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Separation of coal ash into magnetic and non-magnetic fractions facilitates their utilization when processed separately. Due to desulphurization additives added to coal during the fluidised-bed combustion, non-magnetic fractions often contain elevated CaO levels (while magnetic concentrates are typically rich in Fe2O3). Both CaO and Fe2O3 are known for their ability to bind As during the combustion, whose distribution is a crucial parameter in terms of proper utilization of these fractions. Therefore, the study deals with the As partitioning within magnetic and non-magnetic fractions of fluidized-bed coal combustion ashes. Two different (successive) procedures of dry magnetic separation were used to separate each ash into strongly magnetic, less magnetic, and a non-magnetic fraction. Due to their optimal utilization, the concentrations of As and other target elements in these fractions were evaluated and compared. Magnetic concentrates from the first separation step (in vibrofluidized state) contained 60–70% Fe2O3, magnetic concentrates separated manually out of the residues after the first separation contained 26–41% Fe2O3, and the non-magnetic residues contained 2.4–3.5% Fe2O3. Arsenic levels were the highest in the non-magnetic residues and gradually decreased with the increasing Fe2O3 content in the magnetic fractions. The dominant As association in the studied samples was to CaO (r = +0.909) and with SO3 (r = +0.906) whereas its joint occurrence with Fe2O3 was improbable (r = −0.834).

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