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Old 07-10-2021, 07:22 PM
Michael Ahlefeldt-Laurvig Michael Ahlefeldt-Laurvig is offline
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Stannous chloride

I have asked this before but have never gotten a clear answer. I have maybe 30 kilos of tin 2 gel. , - when using stannous chloride dissolved in ethanol, for fuming, there is always a bit leftover and turns into a gel when you pour the leftover it into a jar in the end of the day.
Stannous chloride is quite expensive and Id like to reclaim it, if possible
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Old 07-11-2021, 01:22 AM
Brian Bradshaw Brian Bradshaw is offline
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It's been a while since I used it, but here's my take. All ethanol (except 200 proof) is diluted in water so your gel is coming from some chemical reaction in the water. I started out using ethanol, but switched to distilled (pure) H2O. I was always able to re-use what was left over by mixing into a fresh batch. Stannous never gave me any problems. I always had problems with ferric, but ended up switching to a custom all glass sprayer in a filtered pvc booth. Just my 2c...
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Old 07-11-2021, 03:57 AM
Michael Ahlefeldt-Laurvig Michael Ahlefeldt-Laurvig is offline
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Since I thought it was the water that caused the gel, I never thought of using pure water, thats interesting, thanks
I read a long time ago, that using some acid, you could make crystals again. Never have been able to find the info again though

Last edited by Michael Ahlefeldt-Laurvig; 07-11-2021 at 04:00 AM.
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Old 07-11-2021, 07:32 AM
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Sky Campbell Sky Campbell is offline
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It can be recovered but the process isn’t as simple as I would have thought. You can read this it contains a link to the process.

https://www.researchgate.net/post/St...ck_for_lab_use

I do believe your answers are in “PURIFICATION OF LABORATORY CHEMICALS” -Fifth Edition- Wilfred L. E Armarego and Christina Li Lin Chai for the anhydrous form
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Old 07-11-2021, 10:07 AM
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Pete VanderLaan Pete VanderLaan is offline
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When I was first starting out at this. The two Univ of Iowa people I spent my early time with would simply take a hot gather of glass, punch a dent in the center and drop some tin chloride in the gather. The resultant fume gassed off and the blown piece was rotated over the gather until it irridized.

While I recognize that this is very crude, so much was, but what happens with the gel if you slop a bit onto a hot gather the way I described?

My later stuff with the stuff involved stirring it into a variety of liquids, water, hydrochloric acid, isopropyl alcohol were the mediums and it was lifted from a jar via a venturi over an eye dropper, atomized and sprayed on the surface of the piece in question.

This all involved liquids which were mixed up with the stannous crystals. What I want to know is why the gel as you describe it simply can't be used in this fashion? Is it a case of you doing something quite different with it now?
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Old 07-11-2021, 10:43 AM
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I use ethanol mixed with stannous crystals. I have never had a gel form. I use a modified Critter syphon gun- all parts that touch the solution are made of plastic. I will get settling of the solution between work sessions (days) but a quick shake resolves this. I am interested to see what your gel looks like.
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Old 07-11-2021, 01:24 PM
Brian Bradshaw Brian Bradshaw is offline
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Michael, the acid you are looking for is Hydrochloric. Here's the reaction:

Sn (s) + 2 HCl (aq) → SnCl2 (aq) + H2 (g)

You should be able to get it in one molar by liter. (1.0M) I would experiment a little with reducing the molarity before mixing to check your solution. The gel components may be reduced by the acid also. Just my 2c...
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Old 07-11-2021, 07:21 PM
Michael Ahlefeldt-Laurvig Michael Ahlefeldt-Laurvig is offline
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Thank you for the answers, it seems we also got into a lot of other issues about fuming.
I can basically only get one kind of technical ethanol , it says its 95%, but also contains small amounts of foul tasting alcohols that are impossible to distill away, at least in a private setting.
I didnt dilute with acid as suggested in some sources, because it worked fine without. It certainly is corrosive enough without adding acid- it forms hydrochloric acid in contact with moisture, yes?
My mix ( fully saturated more or less) had a definite shelf life of about 3 hours, after that it would still fume but not the really brilliant colors- it would dull, so I mixed about 3 cl at a time- a shotglass.
Any leftover would just be poured in a glass jar to evaporate. That jar would form a opalescent light grey thick gel like goo. You could turn the jar upside-down and it would not pour. It would never dry completely. It would make very dull dusty fuming if stirred up with new alcohol. Unusable.
When I started doing this , there was no one to ask, I had to reinvent the wheel in sorts. I saw photos of Orient and Flume things, and wanted to give it a go. I found a fuel line to a gasoline run automotive heater to make the nozzle with modifications with a 1/10 mm hole, used a cheap airbrush nozzle for the air, foot pedal that sprayed and started a fast response 2800 rpm welding exhaust fan for the booth, with a time relay that ran the fan about 7 sek after releasing foot pedal. Had to custom manufacture a stainless impeller for that fan and coat inside of the housing with several layers of epoxy. On and on.
Going to study the links Sky pointed and Brians suggestions- thanks
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Old 07-12-2021, 06:47 AM
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Pete VanderLaan Pete VanderLaan is offline
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It's interesting to hear you suggest that the mix "goes bad" and fumes with a dull surface. I would get a dull surface if I overfumed or fumed a piece that was too cold. That dull stuff it turned out could be rubbed off of the piece although it was seriusly time consuming. I only used water and put 100 grams of the anhydrous tin chloride in the jar with a pint of water. Other people I knew used hydrochloric acid and we never talked about mix ratios.

What I do wonder is whether dosing up some of your gel- which I never got- with hydrochloric acid might improve the reaction. If I recall properly, the use of the acid was to keep the stuff in solution to the point that heating it might help as I look back.

What I do know is that it's seriously corrosive stuff on metal. I would think long term storage to be an issue. 30KG's is a lot of stuff. I do not think a plastic lined drum would really cut it.
I also think the basic formula for the glass being fumed is important. Again, high potash r lead glasses took fumes exceptionally well.
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Old 07-12-2021, 06:49 AM
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Quote:
Originally Posted by Brian Bradshaw View Post
Michael, the acid you are looking for is Hydrochloric. Here's the reaction:

Sn (s) + 2 HCl (aq) → SnCl2 (aq) + H2 (g)

You should be able to get it in one molar by liter. (1.0M) I would experiment a little with reducing the molarity before mixing to check your solution. The gel components may be reduced by the acid also. Just my 2c...
****
I'm having trouble balancing that equation
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Old 07-12-2021, 10:07 AM
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A bit of additional thought.

HCL as a standalone is concentrated and you will rarely see it. Normally HCL for brick cleaning etc is about 70% with the remainder being water ( usually) . What makes an acid work is all those hydrogen ions and when they interact with whatever ( Chlorine in this case) and some other material the ions are virtually spent making the H+ dilute until quite week. It's true in Nitric acid as well (HN03).

My reason for mentioning this is for Michael, he may have mixed up essentially a weak acid solution and it was spent fairly quickly leaving a fair amount of a chlorine gel that had nothing else to combine with. '
When I make silver nitrate, I'm sloppy with my stoichiometric calculations and I essential put some pure silver casting shot in a baking dish and then cover it with the nitric acid and a spoonful of tap water. Then I heat it up and the reaction gets going when the mix is hot enough. The acid readily attack's the silver leaving crystals in the dish and it's all over in about 20 minutes. Then, I'll have this liquid and these crystals. At that point, I add some more acid and tons of crystals appear like flower blooms as it by magic but it's not magic at all. I have weakened solution of the nitric and when it gets enhanced, it goes back to work and makes more crystals. Being a slob, I just let that dry behind the furnace and get it later where I will have tons of silver nitrate crystals at a far cheaper price than buying the stuff. Tons cheaper. I can always tell if someone tried to short me substituting sterling silver since the present 14% copper makes the stuff turn blue. The quantity of copper in the crystals is sufficient enough to throw off some of my colloidal silver mixes so I'm quite testy about it. Silver coins are rarely fine silver.

So, long windily, I think adding fresh acid to your gel may be just the ticket. It's gotta be at least 70% molar. Do a small batch. I suspect some of that dull look was a weakened solution and the fume did well with the acid strong and present.
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Old 07-27-2021, 10:54 PM
Ron Mynatt Ron Mynatt is offline
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I use 600 gram of stannous chloride 8 oz of muriatic acid 4 oz 90% isopropyl alcohol and 12 oz of water. I let the acid and alcohol dissolve the crystals completely one day then add the water.I use a glass tube on a air foot pedal to spay air onto a glass tube coming out of the jar of stannous. A Venturia siphon pump. (Youtube) .Use glass on all tubes at a 90 degree angle and a plastic barrel, a 12 volt inline blower (jabsco or something similar) from ebay 4 " is the best size not 3 " connected to a 4 " pvc pipe .I hook the inline blower to a 12 volt battery charger attached to a on/ off foot pedal to turn the battery charger on and off .I usually let it vent off any fumes for 30-45 seconds after I finish spraying the glass .This mixture accumulates on the opposite side wall away from the Venturia siphon. Depending on how much you spray in a day it usually dries and I scrape the residue off and keep in a sealed container for when I make my next batch .If you spray a lot in a day drill a hole on the bottom of your barrel and put a jar under the hole to collect the run off .I will usually make sure I clean the barrel of anything I want to save before I shut down for the season because the humidity causes any residue to dissolve over the summer. I can email pics for a better description .
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