navg

It's just not working. Something else finally came to mind. Could it be that there is a different grade of boric makes different crystals? And if that is possible. Is there a way for me to test my sample and identify it's grade?

Thanks

You can usually get bigger better made crystals by cooling a solution slowly so the crystals form slowly.

I am hoping for large and very flaky crystals as in the picture. These crystals are not clear/see through, is that what you had? These are actually a mother of pearl color, soft, silky and very flaky, they slip/flake off each other.

Haven't been on in a white, however, still searching for my answer, any help?

Thanks

Hey, it's been a while and unfortunately still haven't solved my issue. I need crystals like in the photo above. I don't know if some how I could have done something wrong to your method? Can you "John C" tell me that your crystals were identical to mine? I tried your method a couple of times all I get is just boric acid as it is. What can I be doing wrong?

I have also tried with HCL acid and Sulfuric acid, I don't know again if I am doing something wrong, but no luck getting this! I have talked to other people on the subject, everyone who looks at the photo is not sure either but imagine it could be from sulfuric or nitride?

Any help guys?

Weigh out some boric acid (say 100 grams).

Put it in a suitable container. A glass saucepan would be good. Add 4 times as much water (so, for 100 grams you need about 400 ml of water).

Heat the mixture until it boils gently and stir it.

Once the liquid is boiling all the boric acid should dissolve. (Borates have a reputation for dissolving rather slowly so it may take some time. Keep an eye on the water level. If lots of it evaporates as you boil it you might need to add some more hot water.).

Once all, or almost all of the solid has dissolved stop stirring and stop heating the solution. Let any solid material settle out.

Pour the liquid into another container leaving any undissolved material behind.

Let the hot solution cool slowly.

It should form crystals like those in the picture you linked to.

Pour off the liquid from the crystals ( it probably makes sense to put it back in the saucepan.)

Wash the crystals with a little cold water and filter them out of the solution. A fairly fine sieve is probably better than filter paper for this because you won't get bits of paper in the crystals.

 

You should get most (about 60% or 70%) of the boric acid back as crystals.

Yes exactly, I am not sure if it's the fact that the crystals are too big, when I compare it to my sample/photo it's not the same texture at all. Like mentioned before they don't compact together, they aren't slippery feeling, or even smooth and they break into powder very easily.

My sample is pretty much the opposite, soft silky, smooth, slippery, and it will break into small flaky layers. Like mica basically. Even looks like mica.

About the HCl acid, I should have been clear, I mean could it be possible that when borax is transformed into boric that it forms to be like this?

So, when you did the recrystalisation before, letting the solution cool- you said you got the right sort of crystals, but they didn't compact to form the flake?

 

What I feel is likely to have happened was that you got a bigger crystal (same shape and texture, but the increased size wouldn't compact as easy). You could try to induce smaller crystals by precipitating them from solution faster (i.e. rapid cooling (on ice) and scratching the bottom with a glass rod to induce precipitation). As spectulation, I would imagine industry would cool and induce precipitation in such a way because it is easy to do, and quickens the overall process- this might be why they achieve the smaller, more compactable crystals.

In addition, I did the slow boil, didn't really help much, I get what you mean that it produces bigger chunks, however, it's still a completely different texture, but as I said before it does have flakes of very shinny small flakes which is a good thing I guess.

Any help appreciate.

Yes, and by getting a good look at the photo, would you still say your flakes looked like this? Or do you believe something is being added to change texture/appearance?

Why do they add concentrated HCL or H2SO4 do you know?

Sorry the Borax was a mention, I read online that if you crystallize Borax under HCL Acid, then it turns into boric acid flakes, so I wasn't sure which one would result to be what I am looking for.

I also have CHNO and PIXE tests maybe someone can take a look and see if something extra is added?

Carbon: 0.22%

Hydrogen: 4.45%

Nitrogen: <0.05%

Oxygen: 23.36%

PIXE TEST:Check attachment.

Also can you look at better photo and confirm you've made flakes like this once again?

On the same note for curiosity, does Borax crystallize like this? I have tried Borax and it gives salt like crystals which I read people use to make decorative snow flakes. My friend is 99% on the flakes being Boric, but if some how Borax can give the same appearance I can try it and see if it's closer to the sample I have.

Can someone also clear this up for me??

This is what I keep finding online and it confuses me. When I google description of my sample. I get mainly:

Boric acid from Borax :- Concentrated HCL or H2SO4 is added to a hot

and saturated solution of borax, boric acid is produced. The product is cooled, when

pearly white silky crystals of boric acid separate out. These are washed and purified by

recrystallization from hot water.

Hey,

So I tried the experiment, I got basically what I had gotten before, unfortunately it doesn't look entirely like the photo. I got vitreous crystals which is a good thing because it's a property the flakes have the same shine. However, the flakes that I have in my hand, they stick together well in form of layers and it actually flakes, they are softer and slippery feeling. The one I got from water still sort of feels like boric acid/greasy and does not stick together.

My friend had analyzed a sample of the flakes for me, he did identify it as boric acid but, he is not any good with borons so he couldn't help me more, but what he did say was that the solution was more acidic than he would expect boric acid alone to be.

I'm starting to think that maybe they crystallize just the way you told me to do but add an acidic solution so they come out feeling and looking different?

The level of pH of water solution at room temp ~4-5. is what my friend got.

Would you happen to have any more ideas on what I could try? I really appreciate it.

Thanks!

Way to be a show off but I cannot seem to get them!!

I tried 1. Boiling boric in water, waiting for it to cool, upon cooling filtering it out of water, once they had dried, it seemed to be just boric again...

2. I have tried same thing but with adding diluted H2S04 (half weight of boric) so example 2g boric 0.5 H2S04 with 0.5 water dilute. This gave me a paste...

I have been trying to figure this out but no help! I hope you can help!

Thanks!

I have produced crystals of boric acid like those in the picture. I did it when I was a school kid "playing " with chemistry so it certainly isn't difficult.

 

Exactly what did you do that didn't work?

Please check out this link. And take a look at the photo. This is basically what I want to learn. How can I transform boric acid into this?

Thanks!

http://www.ebay.co.uk/itm/Boric-Acid-Flakes-1kg-insecticide-antiseptic-/190577869343

Have a client who wants to buy it crystallized, I tried with water, didn't really seem to work, reverts back to powder, there's a method to make it into crystals/flakes.

Does anyone here know how to crystallize boric acid? I've been reading all sorts of stuff online and don't know what is right.

Borax under HCL acid?

Boric acid under sulfuric acid?

Does anyone have the correct method?

Thanks

any help?

Exactly what my friend said, and yes it does give us a green flame! So what now?

I wondered about boric acid because it would explain why nothing much showed up in the PIXE results.

Anyway, if it is than this is as good a way to prove it as any.

Hello,

I need the help of a boron specialist/chemist. I had an unidentified substance and I posted a thread in the organic chem topics trying to have it identified. After a friend helped do some tests, he believes that the substance is most likely boric acid.

Please check the link below it will lead you to the original topic. You can see photos and info about the substance. My friend is not good with inorganic chem, so he suggested that a boron chemist could probably help me.

I would like to find out which type of boric was used, and how to crystallize it like my photo? If you know of a lab or someone who can help and requires a fee, do not hesitate to let me know, if you require a sample for testing, I can provide this as well.

All help is honestly greatly appreciate.

Thank you!

http://www.scienceforums.net/topic/62954-help-in-identifying-an-unknown-substance-please/

Too scared to do this! The FDA actually doesn't regulate incense, and well it's been tested before and I tried to ask them what it was, they wouldn't tell me, they said that it was non-toxic and not illegal. So they let it pass every time, and in large quantities, lol wish it was that easy!

On the plus side, I have some more data. I hope you geniuses can help narrow this down now!

In water:

Solubility at room temperature - approx 50 mg/mL, or about 5 g/100mL

Solubility at 100C - approx 160 mg/mL, or about 16g/100 mL

These were measured by adding excess solid to water, storing one sample at room temp for two days to equilibrate, and heating the other to reflux. 0.5 mL of each sample was transferred to a vial and the water removed under vacuum. Solid residue was weighed. The solubility measured at 100C may be slightly lower than the true value - the sample cools during the transfer process and the product rapidly recrystallized, leading to some loss of sample

pH of water solution at room temp ~4-5

Well, there you go. Try to bring some across the border, look a little too sleazy (I recommend some bling, dark sunglasses, hip-hop clothing and some scantily-clad chicks women), ... and presto, they test it for you.

 

Seriously though, you might ask some American govt agency (eg, US DEA) to test it or look into it. Tell them what you told us and more ... you use it to make "magic incense", you're worried that it's illegal or otherwise harmful, and would like to know what it is from a consumer safety perspective. You might be surprised ... and you'd be doing the right thing. I wonder if the FDA regulates incense.

lol thanks a lot, I could send you a sample if you'd like to do that idea . It's for not something toxic, it's something really general and it's just not coming to mind, especially because I think it's been worked like recrystallized and then probably compressed together using water or something else.

I wouldn't mind trying to do some tests at home with it, all I've done to it really is burn it with water and burn it without water (tried tasting it ) and smelling of course, noting down the texture. And as for my friend tells me, he's the one that told me what it's been dissolved in DMSO, etc and he says that there is a lot of water in it so it is probably a highly hydrated salt. He suggested to do atomic absorption or atomic emission spectroscopy to determine the presence of the various metal ions - sodium, aluminum, silicon, magnesium, calcium, etc. And then see from there.

Would love to hear back from you guys, but get your sleep first! Good night!

Ok, so inorganic- (edited out now completely irrelevent old post).

 

Not exactly my area, but did it contain any carbon or hydrogen at all? example, HCO₃^- or CO_3^2- ? Or the HNMR would show if it was wet or dry (H₂O). Um. I guess precipitation reactions or AAS may be most beificial to you, the former you can do at home using a variety of household substances. Let me know if this interested you- i'll think of some important ones.

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.

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.

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

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.

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.

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.

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.