[kamikaze762]

I am trying to find out what I have created.  I dissolved calcite (calcium carbonate) from some rocks I had in HCl.  I was trying to recrystalize the calcite to a clearer and more aesthetically pleasing crystal structure from a super-saturated solution in an undisturbed location.  I got impatient and boiled off the solution to get what seem to be yellowish (contaminated HCl) calcium chloride crystals...

Doing some reading, I found that neutralizing the solution with sodium carbonate may precipitate calcium carbonate again...  So I added some sodium bicarbonate instead (knowing that it can sometimes serve as a substitute in some reactions calling for Na2CO3).  Nothing.  I boiled it down and all I get is more yellow crystals with what seems to be a sodium carbonate coating.

Then I read something that said potassium could react with a calcium chloride solution... So I had some potash I extracted from ashes (which is least mostly potassium carbonate, if contaminated). 

I wasn't really expecting a difference.  I figured it would simply form a mixture if no reaction occurred.  I had added a very small amount to it before and noticed that some pink crystals formed amidst the other colors when I boiled it dry.  I assumed this was potash and noticed it was particularly resilient to dissolution in the HCl again. 

Well... I figured I would try to make more of those crystals so I added nearly 10 ml of my improvised potash solution to the mixture of calcium carbonate, sodium carbonate, and HCl.  Some minor bubbling, which I assumed was a simple neutralization reaction of the slightly alkaline potash with the HCl. 

The really strange thing happened when I tried to boil down this new mix.  It nearly ran me out of my house.  Boiling the other solutions produced some hydrogen chloride fumes, but it wasn't too bad since I am using a very small improvised beaker and I am only dealing with maybe a quarter cup of solution or less.  I am somewhat used to muriatic acid fumes, but this was different.  The initial boils resulted in an awful smell... Then much later, the smell was mostly chlorine-like.  The solution is now forming brown crystals and still smells terrible when rehydrated and boiled. 

So my question.  Did I make something toxic besides chlorine gas?  I know hydrogen chloride and chlorine gas are both irritants in a high enough concentration.  But this smell was different than either and much stronger.  I wish I could boil whatever remains of it out of my mixture.

In summary...

Hydrogen Chloride (muriatic acid)
Calcium Carbonate
Sodium Bicarbonate
Potassium Carbonate
* Various trace contaminates

All of this has been mixed and boiled in various stages.  Does anyone know any compounds which may possibly form from this?  And why does it smell so bad when heated?

[Arkcon]

That's quite a missive you've written, we'll try to help you point by point, at least until you've begun to learn what's wrong.

I am trying to find out what I have created.  I dissolved calcite (calcium carbonate) from some rocks I had in HCl.

Great.  Do you know what reaction happened?  If you don't, can you describe what you saw?  It may you understand what's happening.

I was trying to recrystalize the calcite to a clearer and more aesthetically pleasing crystal structure from a super-saturated solution in an undisturbed location.  I got impatient and boiled off the solution to get what seem to be yellowish (contaminated HCl) calcium chloride crystals...

Lots happening there.  Briefly, mixing calcite with acid is not how recrystallizing is done.

Doing some reading, I found that neutralizing the solution with sodium carbonate may precipitate calcium carbonate again... 

Do you have (or can you write)  a balanced chemical equation for what you want to happen?  It will he you know if its possible or not.

So I added some sodium bicarbonate instead (knowing that it can sometimes serve as a substitute in some reactions calling for Na2CO3).  Nothing.  I boiled it down and all I get is more yellow crystals with what seems to be a sodium carbonate coating.

Bummer.

Then I read something that said potassium could react with a calcium chloride solution... So I had some potash I extracted from ashes (which is least mostly potassium carbonate, if contaminated). 

I wasn't really expecting a difference.  I figured it would simply form a mixture if no reaction occurred.  I had added a very small amount to it before and noticed that some pink crystals formed amidst the other colors when I boiled it dry.  I assumed this was potash and noticed it was particularly resilient to dissolution in the HCl again. 

Possibly.  Again, a balanced chemical equation would help.  You have to realize, the potassium won't disappear.  So you have to expect that you're now getting a mixed batch of salts.  And you've previously implied that mixing diverse reagents just "gets back" what you had before.  You'll have to abandon talk like that, because that's not possible.  For example:

Well... I figured I would try to make more of those crystals so I added nearly 10 ml of my improvised potash solution to the mixture of calcium carbonate, sodium carbonate, and HCl.  Some minor bubbling, which I assumed was a simple neutralization reaction of the slightly alkaline potash with the HCl. 

I don't know what you're expecting to get here. 

The really strange thing happened when I tried to boil down this new mix.  It nearly ran me out of my house.  Boiling the other solutions produced some hydrogen chloride fumes, but it wasn't too bad since I am using a very small improvised beaker and I am only dealing with maybe a quarter cup of solution or less.  I am somewhat used to muriatic acid fumes, but this was different.  The initial boils resulted in an awful smell... Then much later, the smell was mostly chlorine-like.  The solution is now forming brown crystals and still smells terrible when rehydrated and boiled. 

I don't know what's happening here.  Some free HCl may have completely evaporated.  Just because you're used to fumes from HCl solution doesn't mean you're ready for all of the HCl to appear at once.

So my question.  Did I make something toxic besides chlorine gas?  I know hydrogen chloride and chlorine gas are both irritants in a high enough concentration.  But this smell was different than either and much stronger.  I wish I could boil whatever remains of it out of my mixture.

In summary...

Hydrogen Chloride (muriatic acid)
Calcium Carbonate
Sodium Bicarbonate
Potassium Carbonate
* Various trace contaminates

All of this has been mixed and boiled in various stages.  Does anyone know any compounds which may possibly form from this?  And why does it smell so bad when heated?

If you potash is made from soaked wood ashes, then you have some potassium carbonate and potassium hydroxide -- and a large amount of random organic compounds.  Unless you've recrystallized the ash water repeatedly, and you won't get enough unless you've process a ton of trees.

[kamikaze762]

Thanks for your response, Arkcon.  I have not done a balanced equation, because frankly, I don't know how.  I know that all the same atoms are present, if bonded differently (unless some escape as gas or some is added from the atmosphere).  There is, of course, water to account for as well, forming some hydroxides or hydrochlorides in some reactions.  That is about the extent of my chem knowledge other than a brief overview of compounds and mixtures.  I know a little about valance and different types of bonds, but all of my knowledge is conceptual only.  I know that the same amount of atoms are present in a balanced equation on both sides... but as for how they are separated and recombined, I'm basically lost.

I know I can't "get back" what went into the reaction per se.  Many or all of my ingredients must have formed chloride salts since these tend to be pretty stable... but I also know that adding energy (heat, electricity) to fuel many reactions can produce less stable compounds than what you start with.  I doubt my little jar over a candle provides enough energy for these kinds of reactions though.

Forgive my lack of knowledge on the subject.  Chemistry has been a passing interest of mine for years, but I bounce between hobbies a lot.

This is not a very accurate approach, but I think I have figured out more of what I have produced.  Once the mixture dried and cooled, I gave it a good smell.   I noticed the distinct smell of chlorine and wood smoke (more like creosote).  The chlorine is obviously from the HCl...  In effect, I was burning tar from the all the condensed and concentrated leaching from my ashes.  I should have used a higher heat method to reduce the ashes completely before leaching them.  So instead of getting some interesting salts to play with, I have a mix of salts and smoke tar... the tar being so many different things that I may as well forget about knowing exactly what I have.

[billnotgatez]

The really strange thing happened when I tried to boil down this new mix.  It nearly ran me out of my house.

OMG
Please do not become another Darwin Award Winner

[Arkcon]

I'm going to try to be brief, in order to save some time.  This part here:

There is, of course, water to account for as well, forming some hydroxides or hydrochlorides in some reactions.  That is about the extent of my chem knowledge other than a brief overview of compounds and mixtures.

Is false.  We can't make hydroxides and hydro- acids that way.  You are simply using the names, and atoms found in water, and mixing them via contemporary English grammar rules.  Chemistry uses different rules.

Many or all of my ingredients must have formed chloride salts since these tend to be pretty stable... but I also know that adding energy (heat, electricity) to fuel many reactions can produce less stable compounds than what you start with.

Uh...

I doubt my little jar over a candle provides enough energy for these kinds of reactions though.

OK.  I'm glad you realize that.  Because the quote I made above it didn't seem likely to me, either.

Forgive my lack of knowledge on the subject.  Chemistry has been a passing interest of mine for years, but I bounce between hobbies a lot.

Everyone has to start somewhere.

This is not a very accurate approach, but I think I have figured out more of what I have produced.  Once the mixture dried and cooled, I gave it a good smell.   I noticed the distinct smell of chlorine and wood smoke (more like creosote).

 

Huh ... what?  Cresote?  I knew your potash was impure but ... that's a lot of weirdness, right there.

The chlorine is obviously from the HCl... 

OK, but ...

In effect, I was burning tar from the all the condensed and concentrated leaching from my ashes.  I should have used a higher heat method to reduce the ashes completely before leaching them.  So instead of getting some interesting salts to play with, I have a mix of salts and smoke tar... the tar being so many different things that I may as well forget about knowing exactly what I have.

And you've lost me again.  Creosote and tar are complex organic mixtures.  We can't describe them, and their reactions, one post at a time.  To understand the reactions of calcium carbonate and acid, you can browse a high school chemistry book.  To learn more about calcite, which is a mineral composed mostly (but not completely) of calcium carbonate, you can try some basic mineralogy texts.  Try that first.

[kamikaze762]

    There is, of course, water to account for as well, forming some hydroxides or hydrochlorides in some reactions.  That is about the extent of my chem knowledge other than a brief overview of compounds and mixtures.

Is false.  We can't make hydroxides and hydro- acids that way.  You are simply using the names, and atoms found in water, and mixing them via contemporary English grammar rules.  Chemistry uses different rules.

One such example is quicklime and slaked lime.  Calcium oxide to calcium hydroxide with the simple addition of water.  Perhaps I overgeneralized the statement.

    Many or all of my ingredients must have formed chloride salts since these tend to be pretty stable... but I also know that adding energy (heat, electricity) to fuel many reactions can produce less stable compounds than what you start with.

Uh...

Sodium Chloride, quite stable, can be reacted by electrolysis with a permeable membrane to produce sodium hydroxide and sodium hypochlorite... so I've read anyway...  Both of these are less stable than the original salt.  I'm not sure how I misstated this.  Which parts of my statement were incorrect?

The premise I am working from with all of this is that chemicals seek equilibrium, and just like other physical phenomena, if you want to introduce any kind deviation from that equal and most energy-efficient state, you must apply work of some sort.  So... adding energy to the system provides that work in some cases... which is why electrolysis can effectively generate chemicals which are more reactive than the original ones... 

Did I go wrong anywhere?

     ...the tar being so many different things that I may as well forget about knowing exactly what I have.

And you've lost me again.  Creosote and tar are complex organic mixtures.  We can't describe them, and their reactions, one post at a time.  To understand the reactions of calcium carbonate and acid, you can browse a high school chemistry book.  To learn more about calcite, which is a mineral composed mostly (but not completely) of calcium carbonate, you can try some basic mineralogy texts.  Try that first.

This is sort of what I stated concerning the wood tar.  Creosote was perhaps the wrong word to use since it indicates some processing of wood tar.  I was thinking barbeque talk.   People who smoke meats often call the bitter taste creosote, forming from a smothered fire.  Wood tar would have been a better term.  The tar is complex as I stated, and knowing what is in what I have mixed and what product have derived from it may be very difficult.