The applicability of a special pilot-scale installation (Short Circulation Device) was studied for demonstrating the enrichment of selected resin and fatty acids in process waters when increasing water reuse during the manufacture of paper. The traditional gas chromatography with flame ionization detection (GC-FID), turbidity, and online sample enrichment (solid phase extraction, SPE) for atmospheric pressure chemical ionization-mass spectrometry (APCI-MS) measurements were used for the analysis of the resin and fatty acids. The data from all the measurements with unbleached thermomechanical pulp (TMP) process waters were in a good agreement, and correlation coefficients (R2) > 0.9 were obtained in each case. Rapid information about the levels of wood extractives in papermaking process waters is of great importance, and it offers a suitable way to predict oncoming pitch problems. It was concluded that the routine control of the extractives level in papermaking process waters is possible by all these methods.