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Doped-Al2O3-fusion
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I actually have more to update on this thread, but I need to try to get some rest before I have to continue working for my day-job.--required 24x7
pretty much and not happy about it.
Anyhow, $13.99 on the left vs. a couple weeks of hard work on the right. Motivation gains...
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S.C. Wack
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Maybe there's a good reason to use sulfite instead of NaOH after all.
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Doped-Al2O3-fusion
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Tons of good reason. LOL.
I did have success with the complete polysulfide oxygenation with this last run, despite my most recent mistake by switching to an aquarium air-stone.
Update soon to follow.
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Doped-Al2O3-fusion
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I made the mistake of switching out my glass bubbling tube for an air-stone thinking that the air-stone would provide better oxygenation absorption
into solution. The solution was also added to a graduated cylinder along with 80mL of distilled water as the air-stone was causing a lot of mist to
escape the test tube. After running over night, two nights ago, I came down to check on my experiment and the solution had turned turbid indicating
sulfur precipitation, and my H2S indicator test strip was completely black. I turned the air off and tested the pH of the solution which measured in
at 7.5 from 10 the night before.
I filtered out the precipitated sulfur which was highly contaminated as indicated as a grayish colored silt. I assume this to be the resultant
product from the blue colored air-stone which I had purchased from stupid Walmart. I'll also assume the addition of the 80mL of distilled water
lowered the pH which was a complete oversight and mistake on my part. The glass air tube was reattached to the air line and some aqueous sodium
hydroxide was added to the solution to raise the pH to 11.
This morning I checked the status of the solution and it is now completely clear. I only had time to turn off the air, but will be able to test the
final pH of the solution before I move onto evaporating enough water to begin crystallization. Hopefully there isn't too much sodium sulfide
remaining in solution as well as any formed sodium sulfate from decomposition. Sodium sulfide should be the first product to crystallize, but I need
to check on the solubility of sodium sulfate in comparison to the thiosulfate. pH adjustments will also be examined in favor of specific product
crystallization and will be implemented as required.
   
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Doped-Al2O3-fusion
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Here is a video I shot a couple nights ago which I stumble over my words as well as ramble on with a presumptuous level of flawed logic in describing
this experiment. This was obviously shot prior to the discovery of the air-stone fail.
https://www.youtube.com/watch?v=Zasc_eM7qNg&t=18s
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S.C. Wack
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SO2 may be preferred over air.
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Doped-Al2O3-fusion
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That very may well work. I still have the 2.5oz of solution sitting in that plastic cup I posted a picture of previously. I could try that out with
that since I haven't been sure what to do with it besides the same boring method that I've been using. Other than the fact that I didn't boil the
sulfur in the sodium hydroxide in that solution, it should technically be pretty much of the same so I might as well do something different.
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Doped-Al2O3-fusion
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Here are some decent crystals that formed on the third recrystallization. I haven't had a chance to measure the mass yet but it did have a good yield
overall to my happy surprise. There is expected to be lower yield results due to the couple of minor mishaps with the pH drop and the mistake of
using the air-stone which reacted with the sodium hydroxide buffer in solution highly contaminating the solution.
I also lost a significant portion of the Na2S2O3 crystals during the final rinse due to a family distraction. I think at least 30% of the crystals
were dissolved from the rinse and absorbed into the coffee filter and a shop towel.--It was supposed to be sitting in the funnel, so the towel soaked
up quite a bit. I just used that towel in a solution for a displacement reaction of some excess lead acetate I had in a dish from making my H2S
detection strips.
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Doped-Al2O3-fusion
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I was just thinking about this again and I don't think SO2 would be suitable as it forms sodium sulfite with sodium hydroxide. I'm not sure how it
would work exactly in a polysulfide solution. I'll do some research.
At the moment, I have my autoclave in the oven at approx 180 Celsius forming iron disulfide. I'm experimenting with the sodium thiosulfate I bought
with a super clean batch of ferrous sulfate I made yesterday. I didn't add any extra sulfur to the mix as I want to see how this turns out
as-is...however this subject is for my other thread on synthesizing pyrite. It is related at the same time because that is the whole reason I became
interested in making Na2S2O3 in the first place.
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S.C. Wack
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So...
...you were bubbling air through NaOH?
...sulfide and SO2 doesn't automatically adjust pH and precipitate S leaving thiosulfate?
...Na2SO3 boiled with S powder doesn't give Na2S2O3 like I suggested here in 2005?
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Doped-Al2O3-fusion
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Quote: Originally posted by S.C. Wack  |
So...
...you were bubbling air through NaOH?
...sulfide and SO2 doesn't automatically adjust pH and precipitate S leaving thiosulfate?
...Na2SO3 boiled with S powder doesn't give Na2S2O3 like I suggested here in 2005? |
I'm not suggesting you are wrong nor the procedures you suggested. I was only stating what I understood to be results from research I've been doing,
including my own experimental observations. I'm still quite a novice and I'm just trying my best to learn on my own. There is a lot of conflicting
info out there and I truly appreciate the academic approach of learning at paced steps. I lack that practiced discipline acquired through a formal
education but I'm trying.
*edit*
"...Na2SO3 boiled with S powder doesn't give Na2S2O3 like I suggested here in 2005?"
I also didn't come across your post in 2005 regarding this. I'll search for it when I get some spare time again.
[Edited on 13-9-2018 by Doped-Al2O3-fusion]
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Doped-Al2O3-fusion
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...I may have some incorrect logic in my understanding of a reaction, so I'm glad others in the community can chime in to correct me or guide me in
the right direction. I appreciate that more than silence.
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