Study of natural nanoparticles of noble metals (NMs) is a rapidly developing area of modern geology and thus requires developing new precise instrumental methods of analysis. Further development of scintillation emission spectral analysis (SES) based on the use of a new spectrum recording system provides unprecedented opportunities for material research. We present the results of studying the samples obtained from hydrotherms near the volcanoes of the Kuril Islands using a modified SES method. It is shown that the proposed method of recording is not only a powerful tool for geochemists in determination of the quantitative content of NMs in a sample, but also provides information about the forms of the element present in the sample.