surprised when I tried and got very concentrated H2O2 solution, which would stain your skin in seconds and also reactions of it were very fast.
The only reason I figured out - the sulphate forming is in the form of hydrate - perhaps decahydrate, which takes a lot of additional water into
precipitate under these conditions so when you filter it out, the liquid is really concentrated H2O2 solution. I think one must try to calculate
optimal acid concentration for the best results, which I didn't do.
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AJKOER
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With respect to organic solvent, I would try a little Ethanol as Na2CO3 does not dissolve in it, while H2O2 does. Other alcohols may work as well.
But can you really physically work with a larger mass of the percarbonate relative to the Ethanol to increase concentration? Wouldn't the alcohol
evaporating be an issue, for example?
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blogfast25
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Considering just how widely available and cheap hydrogen peroxide solutions are this is a waste of time and effort, IMHO.
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ElectroWin
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Quote: Originally posted by blogfast25  | | Considering just how widely available and cheap hydrogen peroxide solutions are this is a waste of time and effort, IMHO. |
if we did all reactions based on the expense of the products we would never learn anything.
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toothpick93
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| Quote: Originally posted by blogfast25 | | Considering just how widely available and cheap hydrogen peroxide solutions are this is a waste of time and effort, IMHO. |
whats the fun in buying hydrogen peroxide when you could be able to make it at home?
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papaya
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If acid doesn't interfere with what you do - the way I described seems best to me - you get fairly concentrated peroxide. You may also neutralize acid
after all if needed, and peroxide is not that easily/safely available everywhere, unlike stain removers. I forgot to say - don't do this with HCL, as
chlorine gas is evolved, and peroxide reduced to water ( I got ''0'' yield).
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blogfast25
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Yeah, I mean, what's the fun in buying doughnuts when you can make them yourself, eh?
Once you start experimenting in earnest you want a chemical larder, so you can use things off the shelf, instead of having to make everything yourself
and waste various science foras' bandwidth. 
Talk about learning: quantitatively determining how much peroxide there is in that commercial product would be an interesting learning curve.
Trying to isolate a product that you can pick up probably from the neighbouring shelf, just isn’t very productive, even didactically speaking.
[Edited on 18-5-2013 by blogfast25]
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papaya
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"Trying to isolate a product that you can pick up probably from the neighbouring shelf, just isn’t very productive, even didactically speaking."
Falling into suspicion because you bought such a 'harmless' compound isn't fun..
[Edited on 18-5-2013 by papaya]
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blogfast25
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| Quote: Originally posted by papaya | "Trying to isolate a product that you can pick up probably from the neighbouring shelf, just isn’t very productive, even didactically speaking."
Falling into suspicion because you bought such a 'harmless' compound isn't fun..
[Edited on 18-5-2013 by papaya] |
This isn't going to happen with a product that is so widely used and has a gazillion applications. It's very OTC. Unless you'd order it by the barrel
load or are seeking 100 % H2O2 you can't really be suspected of anything, lest they want to suspect you of EVERYTHING.
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papaya
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Highly depends where you live, there are places on the globe that even mineral acids are banned, not to say when they catch you, you are guilty a
priori.. but this is offtop, topic starter just asked HOW not IF..
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toothpick93
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| Quote: Originally posted by blogfast25 |
Yeah, I mean, what's the fun in buying doughnuts when you can make them yourself, eh?
Once you start experimenting in earnest you want a chemical larder, so you can use things off the shelf, instead of having to make everything yourself
and waste various science foras' bandwidth.
OK, your right about that. where i live its hard to find good sources of peroxide, i only can find 3-6% stuff for about $5-$8. pretty expensive for
about 50-100mls |
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woelen
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I only partially agree with blogfast25. At some places it indeed is remarkably difficult to obtain hydrogen peroxide at more than 3% concentration.
Where I live is such a place. With the new upcoming EU-regulations, the availability of hydrogen peroxide will be reduced further. I expect this
chemical to be really unavailable by the start of 2014 in more than 3% concentration, maybe halfway 2014.
Sodium percarbonate, on the other hand, can be purchased without limit, as it is sold as a so-called "green" bleach powder. I have found supplies of
100% Na2CO3.xH2O2.H2O (IIRC x = 1.5 or 2). This has a decent amount of peroxide and when treated with moderately concentrated H2SO4 you indeed get
fairly concentrated solutions, with only a small amount of Na2SO4 left in solution. For most experiments it is good enough.
It would, however, be a good thing if the people who try to isolate H2O2 from this "green" bleach work out the gory details of isolating the H2O2 and
work quantitatively so that more can be said about the concentration and the purity. It also would be good to search for sources of pure sodium
percarbonate. They should not be difficult to find. Online sources exist for this chemical as well. It is not a suspect thing if you order this
material.
[Edited on 21-5-13 by woelen]
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Finnnicus
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In my area (Victoria au, if anyone can help!) H2O2 is either 3%/200ml/10$ or 7%/50ml/10%  ! So this seems like a viable way to get it, at least economically. When I am at the supermarket next I will write down my prices -at
100% yield.
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papaya
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According to wiki sodium percarbonate is Na2CO3·1.5H2O2, when you calculate you have only about 32.4% peroxide by mass. In my case the bleaching
powder was written to contain >30% percarbonate, thus 32.4% of 30% gives about 9.7% of H2O2 per mass, and as you add some acid/water you expect to
get even less concentrated H2O2 solution. However, what I want to point out, with sulfuric acid as I mentioned earlier I got very concentrated
solution (didn't do titration to say), this may be due to Na2SO4 complexing water and getting out of solution (precipitates). Only quick test I could
do to estimate concentration (not the best way  ) - to few mls of this acid/H2O2
few ml of acetone were added in the test tube and the volume of liquid turned into gel in a minute due to solid product formation, which you can't
achieve with 30% (I believe, I don't have it and didn't test).
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woelen
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Another advantage of sodium percarbonate over solutions of H2O2 in water is that the former has unlimited shelf life, while H2O2 slowly deteriorates
over time. I purchased 27% H2O2 a few years ago, but its concentration now is much lower. I did a rough test with it and measured how many milliliters
of oxygen were obtained per ml of liquid. I do not remember the details anymore of the computation, but I found that the concentration was well below
20%.
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ScienceSquirrel
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I am not sure how effective these regulations will be on hydrogen peroxide.
It is used on a tonnage scale for all sorts of things from bleaching to waste water treatment and food preparation.
I use a lot for equipment rinsing as it destroys chlorine based chemicals plus it is a strong bactericide itself and breaks down to water and oxygen.
Formalin has been restricted but it is still widely available, the koi carp keepers use it as a general cure all in their ponds. The same goes for
ammonium sulphamate, this was supposed to disappear off the market when it's licence for use as a weedkiller was withdrawn but it is still used a lot,
albeit illegally. The vendors helpfully tell you that it is dangerous to plants!
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papaya
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I want to ask for the easiest(doable) method of quantitative analysis for sodium percarbonate containing powders, titration with KJ and the J2 is out.
Maybe some gas volume determination, will using some 1cm piece of platinum wire as a H2O2 decomposition catalyst work? Please share your
experience/methods in case if I want to do some analysis in the future.
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Bot0nist
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MnO2 catalyst and quantify the released 02 in an inverted graduated cylinder. search the H2O2 concentrating threads. Me and M1tanker made a nice
diagram and explanation in one of those threads.
[Edited on 28-5-2013 by Bot0nist]
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AndersHoveland
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Remember, H2O2 slowly decomposes under alkaline conditions. So the best way would be to add acid (but not hydrochloric, because chloride ions can
slowly catalyze decomposition also).
The basic compounds Na2CO3*H2O2 and CaO2 both seem to be stable, but only because they are solids. Add water and they slowly start to decompose.
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papaya
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Does this imply that it is possible to titrate percarbonate itself without addition of acid ?  (I thought acid is needed always if you want to form H2O2 in solution, or just dissolving in water is enough for
that?)
[Edited on 3-6-2013 by papaya]
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aliced25
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There is at least one brand selling on-line that states it is 100% Sodium Percarbonate, which could be useful:
http://chemistry.mdma.ch/hiveboard/rhodium/pdf/perborate-per...
Read that, see if it gives you any hints, by the looks of this paper (http://www.northeastern.edu/alert/assets/F1-A1_2012.pdf) it will form Triacteone peroxide with Acetone and it has been used to iodinate Arenes (http://www.usc.es/congresos/ecsoc/8/GOS/022/index.pdf). Whether it can be isolated would be interesting, Dioxiranes can be isolated, which would
make it a useful product in its own right (who the fuck wants to isolate peroxide and store it when you have it a nice stable package?) It has also
been used in the oxidative version of the Nef Reaction (http://mutuslab.cs.uwindsor.ca/green/4531/tet-2004-60-1017-b...). This search might give you some ideas (http://tinyurl.com/n8dhfc8) and that is just JACS. The use of it with acetic acid might be bloody useful, I just realised. I'll throw up some
papers on the subject:
Attachment: Bracken.Tietz.Analysis.of.Oxiclean.An.Interesting.Comparison.of.Percarbonate.Stain.Removers.pdf (91kB)
This file has been downloaded 740 times
Attachment: Bracken.Tietz.Supporting.Information.pdf (68kB)
This file has been downloaded 1061 times
Attachment: Kjonaas.Clemons.The.BaeyerVilliger.Reaction.with.TFA.and.Household.Sodium.Percarbonate.pdf (187kB)
This file has been downloaded 906 times
Attachment: Kjonas.Clemons.Supplemental.Material.pdf (189kB)
This file has been downloaded 1201 times
Attachment: Zhao.etal.SolidLiquid.Equilibrium.for.the.Quaternary.System.SodiumCarbonate.SodiumChloride.HydrogenPeroxide.Water.at.293 (44kB)
This file has been downloaded 644 times
What I find extremely interesting is that at least one of the cleaners examined had a lower content of sodium carbonate to percarbonate tjhan that
available from a reputable Chemical Supply Company. I wouldn't take that as
gospel in every case, titrate it and see.
[Edited on 5-6-2013 by aliced25]
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woelen
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| Quote: Originally posted by ScienceSquirrel | I am not sure how effective these regulations will be on hydrogen peroxide.
It is used on a tonnage scale for all sorts of things from bleaching to waste water treatment and food preparation.
I use a lot for equipment rinsing as it destroys chlorine based chemicals plus it is a strong bactericide itself and breaks down to water and oxygen.
Formalin has been restricted but it is still widely available, the koi carp keepers use it as a general cure all in their ponds. The same goes for
ammonium sulphamate, this was supposed to disappear off the market when it's licence for use as a weedkiller was withdrawn but it is still used a lot,
albeit illegally. The vendors helpfully tell you that it is dangerous to plants! |
There is a big difference between these restrictions and the upcoming restrictions for a whole class of chemicals for 2014. The restrictions you
mention is that the chemicals should not be sold anymore for the intended purpose and hence should disappear from the shelves as OTC product. The
chemicals, however, still can be purchased, as the pure chemical, for research purposes (e.g. experimenting). In the Netherlands we have had a
restriction on ammonia. Due to safety concerns (pungent gas, chance of severe respiratory problems) the concentration of ammonia for general household
purposes may not exceed 5%. Since these restrictions have come into effect, ammonia at more than 5% concentration cannot be purchased anymore in
supermarkets, hardware stores and paint stores. But as a general chemical it still can be purchased at 25% concentration or even 30+ % concentration.
The new regulations for 2014, however, state that sale of certain chemicals to private persons in any quantity is prohibited. Possession of these
chemicals is prohibited from 2016. So, here it is said that the chemical itself may not be sold to (and later: in possession of) private persons,
regardless of the intended application. Affected chemicals are hydrogen peroxide, nitromethane, nitrates, chlorates, perchlorates and their acids. I
think that from 2016 it even is illegal if you make KClO3 at home from KCl, using electrolysis. I do not believe that if you make a few grams that it
will give trouble, but if you make several pounds, then I can imagine that this is considered a crime.
Suppliers in the EU now already warn their customers that they stop selling certain chemicals permanently next year, because of the new restrictions:
http://www.pyrogarage.pl/end.htm
I am afraid that this will make the EU one of the most restrictive places in the world for home chemistry. In 2017 the measures will be evaluated,
detected security gaps will be closed, and it will be investigated whether the restrictions can be strengthened further without affecting economy too
much.
[Edited on 5-6-13 by woelen]
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Bezaleel
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[/Rant][Offtopic]This whole European community is one big satanic conspiracy if you ask me. A demon of fear in a society without
answers.[/Offtopic][/Rant]
We may hope that there will be sufficient common sense to allow us continuation of performing experiments for the sake of experimenting.
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papaya
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Excellent research aliced25, indeed peroxide is possible to obtain from oxygen bleaches and I'm even sceptical on the point in one of papers that
extra Na2CO3 will ruin TATP synthesis (they didn't try it with sulfuric at least) as extra water always could be taken out.
Also look here
Leach out peroxide into organic solvent, then let it evaporate and you will get some >90% H2O2? :O Or even no, just use that mixture as an
energetic.. (dreaming here).
It would be interesting to look into following references(don't have access):
[1] Matyas, R; Pachman, J., Study of TATP: Influence of reaction conditions on product composition
[2] Reany, O.; Kapon, M.; Botoshansky, M; Keinan, E., Rich polymorphism in triacetone-triperoxide
It's funny to see how professors go routes already known to many home experimenters (who sometimes get superior results) and get publications/funding
''in sake of safety''
[Edited on 5-6-2013 by papaya]
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