Both boron and zirconium are present in ceramic materials as major silica components and have to be determined for quality control in the ceramic industry. For boron determination, sintering with a mixture of Na2CO3 and ZnO is proposed for decomposition of samples. For zirconium determination, acid digestion using an HF-HClO4 mixture and subsequent fusion with NaKCO3 and H3BO3 is proposed as decomposition step. The AAS absorbance signal of these elements is suppressed by the fusion elements in the samples. Therefore, the calibration solutions for both B and Zr must contain an appropriate concentration of sodium, sodium-potassium, and boron salts. An AIF3 solution was used for signal enhancement and improving the linearity of the Zr calibration curve. The methods proposed are well suited for the determination of higher concentrations of both boron and zirconium in silicate samples.