We approach this problem purely from the sample side and disregard the specific apparatus. Non the less of course an integrating sphere with reabsorbtion correction will be used.

Lets say we want to determine a quantum yield (QY) of a solid, crystalline substance. What i gathered from literature is that particle size matters when You are measuring a solid sample, this is the case also for me:

Example: Crystals formed via vapor diffusion (big orderly crystals suitable for X-Ray) gave QY of ~ 5%, when i ground this material in a pestle a powder like substance was obtained and it gave QY of ~ 19%, on the other hand if the substance was directly precipitated from saturated solution using a solvent in which the material does not dissolve (DCM -> pentane was added) a similar powder like substance was obtained, in this case the QY ~ 22%

All of these measurements were done with the same substance (same batch) at the same purity etc. several X-Ray structures (from different solvent systems) revealed that solvent does not participate in crystallization pattern and the pattern is always the same.

Which of these measurements should i choose?

Are there any other aspects we should take in consideration?

Thanks in advance,

Kaspars

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