Help in identifying an unknown substance please!!

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Hey everyone,

 

First off, thanks for taking a look even if it's just curiosity. I have a chemical or substance that I am trying to have identified, and I can't really seem to get much help or where to turn.

 

I am not really good with chemistry so I was hoping for some good help on this forum. I will list pretty much everything valuable I know about the chemical, you can always msg for more details as I would be glad to discuss about it.

 

Let's just say someone does help me solve this! It would mean a lot and I would be very happy to give some sort of reward on my own! $!

 

At first I thought this chemical was methionine crystals, however, I was told that I am wrong. I have successfully managed to produce methionine crystals that look almost identical to this substance, the only problem is that methionine has a rotten odor that we cannot manage to remove so that did not work out.

 

This substance is in cleavage like flakes, it could be that the flakes were hand pressed but I am not sure, it doesn't really seem to break down into fine powder, it always breaks into smaller and smaller flakes. If you feel the flakes between your fingers, they have a sort of oily and slippery feeling. You don't get a lot of shimmering powder stuck to your hands but yet small flakes.

 

It is white/opaque lustrous and bright.

 

I can't measure it's melting point but for sure it melts quite fast, meaning that it must be as low as 100-200 degrees. It melts into what I would almost say a brown and sticky substance almost like a sugar.

 

Completely soluble in DMSO and methanol, not completely soluble in acetone, chloroform, or water.

As far as I can tell it does completely dissolve in hot water.

 

It's taste is salty at least this is what I find.

It is odorless (if anything it smells like fresh water, slightly)

 

I had a lab do a CHNO test and it has hydrogen only from water.

 

Carbon (wt%) 0.22%

Hydrogen (wt%) 4.45%

Nitrogen (wt%) <0.05%

Oxygen (wt%) 23.36%

 

I also have PIXE test results you can message me for them as they are really long.

 

I really hope to have all the help possible and solve this thing!

 

Last photo "DSC09416" as you can see there is small flakes/powder stuck to the bag so it's sort of free flowing but yet at the same time contained. Maybe because it's been pressed or flaked together which makes it more contained and originally the substance is free flowing.

[hypervalent_iodine]

First things first, and excuse my alarm here, but WHAT WERE YOU DOING EATING UNKNOWN CHEMICALS?! Honestly, what were you thinking? Touching them with you bare skin is bad enough, but eating them is just plain silly. I hope I misinterpretted something when you said that it tastes salty and that you weren't truly eating unidentified substances in a lab, but if you were, please don't do it again. It's for your own good. Anyway, since chemists don't go around eating chemicals as a rule (no really, it's a rule), telling us what it tastes like isn't very helpful.

 

To be honest, a physical description of what a compound looks like isn't very useful for identification purposes. Your characterisation data suggests your crystals were very wet, so it's not very helpful either, except that it tells you it is hygroscopic. This makes sense given your info on solubility. I would recommend running it through a GC-MS and getting a proton NMR. That will tell you what you have.

 

100 degrees C? That's not that low for an organic compound and you should have no trouble figuring outthe m.p. if it's in that range. That it went brown means it decomposed (which isn't melting), so you have likely ramped the temperature up too high, too quickly. It does sound like what happens when you heat sugars up, though (think toffee), so I'm suspicious you have a HCl salt of an amine derivative of some kind (maybe glucosamine hydrochloride). There are a few chemical methods to test for this, but they still won't give you exact information and getting spectral data is really much faster.

 

To conclude: I think what you have is the hydrochloric salt of an amino saccharide. Having said that physical appearance is useless, I'm going to make a hypocrite of myself and say it looks like D-aminoglucosamine hydrochloride, having had worked with it before. Get GC-MS or mass spec data and an NMR spectra to confirm. Finally, do not eat chemicals in the lab. That is a bad, bad idea.

 

Just a quick edit: it may also be N-acetyl glucosamine or similar.

Edited January 13, 2012 by hypervalent_iodine

[Suxamethonium]

I won't lie and say I've never tasted anything in the lab- but only if I've known what it is (and even then I understand that there are risks of impurity, etc so I avoid it). Haha, But I did find it funny- anyway, I agree that this information isn't very helpful and that HNMR, GC-MS, or even just an MS would be much more informative. Even IR would be more helpful than physical appearance. The only reason I wanted to add to this was because if it is a hydrochloride salt, neutralising with ammonia solution would yeild the free base (which should have different physical properties, and may help in identification if the afforementioned in the absence of GC-MS and HNMR).

[hypervalent_iodine]

Yeah, as I said, there are a bunch of chemical tests you could do. Yielding the free base would be useful though, because I am now more convinced it may be the N-acetyl derivative and doing so would eliminate or confirm at least one possibility.

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Hey guys, thanks for the reply! I know I know, eating was a bad idea but I really need to find out what this is! That's not a good answer but I've been working on this for a while, I didn't really clarify that I'm not a chemist and I have no equipment, hence, why it's probably taken so long to get some where and well I still haven't really gotten anywhere, I just have research online.

 

I really appreciate you looking out for me though, and next time I have an unknown substance, I won't eat it, I'll just bug you guys .

 

"hypervalent_iodine"What do you mean that the crystals were very wet? Did I misunderstand something? Because they don't seem to be physically wet. They are very dry.

 

I don't have many methods to test (hence why I can't even get the exact m.p) however, even if there was a cost, I would be willing to send some sample to whoever could help test this item and hopefully finally identify them.

 

Really appreciate the help and I look forward to your replies.

[hypervalent_iodine]

Can I ask if you have any inclination at all as to what it might be? As in, are you able to narrow it down to a certain type of chemical or did you literally just stumble upon a bag of unlabelled white powder? Your best bet in terms of characterisation is to contact a lab willing to run some tests for you. You'll want ¹H NMR and mass spec at least and perhaps a GC-MS trace to ensure purity, etc. It will cost you money (though I have no idea how much, but it will give you your answer. If you can do that, show your results here and we/I can take a look at them for you.

[John Cuthber]

If the analysis given is really

"I had a lab do a CHNO test and it has hydrogen only from water.

 

Carbon (wt%) 0.22%

Hydrogen (wt%) 4.45%

Nitrogen (wt%) <0.05%

Oxygen (wt%) 23.36%"

 

Then it isn't an N acetyl anything.

In fact that's a rather odd anlanysis.

Anyway, the really important question to ask is "where did this stuff come from?".

Without knowing that it's pretty near pointless to speculate.

[michel123456]

I would have a look at the label on the plastic bag.

[hypervalent_iodine]

If the analysis given is really

"I had a lab do a CHNO test and it has hydrogen only from water.

 

Carbon (wt%) 0.22%

Hydrogen (wt%) 4.45%

Nitrogen (wt%) <0.05%

Oxygen (wt%) 23.36%"

 

Then it isn't an N acetyl anything.

In fact that's a rather odd anlanysis.

Anyway, the really important question to ask is "where did this stuff come from?".

Without knowing that it's pretty near pointless to speculate.

 

The results of that test were too convoluted from the water in it to really tell much of anything without calculations, so I ignored it since I was posting on the run and not near a calculator.

 

Edit: I just did a couple of calculations to work out the true oxygen percentage assuming that all of the hydrogen was from water and the results don't really make much sense to me. Perhaps you could shed some more light on it, as I am not terribly familiar with this type of test.

Edited January 13, 2012 by hypervalent_iodine

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Once again thanks for the reply, I am willing to have tests done but I need a good lab, I have contacted many and most say they are not fit to do testing like this etc. Does someone have a recommendation? I will get the tests required done and posted up here.

 

I wish I knew a lot more but this will sound odd to you guys, we are a company that deals in Incense, I am sure most are familiar with fragrance or natural Incense? Well that's what we manufacture and sell. There will be a couple of products we will stumble upon that are like the one above. A company brought into the market the incense above (I've had a similar experience before, someone else brought something similar to the product above before) what usually I find happens (may not be the case this time) is instead of it actually being some sort of incense (the usual with bamboo, resin, etc) it ends up being a cosmetic ingredient or a food/feed ingredient.

 

Basically this product above is being packaged as "magic incense" for novelty use and being sold, it's a pretty popular product. So to stay in the game naturally, we would also need to produce it and get our share of the market.

 

This is why, I don't have too much chem experience (I've done basic chem in school etc but nothing that would really get me far).

 

I sent to one lab before, they did a PIXE and CHNO test, from what I understood, CHNO test shows the amount of carbon, hydro, nitro, oxygen in the substance? And PIXE test is I believe what it could be contaminated with or contain, sulfur, chlorine, etc. It's too long to post up here, so if you guys could message me your email I'd be glad to send that.

 

As for the rest of the tests, willing to get it done, just need someone reliable that can do it.

 

Being that it's being passed off as an Incense novelty item, they have no requirement to give me the real name, use, or ingredients etc.

 

My guess is that it's something that's been some how worked, a substance that's been crystallized, or some substance washed with something, or even a powder/flake just bonded together using a non toxic liquid.

 

The reason that at first I believed this was dl-methionine is because I had an optical rotation test performed on it, and they told me it was dl-m. Once I received dl-m, it's small flake type of substance when you touch it, and shimmers the same way, so I was pretty sure it was that. However, even after having recrystallized dl-m, the appearance was the same, dl-m also dissolves easily I find etc, but the problem is that dl-m with it's sulfuric odor, it defeats the purpose and I could figure out no method to modify it to have no odor. So from there I figured it probably isn't dl-m. Also a friend that looked at it for me, who's test info I have also posted above claims that it is for sure not dl-m. It could even be that it's just some sort of neutral filler, or that, it's being modified to not retain much and be a neutral filler. All that is important about it is that it's appearance and that it dissolves.

 

Thanks again everyone.

 

Just a side note, here's what PIXE test is "Proton Induced X-ray Emission (PIXE), provides a non-destructive, simultaneous analysis for the 72 inorganic elements from Sodium through Uranium on the Periodic Table for solid, liquid, and thin film (i.e. aerosol filter) samples."

[hypervalent_iodine]

It's hard to say without knowing where you are, although even then I would not have anywhere to recommend for getting a sample tested. You might be able to find a pharmaceutical testing company or some other analytical lab that will do the tests for you.

 

Also, dissolves in what?

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I was going to mention that and forgot. I am in Canada, and if it's any help, the product comes from USA. The product dissolves and disappears in hot water as far as I can tell, when heated on it's own with no liquid, like I mentioned before, also dissolves turning into what looks like a clear oil/water. Do you think it could even be an inorganic matter or is it most likely organic? I'm not very knowledgeable on the subject but at first I was sure it's some sort of amino acid, but I could be very wrong.

[hypervalent_iodine]

As JohnCuthber said, speculating is not going to get you anywhere in terms of working out what it is. You need to get tests run on the sample. Also, I was asking what you want it to be able to dissolve in?

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I am going to try to find someone to do the tests that you mentioned, but if someone in this forum is able to do them of course for a fee, I'd be happy to save the time and have them done properly.

 

I'd like it to be able to dissolve in water and on it's own as it already does. I'd like to identify this substance as is so we could re manufacture it on our own.

 

Thanks

 

I realized that I could upload the PIXE test results, I am sure that when you guys take a look at it you'll know what they are. I hope it's of some help! Also lab gave me a sheet on how to interpret their PIXE results, which is also attached.

 

Thanks

 

Also what I am wondering is, even if we are unable to for some reason identify this substance, has no one seen a substance that looks very close to this one? That is I guess look wise micaceous, flaky, etc and also dissolves with heat readily, also dissolves and disappears into water, such as where I got started with dl-m, I find that it looks pretty close to this, it dissolves, only problem was the odor, if somebody even has a suggestion on how to remove the odor on dl-m I think that would still be a good substitute for this, you have to remember that I am just looking for something similar to this, I know from a chem point of view you have to be very to the point and not general, but for my use, it's not for food or anything very important as mentioned before. Any help like that would be great as well.

 

 

 

I am wondering if nobody has seen anything similar to this really, could it be it was chemically engineered by some chemist? It's sort of an original item? Could this be possible as well?

 

Sorry for all the questions just trying to run all possibilities until I can find someone to definitely test it.

[hypervalent_iodine]

Your best and easiest bet is to get a lab from where you are from to do the analysis. IIRC, of the chemists I know of who frequent here, none are from Canada, which makes it difficult (ignoring the fact that it would probably not be allowed anyway).

 

Your PIXE results seem a bit odd to me, but I am by no means familiar with that type of test. It says there is sulphur in there, so it could still be methionine. Again, though, it is impossible to tell without some more data.

[John Cuthber]

It says there are a few ppm of sulphur there. Methionine should be something like 21% sulphur.

On the other hand, as I have said there's something odd about the analytical results- they don't add up to 100% so they have clearly missed something, but we don't know what.

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If you happen to know of some chemists that could do the test please do let me know, as I have looked previously for labs and I didn't find anyone in Canada who was able to test for us. I would probably go with the lab that did the tests above again, they are in USA also, so I would have to mail another sample anyway.

 

Your best and easiest bet is to get a lab from where you are from to do the analysis. IIRC, of the chemists I know of who frequent here, none are from Canada, which makes it difficult (ignoring the fact that it would probably not be allowed anyway).

 

Your PIXE results seem a bit odd to me, but I am by no means familiar with that type of test. It says there is sulphur in there, so it could still be methionine. Again, though, it is impossible to tell without some more data.

 

Is it still a possibility with the test results that it could be methionine and some how sulfur was removed? Or is this something that is "impossible". Keep in mind that someone may have worked some sort of chemical to actually make it harder to identify. I don't think this is something that is naturally flakes or even flakes naturally, I wouldn't be surprised if it was some worked powder and then pressed together to appear as flakes. So maybe they use water to do that?

 

It says there are a few ppm of sulphur there. Methionine should be something like 21% sulphur.

On the other hand, as I have said there's something odd about the analytical results- they don't add up to 100% so they have clearly missed something, but we don't know what.

 

Also a friend seems to think that this maybe talc powder, do you think this is a possibility? I did some quick search on talc and I couldn't find any that is so lustrous and I think it doesn't dissolve in water, where as this completely disappears into water.

[hypervalent_iodine]

You might find it difficult to send to anyone overseas, since you have absolutely no idea what it is. Customs officials tend not to like mysterious white powders.

 

The appearance of the crystals is not unusual. There a few compounds I remember having encountered that look similar, though they are not something you would really want to use for the purposes you state.

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It's actually not difficult, we order this from USA into Canada in large quantities, it's manufactured in the USA and it always stops at the border for a check, sometimes it gets delayed because they test it and it gets released. It's some sort of a neutral filler. I think you made sense, I think it's just a crystal form of some chemical, which chemicals do you have in mind and why would they not be good for our purpose?

 

 

You might find it difficult to send to anyone overseas, since you have absolutely no idea what it is. Customs officials tend not to like mysterious white powders.

 

The appearance of the crystals is not unusual. There a few compounds I remember having encountered that look similar, though they are not something you would really want to use for the purposes you state.

[hypervalent_iodine]

Because they are toxic.

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Yes you are correct, it won't be a toxic chemical. Do you think it might be impossible to identify this?

[hypervalent_iodine]

No, you just need to get the right tests done on your samples.

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Okay, I'll probably go with the lab as before, could you please tell me which tests are necessary?

 

Thanks a lot.

 

No, you just need to get the right tests done on your samples.

[hypervalent_iodine]

¹H NMR (tell them that your sample is soluble in DMSO and MeOH and not chloroform), ¹³C NMR if possible, high res mass spec and maybe see if they can run a GC-MS on it.

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Update, my friend that told me it is soluble in DMSO, etc, just told me that he ran the 1H NMR and 13C NMR and he tells me the compound is for sure an inorganic one. I guess I should link this to inorganic category too? By the way, any closer ideas now knowing it's inorganic?

 

 

¹H NMR (tell them that your sample is soluble in DMSO and MeOH and not chloroform), ¹³C NMR if possible, high res mass spec and maybe see if they can run a GC-MS on it.