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Powder Technology 201 (2010) 283–288

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Powder Technology
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / p ow t e c

Measurement of the floating particle size distribution by a buoyancy


weighing-bar method
Takumi Motoi, Yuichi Ohira ⁎, Eiji Obata
Division of Applied Sciences, Graduate School of Engineering, Muroran Institute of Technology, Muroran, Hokkaido 050-8585, Japan

a r t i c l e i n f o a b s t r a c t

Article history: The particle size distribution of cylinder-shaped solid particles was measured using a buoyancy weighing-bar
Received 17 September 2009 method where the liquid phase density was adjusted to settle or float the particles. The particle size
Received in revised form 13 April 2010 distribution obtained in our experiment agrees with the particle size measured by other method. The present
Accepted 13 April 2010
study demonstrates that a buoyancy weighing-bar method, a novel method for measuring the particle size
Available online 18 April 2010
distribution, is suitable for measuring the particle size distribution of a floating solid. The precision of the
Keywords:
resulting particle size distribution is comparable to that of a laser diffraction/scattering method as well as a
Floating particle direct measurement with a micrometer. Moreover, this buoyancy weighing-bar method can measure the
Particle size distribution particle size distribution even in a mixture of two particles with different sizes.
Buoyant mass © 2010 Elsevier B.V. All rights reserved.
Solid particle
Stokes diameter

1. Introduction This apparatus consists of an analytical balance with a hook for


underfloor weighing, a personal computer, and a weighing-bar, which
Various approaches have been used to measure particle size is used to detect the density change in suspension. This apparatus has
distribution [1]. For solid–liquid systems, it is important to measure a simple structure, is easy to maintain, and does not require special
particle size distribution by the Stokes diameter. However, the skills. Furthermore, it is economical, and is even capable of auto-
Andreasen pipette method [2], sedimentation balance method [3], measurements.
centrifugal sedimentation method [4], etc. can measure particle size We have reported that the particle size distributions of settling
distribution in suspensions because these methods measure the particles can be measured using a buoyancy weighing-bar method
migration velocities of particles in solution and then use Stokes (BWM) [8]. Theoretically, a BWM can be applied not only to settling
formula to calculate particle size. The disadvantages of these methods particles, but also to floating particles, including bubbles and liquid
are that they are time consuming and require special skills. On the droplets. However, the latter has not been verified. In this study, we
other hand, particle size distribution can be analyzed using a different experimentally investigate the applicability of a BWM on measure-
principle through micrographs [5], laser diffraction/scattering meth- ments of the particle size distribution of floating particle. Floating
ods [6], and coulter counter method [7]; the drawbacks to this type of particles include microbubbles, liquid drops, and solid particles, which
method is that numerous samples must be used for accurate particle were smaller than liquid density. In terms of easy handling and
size distribution. Although laser diffraction/scattering and coulter availability of standard samples, we used solid particles in this study.
counter methods produce highly accurate results within a shorter
time, the equipment is extremely expensive. A simple and cost- 2. Theory
effective new method to determine particle size distribution is in high
demand. Let us assume the particles are uniformly dispersed in suspension.
We aim to develop a new method to measure the particle size Schematic diagram of particle floating is shown in Fig. 1. As shown in
distribution using a buoyancy weighing-bar method. In this method, Fig. 1(a), the initial buoyant mass of the submerged weighing-bar WB0
the density change in a suspension due to particle migration is depended on the particles between the top of the weighing-bar and
measured by weighing buoyancy against a weighing-bar hung in the the bottom of that in the suspension. The initial density of suspension
suspension, and the particle size distribution is calculated using the ρS0, the initial buoyant mass of the weighing-bar WB0 and the initial
length of the bar and the time course change in the mass of the bar [8]. apparent mass of the bar GB0 in suspension at t = 0 is given by the
following equations:

C0
⁎ Corresponding author. Tel.: + 81 143 46 5768; fax: + 81 143 46 5701. ρS0 = ρL + ðρ −ρL Þ; ð1Þ
E-mail address: ohira@mmm.muroran-it.ac.jp (Y. Ohira). ρP P

0032-5910/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2010.04.015
284 T. Motoi et al. / Powder Technology 201 (2010) 283–288

GBt = VB ρB −WBt = VB ðρB −ρS Þ: ð6Þ

As shown in Fig. 1(c), concentration of suspension C is finally zero,


because small particles also have floated. The final density of
suspension ρS∞, the final buoyant mass of the weighing-bar WB∞ and
the final apparent mass of the weighing-bar GB∞ in suspension at t = ∞
is given by the following equations:

ρS∞ = ρL ; ð7Þ

WB∞ = VB ρL ; ð8Þ

GB∞ = VB ρB −WB∞ = VB ðρB −ρL Þ: ð9Þ

Fig. 2 schematically illustrates the calculating method of the


particle size distribution used in the present study. Eq. (10) shows the
mass balance of particles in suspension [1].

Fig. 1. Schematic diagram of particle floating.


x x vðxÞt
C0 −C = C0 ∫xmax f ðxÞdx + C0 ∫ximin f ðxÞdx ð10Þ
i
h
WB0 = VB ρS0 ; ð2Þ
From Eqs. (2), (5), (8) and (10),
GB0 = VB ρB −WB0 = VB ðρB −ρS0 Þ; ð3Þ
x x vðxÞt
W0 −W = ðW0 −W∞ Þ∫xmax f ðxÞdx + ðW0 −W∞ Þ∫ximin f ðxÞdx ð11Þ
where the liquid density is ρL, the particle density is ρP, the initial con- i
h
centration of suspension is C0 [kg-solid/m3-suspension], the density of
the weighing-bar in suspension is, the volume of the weighing-bar is where v(x) is the floating velocity of the particle, f(x) is the mass
VB. As shown in Fig. 1(b), concentration of suspension C decreases frequency of the particle size x. Differentiate Eq. (11) with respect to
with the time, because large particles have floated. The density of the time t, we obtain:
suspension ρS, the buoyant mass of the weighing-bar WBt and the
apparent mass of the bar GBt in suspension at t = t is given by the dW x vðxÞ
− = ðW0 −W∞ Þ∫ximin f ðxÞdx: ð12Þ
following equations: dt h

C From Eqs. (11) and (12),


ρS = ρL + ðρ −ρL Þ; ð4Þ
ρP P
 
dWBt
WBt = WRt + t: ð13Þ
WBt = VB ρS ; ð5Þ dt

Fig. 2. Construction method to determine the floating particle size distribution.


T. Motoi et al. / Powder Technology 201 (2010) 283–288 285

Table 1
Sample particles.

Sample particles Shape Particle size [m] Particle density [kg m− 3]

Glassbubbles, K37 Sphere 0.012–0.081 × 10− 3 0.37 × 103


Paraffin particle Sphere 0.060–0.30 × 10− 3 0.89 × 103
NB202(A) Cylinder 0.2 × 10− 3 (nominal) 1.12 × 103
NB303(B) Cylinder 0.3 × 10− 3 (nominal) 1.12 × 103
FNB#400(C) Cylinder 0.4 × 10− 3 (nominal) 1.12 × 103
FNB#600(D) Cylinder 0.6 × 10− 3 (nominal) 1.12 × 103

The apparent mass of the submerged weighing-bar GBt is given by


Eq. (6). It is gradually decreases from GB0 to GB∞. The volume and the
density of the submerged weighing-bar are constant value. Differen-
tiate Eq. (6) with respect to the time t, we obtain:

dGBt dWBt
=− : ð14Þ
dt dt

Therefore, from Eqs. (6), (13) and (14), we obtain:


Fig. 4. Schematic diagram of the experimental apparatus. 1. Analytical balance. 2.
   
dGBt dGBt Personal computer. 3. RS-232C cable. 4. Hanging wire. 5. Measuring cylinder. 6.
GBt = VB ρB −WRt + t = GRt + t; ð15Þ Weighing bar, 7. Thermal insulation vessel. 8. Heating panel. 9. Controller.
dt dt

where GRt = VB ρ B − WRt. Value of GRt calculates from tangent line


where the length of the submerged weighing-bar is h and the time
based on Eq. (15). The cumulative mass percentage oversize is
lapse is t. From Eqs. (17) and (19), time t is a quadratic function of the
reciprocal of particle size x− 1. The particle size distribution of the
x GB0 −GRt
RðxÞ = 100∫xmax f ðxÞdx = × 100 = 100−DðxÞ: ð16Þ suspended particles is prepared by calculating the particle size at each
GB0 −GB∞
time, and then plotting the corresponding mass percentage undersize.
This theory for the floating particles measured by a BWM is the similar
Particle size x is given by the following equation using Stokes
to that for settling particles [8].
formula modified the voidage function:
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
1 18μ L vðxÞF ðεÞ 3. Materials and methods
x= : ð17Þ
ϕ g ðρL −ρP Þ
Table 1 describes the sample particles, which were Glassbubbles
where, ϕ is Wadell's shape factor, g is the gravitational acceleration, μ L (K37, Sumitomo 3M), paraffin particle (Kanto Chemical Co., Inc.)
is the viscosity of the dispersion liquid contained the dispersant, ε is made by spray and Fuji nylon beads (NB202, NB303, FNB#400,
voidage, F(ε) is the voidage function. The voidage function is FNB#600, Fuji Manufacturing Co., Ltd.). The particle densities of the
calculated by the Richardson and Zaki correlation [9]. sample were 0.37 × 103 kg/m3 (Glassbubbles K37), 0.89 × 103 kg/m3
(Paraffin particle) and 1.12 × 103 kg/m3 (Fuji nylon beads). For
−4:65
F ðεÞ = ε ; ð18Þ example, Fig. 3 shows micrographs of sample particles. The shapes
of Glassbubbles (a) and paraffin particle (b) were sphere-shaped. The
The floating velocity of the particles v(x) is calculated using shape of the nylon particles varied to a certain degree, but most of the
Eq. (19): particles were cylinder-shaped and the ratio of diameter and length is
approximately 1 (c). The nylon particles were either used alone or
h mixed (using a volume ratio) at equivalent concentrations. Fig. 4
vðxÞ = ; ð19Þ
t shows a diagram of the apparatus used in the experiment. A floating

Fig. 3. Micrographs of sample particles.


286 T. Motoi et al. / Powder Technology 201 (2010) 283–288

particle suspension was placed in a 1000 ml measuring glass cylinder


(diameter: 65 mm, Sanplatec Co., Ltd.), and an aluminum weighing-
bar (diameter: 10 mm, length: 250 mm, density: 2.70 × 103 kg/m3)
was hung from an analytical balance with a hook for underfloor
weighing (GR-300, minimum readout mass: 0.1 mg, A & D Co., Ltd.)
using a hanging wire. A personal computer was connected to the
analytical balance, and the data were collected in one second interval.
To avoid external effects such as airflow and temperature changes, the
experimental apparatus was placed in a box. A heater connected to
the thermostat was placed within the box to maintain the desired
temperature. A laser diffraction/scattering method (Microtrac
MT3000EX, Nikkiso Co., Ltd.) was used to validate the particle size
distribution obtained from the experiments. Table 2 describes the
properties of sample liquids. Ion exchanged water (density:
1.00 × 103 kg/m3, viscosity: 0.89 × 10− 3 Pa s) was used as the liquid
phase for Glassbubbles and paraffin particle. Sodium chloride (reagent
grade, Kanto Chemical Co., Inc.) solutions were used as the liquid
phase for Fuji nylon beads: one for the floating experiment
(concentration: 24 wt.%, density: 1.17 × 10 3 kg/m 3 , viscosity:
1.55 × 10− 3 Pa s), and the other for settling experiment (concentra-
tion: 10 wt.%, density: 1.07 × 103 kg/m3, viscosity: 1.07 × 10− 3 Pa s).
Fig. 5. Apparent mass of the weighing bar as a function of time (sphere-shaped
The liquid density was adjusted so that the density difference particles).
between the particle density and the liquid density was equal. The
initial volume concentration of the suspension C0/ρP was set at 0.001–
0.01 m3-solid/m3-suspension, and the temperature during the exper- on particle size distributions of Glassbubbles K37. When the volume
iment was maintained at 298 K. concentration is 0.03, the particle size distribution of Glassbubbles
To prepare a suspension, 1000 ml liquid and the particles to be K37 could not be measured by the BWM. The particle size
tested were mixed in measuring glass cylinder. Using a hanging wire, distributions measured by the laser diffraction/scattering method
which did not extend due to the weight of the bar, a bar was hung are indicated by the lines in Fig. 6. The particle size distributions
from the electronic precision weighing balance. After thoroughly measured by the BWM were close to those measured by the laser
stirring the suspension using an agitator, the bar was set with the diffraction/scattering method. We concluded that the particle size
balance, and this was recorded as t = 0. The measuring data, which distribution of floating sphere-shaped particles could be measured by
consisted of time t and the corresponding mass of the bar GB, were the BWM.
recorded on a personal computer. After the measurements, we Brownian motion is observed for particles about 1 μm in diameter
calculated the particle size distribution of the tested particles based [10]. In this work, the range of the particle size is 12–600 μm. Because
on the above-described theory. the particle size order is different by one or two digits, we consider
that the Brownian motion effects are little.

4. Results and discussion


4.2. Cylinder-shaped particles
4.1. Sphere-shaped particles
Fig. 7 shows the time course change in apparent mass of the bar GB
Fig. 5 shows the time course change in the apparent mass of the when nylon particle C was used. In a 10 wt.% sodium chloride solution
weighing-bar GB when Glassbubbles K37 and paraffin particle were
used. The apparent mass of the weighing-bar decreased, at which
point all particles floated above the upper end of the weighing-bar,
and the apparent mass of the weighing-bar became constant. The
change in the apparent mass was due to the change in buoyant mass
against the weighing-bar along with the particle floating. Thus, we
considered that the particle size distribution of floating particle can be
measured using the BWM, and that the results agree with the findings
in the previous report [8]. Fig. 6 shows the particle size distributions
obtained from the floating experiments using Glassbubbles K37 and
paraffin particle. The Wadell's shape factor of the sphere-shaped
particles is theoretically 1.0. Reynolds number of the floating particles
was smaller than 2 in the present study. When the volume
concentration is 0.01 or less, there is no effect of volume concentration

Table 2
Liquid properties.

Liquid Liquid density [kg m− 3] Viscosity [Pa s]

Water 1.00 × 103 0.89 × 10− 3 Glassbubbles K37, Paraffin


10% NaCl 1.07 × 103 1.07 × 10− 3 Particle C (settling)
24% NaCl 1.17 × 103 1.55 × 10− 3 Particles A-D (floating)
Fig. 6. Particle size distributions of sphere-shaped particles.
T. Motoi et al. / Powder Technology 201 (2010) 283–288 287

settling experiments using nylon particle C. The Wadell's shape factor


of the cylinder-shaped particle ϕ was calculated using Eq. (20) [11]:

surface area of a sphere having the same volume as the particle


ϕ= :
surface area of the particle
ð20Þ

The Wadell's shape factor of the cylinder-shaped particle is


theoretically 0.873, because the ratio of diameter and length is 1.
Reynolds number of floating particles was smaller than 2 in the
present study. The comparison studies of the results of the settling/
floating experiment with nylon particle C demonstrated that the
particle size distributions almost coincided. The precision of the
particle size distributions of floating particle measured by the present
method is comparable to that of the particle size distributions of
settling particle reported previously [8]. As for nylon particles A, B,
and D, they were only used in the floating experiment, but the particle
size distribution was almost the same as their respective nominal
sizes. Thus, we conclude the particle size distributions obtained for
nylon particles A, B and D are as reliable as those for nylon particles C.
Fig. 7. Apparent mass of the weighing bar as a function of time (cylinder-shaped We also measured the particle size distributions for nylon particles by
particles). the laser diffraction/scattering method. The particle size distributions
of nylon particles measured by the laser diffraction/scattering method
(upward triangle), which was used as the liquid phase for the settling are indicated by the solid lines in Fig. 8. The particle size distributions
experiments, the apparent mass of the weighing-bar (measured by measured by the BWM were similar to those measured by the laser
the analytical balance) linearly increased for approximately 60 s, at diffraction/scattering method.
which point all nylon particles settled below the lower end of the Next, we used a mixture of nylon particles A and C for the floating
weighing-bar, and the apparent mass of the weighing-bar became experiment. The time course change (filled circle) in the mass of the
constant. On the other hand, with the 24 wt.% sodium chloride bar is shown in Fig. 7. The apparent mass of the weighing-bar
solution (downward triangle), which was used as the liquid phase for decreased over time, and then became constant. The decreasing
the floating experiments, the apparent mass of the weighing-bar trends for the initial 100 s, and that between 100 s and 300 s were
linearly decreased for approximately 90 s, at which point all nylon different. As shown in Fig. 7, in the particle C (upward triangle)
particles floated above the upper end of the bar, and the apparent suspension, the decreasing trend in the apparent mass of the
mass of the weighing-bar became constant. Compared to the settling weighing-bar changed at 90 s, suggesting that the particle size
particles, it takes 1.5-fold longer for the apparent mass of the distribution of particle C was measured in the initial 100 s, while
weighing-bar to become constant, suggesting the floating velocity is that in the particle A suspension was measured between 100 s and
1.5-fold slower than that of the settling velocity of the particles. 300 s. Fig. 9 shows the particle size distribution (filled circle) of the
Although the density difference between the particles and liquid particle mixture. The nominal size of particles A and C are shown as
phase is the same, this difference between the floating and settling broken lines in the figure. The inflection point was at approximately
velocities of the particles is due to the viscosity of the liquid phase, 50% of the mass percentage undersize, suggesting that both particle
which is 1.5-fold greater in the floating experiment than that of the sizes were measured. The figure shows the particle size at 25% was
settling experiment. Fig. 8 shows the particle size distributions approximately 0.25 mm, and that at 75% was approximately 0.48 mm.
obtained from the floating experiments using all nylon particles and These results confirm that each particle size is successfully measured

Fig. 9. Particle size distributions of a nylon particle mixture. Solid line: calculated line of
Fig. 8. Particle size distributions of nylon particles (cylinder-shaped particles). nylon particles A and C.
288 T. Motoi et al. / Powder Technology 201 (2010) 283–288

in the particle mixture. In addition, we calculated the particle size x particle size, m
distribution of the particle mixture, which consisted of nylon particles ε voidage, −
A and C, from independent data obtained using nylon particle A and ϕ shape factor, −
nylon particle C. The results are shown in Fig. 9 (solid line). There is a μL liquid viscosity, Pa s
slight difference between the calculated results and the results ρL liquid density, kg/m3
obtained in the experiment, but they are close. ρB density of weighing tool, kg/m3
Thus, we conclude that the particle size distribution of particles, ρP particle density, kg/m3
which consists of two different sized particles, can be measured using ρS density of suspension, kg/m3
the BWM if the particle density is the same. Taken together, the BWM
is reliable for measuring a particle size distribution. Subscripts
max maximum
5. Conclusions min minimum
0 initial t = 0
Using the BWM, we measured the particle size distribution of the ∞ infinity t = ∞
floating solid particles in the liquid phases where the density was
adjusted with the concentration of sodium chloride. The following
results were determined:
Acknowledgements
(1) Using the BWM, the particle size distributions of floating solid
particles can be measured, suggesting the theory established in A part of this work has been supported by the Japan Science and
particle size distribution of settling particle measurements can Technology Agency (JST). The authors would like to thank our
be applied to floating particles. students for experimental assistance: Mr. Y. Koikeda and K. Nakano.
(2) The particle size distribution for a particle mixture consisting of
two different size particles can be measured using the BWM.
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