Derivatization

[chemistab]

I want to ask how can i derivatize methyl iodide? I try to determine methyl iodide but i think that it reacts with a acid of my sample and i haven't so good recovery. Any suggestion please?

[Don_Hilton]

If you derivatized methyl iodice you will create a methylated compound and iodide ion. Depending on your sample, it may be difficult to separate results arizing from methyl iodide from methylated compunds and iodide ion alredy present.

Tell us about your sample and what you are doing for analysis. Losses may be stongly related to these. Also, are you following any procedures from the literature, if so, at least give us some citations.

[chemistab]

My sample is a medicine which contents tartaric acid. I think that methyl iodide reacts with this acid. I make spiked the methyl iodide in my sample but i have no good recovery. Why you think it happens?

About my method: I make headspace injection (after 30min - 100 OC ) my temperature program: 33 OC (initial temperature) holding 8 min and with a rate 30 OC/min - 240 OC for 3min. Injection mode split (split ratio 5). Injection temperature 140 oC. The column is DB-624.
I tried also to neutralize tartaric acid with NaOH in MeOH.But the result wasn't satisfactory.
Any suggestion please!!!