Dissolution behavior of stone wool fibers in synthetic lung fluids: Impact of iron oxidation state changes induced by heat treatment for binder removal.

Stone wool fiber materials are commonly used for thermal and acoustic insulation, horticulture and filler purposes. Biosolubility of the stone wool fiber (SWF) materials accessed through acellular in vitro dissolution tests can potentially be used in future as an indicator of fiber biopersistence in vivo. To correlate acellular in vitro studies with in vivo and epidemiological investigations, not only a robust dissolution procedure is needed, but fundamental understanding of fiber behavior during sample preparation and dissolution is required. We investigated the influence of heat treatment procedure for binder removal on the SWF iron oxidation state as well as on the SWF dissolution behavior in simulant lung fluids (with and without complexing agents). We used heat treatments at 450 °C for 5 min and 590 °C for 1 h. Both procedures resulted in complete binder removal from the SWF. Changes of iron oxidation state were moderate if binder was removed at 450 °C for 5 min, and there were no substantial changes of SWF's dissolution behavior in all investigated fluids after this heat treatment. In contrast, if binder was removed at 590 °C for 1 h, complete Fe(II) oxidation to Fe(III) was observed and significant increase of dissolution was shown in fluids without complexing agent (citrate). PHREEQC solution speciation modeling showed that in this case, released Fe(III) may form ferrihydrite precipitate in the solution. Precipitation of ferrihydrite solid phase leads to removal of iron cations from the solution, thus shifting reaction towards the dissolution products and increasing total mass loss of fiber samples. This effect is not observed for heat treated fibers if citrate is present in the fluid, because Fe(III) binds with citrate and remains mobile in the solution. Therefore, for developing the most accurate SWF in vitro acellular biosolubility test, SWF heat treatment for binder removal is not recommended in combination with dissolution testing in fluids without citrate as a complexing agent.