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Author: Subject: Preparation of elemental phosphorus
JScott
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[*] posted on 1-9-2018 at 11:40


Quote: Originally posted by Hunterman2244  
Quote: Originally posted by JScott  
@Hunterman2244,

Thanks, when I scale up, it is my intention to work in a metal apparatus. However, I am a ways from there at this point. As mentioned, I really just wanted to recreate what I had seen in that video. Though it only appeared to be partially successful, I thought for me, it would make a good first step.

Partial successes can be instructional, and a bit more fun than absolute failure ;-) Further, I have been stymied by not having any inert gases on hand. I was sent down this path when I found that wine connoisseurs used Ar to replace the air in opened bottles. Though I'm sure 15$ for that much gas is a gouging, it's a lot cheaper than buying even the smallest refillable canister of Argon.

Any experience I can gain using these small, easily located cans of Argon will be helpful until I can afford more substantial supplies.

Still, your advise is right on point and very much inline with what I hope to do as I move further along in my studies. Thank you very much for getting back to me.

[Edited on 9-1-2018 by JScott]

Thanks. My intention was to eliminate the need for inert gasses due to the production of CO2. It also reduces the potential for accidents due to the fact it's not an energetic redox. I hope to try it out myself.


Ah, so you did, and I clearly missed your assist. My apologies, I should have read your advice more carefully. Clearly I had thought my use of the balloon was so clever I stopped listening <LOL>, avoiding the use of the gas would be even better.

But, fascinated by the idea of that particular video I have already purchased the materials. Still, saving that expensive gas would be key.

Also, this was one phosphorus experiment that looked doable in the fume hood. It is sometimes difficult for me to use the yard.
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Hunterman2244
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[*] posted on 1-9-2018 at 13:13


Quote: Originally posted by JScott  
Quote: Originally posted by Hunterman2244  
Quote: Originally posted by JScott  
@Hunterman2244,

Thanks, when I scale up, it is my intention to work in a metal apparatus. However, I am a ways from there at this point. As mentioned, I really just wanted to recreate what I had seen in that video. Though it only appeared to be partially successful, I thought for me, it would make a good first step.

Partial successes can be instructional, and a bit more fun than absolute failure ;-) Further, I have been stymied by not having any inert gases on hand. I was sent down this path when I found that wine connoisseurs used Ar to replace the air in opened bottles. Though I'm sure 15$ for that much gas is a gouging, it's a lot cheaper than buying even the smallest refillable canister of Argon.

Any experience I can gain using these small, easily located cans of Argon will be helpful until I can afford more substantial supplies.

Still, your advise is right on point and very much inline with what I hope to do as I move further along in my studies. Thank you very much for getting back to me.

[Edited on 9-1-2018 by JScott]

Thanks. My intention was to eliminate the need for inert gasses due to the production of CO2. It also reduces the potential for accidents due to the fact it's not an energetic redox. I hope to try it out myself.


Ah, so you did, and I clearly missed your assist. My apologies, I should have read your advice more carefully. Clearly I had thought my use of the balloon was so clever I stopped listening <LOL>, avoiding the use of the gas would be even better.

But, fascinated by the idea of that particular video I have already purchased the materials. Still, saving that expensive gas would be key.

Also, this was one phosphorus experiment that looked doable in the fume hood. It is sometimes difficult for me to use the yard.

Cool, get back with your results, would love to see how it turns out.
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[*] posted on 13-9-2018 at 13:01


Quote: Originally posted by Magpie  
yes, I believe the intimate contact provided by molten aluminum/SHMP greatly augments the reaction rate. I don't understand how Monsanto and FMC get such good production using Apatite, sand, and coke at 1200°C. Perhaps the apatite is molten at that temperature.

I wish I could find a simple way to make briquettes about 1/4" in diameter.


I recently roasted apatite crystals from an igneous rock I crushed up into a fine powder. There was plenty of silicon based mineral as part of the composition. I had noted the previous day, I was observing the apatite crystals to melt into a black glassy substance. At hot temperatures it seemed to be a bit tar like but quickly cools into a glassy like condensate. I used a stainless steel crucible with a narrow tube exhaust port, which condensed a hot black tar like substance on the collection vessel ceiling. I then took this black substance and broke it off into my agate mortise and pulverized it into a fine powder.

I figured I would try to reduce it if I could thinking that would help identify the mystery end result compound. I mixed this with carbon and heated until it was red hot. The inside of the test tube became coated in white substance and the thought occurred to me that this could possible be phosphorus and I assumed it was at first out of pure excitement. The white substance glows brightly under UV light and it appeared to still emit a soft glow with the lights out.

I don't have a sense of smell, so I can't reference that observation. The little bit of exposed white material did seem to react energetically with water, but since my knowledge level and experience are still limited, I can't say for certain "I made phosphorus!" Not when I see all you other guys that have been working so hard over years to produce this element.

The two other test tube pictures that are obviously different than the first two were experiments with ammonium phosphate I created after isolating the phosphoric acid from Naval Jelly. Removing the xanthum gum is a gooey mess, but coagulated fairly well with ethanol and can be twisted around a glass stir rod into a globular mass. I neutralized the phosphoric acid with ammonium hydroxide to form ammonium phosphate, then heated the salt mixed with carbon dust. I don't know if any of the residue that formed in those last two test tubes were anything buy recrystallized salt. It didn't seem to glow under UV light like the first test tube did.

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