Particulate Science and Technology

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Comparison of Subsieving Techniques Based on the

Relation of Particle Size and Specific Surface Area in
Mineral Processing

Murat Kademli

To cite this article: Murat Kademli (2013) Comparison of Subsieving Techniques Based on the
Relation of Particle Size and Specific Surface Area in Mineral Processing, Particulate Science
and Technology, 31:4, 326-331, DOI: 10.1080/02726351.2012.736457

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Particulate Science and Technology, 31: 326–331
Copyright # 2013 Taylor & Francis Group, LLC
ISSN: 0272-6351 print=1548-0046 online
DOI: 10.1080/02726351.2012.736457

Comparison of Subsieving Techniques Based on the

Relation of Particle Size and Specific Surface Area
in Mineral Processing
MURAT KADEMLİ
Hacettepe University, Vocational School of Higher Education, Hacettepe University Beytepe Campus Hacettepe, Ankara, Turkey

This investigation is concerned with the comparison of the advantages and disadvantages of subsieving techniques widely used in
mineral processing throughout the world. With this purpose, the subsieving techniques of Andreasen pipette, Coulter counter, and
laser diffraction methods were compared each other by determining the relationship between specific surface area and particle size
distribution. In the tests, the two different standard quartz sand samples (A and B) from the Official Material Testing Institute for
Nonmetallic Minerals, Clausthal-Zellerfeld with a particle density of q ¼ 2.65 g=cm3 were used. As a result, the Coulter counter
method had the most favorable results in terms of calculated specific surface areas of 3848 cm2=g for sample A and 2852 cm2=g
for sample B, with standard deviations 41.29 and 32.48, respectively.
Keywords: Andreasen pipette, coulter counter, laser diffraction, specific surface area, subsieving

1. Introduction Therefore, Andreasen pipette, Coulter counter, and laser

diffraction methods were chosen for the investigations in this
Sieve analysis is one of the oldest methods of size analysis paper and were compared in terms of their advantages and
and is accomplished by passing a known weight of sample disadvantages. Typically, in particle size analysis, size is
material successively through finer sieves and weighing the expressed as an ‘‘equivalent sphere diameter’’ based on the
amount collected on each sieve to determine the percentage response of the particle to the particular measurement used.
weight in each size fraction Wills (1985). It has been used An important consequence is that, for irregular particles, dif-
since early Egyptian times for preparation of foodstuffs. ferent kinds of measurements (e.g., sieving, sedimentation,
The simplest sieves would be made of some woven material, and light scattering) give different apparent sizes for the same
but punched plate sieves are recorded in early Egyptian particle. Ideally, particles of identical size and shape would
drawings. It is a particularly useful technique since particles give the same response to sieving or sedimentation or to
are sorted into categories on the basis of size alone, indepen- volume-based methods such as the Coulter counter method
dently of their other properties such as density, surface (Hogg et al. 2004). Although each method has a different
properties, etc. (Allen 1992). Moreover, it has an important theory to determine particle size distribution, the differences
role for the determination of particle size distribution, par- of size distribution curves depend not only on the particular
ticle liberation degree, and designing of comminution, grind- instrument and material tested but also on the shape of the
ing, and drying units (Saklara et al. 2000). However, it is size distribution of the sample being measured (Austin 1997).
rarely carried out on a routine basis below about 38 mm; This study aimed to investigate of advantages and disad-
below this size, the operation is referred to as subsieving. vantages of these various methods by using standard quartz
The subsieving techniques are also used in different indus- sand samples with certain specific surface areas. The subsiev-
tries such as chemistry, fertilizer, pharmacology, astronomy, ing techniques, widely used in mineral processing industry,
meteorology, cement, blood analysis, etc. There are over 400 are compared with each other in order to determine the
subsieving techniques in different industry for different relationship between particle size and specific surface area.
purposes Bart and Flippen (1995). However, the most widely For this purpose, the specific surface areas of samples were
used procedures are sedimentation, electronic sensing, and calculated by using different particle size distributions,
laser diffraction methods in the mineral processing industry. (obtained from all subsieving methods) and compared with
actual specific surface area values of samples. In the per-
Address correspondence to: Murat Kademlı̇, Hacettepe meability method, the outer surface area of a particle collec-
University, Vocational School of Higher Education, Hacettepe tive is measured, which corresponds approximately with the
University Beytepe Campus Hacettepe Vocational School of geometric surface area. This allowed the samples to be tested
Higher Education, Ankara 906800, Turkey. E-mail: kademli@ with a Blaine apparatus and the results evaluated together.
hacettepe.edu.tr
Subsieving Techniques Based on Particle Size and Surface Area 327

Fig. 1. Andreassen pipette technique.

Fig. 2. Working sketch of Coulter–counter technique (http.==

1.1 Andreasen Pipette Technique folk.uio.no). (Figure available in color online.).
The Andreasen pipette method, which is one of the sedimen-
tation methods, is among the most widely applied methods The basic assumption underlying the operation of the
for subsieving measurements. The method is simple, cheap, Coulter counter is that the response is directly proportional
and readily available (Ulusoy et al. 2006). It has the advan- to particle volume. The reliability of the instrument depends
tage of producing a true fractional size analysis. The device on the accuracy of this assumption.
is suitable for size measurement in the range of 1 to 50 mm. Since analyses may be carried out rapidly with good
This method has same principle with decantation methods; reproducibility using semi-skilled operators, the method
however, it supplies to take experiments’ conditions under has become popular in a wide range of industries.
control (Saklara et al. 2000). On the other hand, it is The instrument response essentially is to particle volume.
extremely tedious, as long settling times are required for very It has been claimed that particle shape, roughness, and the
fine particles, and separate tests must be performed for each nature of the material have little effect on the analysis, but
particle size. there is considerable evidence that the size parameter mea-
The apparatus is a glass cylinder with an Andreasen pip- sured is, in fact, the envelope of the particle. Comparison
ette and a suspension column of initial height 200 mm. It with other techniques has been found to be good for spheri-
consists of a thin, capillary pipette with tip fixed at a known cal particles; for nonspherical particles, results may differ
depth in a vertical cylinder containing an initially homogen- with porous materials such as nylon the measured volume
ous suspension (see Figure 1). may be several times skeletal volume (see Figure 2).

1.2 Coulter Counter Technique 1.3 Laser Diffraction Technique

The Coulter counter technique is a method for determining For particle size analysis, optical instruments based on the
the number and size of particles suspended in an electrolyte measurement of laser light scattered by the particles in the
by causing them to pass through a small orifice on either side forward direction have now become a popular and standard
of the orifice, which is immersed an electrode. A known technique in the laboratory. Since the light scattered in the
volume of an extremely dilute suspension of particles in forward direction can often be accurately approximated by
a conducting fluid flows through a standard interchangeable diffraction theory, the class of instruments have become gen-
aperture having an immersed electrode on either side. The erally known as laser diffraction instruments. Compared
particles traverse the aperture substantially one at a time, caus- with other particle sizing techniques, laser diffraction has
ing an attendant change in electrical resistivity proportional the advantage of high speed, good reliability, and high
to the volume of the particle passing through the aperture. reproducibility. It is increasingly being applied for direct
The amplified signals pass through a gate circuit, which online process and quality control of powder processes
ensures that only pulses greater than a preselected threshold (Zhanhua et al. 2000).
value are counted; thus, the pulse count records the number This technique is based on the fact that the grain diameter
of particles greater than a certain size (Harris 1965). is inversely proportional with the refraction angle of the
328 Kademlı̇

multiplying the cumulative undersize value of 38 mm as

determined by the sieving techniques.
In the Andreasen pipette experiments, the 2% solid con-
tents by weight suspension were used. The samples were con-
tinuously taken to 10 ml cell in determined time intervals,
which were doubled each time, starting from 60 s and ending
at 1920s in each experiment. The particle size distributions
were calculated by using Stoke’s law.

d 2 gðDs
Df Þ
n¼ ð1Þ
18l
where l is viscosity, centipoises (g=cm.sec); n is velocity, cm=
sec.; Ds is density of solid particle, g=cm3; Df is density of
fluid, g=cm3; d is diameter of a sphere, cm; and g is acceler-
ation due to gravity, cm=sec2.
Fig. 3. Working scheme of laser diffraction technique.
In the Coulter counter experiments, the 1% solid contents
by weight suspension were used. During the tests, the thresh-
laser light. In other words, larger diameter grains refract old values were changed to obtained different pulses, which
laser light with small angles where as small diameter grains identify different particle sizes.
refract laser light with grater angle. As particle size In the laser diffraction experiments, the 10 g sample was
decreases, the observed scattering angle increases logarithmi- used. The particle size distributions were calculated auto-
cally (Rawle 1995a:1995b; Kippax 2005; Ulusoy et al. 2008). matically by a computer program.
The most important difference of the laser diffraction sys- The specific surface areas of test materials were then
tem is that it determines grain-size distribution according to determined with a Blaine apparatus, which is a test appar-
volumetric basis. By using the density of scattered laser light, atus for determining the specific surface area by using the
the volumes of grains are calculated and results are pre- permeability of a fluid through a particle bed. In the per-
sented. The laser diffraction technique utilized equivalent meability method, the experiments are performed repeatedly
sphere theory for the calculation of grain sizes. The most in order to compare actual values. In scope of this research,
important advantage of this technique is that it does not the average mean of measured specific surface areas from 10
require the specific gravity and weight of grains. By this measurements were 3959 cm2=g with the 5.49 standard devi-
way, mistakes during the calculation of weight is avoided ation for sample A and 2892 cm2=g with the 6.80 standard
(Orhan et al. 2004). On the other hand, the laser diffract- deviation for sample B. The tests were repeated 10 times
ometer uses a very small sample, usually about 4 g, and spe- and standard deviations were calculated and conducted at
cial care is required to ensure the sample is representative. room temperature.
The equipment has alternative configurations for predicting The relationship between particle size distribution and
the light scattering pattern of particles, using the Fraunhofer specific surface area have investigated in many other studies
approximation or the complete Mie theory (Schneider et al. and are presented by Equations (2)–(4) (Hewlett 1998;
2006) (see Figure 3). Summer et al. 1989; Zhang et al. 1995; Kalkert 2000;
Gultepe and Ergun 2009).
n

2. Materials and Methods 6 X Wi
SSA ¼  ð2Þ
In the present study, the standard substance quartz sand q i¼1 Xmi
from the Official Material Testing Institute for nonmetallic n

6 X Wi
minerals, Clausthal-Zellerfeld, with a particle density of SSA ¼  u  ð3Þ
q ¼ 2,65 g=cm3, was chosen as the test material. Two differ- q i¼1
Xmi
ent test samples were used; sample A had specific surface
area of 3970 cm2=g and sample B had specific surface area Actual Value of SSA
u¼ ð4Þ
of 2930 cm2=g. The samples were sieved at the same sieving Calculated Value of SSA
sizes, but with different size distributions. (The quartz sands,
used in our tests, were a special production for the cali-
bration of the Blaine-specific surface area analyzer and Equation (2) is used for spherical shape particles and
had certain specific surface areas.) First, the samples were Equation (3) is usually used for nonspherical shape particles.
sieved to under 38 mm with the classical wet screening Much work has been done to study the effect of particle
method; then our subsieving techniques (Andreasen pipette, shape on size distribution as measured by different techniques.
Coulter counter, and laser diffraction) were applied for It has been shown that particle shape has a strong influence on
determination of finer size distributions; this was done size distribution measured by light diffraction, electrical sens-
repeatedly and then combined to obtain the sieving data. ing zone, x-ray sedimentation, photo-sedimentation, light-
The combined particle size distributions were obtained by obscuration, and image analysis (Barreiros et al. 1996; Kaye
Subsieving Techniques Based on Particle Size and Surface Area 329

et al. 1997, 1999; Endoh et al. 1998; Xu and Guida 2003; Li

et al. 2005; Taşdemir et al. 2011).
In this case, the samples, used in our tests, are special a pro-
duction of standard quartz sands (samples A and B) from
the Official Material Testing Institute for Nonmetallic
Minerals, Clausthal-Zellerfeld, with certain specific surface
areas and their shapes are rounded specially. The shapes
of the samples have high sphericity (S) values and the shapes
of samples are highly close to sphere.
Thus, Equation (2) was used for all calculations and then
the adjusting coefficients were defined in place of shape factors
for each sample by using Equations (3) and (4), where SSA is
specific surface area (cm2=g), q is density of particles (g=cm3),
wi is the weight percentage of fractions, Xmi is mean particle sizes
of xi and xiþ1 fractions, u is the adjusting coefficient (i.e., it is
rounded in shape, so it is called as adjusting coefficient).
Moreover, there are some different approaches in order to
find the mean particle sizes of xi and xiþ1 fraction such as arith-
metic mean, geometric mean, harmonic mean, and quadratic
mean (see Equations (5)–(8)). The specific surface area values
were calculated by using all approaches in terms of different
mean calculations for each subsieving technique. They then
were compared with actual specific surface area of samples. Fig. 4. Combined particle size distributions. (Figure available in
color online.).
xi þ . . . þ xn
xmi ¼ arithmetic mean ð5Þ
n
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
xmi ¼ n xi . . . xn geometic mean ð6Þ Table 1. Calculated specific surface areas and their standard
n deviations for sample A
xmi ¼ 1 1
harmonic mean ð7Þ
xi þ . . . þ xn Andreasen Coulter Laser
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi pipette counter diffraction
x2i þ . . . þ x2n
xmi ¼ quadratic mean ð8Þ Number of SSA SSA SSA
n
equation (cm2=g) STD (cm2=g) STD (cm2=g) STD

Equation (5) 2537.48 26.22 3010.18 37.41 2326.52 14.25

3. Results and Discussions
Equation (6) 3015.27 31.05 3848.18 41.29 2794.93 19.67
According to theory difference between methods, the differ- Equation (7) 3654.36 35.55 5023.85 55.84 3432.28 30.06
ent particle size distributions were obtained and combined Equation (8) 2297.02 24.27 2631.47 24.21 2101.59 13.92
with wet screening results (Figure 4). The minimum particle size is assumed as 1 mm.
The combined particle size distributions, obtained from SSA ¼ specific surface area.
STD: standard deviation.
each method, were used for calculations of specific surface
SSA ¼ specific surface area.
area in the terms of different equations (see Equations STD: standard deviation.
(5)–(8)). The calculated specific surface areas and their stan-
dard deviations by using the above equations are given in
Tables 1 and 2 and the adjusting coefficients were calculated Table 2. Calculated specific surface areas and their standard
for each approach are given in Tables 3 and 4. Figure 5 shows deviations for sample B
the relationship between adjusting coefficients and equations,
which were used for calculating of particle size mean. Andreasen Coulter Laser
This study mainly focused on comparing the subsieving pipette counter diffraction
techniques based on different physical properties and the-
ories. Thus, no specific inferences about which technique is Number of SSA SSA SSA
best for particle size distribution can be made. equation (cm2=g) STD (cm2=g) STD (cm2=g) STD
There are some advantages and disadvantages of all tech- Equation (5) 2537.48 26.22 3010.18 37.41 2326.52 14.25
niques. Thus, it is not surprising that the consistent compari- Equation (6) 3015.27 31.05 3848.18 41.29 2794.93 19.67
son of size distributions measured by one technique with Equation (7) 3654.36 35.55 5023.85 55.84 3432.28 30.06
those measured by another has proved difficult. According Equation (8) 2297.02 24.27 2631.47 24.21 2101.59 13.92
to calculated specific surface areas and adjusting coefficient The minimum particle size is assumed as 1 mm.
values, the best reliable results were obtained from Coulter SSA ¼ specific surface area.
counter technique, then the Andreasen pipette and laser STD: standard deviation.
330 Kademlı̇

Table 3. Calculated adjusting coefficient and their standard diffraction, respectively. In a similar study, Xu and Guida
deviations for sample A (2003) investigated the comparison of laser diffraction, elec-
trical sensing zone (Coulter counter principal), and image
Andreasen Coulter Laser
analysis methods by using unimodal sphere glass bead parti-
pipette counter diffraction
cles; they indicated that particles with mean values obtained
Number of Adj. Adj. Adj. from the three technologies agree well. The trend in the devi-
equation coeff. STD coeff. STD coeff. STD ation of laser diffraction results from those of electrical sens-
ing zone and dynamic image analysis is very clear as the
Equation (5) 1.56 0.0066 1.32 0.0094 1.71 0.0036 shape of particles departs from that of a sphere. On the
Equation (6) 1.32 0.0078 1.03 0.0104 1.42 0.0050 other hand, electrical sensing zone and dynamic image
Equation (7) 1.09 0.0090 0.79 0.0141 1.16 0.0076 analysis are more appropriate in obtaining equivalent
Equation (8) 1.73 0.0061 1.51 0.0061 1.89 0.0035 spherical diameters.
3970 cm2=g was used as actual value of specific surface area according to However, the Coulter counter technique has disadvan-
data of Clausthal-Zellerfeld Institute. tages such as having narrow analysis intervals, low analysis
SSA ¼ specific surface area.
STD: standard deviation.
speed, operational difficulties, and only being able to be used
in wet applications. Advantages to the laser diffraction
technique include analysis speed, ability to be used in dry
and wet application, wide analysis intervals, easy usage,
Table 4. Calculated adjusting coefficient and their standard and adaptation of online analysis systems. The Andreasen
deviations for sample B
pipette technique generally shares disadvantages of the
Andreasen Coulter Laser Coulter counter technique, but it has important advantages
pipette counter diffraction such as being a cheap and easy method for analysis under
38 mm particles.
Number of Adj. Adj. Adj.
equation coeff. STD coeff. STD coeff. STD 4. Conclusion
Equation (5) 1.56 0.0162 1.32 0.0164 1.71 0.0105 In this study, the methods were evaluated by means of their
Equation (6) 1.32 0.0136 1.03 0.0111 1.42 0.0100 relationship between particle size distributions and specific
Equation (7) 1.09 0.0106 0.79 0.0088 1.16 0.0101
surface areas. In this manner, the specific surface areas were
Equation (8) 1.73 0.0183 1.51 0.0139 1.89 0.0125
calculated by using different approaches for each method
2930 cm2=g was used as actual value of specific surface area according to with two different fractions of quartz sand samples.
data of Clausthal-Zellerfeld Institute.
SSA ¼ specific surface area.
The results show that the Coulter counter method was the
STD: standard deviation. most favorable technique in order to obtain a ratio between
calculated specific surface area and actual surface area
values (Figure 5). The most favorable results were found
as 3848.18 cm2=g for sample A, with the actual specific sur-
face area of 3970 cm2=g, and 2852.78 cm2=g for sample B,
with the actual specific area of 2930 cm2=g.
The second most favorable technique was the Andreasen
pipette, giving the calculated specific surface area of
3654.36 cm2=g for sample A, and 2796.13 cm2=g for sample
B. The laser diffraction technique gave specific surface of
3432.28 cm2=g and 2439.72 cm2=g for samples A and B,
respectively. The Coulter counter technique had the mini-
mum adjusting coefficient value of 1.03. Normally, it can
be described as shape factor of sample. In this case, the
quartz samples, as used in our tests, were a special pro-
duction from the Clausthal–Zellerfeld Institute. Thus, the
shapes of sample were rounded specially. Therefore, the
shape factor was ignored and it was defined as adjusting
coefficient as discussed in this article.
In specific surface area calculations, the mean of fractions
were calculated by four different approaches: arithmetic
mean, geometric mean, harmonic mean, and quadratic mean
(see Equations (5)–(8)). The best results were obtain from
geometric mean for Counter coulter technique, whereas the
harmonic mean was found to be best for others. The adjust-
Fig. 5. The variation of adjusting coefficients in order to differ- ing coefficients in order for each equation are shown in
ent mean approaches. (Figure available in color online.). Figure 5.
Subsieving Techniques Based on Particle Size and Surface Area 331

Finally, in the evaluation of all methods, the most favor- Li, M., D. Wilkinson, and K. Patchigolla. 2005. Comparison of particle
able sizing method was determined to be the Coulter counter size distributions measured using different techniques. Particulate
under 38 mm particles. However, the laser diffraction method Science and Technology 23: 265–284.
Orhan, M., M. Ozer, and N. S. Isık. 2004. Investigation of laser
has very important advantages (as discussed above). diffraction and sedimentation methods which are used for the
determination of grain size distribution of fine grained soils. Gazi
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