How can I distinguish between the first stretching overtone N-H and O-H bands in NIR region as both of them has the adsorption bands in 1400–1500 nm?

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Jacques Lavau

I understand that your aim is in analytic chemistry, for molecules or conglomerate of crystals of high molecular weight ?

So no hope with this mean of investigation. You must turn elsewhere to have the missing informations.

I suggest you to correct your "adsorption" into "absorption".

Gyorgy Banhegyi

I agree, mid-IR will be more useful for your purposes. Once you have the basic frequency, you can find out the overtone. but the poblem is that in the case of H-bonded (associated) NH or OH bands these bands are rather broad, so there can be an overlap between the NH and OH ranges.