Studies on emulsion polymerization (EP) of poly(styrene‐co‐butyl acrylate) [P(S‐co‐BA)] can be accessed in open literature. However, these studies are mostly focusing on lab‐scale polymerization and subsequently characterization, of which discussion on pilot‐scale or mass‐production‐scale of the polymerization is scant. This paper focuses on the batch‐to‐batch reproducibility of P(S‐co‐BA) with 78.7 mol% of styrene and 21.3 mol% of butyl acrylate via EP in 3 metric‐ton (MT) pilot‐scale reactor. Polymerization efficiency, molecular, and physical characterization of the copolymers are examined using gravimetric analysis. Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), gel permeation chromatography (GPC), thermal gravimetry analysis (TGA), differential scanning calorimeter (DSC), viscometer, capillary rheometer, particle size analyzer (including dynamic light scattering and laser diffraction techniques), and scanning electron microscope (SEM). The gravimetric analysis on the monomer conversion reveals that the polymerization in 3‐MT reactor is efficient with 100% conversion. Besides, 1H‐NMR results reveal that the styrene‐to‐butyl acrylate mole ratio of the copolymer is of close approximation of the monomer feed amount while FTIR is a rather convenient quality control (QC) tool for batch‐to‐batch reproducibility on the copolymer molecular structured. The physical characteristic of [P(S‐co‐BA)] for all five batches are considered reproducible.