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84 Part. Part. Syst. Charact.

19 (2002) 84 ± 95

Estimating Average Particle Size by Focused Beam Reflectance


Measurement (FBRM)

Alex R. Heath*, Phillip D. Fawell**, Parisa A. Bahri*, Jean D. Swift**


(Received: 5 April 2001; resubmitted: 11 January 2002)

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.

Keywords: FBRM, on-line, particle size analysis

1 Introduction many applications this distinction is not important


because the relevant process variable can be correlated
Various techniques are available for determining particle with some aspect of the chord data, and accurate particle
size [1 ± 5]. However, few can be applied in situ/in-line, or sizing is not specifically required.
over a wide range of solid concentrations. Ultrasonic The instrument×s rapid in-line analysis make it attractive
techniques have been developed [6], but require lengthy to workers modelling the kinetics of flocculation [29, 35]
measurement times, making them unsuitable for dynam- or crystallisation [13, 18, 20] by population balance.
ic systems. Standard laboratory laser diffraction instru- However, in dynamic modelling, both accurate sizing
ments have also been modified [7 ± 10] to allow on-line and counting of particles are desirable for the estimation
sizing of a side stream, but are inconvenient for field or of model parameters, and the raw chord length data may
plant use and typically require some degree of dilution. not be suited to this.
Alternatively, in-process measurements can be made by In this paper both theoretical and empirical methods for
focused beam reflectance measurement (FBRM). The estimating particle diameters from chord data are
FBRM probe has a wide range of applications, frequently reviewed. These methods are then applied to chord
in the process environment (Table 1). The instrument data collected from a range of sieved particles, and the
gives a particle chord length distribution, which is a calculated diameter data compared with conventional
function of the true particle diameter distribution. For sizing for the same samples. The effect of length-
weighting has been examined, and different averaging
* A. R. Heath Ph.D student, Dr. P. A. Bahri, A. J. Parker
methods (mean, median, and mode) compared. Factors
Cooperative Research Centre for Hydrometallurgy, School of affecting the FBRM data were also examined, in
Engineering, Murdoch University, (Rockingham Campus), particular the influence of the solid volume fraction.
Murdoch, WA 6150 (Australia).
** Dr. P. D. Fawell (to whom correspondence should be ad-
dressed), J. D. Swift, A. J. Parker Cooperative Research Centre
for Hydrometallurgy, CSIRO Minerals, Box 90, Bentley, WA
6982 (Australia).
E-mail: phillip.fawell@csiro.au

¹ WILEY-VCH Verlag GmbH, 69469 Weinheim, Germany, 2002 0934-0866/02/0205-0084 $ 17.50+.50/0


Part. Part. Syst. Charact. 19 (2002) 84 ± 95 85

Table 1: Summary of common FBRM process applications.


Application Reference Application Reference
Control [11 ± 16] Grinding [16, 37 ± 41]
Crystallisation/precipitation [13, 15, 17 ± 23] Paper manufacture [42 ± 45]
Estuarine solids [9, 10, 24 ± 27] Petroleum [46 ± 48]
Flocculation [28 ± 40] Pharmaceutical [49, 50]

Several descriptions are given of previous instruments


and data processing regimes [16, 17, 37]. Data processing
of the detector response uses both the signal strength and
slope. Current instrument data processing is adjustable
through the use of either F (fine) or C (coarse)
electronics modules, with the main difference being in
the faster preamplification and greater edge definition
with the former. Although rarely identified in publica-
tions, it can be assumed the F-electronics have been
preferred for most particle studies, due to sharper
resolution and higher sensitivity to fine chords. The C-
electronics is required for studies of aggregated particles,
i.e. for flocculation applications [39].

2.2 Estimating Particle Size from FBRM Data


Fig. 1: Schematic of the FBRM probe (not to scale).
2.2.1 Theoretical Methods
Several papers deal with the transformation of chord to
diameter distributions from first principles [8, 22, 28, 48,
2 Background
52 ± 56]. Most workers assumed that the particles are
2.1 Principle of FBRM
The Lasentec FBRM instrument directs a 780 nm laser
through a lens rotating at 4500 r.p.m., giving a beam of
light highly focused at a point near the instrument×s
window (Figure 1). The position of the focal point is
adjustable, depending on the particle properties [51].
The diameter of the circular path of the laser beam is
8.5 mm, focused to a beam waist of approximately 0.7 
2 mm and a focal depth of approximately 10 mm [37].
However, the exact width of the beam appears to be
dependent on both the focal position and the size and
distance of the particle from the focal position [16, 17].
When the moving laser beam intersects the path of a
particle some of the light is reflected back to the
instrument×s detector. Since the tangential velocity of
the beam is known ( 1.9 m s 1), the duration of the
reflected light pulse is directly proportional to the width
of the particle intersected. The tangential beam velocity
is assumed to be much larger than the particle velocity
relative to the instrument window. However, since it is
unlikely that the laser beam will pass directly across the
centre of the particle (i.e. its diameter), a chord length is Fig. 2: Method of determining the chord distribution expected
measured. from a spherical particle of diameter Dp.
86 Part. Part. Syst. Charact. 19 (2002) 84 ± 95

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

ˆ Ni Ni : …1†
Np
ratio (ratio major:minor axis) approaching 1 : 1. As the iˆ1

aspect ratio increases, and the particles or crystals tend


M  12  12
towards needles/plates, the chord distribution broadens  
X
2 2 2 2
N ˆN
i p D p C i;1 D p C
i;u : …2†
[22, 28]. iˆ1
Most descriptions assume that the focused laser beam
has no width, and that light is reflected immediately the The resulting calculated diameter distribution is a
beam reaches the edge of the particle. However, Hobbel number distribution, and is converted to the conven-
et al. [8] proposed a parameter (k) to account for the tional particle volume distribution by applying a length-
™arch of rejected reflection∫. Sparks and Dobbs [17] cube weighting (as discussed in Section 4.1).
considered the physics of the laser/lens interaction and
suggest that the beam may be broadened in some
2.2.2 Empirical Methods
conditions. Spreading of the beam away from the optimal
focal point may also affect the chord measurement [16], FBRM results have been compared with alternative
and beam spreading is likely to be a function of solids particle sizing techniques (Table 2) for a variety of
loading, fines, solution and particle surface character- particle sizes and materials. Early Lasentec FBRM
istics. software included a spherical-equivalent size algorithm

Table 2: FBRM comparisons with other sizing techniques.


Reference Particle material Alternative sizing method (size) FBRM size or size relationship (mm)
Hobbel et al. [8] Glass beads Helos laser diffraction 170
(66 mm)
Sparks and Duke standards, carbon, sand, Microtrac laser diffraction, certified Spherical equivalent,
Dobbs [17] alumina standards (0.8 ± 410 mm) FBRM ˆ 52.35 ‡ 1.036Duke
over the range 10 ± 162 mm
Murphy et al. Ground silica BET, SEM, Micromeritics sedigraph Oversized, could not be calibrated in
[33] (2.1 mm) this range
Monnier et al. Glass beads, latex, micronized phar- Cilas laser diffraction, Coulter Undersizes > 100 mm,
[51] maceutical product. Various support- Counter -electrical sensing zone, oversizes < 100 mm
ing fluids microscopy (4.1 ± 396 mm)
Dijkstra et al. Sugar Sieved (30 ± 250 mm) Sieve ˆ 2.04  10 3( FBRM )2.28
[15]
El-Hamouz and Oil/water emulsions Malvern laser diffraction Sauter mean (d32 ˆ 130 ± 210 mm),
Stewart [47] (d32 ˆ 60 ± 350 mm) undersizes > 180 mm,
oversizes < 180 mm
Law et al. [27] Pollen, glass and latex Duke stan- Malvern laser diffraction, Coulter FBRM Par-Tec spherical equivalent,
dards, fractionally settled sediment, Counter, certified standards undersizes > 500 mm, oversizes
sieved sand (6.5 ± 766 mm) < 150 mm
Phillips and Sieved river sediment Coulter laser diffraction FBRM Par-Tec spherical equivalent
Walling [25] (1 ± 355 mm) Coulter d50 ˆ 19.24 ‡ 1.064FBRM
Tadayyon and Sieved ion-exchange resin Sieve (212 ± 850 mm) FBRM undersized, better with cube-
Rohani [56] weighting
Daymo et al. [57] Bentonite, graphite, gibbsite, kaolin, Sieve Horiba sedigraph (0.3 ± 663 mm) Kaolin (5% w/v) 53 mm by FBRM
mica, silica, plastic beads (cube-weighted), 57 mm by sedigraph.
Weak correlation for other samples
Alfano et al. [40] Aggregated silica Malvern laser diffraction FBRM ˆ 10.09 ‡ 0.586 Malvern
(20 ± 180 mm)
Part. Part. Syst. Charact. 19 (2002) 84 ± 95 87

[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

was found to be sufficient to disperse the solid. The


measurements were then taken rapidly, as some fines
were released from calcite particles on extended stirring.
The use of dispersants can be advantageous in some
systems where aggregation is a factor [51], but were
found to give no significant improvement for the samples
studied here.
The FBRM control software (version 6) allows the
acquired chord length data to be discretised into a series
of user-defined intervals (channels). Data was collected
using 90 log ± channels over the range 1 to 1000 mm unless
otherwise stated. While the chord length distributions
should technically be viewed as histograms, for ease of
comparison they are presented as line graphs. A meas- Fig. 4: Unweighted chord length distributions for 10% w/v
urement duration of 10 seconds was used, with each sieved aluminium fractions produced by sieving.
distribution the average of five consecutive measure-
ments. For simplicity, the counts axis on all distributions
represents the number of counts per second.
Fluid flow past the probe window generally ensures that
the window is kept clean. However, fine particles are
prone to adhere to the window, and can increase the
count rate and affect the measured size. Window
cleaning was therefore performed regularly (  5 min.
measurement time) to give a total background count of
less than 50 counts per second in air.
Laser diffraction and electrical sensing zone instruments
(Malvern Mastersizer MS10 and Coulter Multisizer II,
respectively) were used as alternative sizing techniques,
with concentrated samples typically diluted to less than Fig. 5: Effect of applying various length-weightings (moments)
2% w/v for analysis. to the FBRM chord distribution for aluminium particles (sieved
45 ± 53 mm). Laser diffraction volume-weighted distribution also
shown.

4 Results and Discussion


diameter weighting (moment) of the chord distribution.
On this basis, applying the square-weighting is then
4.1 Effect of Applying Weightings to FBRM Chord
effectively a cube (volume) weighting, comparable to the
Distributions
volume-based distribution from laser diffraction.
The raw (unweighted) chord length distributions meas-
ured by FBRM for a series of sieved aluminium fractions
4.2 Sample Presentation Effects
at a constant solid concentration are shown in Figure 4.
As expected, the larger particles gave longer chord
4.2.1 Focal Position
lengths, and a reduced count rate due to the decreased
number of particles. The position of the focal point of the laser is manually
Figure 5 shows the effect of applying length weightings adjustable in relation to the instrument window. This has
(moments) to the chord distribution given by FBRM, i.e.: the effect of moving the position of the viewing region
further into the suspension, or, as negative settings
Ni;n ˆ Ni;o Cni;A : …3† indicate, behind the window/suspension interface (Fig-
ure 1). The effect of focal position on an early version of
It can be seen from Figure 5 that the square-weighted FBRM was examined by Monnier et al. [51] and Law
(n ˆ 2) chord distribution gave the best agreement with et al. [27], who varied the positioning into the solution by
the conventional laser diffraction distribution, although up to 6 or 4 mm, respectively. Law et al. [27] made use of
the FBRM distributions remained broader. This is in a spherical equivalent diameter algorithm, while Mon-
general agreement with the theoretical analysis (Section nier et al. [51] monitored total counts and unweighted
2.2.1) which suggests that FBRM measures the first mean chord lengths.
Part. Part. Syst. Charact. 19 (2002) 84 ± 95 89

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

Fig. 6: Effect of laser focus position on (a) unweighted and (b)


square-weighted chord length distributions for 20% w/v calcite, Fig. 7: Effect of impeller speed on square-weighted chord length
(sieved 106 ± 125 mm, 500 r.p.m. impeller speed). distributions for 20% w/v calcite particles (sieved 106 ± 125 mm).
90 Part. Part. Syst. Charact. 19 (2002) 84 ± 95

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).

Fig. 8: Comparison of median average sizes given by various


techniques and chord weightings for sieved/cyclosized aluminium Fig. 9: Comparison of mode average sizes from the FBRM
fractions, showing the square-weighted chord gives the best square-weighted distributions, with median values from laser
agreement with laser diffraction and sieve analysis. FBRM diffraction and electrical sensing zone analysis for sieved/cyclo-
suspensions 5% w/v. sized calcite particles (5% w/v).
Part. Part. Syst. Charact. 19 (2002) 84 ± 95 91

Fig. 11: Effect of solid fraction on the square-weighted mode of


the chord length for sieved calcite particles (5% w/v).

Fig. 10: Effect of solid fraction on the unweighted and square-


weighted chord length distributions for aluminium particles sieved
125 ± 150 mm.

The effect of solid volume fraction was studied over a


Fig. 12: Effect of solid concentration (% w/v) on transformed
wide range of sizes (Figure 11). The mode of the square- chord data for aluminium particles (sieved 38-45 mm), showing
weighted chord length remained essentially constant that the model (Equation 2) over-estimated the particle size in
over the entire range, except for some deviation at large dilute suspensions.
size fractions. This may be due to release of fines from
these larger particles as a consequence of stirring.
The chord-to-diameter models described in Section 2.2.1 solid fraction, tapering off at high particle concentrations
(Equation 2) are based on the unweighted chord (Figure 13a). Similar results are reported by Barrett and
distribution. As shown in Figure 10, the unweighted Glennon [22] and Daymo et al. [57]. This effect is
distributions are dependent upon the solid fraction, and probably due to an increase in the instrument dead-
this effect is extended to the application of Eq. (2) time at higher solid fraction, because the instrument can
(Figure 12). This limits the usefulness of such algorithms, only count one particle at a time. At a low solid fraction
and further model parameters would be required to only a small portion of the 1.9 m s 1 scanned by the laser
compensate. The calculated distributions are also notice- intersects a particle, and the likelihood of particles
ably broader than the laser diffraction volume-weighted overlapping in the viewing zone is low. However, at a
distribution, and are likely to be worse for particles that higher solid fraction, the high number of counts becomes
deviate further from the sphericity assumed by the a significant portion of the 1.9 m s 1, reducing the time
model. available to detect other particles in the measurement
zone. This dead-time will be slightly larger than the time
spent traversing the particle, because the reflected light
4.5 Effect of Solid Fraction on Particle Counts
must return to zero for a short period between particles.
Estimation of total particle number is desirable for mass The signal processing algorithm also requires the re-
balancing or estimation of aggregate porosity. Unfortu- flected light pulse to rise and fall quickly before and after
nately, total FBRM counts did not correlate well with each particle, and counts from overlapping particles (or
92 Part. Part. Syst. Charact. 19 (2002) 84 ± 95

though the dead-time varies with the substrate, the value


of Equation 4 is that it allows the estimation of solid
fraction from FBRM counts for a particular substrate.

4.6 Effect of Particle Material


Particle shape [22, 28] and reflectivity [16, 17] were
expected to affect the reflection of the laser beam to
some extent. However, Daymo et al. [57] added food
colouring to a suspension of 4% w/v bentonite and
reported no change in the average size. Sparks and
Dobbs [17] studied various particles and found that
transparent particles (oil droplets, latex particles) were
generally poorly sized by FBRM compared to opaque,
reflective particles. The suspension of transparent mono-
sized spherical latex spheres (19.9 mm, Duke Dyna-
spheres), used in this study was also poorly sized by
FBRM, giving unweighted and square-weighted mean
chord lengths of 26 and 51 mm, respectively.
The aluminium and calcite particles used in this study
have quite distinct morphologies (Figure 3), but similar
densities (ral. ˆ 2.702, rcal. ˆ 2.710), giving them similar
volume fractions when made up by weight, and similar
flow requirements to keep the particles suspended.
Figure 14 compares aluminium and calcite particles at
the same solid fraction and size. The increased fine
counts shown by the unweighted distribution for calcite
is largely caused by fine material abraded from surfaces
during suspension mixing. The count rate increased in
this region with time, but was reduced by washing and
decantation. In addition, the sharper edges of the calcite
Fig. 13: (a) Total counts and (b) total corrected counts as a may result in a greater proportion of fine chords. The
function of solid fraction for various sieved calcite fractions. equivalent aluminium particles, with more spherical
shape, and no fines, gave a more symmetrical unweighted
chord distribution.
particles outside the viewing zone) are rejected, further
increasing the dead-time.
It has been suggested that the measured counts can be
corrected for such effects [8, 58]. Figure 13b shows the
effect of correcting for the dead-time according to
Equation 4. A parameter (k) is included to account for
the additional dead-time required before (and after) the
laser intersects the particle:

1:9  106
Nt ˆ Nt  M  : …4†
P 
1:9  106 Ni Ci;A ‡ 2k
iˆ1

The dead-time may then be simply derived from k and


the laser velocity. The optimum value for k was found
numerically by maximising the sum of the correlation
coefficients to produce the most linear relationships. For
calcite particles the dead-time was found to be 13.8 ms, Fig. 14: Comparison between chord length distributions of
compared to 5.74 ms for the aluminium particles. Al- aluminium or calcite (sieved 45 ± 53 mm, 5% w/v).
Part. Part. Syst. Charact. 19 (2002) 84 ± 95 93

fraction, correction for the instrument dead time can


substantially improve this relationship. FBRM square-
weighed average sizes were found to be essentially
independent of suspension bulk flow velocity, focal
position, or solid fraction in the range 0.1 ± 20% w/v.

6 Acknowledgements

This research has been supported by the Australian


Government×s Cooperative Research Centre (CRC)
program, through the AJ Parker CRC for Hydrometal-
lurgy. This support is gratefully acknowledged. One of us
(A.R. Heath) is grateful for support from the AMIRA
P266C ™Improving Thickener Technology∫ project.
Thanks are also extended to Phan Khanh and Mark
Schibeci for providing alternative particle sizing, and to
Dean Ilievski, Peter Austin and Rich Becker for useful
Fig. 15: Comparison between square-weighted median FBRM discussions.
results given by various sieved or cyclosized calcite and aluminium
fractions. FBRM suspensions 5% w/v.

7 Symbols and Abbreviations


In contrast, the corresponding square-weighted chord
Ci, u length of the upper boundary of the ith channel
distributions for the aluminium and calcite fractions are
(mm)
remarkably similar (Figure 14) despite the different
Ci, l length of the lower boundary of the ith channel
morphologies (and presumably different reflectivities)
(mm)
of the two materials.
Ci,A geometric average length of ith channel (mm) ˆ
A comparison of the median square-weighted chord
(Ci, u  Ci, l)1/2
lengths across all the sieved fractions (Figure 15) also
Dp diameter of pth particle (mm)
shows that the FBRM results were essentially unaffected
k additional dead time before (and after) particle
by particle material. This is certainly not expected to be
(mm)
applicable to all materials, but is more a consequence of
minf objective function
the relatively low aspect ratio of the two materials
M maximum number for i
studied.
Ni number of i sized chord counts observed (s 1)
Ni* number of i sized chord counts predicted (s 1)
5 Conclusions Ni, n number of n-weighted chord counts in the ith
channel (mmn s 1)
Np* number of pth sized particles predicted (s 1)
The FBRM instrument provides rapid on-line, in situ,
Ni, o raw unweighted chord counts in the ith channel (s 1)
particle characterisation of concentrated pulps. While
Nt* corrected total chord counts (s 1)
FBRM gives a particle chord distribution, as opposed to
Nt total observed chord counts (s 1)
a conventional diameter-based distribution, mean or
n exponent (0: unweighted; 1: length-weighted; 2:
mode averages of the square-weighted chord lengths are
square-weighted; 3: cube-weighted)
comparable to conventional sizing techniques over the
Wp, i width of pth particle giving chords in the ith channel
range approximately 50 ± 400 mm.
(mm)
This range may be extended by using the length-
weighted average for smaller particles, and by applying
a cube-weighting to larger particles. However, using a
lower weighting increases the instrument×s susceptibility 8 References
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