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Waller solution / Super Iron Out
  
  Index -> Conserving, Preparing and Cleaning Minerals
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Rei




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PostPosted: Jul 01, 2014 19:09    Post subject: Waller solution / Super Iron Out  

So at long last I got a bottle of super iron out for mineral cleaning. I put a bunch of samples in a 3% solution - calcite, some with chalcedony, zeolites, etc, plus a matrix (basalt or similar). I was a bit concerned when from all samples except the calcite I saw streams of tiny bubbles forming (and I must stress tiny, I'm not used to seeing bubbles that small, it was kind of weird - one sample formed a column of bubbles from underneath that was so fine I thought it was a hair and tried to pluck it out). Anyway, very concerned that I might be destroying my samples, I removed the non-calcite samples.

I must ask, is this normal, for super iron out to have some reaction that causes bubbling? Or was that indeed something being destroyed? I just want to get rid of surface oxides.
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PostPosted: Jul 01, 2014 19:22    Post subject: Re: Waller solution / Super Iron Out  

I can't speak specifically to the bubbles - they could be reaction products or they could just be trapped air oozing out of a thin crack. The general rule is to try whatever you use on a sample you can afford to lose before you use it for real.

Waller solution is buffered, so at least until the buffer gets used up, the pH should remain stable. I'm not sure the same is true of Super Iron Out, though I think the other chemicals are similar.

There is a danger that either of these can attack calcite, fluorite, and other minerals if iron oxides are not present, or even if they are. I have ruined fluorite specimens using the Waller solution (as I recall - or was it Super Iron Out?).

So, again, test and observe before you use them on "real" specimens. And test for longer than you think the "real" application will require. And rinse well!

Good luck!

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Collecting and studying crystals with interesting habits, twinning, and epitaxy
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Rei




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PostPosted: Jul 01, 2014 19:35    Post subject: Re: Waller solution / Super Iron Out  

I did choose some of my least impressive specimens. No, it was definitely not air oozing out, I'm 100% about that. So you're saying that a bubbling reaction is not normal with iron out?
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PostPosted: Jul 01, 2014 19:48    Post subject: Re: Waller solution / Super Iron Out  

SIO is slightly acidic. Won't hurt most minerals, but I wouldn't use it on calcite - at least not for more than a minute or two.
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Rei




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PostPosted: Jul 01, 2014 20:06    Post subject: Re: Waller solution / Super Iron Out  

Funny, calcite is the only one that's *not* bubbling ;)

Besides, what other cleaning solution could one use on calcite?
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Dale Hallmark




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PostPosted: Jul 01, 2014 20:12    Post subject: Re: Waller solution / Super Iron Out  

Maybe....a little baking soda...maybe ;-)

Dale


Rei wrote:
Funny, calcite is the only one that's *not* bubbling ;)

Besides, what other cleaning solution could one use on calcite?
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GneissWare




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PostPosted: Jul 01, 2014 21:01    Post subject: Re: Waller solution / Super Iron Out  

The pH of SIO is 5.5 to 6. You can buffer it up to near pH 7 by adding a small amount of baking soda (Sodium bicarbonate). This will not significantly affect the active ingredients of SIO, sodium hydrosulfite and sodium metabisulfite.

The fine bubbling is normal. You can get more info in Rock's article at https://www.mindat.org/article.php/403/Cleaning+Quartz
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Rei




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PostPosted: Jul 01, 2014 21:10    Post subject: Re: Waller solution / Super Iron Out  

Rock's article didn't mention the bubbling but good to know that it's okay! :) I'll put my test specimens back in.
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PostPosted: Jul 01, 2014 22:17    Post subject: Re: Waller solution / Super Iron Out  

John Betts has an article on cleaning with Waller soultion (essentially SIO). He rightly describes the reaction as "the solution works by reducing Fe+3 to Fe+2 and then dissolving Fe+2 in the Citric Acid." This reduction reaction causes the bubbling by release of O2, if I remember correctly.
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Jordi Fabre
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PostPosted: Jul 02, 2014 01:34    Post subject: Re: Waller solution / Super Iron Out  

Just in case you didn't see it: How to remove iron stains?
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lluis




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PostPosted: Jul 02, 2014 08:18    Post subject: Re: Waller solution / Super Iron Out  

Hi, All

If a chemist serves for something
-The hydrosulphite in Waller's solution, when oxidized releases sulphuric acid, and for that there is an extra sodium bicarbonate: to neutralize free sulphuric acid
-Hydrosulphite never releases O2. So, I fear that the bubbling is CO2 being released...

In wikipedia
https://en.wikipedia.org/wiki/Sodium_dithionite
And this article is right.

Also, can anyone tell me what is SIO? If pH is acidic (very few, but acidic), it cannot be Waller's, that is slightly basic (over 7)

With best wishes

Lluís
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Rei




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PostPosted: Jul 02, 2014 08:19    Post subject: Re: Waller solution / Super Iron Out  

GneissWare wrote:
John Betts has an article on cleaning with Waller soultion (essentially SIO). He rightly describes the reaction as "the solution works by reducing Fe+3 to Fe+2 and then dissolving Fe+2 in the Citric Acid." This reduction reaction causes the bubbling by release of O2, if I remember correctly.


I had the pieces in overnight and I don't see any damage to any of them, so that's a great start :) And there's definitely a whole lot of cleaning that's been going on. I'll leave them in for a couple more days to see if I get any more progress, but it's definitely good to see as it is.

Hmm, I read before about the Fe+3 to Fe+2 reaction before, but I never put two and two together... *of course* you're liberating oxygen - 2 Fe(+3)2O3 -> 4 Fe(+2)O + O2. :) I mean, something has to happen to that O2...
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Rei




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PostPosted: Jul 02, 2014 08:22    Post subject: Re: Waller solution / Super Iron Out  

lluis wrote:
If a chemist serves for something
-The hydrosulphite in Waller's solution, when oxidized releases sulphuric acid, and for that there is an extra sodium bicarbonate: to neutralize free sulphuric acid
-Hydrosulphite never releases O2. So, bubbling I fear that is CO2 released...


Hmm, okay, then scratch what I wrote above, if that's correct. Still, if that's CO2 being released, aka it's getting carbon from somewhere, strange that I wouldn't see any damage to the calcite. The calcite was the only one that I *didn't* notice bubbling on (though it still got clean).

In case you're curious, SIO's active ingredients are reportedly Sodium metabisulfite (20-65%) and Sodium hydrosulfite (20-65%). And the reason for the range is not that it's a trade secret, but because one degrades into the other with time and it's hard to guarantee a specific quantity of each. But I'm not too familiar with the reaction. Sodium carbonate and citric acid are the buffering agents. Maybe the bubbling has to do with the sodium carbonate?

Oh, and before I try it... any clue whether it'd work to dissolve SIO in isopropyl alcohol instead of water? I have a couple fibrous zeolites that I'd like to try cleaning with SIO that I've read it's better to clean with alcohol than water.
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lluis




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PostPosted: Jul 02, 2014 09:56    Post subject: Re: Waller solution / Super Iron Out  

Hi, Rei

Sorry to be the sorcerer... Chemists are used to be seen as the bad ones.... :-)

The mixture of sodium metabisulfite and sodium hydrosulfite has a small trouble. Sodium metabisulfite is acidic, and to place a product that is acid sensitive, like sodium dithionite (aka sodium hydrosulphite), well, is a nice way to get big troubles. A fire somehow great (great is for *GREAT*) happened one time in Switzerland because some packages of sodium hydrosulphite got wet and at the end, ignited. Firemen were not informed and they shot more water, and flames got bigger.... Not nice.

Sodium hydrosulphite decays to sodium bisulphite only in presence of water (with sodium thiosulphate) or if in presence of water and oxygen, to sodium bisulphite and sdoium bisulfate. In both cases, with a release of heat that increases the rate of decomposition.

If you say that they have the buffering agents (sodium carbonate), then the sodium bisulfate means that the sodium sulphite used to produce the sodium hydrosulphate is not completely exhausted...
2 NaHSO3 + Zn → Na2S2O4 + Zn(OH)2
bisulphate hydrosulphate

The CO2 released, as you say, would come first from sodium carbonate. For that, calcite would not be damaged: it is the reason why Waller's solution has been created: to clean iron from acid sensitive items, as calcite....

And no, when you reduce Fe3+ to Fe2+ you do not liberate oxygen, you only give an electron to Fe3+ to produce Fe2+
Fe3+ + e- -> Fe2+

Hydrosulphite gives the electrons, oxidizing it to sulphate....

Sorry for long rant.... :-(

With best wishes

Lluís
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Rei




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PostPosted: Jul 02, 2014 12:39    Post subject: Re: Waller solution / Super Iron Out  

lluis wrote:
...And no, when you reduce Fe3+ to Fe2+ you do not liberate oxygen, you only gives an electron to Fe3+ to produce Fe2+
Fe3+ + e- -> Fe2+...

Except that there's not simple "Fe(3+)" in the mixture; there's Fe(3+)2O3 in there. You can't simply change that to Fe(2+)2O3, that's not stable. The stable Fe(2+) equivalent is FeO.

So if I understand right, the excess oxygen is going to change sulfite to sulfate, and the sodium carbonate is neutralizing the sulphuric acid to sodium sulfate and releasing CO2?
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lluis




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PostPosted: Jul 02, 2014 15:06    Post subject: Re: Waller solution / Super Iron Out  

Hi, Rei

Well, if you want to be extremely exhaustive, yes, that is not that easy.
If you place all intermediate states and intermediate compounds, could be a nightmare for the rest.... :-(

But the fact, taking apart that is a reaction in heterogenous phase (rust is solid, and Waller's or SIO is liquid....) is that Fe3+ is reduced to Fe2+, and the solid with Fe2+ is complexed by citrate anion, that is a good chelant for Fe2+, but not enough to solubilize Fe3+ quick enough.

Anyway, yes, the extra oxygen in oxide could be used in the extra oxygen in sulfate or sulphite or used to build water...Sometimes, mechanisms looked using isotopes show that what is expected is not what is done. And in this case, I can place the equations, but I could not say from where things come....

For CO2, yes, the carbonate is releasing the CO2 when neutralizing the sulphate (and sulphite)

With best wishes

Lluís
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PostPosted: Jul 02, 2014 15:37    Post subject: Re: Waller solution / Super Iron Out  

Or, the engineer's way of saying it, is -- "this stuff works."

It's kind of like the old joke illustrating the differences between scientists and engineers (btw, geologists are practical like engineers):

A scientist and an engineer agreed to take part in an experiment. They were both placed in a room and at the other end was a beautiful woman. The experimenter said every 30 seconds they would be allowed to travel half the distance between themselves and the woman.

The scientist said “This is pointless” and stormed off. The engineer agreed to go ahead with the experiment anyway.

The scientist exclaimed on his way out “don’t you see, you’ll never actually reach her?”. To which the engineer replied, “So what? Pretty soon I’ll be close enough for all practical purposes!”

;=))
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lluis




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PostPosted: Jul 02, 2014 15:46    Post subject: Re: Waller solution / Super Iron Out  

Hi, GneissWare

I am by title an engineer.... Chemical engineer...
But, I am sorry, the scientist was right: never get her,,,, (maybe near enough...but never reached; and being from Jesuit formation (although feeling Buddhist...), you never know which is distance gap...Maybe too big enough....)

Being bad

With best wishes

Lluís
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Rei




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PostPosted: Jul 07, 2014 04:40    Post subject: Re: Waller solution / Super Iron Out  

GneissWare wrote:
Or, the engineer's way of saying it, is -- "this stuff works."

It's kind of like the old joke illustrating the differences between scientists and engineers (btw, geologists are practical like engineers):

A scientist and an engineer agreed to take part in an experiment. They were both placed in a room and at the other end was a beautiful woman. The experimenter said every 30 seconds they would be allowed to travel half the distance between themselves and the woman.

The scientist said “This is pointless” and stormed off. The engineer agreed to go ahead with the experiment anyway.

The scientist exclaimed on his way out “don’t you see, you’ll never actually reach her?”. To which the engineer replied, “So what? Pretty soon I’ll be close enough for all practical purposes!”

;=))


I have to say, that joke is straying a bit close to "Your Princess Is In Another Castle" territory:

https://www.thedailybeast.com/articles/2014/05/27/your-princess-is-in-another-castle-misogyny-entitlement-and-nerds.html
(link normalized by FMF)

I know it was only meant as a joke, and I mean no offense by pointing this out. But to sum up, when was the last time you saw a joke, or a TV show, or movie, or video game, or whatnot where a guy was treated as a "prize" to some sort of challenge, but otherwise has no defining human characteristics, just the assumption that he's into whatever girl wins said challenge? Because the converse (as in this joke) of "getting a woman as a prize" is exceedingly common, and it's a dangerous motif because when we see this mirrored (often) in society, it becomes people feeling entitled to their "prize" and taking reprehensible actions when they're not "given" it.

I know this is just a joke. It's just, next time... you might consider having the inanimate, inhuman object of desire in the joke that automatically goes to the victor be an actual inanimate, inhuman obect of desire that automatically goes to the victor. Say, for example, ice cream? ;) Again, not telling you how to tell a joke, just raising an issue you might not have thought of but that matters.

(I'm not even going to touch the automatic assumption that both the engineer and scientist are men)
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bugrock




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PostPosted: Jul 07, 2014 21:42    Post subject: Re: Waller solution / Super Iron Out  

Actually I think the joke works a bit better if done with a mathematician and an engineer.

Some would argue with calling both geologists and engineers practical. I know both a geologist and an engineer in the field of environmental engineering The geologist does not like to work with engineers since they seem to never have enough measurements to be satisfied. The engineer tells me there are geologists working for the firm who work on a project, plot six dots on a map an they think they are done!

Sorry, we are wondering far afield from the focus of this forum.

George
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