Air-blast atomizers are widely used atomizers in a variety of applications such as the aerospace industry, internal combustion engines, spray drying, etc. An experimental setup including novel twin-fluid atomizers has been investigated with real-time monitoring of the acoustic signal data. It is based on the fact that all flow processes emit some energy output signals, which can be recorded and analyzed to extract reliable information. A new non-intrusive approach based on acoustic chemometrics which includes vibration signal collection using glued-on accelerometers was assessed for the determination of the different flow (breakup) regimes spanning a whole range of fluids (water and air) flow rates in this novel twin-fluid atomizer (one-analyte system). This study aims to determine the flow regimes based on the dimensionless number B, whose unique set of values corresponds to different flow (breakup) regimes. The principal component analysis (PCA) intends to be performed to visually classify the breakup regimes using PCA score plots. The preliminary results showed clearly the subsets for all different flow regimes. Partial least squares regression (PLS-R) will be done on the conditioned acoustic signals to get a prediction model using the reference (measured) data values. The predicted Vs reference plot shows a correlation with a certain permissible (%) limit for root mean square of prediction (RMSEP) value for a range of dimensionless number, B. This primary study result will suffice the complex physical understanding behind the fluid flow regimes. A further detailed study is still rendered necessary to understand the feasibility of acoustic studies for the flow regime characterization for different types of atomizer design.