Microwave (MW) H 2 plasmas with small admixtures of CH 4 and/or B 2 H 6 used for doped diamond deposition have been studied by infrared absorption and optical emission spectroscopy (OES) techniques. The experiments were carried out in order to analyze the dependence of the plasma chemistry on several parameters in the MW discharges, such as power, pressure and gas mixture, at relatively high pressures, ie up to 300 mbar, and power values, ie up to 4 kW. The evolution of the concentrations of five stable molecules, CH 4, C 2 H 2, C 2 H 4, C 2 H 6 and B 2 H 6, was monitored in the plasma processes by in situ infrared tunable diode laser absorption spectroscopy. OES was used simultaneously to gather complementary information about the concentration of the boron atom. One target was the determination of the precursors' fragmentation rates and the conversion rates to the molecular reaction products. The analysis of correlations between the power and pressure of the plasma and molecular concentrations, and the differences found with CH 4 and B 2 H 6 admixtures were another focus of interest. The degree of dissociation of the carbon containing precursor molecule CH 4 varied between 35% and 75%, while the decomposition of diborane, the boron precursor, varied between 85% and 97%. By analyzing the development of the molecular concentrations with changes of gas mixtures, pressure and plasma power values, it was found that (i) C 2 H 2 is the most abundant reaction product in the plasma in the case of methane admixture and (ii) the boron atom concentration depends strongly on the presence of hydrocarbons in the plasma. The fragmentation efficiencies of methane and of diborane (R F (CH 4)≈(1–2)× 10 15 molecules J− 1, R F (B 2 H 6)≈(0.4–1.4)× 10 13 molecules J− 1) and the conversion efficiencies to the molecular products (R C (product)≈ 10 13–10 15 molecules J− 1) have been determined for different gas mixtures and plasma power, and pressure values. The boron atom balance, in relation to the dissociated B 2 H 6 molecules was found to vary between 10% and 40% depending on the discharge conditions.