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In this manuscript the purpose is to present and evaluate the developed non‐destructive method for analysing the phase composition of LTCC Du Pont “Green Tape 951” material fired in the temperature range from 800 to 1,000°C using X‐ray powder diffraction and Rietveld refinement.

The method uses the crystalline Al2O3 which is already present in the material as an internal standard since its mass fraction was previously found to be constant in the described temperature range.

The results of the non‐destructive analyses and the classical destructive analyses are comparable and the estimated error of the destructive phase analyses and the calculated errors for the non‐destructive phase analyses are of the same order.

The described method can be used also for analysing another type of LTCC material. In this case it is necessary to check whether the mass fraction of any crystalline phase present in the sample is constant in the given temperature range, because only in this case can it be used as an internal standard for a determination of the phase composition.

The non‐destructive method is a fast and easy approach for analysing the fired samples and is also suitable for controlling the phase composition of LTCC materials on 3D complex structures without destroying them, just by using the X‐ray diffraction patterns collected from their surface.