Sciencemadness Discussion Board - Unknown product made by accident

Unknown product made by accident

Xrpdguy - 9-7-2018 at 03:18

Hello guys again. Yesterday i discovered one interesting product (in crystal state ) in my lab.
The main idea was making elemental iodine from povidon solution (by Nilered instructions )but it didn't work. So i left in for some time.

In the meanwhile i worked on mixture HCl-H2O2 (one of my previous posts) and benzoic acid+H2O2, so somehow one part of benzoic acid and hydrogen-peroxide i dropped in the povidone mixture.

I was disappointed cause i thought that nothing will happen and left the contaminated povidone mixture in one large beaker for some time (2months). From that day till yesterday no one touched that beaker and a whole liquid disappeared. At the bottom were beautiful crystals (i gave it name X).
X crystals are highly hygroscopic but only on their surface and very sticky.
Today i am gonna check its reaction with reagents, but i am curious did you ever see something like this.

At the bottom of the beaker was yellow layer and after some time a lot of foam was present.

Xrpdguy - 10-7-2018 at 04:20

What do you think about this? Did you see it somewhere or know which compound it should be?

woelen - 10-7-2018 at 05:11

The foam can be explained by assuming that H2O2 slowly decomposed, giving oxygen, which leads to formation of bubbles (and hence foam) in this solution.

I cannot say anything about the crystals. I do not know the Povidon solution you used, I assume it is a complicated mix of all kinds of chemicals and for such things it is very difficult to say anything useful about their composition.

I suggest you to buy some real reagents, like KI, and some acid (e.g. 10% HCl will do) and do experiments with that. That allows you to make iodine and isolate it.

Xrpdguy - 18-7-2018 at 04:24

Quote: Originally posted by woelen

The foam can be explained by assuming that H2O2 slowly decomposed, giving oxygen, which leads to formation of bubbles (and hence foam) in this solution.

I cannot say anything about the crystals. I do not know the Povidon solution you used, I assume it is a complicated mix of all kinds of chemicals and for such things it is very difficult to say anything useful about their composition.

I suggest you to buy some real reagents, like KI, and some acid (e.g. 10% HCl will do) and do experiments with that. That allows you to make iodine and isolate it.

I have mixed the Betadine 10% povidon solution with 30% hydrogen-peroxide and 5M NaOH (98%).

Crystals are insoluable in water and ethanol.
With HCl only the liquid on their surface react so the end at the bottom of the test tube are crystals with some dark orange precipitate.
In the flame crystal explode :p
With CuSO4 solution it makes light green precipitate.
Only with a mixture of NaOH+H2O2 crystals react and give some foam and blurry solution. Also some gas was produced.

After standing light-green precipitate is down layer and green clear solution is upper layer. Green solution is sensitive on light so it became brown.

More analysis i will do tomorrow.

XeonTheMGPony - 18-7-2018 at 04:35

Sodium iodide?

Sigmatropic - 18-7-2018 at 08:09

Sodium iodate?

Deathunter88 - 18-7-2018 at 18:51

There is zero point in trying to figure out what you made. As woelen said, go buy some real reagents and try do something useful.

Xrpdguy - 19-7-2018 at 04:59

Quote: Originally posted by Deathunter88

There is zero point in trying to figure out what you made. As woelen said, go buy some real reagents and try do something useful.

Well, not very much people make something new or undiscovered things here.
These crystals can be very usefull as a catalyst for an oxidation of alcoholes and i started a research.
The structure and formula can be determined by some instruments, like XRD or XRPD, but i want try a determination by using some simple reactions and discusion about it.

This post wasnt about getting iodine but determination of some unknown thing. It can be simple as NaI or NaIO3, but can be also more complicated.

Xrpdguy - 29-7-2018 at 10:48

As i said crystals react with CuSO4 and make green precipitate and clear solution above it.
That solution is light-green and after some time it become dark orange, almost brown.
That brown solution i have mixed with 0.5ml of potassium-metabisulfite and got clear light-blue solution with some white precipitate.
Can you tell me what it can be?

weilawei - 29-7-2018 at 11:14

Well, how about taking a melting point for starters?

Abromination - 29-7-2018 at 12:23

You might have to do some hard core spectroscopy here. It would help to know the melting point of the crystals, and try doing some experiments leaning towards the idea that it is not organic as the yellow polyme was left behind. Also be careful experimenting as anything can happen when you dont know what it is.

Hendrik - 29-7-2018 at 12:40

Could the crystals be peroxybenzoic acid? Maybe H2O2 reacted with the benzoic acid in order to make peroxybenzoic acid which would explain the explosive nature of the crystals. Also, try to take a better picture of the copper precipitate. If it is actually pale blue instead of green, the precipitate would be copper benzoate.

Abromination - 30-7-2018 at 20:49

If it is peroxybenzoic acid, the melting point of the crystal should theoretically be between 41 and 42. In what way did it explode when heated?

Xrpdguy - 1-8-2018 at 21:50

Quote: Originally posted by Hendrik

Could the crystals be peroxybenzoic acid? Maybe H2O2 reacted with the benzoic acid in order to make peroxybenzoic acid which would explain the explosive nature of the crystals. Also, try to take a better picture of the copper precipitate. If it is actually pale blue instead of green, the precipitate would be copper benzoate.

Precipitate is white and solution above it is pale blue.