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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Particle size analysis is important in both process and quality control. Different techniques are currently available. In this contribution, the characteristics of three techniques, based on Static Light Scattering (SLS), Time‐of‐Transition (TOT), and Dynamic Image Analysis (DIA), are compared using various aqueous dispersions. Hereby, the techniques were connected in series, so that simultaneous measurements could be performed on the same sample. The experimental results demonstrated that each of the investigated techniques has its strengths and limitations. Thus, SLS results may be largely affected by the choice of the refractive index of the dispersed particles as well as by the choice of the inversion algorithm to convert the angular spectrum to a particle size distribution. As neither TOT or DIA require information concerning the (complex) refractive index of the particles and are based on the detection of individual particles, these techniques are claimed to be very useful for measuring particles in the micrometer size range, although the measurement can be heavily affected by the particle transparency and concentration. Furthermore, all the techniques appear more suited to discerning small particles within a population of large particles than to detecting large particles within a population of small particles. Finally, TOT is much less sensitive towards submicron particles, as compared to SLS. The latter technique does not only have a broader dynamic range, which extends down to the submicron range, but also produces reliable results at higher sample concentrations as compared to TOT and DIA.

Impact of model-based operation of nutrient removing SBRs on the stability of activated sludge population was studied in this contribution. The optimal operation scenario found by the systematic model-based optimisation protocol of Sin et al. (Wat. Sci. Tech., 2004, 50(10), 97-105) was applied to a pilot-scale SBR and observed to considerably improve the nutrient removal efficiency in the system. Further, the process dynamics was observed to change under the optimal operation scenario, e.g. the nitrite route prevailed and also filamentous bulking was provoked in the SBR system. At the microbial community level as monitored by DGGE, a transient shift was observed to gradually take place parallel to the shift into the optimal operation scenario. This implies that the model-based optimisation of a nutrient removing SBR causes changes at the microbial community level. This opens future perspectives to incorporate the valuable information from the molecular monitoring of activated sludge into the model-based optimisation methodologies. In this way, it is expected that model-based optimisation approaches will better cover complex and dynamic aspects of activated sludge systems.

The activated sludge floc size distribution (FSD) is investigated by using different measurement techniques in order to gain insight in FSD assessment as well as to detect the strengths and limitations of each technique. A second objective was to determine the experimental conditions that allow a representative and accurate measurement of activated sludge floc size distributions. Laser diffraction, Time Of Transition (TOT) and Dynamic Image Analysis (DIA) devices were connected in series. The sample dilution liquid, the dilution factor and hydraulic flow conditions avoiding flocculation proved to be important. All methods had certain advantages and limitations. The MastersizerS has a broader dynamic size range and provides accurate results at high concentrations. However, it suffers from an imprecise evaluation of small size flocs and is susceptible to particle shape effects. TOT suffers less from size overestimation for non-spherical particles. However, care should be taken with the settings of the transparency check. Being primarily a counting technique, DIA suffers from a limited size detection range but is an excellent technique for process visualization. All evaluated techniques turned out to be reliable methods to quantify the floc size distribution. Selection of a certain method depends on the purpose of the measurement.