Chromatography Forum

Hi All,

Since our GC/MS isn't equipped with a headspace. I was wondering what other possible ways to identify the solvents used in nail polish.

at the moment I'm thinking of putting a vial containing the nail polish in hot water bath then quickly take the head-space gas with a syringe and manually inject it to the GC/MS.

Just wondering has anyone ever experience doing this before?

Tarapan.

Quantitative or just qualitative?

Quantitative or just qualitative?

qualitative for the moment

I've never analyzed nail polish, but for a quick scan you can use a headspace vial and put it into a standard lab oven at about 80 °C. You need to heat the syringe, too. Temp gradient should start at a very low temperature to be able to cut off the air injected with the sample.

Ah, and you should wear cotton gloves - the syringe is hot...

Hi

Agreed might work for qualitative purposes.

But also consider what your looking for. On top of my head I would guess you will find "a lot" of ethyl/buthyl actetate possibly toluene. Acetone is "usually" in removers rather than in the polish.
The acetate peaks may be huge and might interfer if you not chose column and oven program wisely.

Back In the past,we "jury rigged" the autosampler on our old 5890 GC to do headspace work.

You can connect the sections of the sample tray with tubing and connect these into a circulating water bath which will pump heated water through the trays and around the samples.

We inserted squares of filter paper, rolled into a cylindrical shape into 2 mL chromatograpy vials. If you add liquid into the vials, caplillary action draws it into the paper ensuring no liqid gets into the injection syringe.

We the fitted the 7673 injector with a syringe capable of injecting 100 µL on the largest setting. We couldnt use a gas-tight syringe of this size in the auto sampler but if you use a non gas-tight one and lubricate it with a viscous mineral oil, it can work.

We developed a successful method for an anasthetic in blood on that type of system.

thanks everyone for the ideas.

I like the filter paper in the vials idea.

Just one thought though, since the solvents in nail polish are volatiles. it might make more sense leaving the vials simply at room temperature for a while to saturate the headspace and then injecting the headspace gas. my only worries now is if the vapour are sufficient for detection.

need to try it out after the weekend though.

Tarapan

Hi all; I just wonder what about SPME - HS?

I've never analyzed nail polish, but for a quick scan you can use a headspace vial and put it into a standard lab oven at about 80 °C. You need to heat the syringe, too. Temp gradient should start at a very low temperature to be able to cut off the air injected with the sample.

Ah, and you should wear cotton gloves - the syringe is hot...

We do this three ways:
1. We put some product into a septum-capped vial, put in oven like above, use a 1 ml gas syringe with an on-off valve, inject and over-ride the solvent delay.

2. We use a traditional 10ul syringe, rinse it a few times with product, expel it, then inject the empty syringe contents into GCMS, and over-ride the solvent delay.

3. Our headspace unit.

In U.S., personal care products have ingredients statements, or manufacturers and retailers can can contacted for MSDS sheets.

Tarapan,

Run a big split. 500:1 or 1000:1 for example. Petroleum industry shoots neat gasoline like this so I cannot see why it would not work in your case. Of course you are only looking at major components but you can get away with using your current autosampler, especially if you tell it to only shoot 0.1 or 0.2 microliters.

Best regards.

tarapan,

Being a bit rusty.... The other possible solution is that you set the needle depth. Depending on which autosampler you have you could just tell it to sample the headspace by only putting the needle just in the vial. The newest Agilent autosamplers have this capability.

Best regards.