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Draeger
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[*] posted on 25-4-2020 at 13:24
Evaporating bleach - what would come out?


So, I know that boiling bleach produces sodium chlorate, but what comes out from gently evaporating the bleach at room temperature?

I'm not really sure if the disproportionation of the sodium hypochlorite needs heat or just happens on the evaporation of water anyway.




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Al, Cu, Ga, C (coal), S, Zn

Collected compounds:

Inorganic:
NaOH; NaHCO3; MnCl2; MnCO3; CuSO4; FeSO4; aq. 30-33% HCl; aq. NaClO; aq. 9,5% ammonia; aq. 94-96% H2SO4; aq. 3% H2O2

Organic:
citric acid, sodium acetate, sodium citrate, petroleum
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S.C. Wack
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[*] posted on 25-4-2020 at 14:18


Smell hypochlorite as liquid or solid...it's Cl that's coming out, yes? Whether this is the result of inherent instability or CO2 is not important...time is not on your side and neither is exposure to air. BTW the bleach already has chloride and chlorate in it.

[Edited on 25-4-2020 by S.C. Wack]




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AJKOER
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[*] posted on 25-4-2020 at 14:24


To create chlorate, you have to add some energy in the form of heat or light. A source of hydroxyl radicals is also good in the presence of HOCl.

Something I may be able to try is first prepare Mg(OCl)2 from adding NaOCl in excess to MgSO4 (Epsom's Salt). Freeze out the Na2SO4.7H2O, leaving magnesium hypochlorite. Add a small amount of Aluminum foil, a piece of high surface-area carbon, and finally some vinegar. This creates a bleach battery based on OCl-/HOCl with anodic Al and a noble cathode, where the electrons generated in the battery cell stay in the solution and can interact with pumped in O2. Warm the solution to over 60 C and try not to boil (reduces chlorate yield).

Reaction logic: Battery cell has solvated electrons, e-(aq). Then, in the presence of supplied oxygen:

e- (aq) + O2 = *O2- (the superoxide radical anion)

OCl- + H+ = HOCl (hypochlorous acid from the action of a weak acid on hypochlorite)

*O2- + HOCl-> .OH + Cl- + O2 (the source of hydroxyl radicals)

Why Magnesium hypochlorite? Because it is reportedly oxygen-sensitive creating chlorates on warming. The chemistry of Mg++ parallels Al3+ and Ca2+ in forming a weak mixed salt with superoxide (see discussion and references at https://www.sciencemadness.org/whisper/viewthread.php?tid=96... ), which extends the effective longevity/reactivity of the superoxide radical.

Supporting basis, my prior comments on SM at https://www.sciencemadness.org/whisper/viewthread.php?tid=15... to quote:

"Apparently, burnt vegetables in contact with air and food acids can convert chlorine bleach to ClO3- (in place of IO3- here) and boom, as I noted previously on SM:

"Carbon produced by accidentally burning vegetables is also a source of radicals especially in a pan (of Al or Fe?) with boiling bleach. In fact, there is a report in Bretherick on an explosion occurring by someone trying to clean a pot with burnt vegetables on boiling with NaOCl, and forgetting it was on the stove! An accidentally revealed chlorate route!"

Also, some interesting comments from this patent https://patents.google.com/patentUS4380533A/en) which focuses on making Mg(OCl)2 absence chlorate, but, to quote:

"High rates of addition and high rates of reaction are desired so that chlorine gas is rapidly evolved from the reaction mixture. This enables the evolved chlorine to be recovered and, for example, recycled to the calcium hypochlorite process. At low rates of addition and subsequently low reaction rates such as those employed in a process in which the reactants are in solution, the chlorine is evolved slowly and considerable amounts of chlorate ion are formed in the solution. For example, generally about 25 percent or more of the available chlorine in the solution is converted."

So, my acidification of the hypochlorite leads to HOCl. Relatedly, free Cl2 in solutions that is not released as gas, also produces HOCl, a likely precursor to chlorate.

Also, per this patent https://patents.google.com/patent/EP0498484B1/en to quote:

"In the cyclic chlorate process the pH is regulated in several positions within the range 5.5 - 12, to optimize the process conditions in each unit operation."

where a pH above 4.88 is consistent, with superoxide creation and not acidic *HO2 (perhydroxyl radical).

[Edited on 25-4-2020 by AJKOER]

[Edited on 25-4-2020 by AJKOER]
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Draeger
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[*] posted on 25-4-2020 at 14:33


Quote: Originally posted by S.C. Wack  
Smell hypochlorite as liquid or solid...it's Cl that's coming out, yes? Whether this is the result of inherent instability or CO2 is not important...time is not on your side and neither is exposure to air. BTW the bleach already has chloride and chlorate in it.

[Edited on 25-4-2020 by S.C. Wack]

Ah. Thank you. Short side question: does boiling bleach generate dangerous amounts of chlorine? I'm suspecting it does, but if so that means I can't do it, so I'd like to check.




Collected elements:
Al, Cu, Ga, C (coal), S, Zn

Collected compounds:

Inorganic:
NaOH; NaHCO3; MnCl2; MnCO3; CuSO4; FeSO4; aq. 30-33% HCl; aq. NaClO; aq. 9,5% ammonia; aq. 94-96% H2SO4; aq. 3% H2O2

Organic:
citric acid, sodium acetate, sodium citrate, petroleum
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S.C. Wack
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[*] posted on 25-4-2020 at 14:43


Quote: Originally posted by AJKOER  
To create chlorate, you have to add some energy in the form of heat or light.


Anything above freezing is heat.

Quote: Originally posted by AJKOER  
Why Magnesium hypochlorite? Because it is reportedly oxygen-sensitive creating chlorates on warming.


They all form chlorates...Mg is preferred because it gives the best isolated yield of KClO3 from the theoretical amount of KCl and chlorate.




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S.C. Wack
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[*] posted on 25-4-2020 at 14:54


Quote: Originally posted by Draeger  
does boiling bleach generate dangerous amounts of chlorine?


Try it in a test tube. I doubt it but can't speak for all products. I would think the rate of loss is lessened by the atmosphere of water.




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Draeger
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[*] posted on 25-4-2020 at 16:19


Quote: Originally posted by S.C. Wack  
Quote: Originally posted by Draeger  
does boiling bleach generate dangerous amounts of chlorine?


Try it in a test tube. I doubt it but can't speak for all products. I would think the rate of loss is lessened by the atmosphere of water.

Would boiling just a little amount of bleach in a normal beaker work as a test? I don't have any glass test tubes, sadly.




Collected elements:
Al, Cu, Ga, C (coal), S, Zn

Collected compounds:

Inorganic:
NaOH; NaHCO3; MnCl2; MnCO3; CuSO4; FeSO4; aq. 30-33% HCl; aq. NaClO; aq. 9,5% ammonia; aq. 94-96% H2SO4; aq. 3% H2O2

Organic:
citric acid, sodium acetate, sodium citrate, petroleum
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[*] posted on 25-4-2020 at 21:07


Quote: Originally posted by Draeger  
Quote: Originally posted by S.C. Wack  
Quote: Originally posted by Draeger  
does boiling bleach generate dangerous amounts of chlorine?


Try it in a test tube. I doubt it but can't speak for all products. I would think the rate of loss is lessened by the atmosphere of water.

Would boiling just a little amount of bleach in a normal beaker work as a test? I don't have any glass test tubes, sadly.


Order a few off eBay they only cost a few dollars delivered.a glass cigar tube could also be used.
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[*] posted on 26-4-2020 at 04:06


There are two competing reactions for hypochlorite:
2ClO->2Cl-+O2
3ClO->2Cl-+ClO3-
Both are effectively irreversible. Both should be promoted by higher temperature but also higher concentration of hypochlorite. So which conditions favour which?
Hypochlorite solutions can exist at temperatures below freezing, too. Not its own, but solutes lower water freezing point. Instead of evaporation, you could concentrate bleach by freezing and skimming off pure ice as it floats to top... which still would increase the concentration and thereby promote decay.
At low temperatures, sodium hypochlorite precipitates from saturated solutions as NaClO*5H2O.
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Draeger
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[*] posted on 26-4-2020 at 06:24


Quote: Originally posted by draculic acid69  
Quote: Originally posted by Draeger  
Quote: Originally posted by S.C. Wack  
Quote: Originally posted by Draeger  
does boiling bleach generate dangerous amounts of chlorine?


Try it in a test tube. I doubt it but can't speak for all products. I would think the rate of loss is lessened by the atmosphere of water.

Would boiling just a little amount of bleach in a normal beaker work as a test? I don't have any glass test tubes, sadly.


Order a few off eBay they only cost a few dollars delivered.a glass cigar tube could also be used.

And how do I heat the test tube?

Quote: Originally posted by chornedsnorkack  
There are two competing reactions for hypochlorite:
2ClO->2Cl-+O2
3ClO->2Cl-+ClO3-
Both are effectively irreversible. Both should be promoted by higher temperature but also higher concentration of hypochlorite. So which conditions favour which?
Hypochlorite solutions can exist at temperatures below freezing, too. Not its own, but solutes lower water freezing point. Instead of evaporation, you could concentrate bleach by freezing and skimming off pure ice as it floats to top... which still would increase the concentration and thereby promote decay.
At low temperatures, sodium hypochlorite precipitates from saturated solutions as NaClO*5H2O.

Wouldn't that be risky, since solid NaClO is very unstable, and if it precipitated shock could set it off?




Collected elements:
Al, Cu, Ga, C (coal), S, Zn

Collected compounds:

Inorganic:
NaOH; NaHCO3; MnCl2; MnCO3; CuSO4; FeSO4; aq. 30-33% HCl; aq. NaClO; aq. 9,5% ammonia; aq. 94-96% H2SO4; aq. 3% H2O2

Organic:
citric acid, sodium acetate, sodium citrate, petroleum
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[*] posted on 26-4-2020 at 09:57


If you dry bleach there's a fair to middling chance that you will get salt.
Bleach slowly evolves oxygen.(It's rather faster if you add a cobalt catalyst)
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[*] posted on 26-4-2020 at 12:33


The Cl you smell is hypochlorous acid from CO2 and hypochlorite, which also oxidizes hypochlorite while neutralizing alkalinity, further encouraging chlorate.



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[*] posted on 27-7-2020 at 08:47


I did this very thing last summer. Unionised is right. The crystals left behind from evaporating common bleach were pure salt. I tasted it. Just salt with a very faint hint of bleach smell. I’d read somewhere that that was what would happen. I just had to try it.



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[*] posted on 27-7-2020 at 09:06


It is not pure salt, it is a mixture of sodium chloride and chlorate, depending on the pH one of the two will predominate.
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[*] posted on 27-7-2020 at 09:44


Sorry for the OT, but the smell of hypochlorite, isn't that hypochlorous acid and not chlorine?
I know that chlorine does not smell like hypochlorite salts.
And that the "public pool smell", which is the same as hypochlorite salts, must come from hypochlorous acid too(unlike the public opinion which says it is the reaction of urine with chlorine:o).
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[*] posted on 29-8-2020 at 04:35


Quote: Originally posted by karlos³  
Sorry for the OT, but the smell of hypochlorite, isn't that hypochlorous acid and not chlorine?
I know that chlorine does not smell like hypochlorite salts.
And that the "public pool smell", which is the same as hypochlorite salts, must come from hypochlorous acid too(unlike the public opinion which says it is the reaction of urine with chlorine:o).


Yes, I agree that the smell from the interaction CO2 (contained in air), or HCl added to very dilute hypochlorite in the pool, resulting in acidification of the NaOCl, is a path to HOCl. But as:

2 HOCl <--> Cl2O + H2O

the answer may also be the smell of the more problematic oxidizing gas dichlorine oxide. The presence of CO2 with hypochlorite not only creates the latter, but may even assist in stripping out of solution. Also support from the long known report (in Watts Dictionary of Chemistry) that distilling dilute HOCl halfway results in a mix containing over 2/3 of the HOCl, so either the HOCl is volatile or the Cl2O is driven out by heat/air contact.

Home Experiment Test:

You just cleaned a bathroom with chlorine bleach. It smells. Turn on the shower at the hotest setting, leave the bathroom and close the door. Return in a few minutes, and ventilate out the steam. How does it smell? My experience, it is much better suggesting the gaseous smell has been largely removed by the water vapor. This is in support of a highly soluble, chemically active specie.

Also, the fact that indoor pools are associated with creating respiratory issues (like so-called swimmer's asthma) suggests the presence of the more powerful oxidizing agent Cl2O (which is also highly soluble in water in contrast to Cl2). I believe the latter as if you inhale Cl2O, HOCl forms in your lungs, which in the presence of transition metal rich dust, further can engage in a fenton-type reaction creating the powerful hydroxyl radical. More precisely:

Fe(II)/Cu(I)/... + HOCl -> Fe(III)/Cu(II)/... + .ClOH-

Source: See comments and links here https://www.sciencemadness.org/whisper/viewthread.php?tid=86...

At pH > 5: .ClOH- -> Cl- + .OH

But pH < 5: .ClOH- -> .Cl + OH-

And: .Cl + .Cl -> Cl2
.Cl + Cl- <-> .Cl2-

all of which is not healthy chemistry one would want occurring in their lungs. By the way, if I was a manufacturer of NaOCl, I would want people to believe the very less likely chemistry that the smell is from less chemically active dry Cl2 gas and not gaseous Cl2O (the latter being easily assimilated and highly active). Further, I would put up web pages with this alternate reality (see how many you can find now).

[Edited on 29-8-2020 by AJKOER]
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[*] posted on 29-8-2020 at 08:09


You should be able to concentrate sodium hypochlorite at reduced pressure but it is unstable and will decompose more rapidly with added heat. Vacuum drying at freezing temperatures is going to give the best yield and no matter what you will have contaminants.
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[*] posted on 29-8-2020 at 14:43


Quote: Originally posted by Draeger  

Ah. Thank you. Short side question: does boiling bleach generate dangerous amounts of chlorine? I'm suspecting it does, but if so that means I can't do it, so I'd like to check.


I did it long ago in a kitchen at the 500ml scale and all I had to do is keep the window open, but your bleach concentration may be higher so always be careful.

There was also a video by NurdRage which explained how to make potassium chlorate from bleach by boiling it and adding potassium chloride to separate it from sodium chloride, but I checked right now and couldn't find it.
I still have that video on my computer, though.
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[*] posted on 29-8-2020 at 15:45


Quote: Originally posted by Draeger  
Quote: Originally posted by S.C. Wack  
Smell hypochlorite as liquid or solid...it's Cl that's coming out, yes? Whether this is the result of inherent instability or CO2 is not important...time is not on your side and neither is exposure to air. BTW the bleach already has chloride and chlorate in it.

[Edited on 25-4-2020 by S.C. Wack]

Ah. Thank you. Short side question: does boiling bleach generate dangerous amounts of chlorine? I'm suspecting it does, but if so that means I can't do it, so I'd like to check.


The reaction that goes on is a disproportionation reaction into NaCl and NaClO3. No gaseous chlorine. As long as you have no acid in there (the bleach is stabilized in basic condition anyway so you're fine) then no chlorine will form. The vapors do smell strongly of hypochlorite though. Just do it outside with a fan or something and wear gloves.

I've done this reaction before by the way and it's not bad. Boil until a precipitate (NaCl) crashes out. Wear splash proof chemically resistant goggles as well and add boiling chips as this had a tendency to bump for me. Cool, filter, and add saturate KCl and chill to get KClO3. You may need to recrystallize the product as there will be a lot of NaCl impurity.

Also if you were able to somehow get a highly concentrated solution or pure sodium hypochlorite, you'd be on the verge of an explosion since it is highly unstable. Boiling or evaporating the bleach won't do that though as the disproportionation reaction is too fast and is also concentration sensitive. So the higher the concentration, the faster it happens. That's why pool bleach (10%) decomposes faster than household bleach (6%).

[Edited on 29-8-2020 by aromaticfanatic]
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[*] posted on 29-8-2020 at 16:46


Quote: Originally posted by aromaticfanatic  
The reaction that goes on is a disproportionation reaction into NaCl and NaClO3. No gaseous chlorine.


Context? Big picture? It needs to be pointed out, it needs to be known, what form the Cl is in? That's not the point. The point is that Cl is obviously being lost continuously over time. BTW you don't know the proper conditions for making chlorate, and if one smells Cl* while making it and needs to do it outdoors, it's being done wrong.

* anything containing the chlorine atom




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[*] posted on 29-8-2020 at 18:17


Quote: Originally posted by S.C. Wack  
Quote: Originally posted by aromaticfanatic  
The reaction that goes on is a disproportionation reaction into NaCl and NaClO3. No gaseous chlorine.


Context? Big picture? It needs to be pointed out, it needs to be known, what form the Cl is in? That's not the point. The point is that Cl is obviously being lost continuously over time. BTW you don't know the proper conditions for making chlorate, and if one smells Cl* while making it and needs to do it outdoors, it's being done wrong.

* anything containing the chlorine atom


https://en.wikipedia.org/wiki/Hypochlorite#:~:text=Preparati...

https://www.nrcresearchpress.com/doi/pdfplus/10.1139/v56-068

https://www.researchgate.net/publication/237847676_Decomposi...

This reaction is very well known.... also yes I do know the conditions of making chlorate. It happens on its own. There is literally 0 chlorine gas being made... unless you acidify the reaction. And I said I smelled the hypochlorite which means I'm doing nothing wrong. I didn't smell chlorine. Two very different smells. I do it outdoors because the bleach stinks. Go ahead and open a concentrated bleach bottle and pour it in into a big dish. Take a big whiff and you'll smell it. I was able to smell it out of the pool bleach bottle. You can do it inside but I prefer to not stink up the lab with hypochlorite. Just because something has chlorine in it doesn't automatically mean it produces toxic chlorine gas. That is common knowledge for a chemist.


[Edited on 30-8-2020 by aromaticfanatic]

[Edited on 30-8-2020 by aromaticfanatic]

[Edited on 30-8-2020 by aromaticfanatic]
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[*] posted on 29-8-2020 at 22:11


Quote: Originally posted by aromaticfanatic  
Also if you were able to somehow get a highly concentrated solution or pure sodium hypochlorite, you'd be on the verge of an explosion since it is highly unstable. Boiling or evaporating the bleach won't do that though as the disproportionation reaction is too fast and is also concentration sensitive. So the higher the concentration, the faster it happens. That's why pool bleach (10%) decomposes faster than household bleach (6%).


But it is also temperature sensitive.
When you freeze bleach and pure water ice floats to the top, does the remaining highly concentrated mother liquor explode, or just dismute to chloride and chlorate?
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[*] posted on 30-8-2020 at 00:52


Quote: Originally posted by chornedsnorkack  
Quote: Originally posted by aromaticfanatic  
Also if you were able to somehow get a highly concentrated solution or pure sodium hypochlorite, you'd be on the verge of an explosion since it is highly unstable. Boiling or evaporating the bleach won't do that though as the disproportionation reaction is too fast and is also concentration sensitive. So the higher the concentration, the faster it happens. That's why pool bleach (10%) decomposes faster than household bleach (6%).


But it is also temperature sensitive.
When you freeze bleach and pure water ice floats to the top, does the remaining highly concentrated mother liquor explode, or just dismute to chloride and chlorate?


Oh yea of course sorry haha. Temperature is what helps drive the reaction. If you were to freeze the bleach to make it more concentrated I think you would be fine. Problems will probably arise at around 90%+ concentration. Think of it a little like hydrogen peroxide. The pure stuff is explosive but a 3% solution will slowlyyy decompose with light and heat as well as metal ions. The higher the concentration, the higher the decomposition rate.

While I doubt you'd get a solution concentrated enough to explode (unless you begin to heat the solution quickly, then you may generate a runaway r if pure enough an explosion), I'd suggest doing some more research on it. I had thought of making a highly concentrated hypochlorite solution using calcium hypochlorite and baking soda and then heating it to make lots of chlorate, but I never found an answer as to if I would generate a runaway or some type of dangerous situation.

So while I think the concentrations from bleach you could get would likely not be of concern ( I think, but double check) I think using calcium hypochlorite to make sodium hypochlorite and letting it get hot is cause for concern.

And to answer your second part of your question, unless pH or some more extreme condition changes occur, hypochlorite will disproportionate into chloride and chlorate. The difference between a calm disproportionation and explosion is just how fast the disproportionation occurs. The pure stuff will almost certainly explode but it is extremely hard if not impossible to get the pure sodium hypochlorite in an amateur setting.

[Edited on 30-8-2020 by aromaticfanatic]
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[*] posted on 30-8-2020 at 06:31


Quote: Originally posted by aromaticfanatic  
This reaction is very well known.... also yes I do know the conditions of making chlorate.


You post links but I'm beginning to doubt your comprehension...BTW crystals of the pentahydrate do not explode; they can be kept in the refrigerator for a long time.

It would probably be best to take care of alkali before attempting to concentrate bleach in vacuo, if the object is chlorate. Otherwise one may run into the vigorous loss of O and Cl.

PS I've heated gallons of conc. filtered HTH on the stove, not a whiff of anything. Must have done it wrong. I would edit one of my posts above if I could; the Cl you smell is still best described just as Cl, in the absence of proof it is something pure...referring again to the action of CO2.

[Edited on 30-8-2020 by S.C. Wack]




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[*] posted on 30-8-2020 at 14:34


Quote: Originally posted by S.C. Wack  
Quote: Originally posted by aromaticfanatic  
This reaction is very well known.... also yes I do know the conditions of making chlorate.


You post links but I'm beginning to doubt your comprehension...BTW crystals of the pentahydrate do not explode; they can be kept in the refrigerator for a long time.

It would probably be best to take care of alkali before attempting to concentrate bleach in vacuo, if the object is chlorate. Otherwise one may run into the vigorous loss of O and Cl.

PS I've heated gallons of conc. filtered HTH on the stove, not a whiff of anything. Must have done it wrong. I would edit one of my posts above if I could; the Cl you smell is still best described just as Cl, in the absence of proof it is something pure...referring again to the action of CO2.

[Edited on 30-8-2020 by S.C. Wack]


Yea I just reread what you said and I mistook the part where you said context as you asking for sources of the information since you quoted the part about the disproportionation reaction. And those links discuss the context behind it and reaction itself.

Yes I'm aware of the pentahydrate but we were discussing the pure hypochlorite. I have no idea how you don't smell anything. Even the bleach bottles themselves smell if left open for a little in the garage. I 100% did absolutely nothing wrong.

Why are you referring to the ClO- smell as Cl smell? Cl makes people think of chlorine gas (Cl2 would be the formula though) and the two are very very different.

Maybe you don't smell hypochlorite but even opening a bottle of bleach and smelling it has a distinct smell to it. I'm not sure how smelling the bleach makes it wrong.
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