Using IR–Fourier spectrometry (FTIR) and simultaneous thermal analysis combined with quadrupole mass spectrometry of thermal decomposition products (STA + QMS), olivines and clinopyroxene from xenolites of spinel and garnet lherzolites contained in kimberlites and alkaline basalts were studied to confirm the occurrence of hydrogen and carbon within the structure of the minerals, as well as to specify the forms of H and C. The presence of hydroxyl ions (OH–) and molecules of crystal hydrate water (H₂Ocryst) along with CO₂, CH, CH₂, and CH₃ groups was detected, which remained within the structures of mantle minerals up to 1300°C (by the data of both techniques). The total water (OH–and H2Ocryst) was the prevailing component of the C–O–H system.