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Annealing in air and vacuum were obtained glass samples Li2B4O7:Ag,Gd with Ag NPs. Three methods: the half-width strip plasmon resonance, X-ray diffraction and Small-angle X-ray scattering, in these samples by size NPs Ag. Revealed that the size of NPs Ag, defined by half-widths plasmon resonance band much smaller than obtained by other methods. It is concluded that the methods of X-ray diffraction and small-angle X-ray scattering give results closer to reality than the method plasmon resonance.