A systematic study has been described on the laser diffraction (LD) and static image analysis (SIA) of rectangular particles [1]. To rule out powder sampling, sample dispersion and particle orientation as a possible root cause for differences in size distribution profile, powder samples were initially immobilized by means of a dry disperser onto a glass plate. For a defined region of the glass plate the diffraction pattern as induced by the dispersed particles, and the 2D dimensions of the individual particles were measured by LD and optical microscopy, respectively. Correlation between LD and SIA could be demonstrated considering the scattering intensity of the individual particles as the most dominating factor. For both spherical and rectangular particles, theory explains the latter to relate to the square of their projected area. In traditional LD, the size distribution profile is dominated by the maximum projected area of the particles (A), and the diffraction diameters of a rectangular particle with length L and breadth B are perceived by the LD instrument to correspond by approximation with spheres having a diameter of ∅ L and ∅ B , respectively. Weighting for differences in scattering intensity between spherical and Page 3 of 56 rectangular particles exlains each rectangular particle to contribute to the overall LD volume probability distribution proportional to A 2 /L and A 2 /B. Accordingly, for rectangular particles this scattering intensity weighted diffraction diameter (SIWDD) concept explains an overestimation of their shortest dimension and an underestimation of their longest dimension. For this study various samples have been analysed with the longest dimension of the particles ranging from ca. 10 to 1000 µm. For a variety of pharmaceutical powders all with a different rectangular particle size and shape, the demonstrated correlation between LD and SIA aims to facilitate the user in a better validation of LD methods based on SIA data.

A technique based on laser light diffraction is shown to be successful in collecting on-line experimental data. Time series of floc size distributions (FSD) under different shear rates (G) and calcium additions were collected. The steady state mass mean diameter decreased with increasing shear rate G and increased when calcium additions exceeded 8 mg/l. A so-called population balance model (PBM) was used to describe the experimental data. This kind of model describes both aggregation and breakage through birth and death terms. A discretised PBM was used since analytical solutions of the integro-partial differential equations are non-existing. Despite the complexity of the model, only 2 parameters need to be estimated; the aggregation rate and the breakage rate. The model seems, however, to lack flexibility. Also, the description of the floc size distribution (FSD) in time is not accurate.

The activated sludge floc size distribution (FSD) is investigated by using different techniques and the results are compared against each other in order to gain insight into the FSD characteristics, as well as to detect the limitations of each measurement technique. The experimental set-up consisted of three devices coupled in series: a MastersizerS, an automated image analysis system (IMAN) and a CIS-100. The latter instrument has two measurement channels, based on time of transition (TOT), and image analysis (SHAPE) principles. In order to minimise the variability between successive measurements, the activated sludge samples collected from a pilot-scale SBR were flocculated until steady state was achieved. The results show that the MastersizerS and SHAPE devices yield similar volume weighted FSD. In contrast, the IMAN overestimated the floc size and TOT frequently showed a bimodal distribution. The number distributions from TOT and SHAPE were in agreement, while those generated by the MastersizerS were mainly located in the submicron range and those of IMAN corresponded to larger sizes. The experimental distributions show a good fit to the log-normal model. It is shown that the measurement principle is of utmost importance and results transformation may lead to data misinterpretation.

Over a period of 227 days properties of activated sludge grown in an sequencing batch reactor (SBR) operated under stable conditions were analyzed. Settling properties (sludge volume index (SVI)) of the activated sludge were compared with on-line measurements of floc size and size distribution obtained by using a laser light scattering technique (Malvern Mastersizer/S, Malvern, UK), and with measurements of microbial community dynamics analyzed by denaturing gradient gel electrophoresis (DGGE) patterns of 16S rRNA genes. In addition, microscopical observations were used to confirm the results. Three distinct stages in the SBR evolution were observed. In the first stage the structural floc properties showed predominant presence of floc-forming bacteria in the activated sludge. A good correlation between floc size, properties and microbial community evolution was observed. The second stage showed a good balance between floc-forming and filamentous bacteria, with good settling properties and a highly dynamic community in the SBR. In the third stage, an increase in the filamentous bacteria, which became predominant in the system was observed. Again, a good correlation between settling properties and floc size distribution was obtained and a new dominant species was observed in the DGGE patterns, which can be assumed to be a filamentous organism.

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