You need to specify the spectroscopic technique, as different considerations may apply to IR, UV/VIS, NMR, XPS MS etc. depending on the technique. Optical spectroscopies are limited by the beam size and homogeneity, on the technique (transmission, reflection - total or diffuse -, on the sensitivity of the instrument etc. In optical spectroscopies usually the path length should be carefully selected, or if you use solutions, the solution concentration. Usually these parameters are selected so that the transmission is bwtween 30% and 60% (it gives the best signal to noise ratio). In the case of NMR the sample size is determined by sensitivity and manetic field homogeneity. And so on.
I guess you refer to NMR spectroscopy.
Based on my experience,
the main thing is first to determine the time resolution you need for your experiment,
then you evaluate experimentally the volume which allows to obtain a spectrum with an acceptable signal to noise ratio (>10) during that choosen acquisition time.
In my case, I will use High resolution UV-NIR spectrometer to determine reflectance and absorbance properties of insect. How many time I have to collect the data per sample? Is it n = 30. Any ref.?
No reference. But weak radiation (NIR with a lot of overtones) means you will get a weak response. N = 30 sounds reasonable but try a spike sample to confirm.
From your side, what is the most suitable spectroscopic technique to handle short wavelength sample, < 1000 nm. Any suggestion?
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