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19 (2002) 84 ± 95
Abstract
The Lasentec focused beam reflectance measurement The FBRM response has been compared to conven-
(FBRM) probe provides in situ particle characterisa- tional particle sizing techniques (laser diffraction and
tion over a wide range of suspension concentrations. electrical sensing zone) for a range of sieved aluminium
This is a significant advantage over conventional or calcite suspensions. The mode average of the square-
instruments that require sampling and dilution. How- weighted chord length was found to be comparable to
ever, FBRM gives a chord distribution, rather than a other sizing techniques over the range from 50 to
conventional diameter distribution. Both theoretical 400 mm. The square-weighted FBRM results were
and empirical methods for converting from chord to essentially unaffected by changes to the instrument
diameter data are available, but the empirical method focal position, the suspension fluid flow velocity, or the
was found to be more successful. solid fraction in the range 0.1 ± 20 % w/v.
spherical to simplify the mathematics, and most analysis The probability of a particle being detected is propor-
of non-spherical particles is limited to two dimensional tional to its diameter, introducing a bias. Therefore, for
ellipses [52 ± 56]. Assuming the particles are spherical modelling purposes the FBRM is assumed to measure
simplifies the mathematics, because regardless of the the first diameter moment of the chord distribution [48,
particle×s orientation it always presents a circular profile 56]. Calculating a chord distribution from a given
(Figure 2). spherical particle distribution is relatively straightfor-
This assumption may be valid for suspensions of ward, however the reverse algorithm is more difficult,
spherical latex or glass beads, or emulsions of immiscible usually requiring a numerical solution in the form:
liquids. Assuming the particles are spherical may also be M
X 2
reasonable for suspensions of particles with an aspect min
Ni Ni :
1
Np
ratio (ratio major:minor axis) approaching 1 : 1. As the i1
[14, 17, 25, 27, 29, 32]. Comparisons between the resulting
average size and alternative sizing methods showed that
the FBRM oversized small particles (< 150 mm [27],
< 300 mm [25]) and undersized larger ones (> 500 mm [25]).
Current software computes various chord statistics:
median (d50), mean and mode with various chord
weightings. Daymo et al. [57] found good agreement
between the cube-weighted mean size and sieve analysis
of kaolin suspensions with a mean size of around 55 mm.
Alfano et al. [40] show a good correlation between laser
diffraction volume-based mean size and unweighted
FBRM chord lengths for suspensions of aggregated silica
20 ± 200 mm. However, the unweighted FBRM results
again underestimated the size of the larger particles. El-
Hamouz and Stewart [47] compared FBRM mean
square-weighted chord lengths and laser diffraction
mean sizes for droplets of oil/water emulsions and found
the FBRM over-estimated smaller (< 180 mm) droplets,
but underestimated larger (> 180 mm) droplets.
3 Experimental
3.1 Samples
Most samples were either calcite (Omya Southern,
Commercial Minerals) or aluminium (Valimet, Stockton
California). SEM micrographs were obtained using a
JEOL JSM-5800LV, with the calcite particles gold-
coated for imaging purposes (Figure 3). The calcite
Fig. 3: SEM images of unsieved (a) calcite and (b) aluminium
particles were blocky in shape, while the aluminium particles (white bar represents 200 mm).
particles were more spheroidal. In general, most par-
ticles had a low aspect ratio. A single suspension of
mono-sized latex spheres (Dynaspheres, Duke Scientif-
3.2 Equipment
ic) with a specified size of 19.9 mm was also measured.
The particles were separated into narrow size fractions by FBRM measurements were made with a M500 field unit
screening or cyclosizing. Dry sieving used conventional (Lasentec, Redmond, Washington, USA). The probe has
Endecotts screens (38, 45, 53, 63, 75, 106, 125, 150, 180, 212, a 12 mm diameter flat sapphire window set in a 25 mm
250, 300, 425, 500, 600, 710, 850, 1000, 1180 mm) in a Rotap diameter stainless steel casing. As this study was
RX ±29 ±10 mechanical shaker, while smaller size fractions confined to non ± aggregated systems, only the F (fine)
obtained by cyclosizing with a Warman M-4 cyclosizer. electronics data are presented. Unless otherwise stated,
The solids were weighed to 0.1 mg and made up to the focal point was set to 0 mm (external face of the
concentrated aqueous stock suspensions in a volumetric window) as calibrated by the manufacturer. This position
flask. A series of more dilute suspensions were obtained was also confirmed experimentally by placing a film of
by dilution of the stock suspension from a stirred tank, marking pen ink on the window and adjusting for
baffled to ensure uniform solids distribution. The dry maximum counts.
sieved calcite samples were found to contain some fines Suspensions of various particle size and solid fraction
(possibly from surface abrasion or aggregation) and were presented to the FBRM probe using a dedicated
where possible were washed and decanted. Suspensions stand (Lasentec¾). The impeller (four angled blades,
of aluminium particles were reactive, producing a gas diameter 50 mm) was set to 650 r.p.m. unless otherwise
(presumably hydrogen), and were kept on ice to reduce stated. The probe acts as a baffle in the 500 mL tall-form
the reaction rate. Solids concentrations are expressed in beaker (internal diameter 75 mm), and is positioned with
terms of solid weight as a percentage of suspension the probe window 3 mm above the impeller tip to ensure
volume (% w/v). optimal sample presentation. A 30 s period of stirring
88 Part. Part. Syst. Charact. 19 (2002) 84 ± 95
Both groups observed substantial changes with focal focal position was changed, its position did not shift. On
position, suggesting that setting the position further into the basis of these results, a focal position setting of 0 mm
solution (in the range 0.8 to 2 mm) gave better results for was chosen for all subsequent measurements.
larger particles. However, they did not report settings
closer to the probe window. While large focal positions
4.2.2 Suspension Agitation
may give some improvement for very dilute suspensions,
in this work optimal performance was achieved when Accurate sizing by FBRM requires a representative
focused close to the window (Figure 6). For large sample of particles to pass through the measurement
particles it is suggested [58] that the focal position be zone near the window, consequently the effectiveness of
set to approximately 20 mm inside the window. mixing becomes an issue for suspensions containing
Figure 6 shows the effect of varying the focal position larger particles. The effect of the suspension agitation on
between 100 and 100 mm from the window. As the measured size has been previously investigated, with
expected, setting the position into the suspension contradictory results reported. No significant effect of
increases the number of longer chords, but by 50 mm stirring speed on the indicated size in the range 500 ±
there was a significant loss of total counts. At 100 mm into 1000 r.p.m. was observed by Law et al. [27]. Monnier
the suspension the counts dropped below a usable level. et al. [51] found that increasing the impeller speed from
This is most likely a consequence of the high solids 500 ± 1000 r.p.m. dramatically increased both the meas-
concentration, with such focal positions only applicable ured size and total counts of glass beads, although
in dilute solutions. transparent particles are generally reported to be poorly
Larger particles may have difficulty entering the viewing sized by FBRM [17]. Daymo et al. [57] reported that
region as the focal position is brought back towards the increasing the flow velocity of a kaolin suspension from
window, leading to an increased sensitivity of the 1.3 to 2.4 m s 1 in a 76 mm ID pipe reduced the indicated
unweighted distribution to fine chords, which peak at size by 13%. However, these changes may have been due
between 20 and 10 mm (Figure 6a). In contrast, the to particle setting at low flow rates, or particle breakage
square-weighted chord distribution (Figure 6b) remains at high flow rates.
insensitive to the presence of the fine chords, and while The tangential velocity of the focused laser beam is
the peak in this distribution varied in intensity as the approximately 1.9 m s 1, and is assumed (see Section
2.2.1) to be far greater than the particle velocity with
respect to the instrument window. At approximately 750
r.p.m. the tip velocity of the 50 mm diameter pitched
blade impeller reaches 2 m s 1. However, since the
viewing region is adjacent to the window, the flow
velocities in the viscous sub-layer are likely to be
considerably lower than for the bulk of the fluid flow.
In practice, changing the impeller speed had little effect
(Figure 7) on the observed square ± weighted chord
distribution. Larger particles (> 500 mm) tended to
visibly settle at low stirring speeds (< 500 r.p.m.), leading application of a cube-weighting may improve the esti-
to a reduction in the average measured size. mation of larger particle sizes.
The mean, and to a lesser extent also the median,
averages were affected by the instrument×s sensitivity to
4.3 Comparison of Average Particle Size by Various
fine particles. However, the modes (distribution max-
Techniques
ima) were less affected. Figure 9 shows direct compar-
Particle size distributions can be weighted and averaged ison of average sizes by the techniques for a series of
in a variety of ways [5, 59 ± 61]. Figure 8 plots various sieved or cyclosized suspensions. Linear correlation
length-weighted median FBRM average sizes with d50 equations (Figure 9, see labels) could be re-arranged to
values from laser diffraction for a range of sieved or give a 2-parameter calibration, to give reasonable agree-
cyclosized fractions. Calculated geometric average val- ment over the range 20 to 500 mm.
ues from sieving are also included for comparison. Laser
diffraction data is presented on the x-axis because it was
4.4 Effect of Solid Volume Fraction on Indicated Size
the only alternative technique that covered the entire
size range, but this is not meant to imply that the Early studies with FBRM showed that the spherical-
technique provides a more accurate particle size. equivalent size was essentially unaffected by solid
While all the relationships shown in Figure 8 exhibited fraction [17, 27]. More recently, Daymo et al. [57] used
good linearity over the size range studied, applying the chord cube-weighting and also found little variation
length-weightings served to improve the measured slope, in the indicated size as the solid fraction was varied.
increasing from 0.530 for the median unweighted chord Figure 10a shows that increasing the solid volume
length to 0.898 for the median length square-weighted fraction has the effect of increasing the sensitivity of
chord length. The latter slope was comparable to that the unweighted chord length distribution to fine par-
achieved for sieve analysis (0.885). ticles, probably due to fines crowding the measurement
For the calcite particles (which covered a larger range of zone near the window. However, this effect is largely
sizes) the length square-weighting was also found to give overcome by applying a chord square-weighting to the
the best correlation up to 400 mm. Above this size the distribution (Figure 10b). Over most of the volume
fraction range the position of the mode for the square-
weighted distribution remains constant at 140 mm, dis-
playing a shift only at 20% w/v (to 110 mm).
1:9 106
Nt Nt M :
4
P
1:9 106 Ni Ci;A 2k
i1
6 Acknowledgements
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