Flow injection systems for process analytical chemistry

Sammanfattning: Flow injection systems have great potential for sample handling and analysis in process analytical chemistry. The flexibility and versatility of flow injection manifolds can he utilized in specific applications of sample conditioning and analysis. An overview of various flow injection methods, including flow reversals, double injection, and sequential injection is given, as well as different clean-up methods, such as gas diffusion, solid phase extraction, dialysis, and solvent extraction. Calibration techniques, such as single standard and multivariate calibration are also discussed. In addition, different aspects of process analytical chemistry, in particular sampling and sample handling, are discussed.The papers in this thesis describe a number of flow systems, where gradient-, gas diffusion-, and solid phase extraction- methodologies are applied, all of which have potential use in process analytical chemistry. Paper I is focused on multicomponent analysis of mixtures of organic acids by mathematically extracting information from complex spectra. The selectivity is improved by generating pH-gradients in the flow system. In paper II, the methodology of sensor injection is described and electrochemical and spectroscopic sensors are implemented in a sequential injection system. The method is illustrated by using pH sensors and a glucose electrode. Ammonia and ammonium ions are determined on-line to a bioprocess by gas diffusion in paper III. The benefit of frequent re-calibrations and in-line cleaning sequences are demonstrated. Finally a method for on-line determination of o-diphenols in the kraft process has been developed (paper IV). The o-diphenols are isolated from black liquor samples by solid phase extraction and thereafter transferred to a high performance liquid chromatography system for separation and quantification.