This reference describes a method for the determination of hydroxylamine with Vanillin that is linear down to 20ng on column.

Korte, W. D."Determination of hydroxylamine in aqueous solutions of pyridinium aldoximes by high-performance liquid chromatography with UV and fluorometric detection" Journal of Chromatography (1992), 603(1-2), 145-50.

Thanks a lot for suggestions, I will try...

Dear Bharani,

The simplest method for direct and highly sensitive hydroxylamine determination is the ion chromatography with amperometric detection. You need an electrochemical detector and cation exchange column. There are a lot of publications in literature on this analysis, foe example:

http://www.sciencedirect.com/science/article/pii/S0021967302001450

Thanks a lot Dmitry,

We have IC with conductivity detector, we could reach up to 300ppm. I will check it for electrochemical detector.

Dear Bruce

I have tried vanillin oxime method, works out really good.

we could reach the required 1 ppm level, but the standard area is keep on increasing, trials are going on. any suggestion.

Thanks once again

Bharani

Did you use pure hydroxylamine? The authors of the paper indicate they recrystallized the hydroxylamine from ethanol and methanol. To make up the vanillin solution the vanillin is first dissolved in absolute ethanol (make sure it has a low aldehyde content) to give a clear solution, then diluted with an equal volume of deionized water. If you think the vanillin oxime is not forming all the way you could try a longer reaction time (>30min) and/or a higher reaction temperature (>25C). The autosampler rinse solution should be pure methanol for this assay; you might be seeing carry over from the higher concentration standards.

Hi Bruce

I have applied the same procedure that you have mentioned. Observed that after 24 hours the standard area looks consistence. I will check the recovery...any inputs on this regard.

Thanks Bharani

Hi Bharani,

Can you attach the publications for hydroxylamine content (by HPLC and by ion chromatography) if possible.

Thank you

Hi Krish

Please check Mr. Bruce reply, he mentioned about the article details(Korte, W. D."Determination of hydroxylamine in aqueous solutions of pyridinium aldoximes by high-performance liquid chromatography with UV and fluorometric detection" Journal of Chromatography (1992), 603(1-2), 145-50)

 I have tried the same. right now i don't have the IC details.

Have a nice day.

I am unable to access it since both are behind a pay wall.  If possible can you please attach the paper if you have it