Closed-loop system identification and fault detection and isolation are the two fundamental building blocks of process monitoring. Efficient and accurate process monitoring increases plant availability and utilisation. This dissertation investigates a subspace system identification and fault detection methodology for the Benfield process, used by Sasol, Synfuels in Secunda, South Africa, to remove CO2 from CO2-rich tail gas. Subspace identification methods originated between system theory, geometry and numerical linear algebra which makes it a computationally efficient tool to estimate system parameters. Subspace identification methods are classified as Black-Box identification techniques, where it does not rely on a-priori process information and estimates the process model structure and order automatically. Typical subspace identification algorithms use non-parsimonious model formulation, with extra terms in the model that appear to be non-causal (stochastic noise components). These extra terms are included to conveniently perform subspace projection, but are the cause for inflated variance in the estimates, and partially responsible for the loss of closed-loop identifiably. The subspace identification methodology proposed in this dissertation incorporates two successive LQ decompositions to remove stochastic components and obtain state-space models of the plant respectively. The stability of the identified plant is further guaranteed by using the shift invariant property of the extended observability matrix by appending the shifted extended observability matrix by a block of zeros. It is shown that the spectral radius of the identified system matrices all lies within a unit boundary, when the system matrices are derived from the newly appended extended observability matrix. The proposed subspace identification methodology is validated and verified by re-identifying the Benfield process operating in closed-loop, with an RMPCT controller, using measured closed-loop process data. Models that have been identified from data measured from the Benfield process operating in closed-loop with an RMPCT controller produced validation data fits of 65% and higher. From residual analysis results, it was concluded that the proposed subspace identification method produce models that are accurate in predicting future outputs and represent a wide variety of process inputs. A parametric fault detection methodology is proposed that monitors the estimated system parameters as identified from the subspace identification methodology. The fault detection methodology is based on the monitoring of parameter discrepancies, where sporadic parameter deviations will be detected as faults. Extended Kalman filter theory is implemented to estimate system parameters, instead of system states, as new process data becomes readily available. The extended Kalman filter needs accurate initial parameter estimates and is thus periodically updated by the subspace identification methodology, as a new set of more accurate parameters have been identified. The proposed fault detection methodology is validated and verified by monitoring process behaviour of the Benfield process. Faults that were monitored for, and detected include foaming, flooding and sensor faults. Initial process parameters as identified from the subspace method can be tracked efficiently by using an extended Kalman filter. This enables the fault detection methodology to identify process parameter deviations, with a process parameter deviation sensitivity of 2% or higher. This means that a 2% parameter deviation will be detected which greatly enhances the fault detection efficiency and sensitivity. / Dissertation (MEng)--University of Pretoria, 2008. / Electrical, Electronic and Computer Engineering / unrestricted