applied

sciences
Article
Correlation between Material Properties and
Breakage Rate Parameters Determined from
Grinding Tests
Evangelos Petrakis * and Konstantinos Komnitsas ID

School of Mineral Resources Engineering, Technical University of Crete, University Campus, Kounoupidiana,
73100 Chania, Greece; komni@mred.tuc.gr
* Correspondence: vpetraki@mred.tuc.gr; Tel.: +30-28210-37608

Received: 22 December 2017; Accepted: 28 January 2018; Published: 31 January 2018

Abstract: The present study investigates four materials, namely quartz, marble, quartzite and
metasandstone and aims to establish correlations, with the use of simple and multiple regression
analysis, between their properties and breakage rate parameters. The material properties considered
in this study derived from the application of destructive and non-destructive tests and include P-wave
velocity (Vp ), Schmidt rebound value (RL ), uniaxial compressive strength (UCS) and tangent modulus
of elasticity (Et ), while the breakage rate parameters determined from batch grinding tests, include
breakage rate Si , maximum breakage rate Sm , αT and α, and optimum particle size xm . The results
indicate that the properties of all materials examined show very good correlation and can be used
to predict Si or αT . Furthermore, parameter α is well correlated with Vp , RL and Et using inverse
exponential functions, while Sm is strongly correlated with RL and UCS. Overall, it is deduced that
multiple regression analysis involving two independent variables is a reliable approach and can be
used to identify correlations between properties and breakage rate parameters for quartz, quartzite
and metasandstone, which are silica rich materials. The only exception shown is the determination
of xm for marble.

Keywords: comminution; grinding; material properties; population balance model; breakage

rate parameters

1. Introduction
Comminution and especially grinding is one of the most important operations of the materials
processing industry. For many decades, it has been the subject of intensive research in several
industrial sectors including mineral processing [1,2], metallurgy [3], cement, chemicals and ceramics
production [4,5]. In addition, interest has been paid in recent years on the production of ultra-fine
materials due to their improved physical and mechanical properties [6]. It is also known that
comminution is an energy intensive process and has low efficiency, due to the fact that most energy
consumed is absorbed by the device and only a small share is used for size reduction [7]. Considering
these factors, it is deduced that improvement of process efficiency will definitely have a large impact
on the operating cost of the mill, the environment and the conservation of resources.
Scientific research, aiming to improve grinding efficiency, was initiated with the empirical
relationships of Rittinger, Kick, Bond as well as Walker and Shaw, which described the energy-particle
size relationship [8]. Later, theories which incorporated the concept of particle size distribution were
developed [9,10], while recently research focused on the use of the mechanistic approach which is
based on the recognition of physical events that take place during grinding [11–13]. The mechanistic
approach includes the matrix model, which considers grinding as a series of breakage events and
the population balance model, which considers grinding as a continuous process. The population

Appl. Sci. 2018, 8, 220; doi:10.3390/app8020220 www.mdpi.com/journal/applsci

Appl. Sci. 2018, 8, 220 2 of 17

balance model considers first order kinetics and uses two functions, namely the breakage rate Si and
the breakage function bi,j [14,15]. These functions generate the fundamental size-mass balance equation
which is applied for fully mixed batch grinding operations. It is mentioned that many researchers have
underlined the advantages of these functions [16,17], while the scale-up from laboratory to industrial
mills has also been discussed in a number of studies [18–21].
The variation of breakage rate Si (min−1 ) as a function of particle size xi (mm) has been considered
by Austin [15] and is expressed with Equation (1), which is accepted by many researchers [22–24].
 α
xi
Si = α T · · Qi (1)
xo

where, xi (mm) is the upper size of class i, x0 is the standard size (1 mm), αT (parameter that depends on
milling conditions) is the breakage rate for size xi = 1 mm and α is a characteristic parameter depending
on material properties. Qi is a correction factor, which is 1 for small particles (normal breakage) and
smaller than one for large particles that need to be nipped and fractured by the grinding media. In the
abnormal breakage region, the material behaves as it consists of a soft and a harder fraction [16]. Qi is
calculated from Equation (2) [15], !
1
Qi = (2)
1 + ( xi /µ)Λ
where, µ is a parameter that depends on milling conditions and Λ is a positive number that depends on
material type and shows how rapidly the breakage rate decreases as size increases (Λ ≥ 0). In addition,
the particle size xm for which the breakage rate reaches its maximum value is related with parameter µ
through the following equation [25,26],
 1/Λ
α
xm = µ· , Λ>α (3)
Λ−α

Equation (3) shows that xm is directly proportional to µ since for the same material α and Λ
are constants.
The physical and mechanical properties of a material play a crucial role in the design of a mineral
processing circuit. The reliable determination of these properties enables the prediction of milling
results and in this case no extensive milling tests that require large amounts of time and material are
needed [27]. In this respect, several researchers [28–36] have attempted to identify the relationship
between various material properties and P-wave velocity. These studies indicated that sound velocity
is closely related to physico-mechanical properties such as uniaxial compressive strength, modulus of
elasticity, hardness, effective porosity, water absorption and both saturated and dry density. P-wave
velocity test is non-destructive, offers several advantages to researchers and can be easily applied both
in laboratory and in situ. It is mentioned that P-wave velocity is related with the characteristics of the
whole body of the material tested [29].
The Schmidt hammer test is equally acceptable and used for estimating indirectly material
hardness and strength, through the determined RL value, which depends on the properties of the
specimen. The operation of the device is based on the principle that the rebound of an elastic mass
impacting on a surface depends on its hardness and thus the harder the surface the higher is the
rebound distance [37]. Several societies, including the International Society for Rock Mechanics [38,39]
and the American Society for Testing and Materials [40], have proposed test methods and standards,
respectively, for the proper operation of the device [41]. Other options for determining such material
properties with the use of the Schmidt hammer have also been proposed [42–44].
Breakage rate parameters depend on material properties, so it is very useful and practical from
a laboratory and industrial point of view if correlations between them are established. In this regard,
Deniz [45] used limestone as test material and identified the relationship between Bond’s grindability
and breakage rate parameters, while Aras [46] established important correlations between the point
Appl. Sci. 2018, 8, 220 3 of 17

load index and Bond’s grindability as well as breakage rate parameters. However, so far no correlations
between other material properties such as uniaxial compressive strength or modulus of elasticity and
breakage rate parameters have been established.
This study has a certain degree of novelty since it attempts to establish potential correlations
between material properties derived from the application of destructive and non-destructive tests, and
breakage rate parameters.

2. Materials and Methods

The materials used in the present experimental study were obtained from several Greek sites,
namely quartz from Assiros, near Thessaloniki; marble from west Crete, Chania region; and quartzite
and metasandstone from west Crete, Kissamos area. More than 100 kg of each material was sampled
from several locations of the same site in order to obtain representative samples. Mineralogical analyses
show that marble consists mainly of calcite, while quartzite and metasandstone of quartz and some
mica. The quartz samples used in this study were of high purity white quartz. The main difference
between quartzite and metasandstone is the degree of transformation. Quartzite, due to dynamic
re-crystallization, consists of fine crystalline and elongated quartz grains, which are well oriented;
due to the mechanical strain imposed, individual quartz crystals are present. However, metasandstone
consists of a fine crystalline matrix with individual quartz crystals, which exhibit lack of orientation
due to the lower degree of transformation compared to quartzite. In addition, large gaps are observed
between its grains due to the high porosity. Table 1 presents the porosity and density of each raw
material, as determined with the use of Archimedes method [47]; all measurements were carried
out in triplicate and average values are shown. The standard deviation of porosity and density was
0.002 and 0.005 respectively, for all materials tested.

Table 1. Porosity and density of the raw materials used.

Material Porosity % Density g/cm3

quartz 0.02 2.65
marble 0.3 2.72
quartzite 0.9 2.59
metasandstone 8.0 2.11

Cylindrical cores of representative samples with NX size (diameter 54.7 mm) were used to
determine the physico-mechanical properties of each material. Both ends of the core specimens were
cut flat and polished using a cut-off and a special polishing machine, respectively. The height to
diameter ratio of all specimens was kept equal to 2 in order to minimize the size effect. From each
material type 6–8 specimens were cored (Figure 1a,b). Specimens exhibiting cracks, discontinuities,
or alteration phenomena as a result of coring were not used in tests and replaced with new specimens.
In this study, the non-destructive P-wave velocity and Schmidt hammer rebound tests were
carried out. The P-wave velocity test was performed using the PUNDIT 6 (Portable Ultrasonic
Non-destructive Digital Indicating Tester) device (CNS Farnell, London, UK) at a frequency of 1 MHz.
According to the procedure, two transducers were placed opposite the two parallel surfaces of the core
samples (Figure 2a,b) and the travel time of the ultrasonic waves, from one transducer to the other,
was recorded. By taking into account that the distance between the two surfaces of each specimen
is known, the velocity of the ultrasonic waves can be calculated [48]. It is known that the ultrasonic
velocity depends on density and the elastic properties of each material and is higher when the sample
has adequate density, uniformity and homogeneity [49].
 Cylindrical cores of representative samples with NX size (diameter 54.7 mm) were used to
determine the physico-mechanical properties of each material. Both ends of the core specimens were
cut flat and polished using a cut-off and a special polishing machine, respectively. The height to
diameter ratio of all specimens was kept equal to 2 in order to minimize the size effect. From each
material
Appl. Sci. type
2018, 8,6–8
220 specimens were cored (Figure 1a,b). Specimens exhibiting cracks, discontinuities,
4 of 17
or alteration phenomena as a result of coring were not used in tests and replaced with new specimens.

Appl. Sci. 2018, 8, x FOR PEER REVIEW 4 of 18

In this study, the non-destructive P-wave velocity and Schmidt hammer rebound tests were
carried out. The P-wave velocity test was performed using the PUNDIT 6 (Portable Ultrasonic Non-
destructive Digital Indicating Tester) device (CNS Farnell, London, UK) at a frequency of 1 MHz.
According to the procedure, two transducers were placed opposite the two parallel surfaces of the
core samples (Figure 2a,b) and the travel time of the ultrasonic waves, from one transducer to the
other, was recorded. By taking into account that the distance between the two surfaces of each
(a)
specimen is known, the velocity of the ultrasonic waves can be calculated(b) [48]. It is known that the
ultrasonic velocity depends
Figure on density and the (a)
elastic properties of each material and is higher when
Figure1.1.Core
Corespecimens
specimensof
of (a)marble
marbleand
and(b)
(b)metasandstone.
metasandstone.
the sample has adequate density, uniformity and homogeneity [49].

(a) (b)
Figure
Figure 2.
2. P-wave
P-wave velocity
velocity test
test for
for (a)
(a) marble
marble and (b) metasandstone.
and (b) metasandstone.

The Schmidt hammer rebound test was performed using an L-type hammer with impact energy
The Schmidt hammer rebound test was performed using an L-type hammer with impact energy
0.735 Nm. Core specimens were tested in a V-shaped cradle block with an approximate weight of 23
0.735 Nm. Core specimens were tested in a V-shaped cradle block with an approximate weight of 23 kg.
kg. Prior to test execution the circular ends of each specimen were divided into eight equal arcs, from
Prior to test execution the circular ends of each specimen were divided into eight equal arcs, from the
the ends of which eight straight parallel lines along their longitudinal axis were drawn (Figure 3).
ends of which eight straight parallel lines along their longitudinal axis were drawn (Figure 3). The test
The test was performed by placing the core specimens in the cradle and impacting the hammer
was performed by placing the core specimens in the cradle and impacting the hammer vertically
vertically along the drawn lines, starting from line No1 (Figure 4). In this manner, five individual
along the drawn lines, starting from line No1 (Figure 4). In this manner, five individual impacts were
impacts were conducted at equal spacing and consequently five rebound values RL were recorded
conducted at equal spacing and consequently five rebound values RL were recorded along the first
along the first line drawn. Then, the same procedure was repeated by rotating◦the specimen 45°. In
line drawn. Then, the same procedure was repeated by rotating the specimen 45 . In total, depending
total, depending on the number of the specimens used, 40 rebound values for each specimen and 240
on the number of the specimens used, 40 rebound values for each specimen and 240 or 280 for each
or 280 for each material were recorded. The rebound values given in this study for each material are
material were recorded. The rebound values given in this study for each material are the average of all
the average of all recorded values.
recorded values.
After the execution of non-destructive tests, the cylindrical specimens were used for the determination
of their uniaxial compressive strength (UCS) and tangent modulus of elasticity (Et). The uniaxial compression
tests were performed using a 1600 KN hydraulic device, manufactured by MTS (Mechanical Testing System)
corporation (Kalamazoo, MI, USA). According to the procedure, the cylindrical specimens were subjected
to a load acting on both ends (Figure 5a), using a loading rate 0.01 mm/s under displacement control mode;
the failure of specimens occurred in less than 5 min. The peak stress value and the tangent modulus of
elasticity of each specimen were calculated from the complete stress-strain curve (Figure 5b).

Figure 3. Straight parallel lines drawn along the longitudinal axis of each specimen.
vertically along the drawn lines, starting from line No1 (Figure 4). In this manner, five individual
impacts were conducted at equal spacing and consequently five rebound values RL were recorded
along the first line drawn. Then, the same procedure was repeated by rotating the specimen 45°. In
total, depending on the number of the specimens used, 40 rebound values for each specimen and 240
or 280
Appl. Sci.for each
2018, material were recorded. The rebound values given in this study for each material
8, 220 5 ofare
17
the average of all recorded values.

Appl. Sci. 2018, 8, x FOR PEER REVIEW 5 of 18

Figure 3. Straight parallel lines drawn along the longitudinal axis of each specimen.
Figure 3. Straight parallel lines drawn along the longitudinal axis of each specimen.
Appl. Sci. 2018, 8, x FOR PEER REVIEW 5 of 18

Figure 4. The Schmidt hammer rebound test.

After the execution of non-destructive tests, the cylindrical specimens were used for the
determination of their uniaxial compressive strength (UCS) and tangent modulus of elasticity (Et).
The uniaxial compression tests were performed using a 1600 KN hydraulic device, manufactured by
MTS (Mechanical Testing System) corporation (Kalamazoo, MI, USA). According to the procedure,
the cylindrical specimens were subjected to a load acting on both ends (Figure 5a), using a loading
rate 0.01 mm/s under displacement control mode; the failure of specimens occurred in less than 5
min. The peak stress value and the4.tangent
Figure modulus
The Schmidt of elasticity
hammer of each specimen were calculated
rebound test.
Figure
from the complete stress-strain 4. The
curve Schmidt
(Figure 5b).hammer rebound test.
After the execution of non-destructive tests, the cylindrical specimens were used for the
determination of their uniaxial compressive strength (UCS) and tangent modulus of elasticity (Et).
The uniaxial compression tests were performed using a 1600 KN hydraulic device, manufactured by
MTS (Mechanical Testing System) corporation (Kalamazoo, MI, USA). According to the procedure,
the cylindrical specimens were subjected to a load acting on both ends (Figure 5a), using a loading
rate 0.01 mm/s under displacement control mode; the failure of specimens occurred in less than 5
min. The peak stress value and the tangent modulus of elasticity of each specimen were calculated
from the complete stress-strain curve (Figure 5b).

(a) (b)
Figure 5. (a) Cylindrical specimen subjected to loading; (b) Stress-strain curve for the determination
Figure 5. (a) Cylindrical specimen subjected to loading; (b) Stress-strain curve for the determination of
of UCS and Et.
UCS and Et .

For the determination of the breakage rate parameters, experiments were performed in a
laboratory-scale ball mill with a volume of 5423 cm3 (Table 2) operating at a constant speed of Ν = 66
rpm (1.1 Hz), which is 70% of its critical speed. The core samples as well as other materials with the
same properties (porosity, density, mineralogy etc.) were crushed and prepared for the grinding tests.
The mill charge consisted of(a) 25.4 mm (1 inch) stainless steel (b)
balls with density ρb = 7.85 g/cm3. The
parameters J (ball filling volume) and fc (material filling volume), were calculated from Equations (4)
Figure 5. (a) Cylindrical specimen subjected to loading; (b) Stress-strain curve for the determination
andof(5), respectively.
UCS and Et.
1
Appl. Sci. 2018, 8, 220 6 of 17

For the determination of the breakage rate parameters, experiments were performed in
a laboratory-scale ball mill with a volume of 5423 cm3 (Table 2) operating at a constant speed of
N = 66 rpm (1.1 Hz), which is 70% of its critical speed. The core samples as well as other materials
with the same properties (porosity, density, mineralogy etc.) were crushed and prepared for the
grinding tests. The mill charge consisted of 25.4 mm (1 inch) stainless steel balls with density
ρb = 7.85 g/cm3. The parameters J (ball filling volume) and fc (material filling volume), were calculated from
Equations (4) and (5), respectively.
 
Volume o f solid balls 1
J= · (4)
mill volume 1−ε
 
Volume o f solid material 1
fc = · (5)
mill volume 1−ε
where, ε is the bed porosity of balls and material (assumed to be 40%) [15].
The material filling volume fc was kept constant at 4%, corresponding to 345.0 g, 351.5 g, 342.5 g and
273.3 g of quartz, marble, quartzite and metasandstone, respectively. The fraction of the space between the
balls at rest that is filled with material (interstitial filling, U) was calculated from Equation (6); in this study,
U was kept constant at 0.5.
fc
U= (6)
0.4· J
Four mono-size fractions of each material (−3.35 + 2.36 mm), (−1.7 + 1.18 mm), (−0.850 + 0.600 mm)
and (−0.425 + 0.300 mm) were ground in a laboratory ball mill for various grinding times t (0.5, 1, 2, 4 min).
√ products obtained after each grinding time t were wet sieved using a series of screens with a ratio of
The
2 for the determination of particle size distribution. It should be noted that fresh feed was used in each
test and the mill was loaded using successive layers of balls and feed [50].

Table 2. Grinding conditions.

Mill Balls Material

diameter, D (cm) 20.4 diameter, d (mm) 25.4 quartz (2.65)
length, L (cm) 16.6 number 77 marble (2.72)
volume, V (cm3 ) 5423 weight (g) 5149 density (g/cm3 ) quartzite (2.59)
metasandstone
operational speed, N (rpm) 66 density (g/cm3 ) 7.85
(2.11)
material filling
critical speed, Nc (rpm) 93.7 porosity (%) 40 4
volume, f c (%)
interstitial filling,
ball filling volume, J (%) 20 50
U (%)

3. Results and Discussion

3.1. P-Wave Velocity of Materials

The P-wave velocity for each material is shown in Figure 6 in Box and Whisker plots which were
designed with the use of Statistica v.10 software (StatSoft Inc., Tulsa, OK, USA). In these plots the central
rectangle spans the first to the third quartile, while the segment inside the rectangle represents the median
(second quartile). Whiskers above and below the rectangle show the maximum and minimum values
and identify the non-outlier range. Any value outside that range is plotted as independent point and is
called outlier.
Appl. Sci. 2018, 8, 220 7 of 17
Appl. Sci. 2018, 8, x FOR PEER REVIEW 7 of 18

Appl. Sci. 2018, 8, x FOR PEER REVIEW

7 7 of 18

P-wave velocity Vp, km/s

6
9

5
8
4

7
P-wave velocity Vp, km/s

Median 25%-75% Non-Outlier Range Outliers

6 2
Quartz Marble Quartzite Metasandstone

5 Figure
Figure 6. P-wavevelocity
6. P-wave velocity ofofallall
materials used.used.
materials
3.2. Schmidt Rebound Values
4
Figure 6 Theshows thatrebound
Schmidt outliers are are
values present,
shown in just below
Figure 7. It the minimum
is seen value,
that outliers, more only for
clear in quartz and
this
quartzite. case,
It is also observed
are present only that the descending
for marble and quartzite.order
It isof materials
also observedwith respect
that the to theorder
descending medianof Vp value
3
is quartz, materials
marble,with respect and
quartzite to themetasandstone.
median RL value is Thequartz, quartzite, results
statistical marble and metasandstone.
of P-wave The also show
velocity
statistical results of RMedian
for the25%-75% Non-Outlier
materials Range Outliers
tested also
that the mean Vp values of Lthe
2 as materials follow theshow
samethat the mean RL values follow the same
order as the median values. Furthermore,
descending order observed for the median values. Finally, it is also indicated that the values
low standard deviation
obtained is observed
in this study for Vpthefor
Quartz
are well within all the
Marble
range materials
Quartzite
of values reportedtested and
Metasandstone
in other thusfor
studies thequartz
dataandare clustered
around thequartzite Vp values.
mean [54], marble [55]It isand
also mentioned[56].
metasandstone that similar values were obtained in other studies for
Figure 6. P-wave velocity of all materials used.
marble and quartzite [51], sandstone [52] and quartz [53].
65

3.2.
3.2. Schmidt
Schmidt Rebound
Rebound Values
Values60
The Schmidt rebound
The Schmidt rebound55values
valuesare
areshown
showninin Figure
Figure 7. 7. It seen
It is is seen
thatthat outliers,
outliers, moremore
clearclear in case,
in this this
case, are present
are present only foronly for marble
marble and quartzite.
and quartzite. It is alsoItobserved
is also observed that the descending
that the descending order of
order of materials
Schmidt rebound values, RL

50
materials with respect to the median R L value is quartz, quartzite, marble and metasandstone. The
with respect to the median RL value is quartz, quartzite, marble and metasandstone. The statistical
statistical
results of R results of RL for45the materials tested also show that the mean RL values follow the same
L for the materials tested also show that the mean RL values follow the same descending
descending order as
order as observed forobserved
the median
40
forvalues.
the median
Finally,values. Finally,
it is also it is that
indicated also the
indicated that the values
values obtained in this
obtained
study are well within the35range of values reported in other studies for quartz andfor
in this study are well within the range of values reported in other studies quartz [54],
quartzite and
quartzite [54], marble [55] and
marble [55] and metasandstone [56]. metasandstone [56].
30

65
25

Median 25%-75% Non-Outlier Range Outliers

60 20
Quartz Marble Quartzite Metasandstone

55
Figure 7. Schmidt rebound values (RL) of all materials used.
Schmidt rebound values, RL

50
3.3. Uniaxial Compressive Strength and Modulus of Elasticity
The statistical results of UCS and Et for each material are shown in Tables 3 and 4, respectively.
45
Table 3 shows that the descending order of materials with respect to the mean UCS value is quartz,
quartzite, marble and metasandstone. As far as the modulus of elasticity (Et) is concerned, the
40
descending order of materials with respect to the mean Et value is quartz, marble, quartzite and
metasandstone (Table 4); this indicates, as expected, that quartz is the stiffest material and thus more
35

30

25

Median 25%-75% Non-Outlier Range Outliers

20
Quartz Marble Quartzite Metasandstone

Schmidt rebound values (RLL)) of

Figure 7. Schmidt of all
all materials
materials used.
used.

3.3. Uniaxial Compressive Strength and Modulus of Elasticity

The statistical results of UCS and Et for each material are shown in Tables 3 and 4, respectively.
Table 3 shows that the descending order of materials with respect to the mean UCS value is quartz,
quartzite, marble and metasandstone. As far as the modulus of elasticity (Et) is concerned, the
descending order of materials with respect to the mean Et value is quartz, marble, quartzite and
Appl. Sci. 2018, 8, 220 8 of 17

3.3. Uniaxial Compressive Strength and Modulus of Elasticity

The statistical results of UCS and Et for each material are shown in Tables 3 and 4, respectively. Table 3
shows that the descending order of materials with respect to the mean UCS value is quartz, quartzite,
marble and metasandstone. As far as the modulus of elasticity (Et) is concerned, the descending order
of materials with respect to the mean Et value is quartz, marble, quartzite and metasandstone (Table 4);
this indicates, as expected, that quartz is the stiffest material and thus more resistant to deformation. Similar
UCS values have been reported in other studies for quartz [57], quartzite [58], marble and sandstone [59].

Table 3. The statistical results of uniaxial compressive strength (UCS) (MPa).

Material Observations Mean Minimum Maximum Median Std. Dev.

Quartz 7 135.1 122.0 151.5 132.0 12.4
Marble 8 68.0 58.6 100.4 63.5 13.7
Quartzite 7 80.9 68.0 110.0 76.7 15.4
Metasandstone 7 57.6 42.6 74.6 64.0 14.0

Table 4. The statistical results of Et (GPa).

Material Observations Mean Minimum Maximum Median Std. Dev.

Quartz 7 59.5 47.5 71.2 62.8 9.1
Marble 8 48.2 21.5 64.9 53.0 15.8
Quartzite 7 41.7 26.7 56.2 44.8 11.0
Metasandstone 7 27.1 10.7 39.0 31.0 10.9

3.4. Breakage Rate Parameters

Figure 8a–d shows in normal-log plots the relationship between the remaining mass fraction of each
feed size vs. grinding time for all materials used. The feed size is the upper size of the tested size fractions.
The results indicate that breakage follows a first order law i.e., the breakage rate Si is independent of time
and the Si values can be determined from the slope of the straight lines. Each line refers to a different
feed size. Figure 9 shows on log–log scale the variation of Si values, obtained from the first order plots,
with the upper feed particle size. It is shown that for each material Si increases up to a specified size xm
(optimum feed size), but above this size breakage rates decrease sharply, since particles are too large to
be nipped and fractured by the grinding media used. The optimum size xm for each material is the size
at which, under normal grinding conditions, the highest breakage rate Sm is reached. It is mentioned that
the breakage rate parameters were back calculated using the Moly-Cop Tools™ v.1.0 software and the
determined values are presented in Table 5. The back calculation method is described in detail in a previous
recent publication of the authors [8].

Table 5. Breakage rate parameters for all materials used.

Si αT α Sm xm
Material
min−1 min−1 min−1 mm
Quartz 0.55 0.68 0.80 0.85 1.80
Marble 0.89 1.09 0.90 1.83 2.84
Quartzite 0.83 0.98 0.84 1.29 2.00
Metasandstone 1.05 1.41 1.12 2.45 2.32
 line refers to a different feed size. Figure 9 shows on log–log scale the variation of Si values, obtained
from the first order plots, with the upper feed particle size. It is shown that for each material Si
increases up to a specified size xm (optimum feed size), but above this size breakage rates decrease
sharply, since particles are too large to be nipped and fractured by the grinding media used. The
optimum size xm for each material is the size at which, under normal grinding conditions, the highest
breakage rate Sm is reached. It is mentioned that the breakage rate parameters were back calculated
using the Moly-Cop Tools™ v.1.0 software and the determined values are presented in Table 5. The
Appl. Sci. 2018, 8, 220 9 of 17
back calculation method is described in detail in a previous recent publication of the authors [8].

100 100

Mass % remaining, mi (t)

Mass % remaining, mi (t)
Quartz Marble
10

10 1

Appl. Sci. 2018, 8, x FOR PEER REVIEW 0.1 9 of 18

1 0.01
0 2 4 6 8 0 2 4 6 8
100
Appl. Sci. 2018, 8, x FOR Grinding
PEER REVIEW
time, min 9 of 18
100 Grinding time, min
Mass % remaining, mi (t)

Mass % remaining, mi (t)

(a)Quartzite (b) Metasandstone
10
100
10 100
Mass % remaining, mi (t)

Mass % remaining, mi (t)

Quartzite 1 Metasandstone
10
10
1 1 0.1
0.1
1 0.01
0.01
0.1 0.001
0.1 0.001
0 2 4 6 8 0 2 4 6 8
0 2 4 6 8 0 2 4 6 8
Grinding time, time,
Grinding minmin Grinding
Grinding time, min time, min
(c) (c) (d) (d)
Figure 8. First order plots showing the mass % remaining for each size fraction of each material vs.
FigureFigure 8.
8. First First
order order
grindingplots
plots showing
showing
time; (a) thethe
mass
quartz, (b) marble,
mass%%remaining
remaining
(c) quartzite
for each
for eachsize
and (d) metasandstone. sizefraction of of
fraction each eachmaterial vs.
material vs.
grinding time; time;
grinding (a) quartz,
(a) quartz, (b) marble,
(b) marble, (c) (c) quartziteand
quartzite and(d)
(d)metasandstone.
metasandstone.
10
Quartz
Breakage rate Si, min-1

Marble
10
Quartz
Quartzite
Breakage rate Si, min-1

Metasandstone
Marble
1
Quartzite
Metasandstone

1
0.1
0.1 1 10
Upper feed particle size, mm

Figure 9. Variation of breakage rate Si vs. upper feed particle size.

0.1
0.1 1 10
Table 5. Breakage rate parameters for all materials used.
Upper feed particle size, mm
Si αΤ α Sm xm
Material
min−1 rate
min−1Si vs. upper
min−1feed
mm
Figure 9. Variation of breakage
Figure 9. Variation of breakage rate Si vs. upper feedparticle size.
particle size.
Quartz 0.55 0.68 0.80 0.85 1.80
Marble 0.89 1.09 0.90 1.83 2.84
Table 5.Quartzite
Breakage rate parameters
0.83 0.98 Rate
for all1.29
materials
0.84Parameters2.00
used.
3.5. Correlation between Material Properties and Breakage
Metasandstone 1.05 1.41 1.12 2.45 2.32
Si αΤ α Sm xm
Material
3.5.1. Simple Regression
3.5. CorrelationAnalysis
between Material Propertiesmin −1 min
and Breakage −1
Rate Parametersmin−1 mm
Quartz 0.55 0.68 0.80 0.85 1.80
In the first3.5.1.
part of Regression
Simple this study simple regression analysis involving one dependent and one
Analysis
Marble 0.89 1.09 0.90 1.83 2.84
independent variable was
In the carried
first out,study
part of this while Excel
simple software
regression was used to establish
dependent potential correlations
Quartzite 0.83 0.98analysis0.84involving
1.29 one 2.00 and one
between material independent
properties variable
andwasbreakage
carried out,rate whileparameters.
Excel software was used to
During thisestablish
part, potential
linear or non-linear
correlations between Metasandstone
material properties 1.05and breakage 1.41rate 1.12
parameters.2.45
During 2.32this part, linear or
functions were non-linear
used and the equation with the highest correlation coefficient R 2 was considered for
functions were used and the equation with the highest correlation coefficient R was 2

determining theconsidered
3.5. Correlationbreakage
betweenfor determining the breakageand
rate parameters
Material Properties rate ,parameters
(SiBreakage
αT , α, RateS(Smi, αand
Τ, α, Sm and xm). It is mentioned that no
xm ). It is mentioned that no similar
Parameters
similar functions are given so far in other studies in literature.
functions are givenThe socorrelations
far in other studies in literature.
between Si values and Vp, RL, UCS and Et are presented in Figure 10. It is seen
3.5.1.
The SimplethatRegression
correlations verybetween Analysis
Si values
strong correlation between and VpR,L R
Si and (RL2 ,= UCS
0.98) andand Et correlations
strong are presented betweenin Si Figure
and Vp 10. It is seen
(R2 = 0.85) and Et (R2 = 0.85) are obtained with the 2 use of inverse linear functions. Furthermore, Si is
that very strong correlation
In thevery
first part of between
this study
well correlated with UCS with
Si simple
and R regression
(R = 0.98) and strong
analysis correlations
involving
the useLof an inverse exponential function (R2 = 0.99).
one dependentbetween andSi one
and Vp
(R2 = 0.85)
independent
and Et (R 2 = 0.85)
variable wasarecarried
obtained out,with whilethe Excel
use ofsoftware was used
inverse linear to establish
functions. potentialSi is
Furthermore,
correlations
very well correlated between
with UCS materialwithproperties
the use of and anbreakage
inverse rate parameters.
exponential During(Rthis
function 2 = part,
0.99).linear or
non-linear functions were used and the equation with the
Similar results are obtained for the correlations between αT and Vp , RL , UCS and Et (Figure highest correlation coefficient R2 was 11).
considered for determining the breakage rate parameters (Si, αΤ, α, Sm and xm). It is mentioned that no
Parameter αT , which defines the breakage rate for a feed size of 1 mm, is correlated very well with Vp ,
similar functions are given so far in other studies in literature.
RL and Et using an inverse linear relationship. The very strong correlation (R2 = 1) between αT and
The correlations between Si values and Vp, RL, UCS and Et are presented in Figure 10. It is seen
RL is considered verycorrelation
that very strong importantbetween for the Sdesign of grinding circuits. RL values are
i and RL (R2 = 0.98) and strong correlations
obtained
between from
Si and Vp the
application of the convenient and low-cost Schmidt hammer test, which
(R2 = 0.85) and Et (R2 = 0.85) are obtained with the use of inverse linear functions. Furthermore, Si is can be used both in laboratory
and invery
industrial mills, thus
well correlated enabling
with UCS with the theuse determination of breakage
of an inverse exponential rate for
function (R2a=specific
0.99). material in
a grinding circuit.
 Breakage rate Si
Breakage rate S
0.5 0.5

0 0
Appl. Sci. 2018, 8, 2200 5 10 10 30 50 70 10 of 17
Appl. Sci. 2018, 8, x FOR PEER REVIEW Schmidt rebound values RL 10 of 18
P-wave velocity Vp, km/s
(a) (b)
1.5 1.5
2 2
y = -0.10x + 1.41 y = -0.02x + 1.74
Breakage rate Si, min-1

min-1
-1
y = 21.00x-0.74 R² = 0.85 y = -0.01x + 1.46 R² = 0.98

Breakage rate Si, min-1

rateSSi,i,min
R² = 0.99 R² = 0.85
1 1

Breakagerate
1 1

0.5 0.5

Breakage
0 0
0 0
20 70 120 170 10 30 50 70 90
0 5 10 10
Tangent 30 of elasticity50
modulus Et, GPa 70
Uniaxial compressive strength UCS, MPa
P-wave velocity Vp, km/s Schmidt rebound values RL
(c) (d)
(a) (b)
Figure 10. Correlations between breakage rate Si and (a) P-wave velocity Vp, (b) Schmidt rebound
2 2
values RL, (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et; horizontal

Breakage rate Si, min-1

y = 21.00x -0.74
y = -0.01x + 1.46
Breakage rate Si, min-1

error bars show standard deviation of the measurements.

R² = 0.99 R² = 0.85

Similar results are obtained for the correlations between αΤ and Vp, RL, UCS and Et (Figure 11).
1 1
Parameter αΤ, which defines the breakage rate for a feed size of 1 mm, is correlated very well with Vp,
RL and Et using an inverse linear relationship. The very strong correlation (R2 = 1) between αT and RL
is considered very important for the design of grinding circuits. RL values are obtained from the
application
0 of the convenient and low-cost Schmidt hammer 0 test, which can be used both in
laboratory20 and in 70 industrial 120
mills, thus170enabling the determination 10 of 30
breakage 50 rate for
70 a specific
90
material Uniaxial
in a grinding circuit.
compressive strength UCS, MPa Tangent modulus of elasticity Et, GPa
Figure 12 shows(c) the correlations between parameter α and Vp, RL, UCS(d) and Et. It is seen that
parameter α is very well correlated with Vp, RL and Et with the use of inverse exponential functions.
Figure10.
Parameter 10. Correlations
Correlations
α between
is constantbetween breakage
for the breakage
same rate SSand
material i and (a) P-wave
therefore the velocity
functionsVpobtained
, (b) Schmidt
can be rebound
used
Figure rate i and (a) P-wave velocity Vp , (b) Schmidt rebound
valuesRRL,, (c)
independently
values (c) uniaxial
uniaxial
of compressive
grinding
compressive strength
conditions. UCSand
However,
strength UCS and
a (d)tangent
tangent
moderate
(d) modulus(R
correlation
modulus ofelasticity
of
2 elasticity
= 0.67) E;t;horizontal
between
E horizontal
α and
L t
UCS
erroris indicated.
bars show standard deviation of the measurements.
error bars show standard deviation of the measurements.

Similar results
2 are obtained for the correlations between 2 αΤ and Vp, RL, UCS and Et (Figure 11).
Parameter αΤ, which defines the breakage rate for a feed size of 1 mm, is correlated
y = -0.15x + 1.90 y = -0.03x + 2.37
very well with Vp,
R² = 0.88 R² = 1.00
parameter αΤ, min-1

Parameter αΤ, min-1

RL and Et using an inverse linear relationship. The very strong correlation (R2 = 1) between αT and RL
is considered 1very important for the design of grinding circuits. 1 RL values are obtained from the
application of the convenient and low-cost Schmidt hammer test, which can be used both in
laboratory and in industrial mills, thus enabling the determination of breakage rate for a specific
material in a grinding circuit. 0
0
Figure 12 shows 0 the correlations
5 between
10 parameter α10and Vp,30RL, UCS50and Et. 70It is seen that
Appl. Sci. 2018, 8, x FOR PEERvelocity
REVIEW Schmidt rebound values RL 11 of 18
parameter α is very P-wave well correlated Vp, km/s
with Vp, RL and Et with the use of inverse exponential functions.
Parameter α is constant for (a) the same material and therefore the functions (b) obtained can be used
2 2
independently of grinding conditions. However, a moderate correlation (R2 = 0.67) between α and
y = -0.02x + 1.96
UCS is indicated. R² = 0.88
Parameter αΤ, min-1

Parameter αΤ, min-1

1 1
2 2
y = 34.72x-0.81
y = -0.15x + 1.90 y = -0.03x + 2.37
R² = 0.97 R² = 0.88 R² = 1.00
parameter αΤ, min-1

Parameter αΤ, min-1

0 0

1 20 70 120 170 110 30 50 70 90

Tangent modulus of elasticity Et, GPa
Uniaxial compressive strength UCS, MPa
(c) (d)
Figure 11. Correlations between parameter αΤ and (a) P-wave velocity Vp, (b) Schmidt rebound values
Figure 011. Correlations between parameter αT and (a) P-wave velocity
0 Vp , (b) Schmidt rebound values
RL, (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et; horizontal error
RL , (c) uniaxial
0 compressive
5 strength UCS 10
10 and (d) tangent modulus 30
of elasticity 50
Et ; horizontal 70
error
bars show standard deviation of the measurements. Schmidt rebound values RL
P-wave velocity V , km/s
bars show standard deviation ofp the measurements.
(a) (b)
1.2 1.5
y= 1.74x-0.38 y = 9.29x-0.62
1 R² = 0.85 R² = 0.93
Parameter α

1
Parameter α

0.8

0.5
0.6

0.4 0
Appl. Sci. 2018, 8, 220 11 of 17

Figure 12 shows the correlations between parameter α and Vp , RL , UCS and Et . It is seen that parameter
α is very well correlated with Vp , RL and Et with the use of inverse exponential functions. Parameter α is
Appl. Sci. 2018, 8, x FOR PEER REVIEW 11 of 18
constant for the same material and therefore the functions obtained can be used independently of grinding
conditions. However, a moderate correlation (R2 = 0.67) between α and UCS is indicated.
2 2
The correlations between maximum breakage rate Sm and Vp , RL , UCS and Et are presented in
y = -0.02x + 1.96
Figure 13. Very strong correlation (R2 = 0.96) is shown between Sm and RL with the R² = use
0.88 of an inverse
Parameter αΤ, min-1

Parameter αΤ, min-1

linear function. Furthermore, Sm seems to follow an inverse exponential relationship with UCS, with
correlation1 coefficient R2 = 0.95. However, the prediction of1 Sm from Vp and Et values is somehow
risky due to the moderate correlation between these variables.
y = 34.72x-0.81
Figure 14 shows the correlations between the optimum size xm and Vp , RL , UCS and Et . It is
R² = 0.97
seen that weak correlations exist between xm and Vp (R2 = 0.08) 0
as well as Et (R2 = 0.09) when inverse
0
functions are 20 used. Furthermore,
70 120 similar results between xm and
170 10 RL or 30 UCS50 are also 70 obtained,
90 with
R2 0.35 and 0.57, respectively. It is mentioned
Uniaxial compressive strength UCS, MPa that very good to excellent correlations
Tangent modulus between
of elasticity Et, GPa optimum

size xm and other variables (c) are obtained, if marble is excluded from regression (d) analysis. Thus, it is
deduced that the optimum size xm increases with decreasing P-wave velocity, Schmidt rebound value,
Figure
uniaxial 11. Correlations
compressive between
strength andparameter
tangent αΤ and (a) P-wave velocity Vp, (b) Schmidt rebound values
modulus of elasticity, for all materials tested except for
RL, (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et; horizontal error
marble. It is therefore obvious that as strength or stiffness of a material increases the optimum size
bars show standard deviation of the measurements.
at which the breakage rate obtains its maximum value becomes finer.

1.2 1.5
y = 1.74x-0.38 y = 9.29x-0.62
1 R² = 0.85 R² = 0.93
Parameter α

1
Parameter α

0.8

0.5
0.6

0.4 0
0 5 10 10 30 50 70
P-wave velocity Vp, km/s Schmidt rebound values RL
(a) (b)
1.2 1.2
y = 3.86x-0.33 y = 4.25x-0.41
1 R² = 0.67 R² = 0.85
1
parameter α
Parameter α

0.8
0.8
0.6
0.6
0.4

0.2 0.4
20 70 120 170 10 30 50 70 90
Uniaxial compressive strength UCS, MPa Tangent modulus of elasticity Et, GPa

(c) (d)
Figure12.
Figure 12. Correlations
Correlations between
betweenparameter
parameterααand
and(a)
(a)P-wave
P-wavevelocity
velocityVVp,, (b)
(b) Schmidt
Schmidt rebound
rebound values
values
p
R L, (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et; horizontal error
RL , (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et ; horizontal error
barsshow
bars showstandard
standarddeviation
deviationof
ofthe
themeasurements.
measurements.

The correlations between maximum breakage rate Sm and Vp, RL, UCS and Et are presented in
Figure 13. Very strong correlation (R2 = 0.96) is shown between Sm and RL with the use of an inverse
linear function. Furthermore, Sm seems to follow an inverse exponential relationship with UCS, with
correlation coefficient R2 = 0.95. However, the prediction of Sm from Vp and Et values is somehow risky
due to the moderate correlation between these variables.
 2 2

Sm, min-1

Sm, min-1
1 1

Appl. Sci. 2018, 8, 0220 0 12 of 17

Appl. Sci. 2018, 8, x FOR PEER REVIEW 12 of 18
0 5 10 10 30 50 70
P-wave velocity Vp, km/s Schmidt rebound values RL
3 (a) 3 (b)
y = -0.31x + 3.42 y = -0.07x + 4.59
3 R² = 0.74 3 R² = 0.96
2 y = -0.04x + 3.56
2 y = 297.79x-1.21
Sm, minS-1m, min-1 R² = 0.75

S , min-1
R² = 0.95
2 2

-1
m
1 1

Sm, min
1 1
0 0
0 5 10 10 30 50 70
0 P-wave velocity Vp, km/s 0 Schmidt rebound values RL
20 70 120 170 0 20 40 60 80
(a) strength UCS, MPa
Uniaxial compressive (b) of elasticity E , GPa
Tangent modulus t

3 (c) 3 (d)
y = -0.04x + 3.56
y = 297.79x-1.21
Figure 13. Correlations between R² V
maximum breakage rate Sm and (a) P-wave velocity =p0.75
, (b) Schmidt
R² = 0.95
rebound
2 values RL, (c) uniaxial compressive strength UCS and
2 (d) tangent modulus of elasticity Et;

Sm, min-1
Sm, min-1

horizontal error bars show standard deviation of the measurements.

1 1
Figure 14 shows the correlations between the optimum size xm and Vp, RL, UCS and Et. It is seen
that weak correlations exist between xm and Vp (R2 = 0.08) as well as Et (R2 = 0.09) when inverse
functions0are used. Furthermore, similar results between xm0 and RL or UCS are also obtained, with R2
20 70 120 170 0 20 40 60 80
0.35 and 0.57, respectively. It is mentioned that very good to excellent
Uniaxial compressive strength UCS, MPa
correlations
Tangent modulus between
of elasticity optimum
Et, GPa
size xm and other variables (c) are obtained, if marble is excluded from regression (d) analysis. Thus, it is
deduced that the optimum size xm increases with decreasing P-wave velocity, Schmidt rebound value,
Figure
uniaxial 13. Correlations between maximum breakage
modulusrate Sm and (a) P-wave velocity Vp,tested
(b) Schmidt for
Figure 13.compressive
Correlationsstrength
betweenand tangentbreakage
maximum of elasticity,
rate Sm and (a)for all materials
P-wave velocity Vp , (b)except
Schmidt
rebound values RL, obvious
(c) uniaxial compressive strength UCS of
and (d) tangent modulusthe of optimum
elasticity Esize
t;
rebound values RL , (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Eatt ;
marble. It is therefore that as strength or stiffness a material increases
horizontal
which the error error
breakage bars show standard deviation of the measurements.
horizontal bars rate
show obtains
standardits maximum
deviation ofvalue becomes finer.
the measurements.
Figure 14 shows the correlations between the optimum size xm and Vp, RL, UCS and Et. It is seen
that weak3 correlations exist between xm and Vp (R2 = 0.08)3 as well as Et (R2 = 0.09) when inverse
functions are used. Furthermore, similar results between xm and RL or UCS are also obtained, with R2
0.35 and 0.57,
2
respectively. It is mentioned that very good to2excellent correlations between optimum
size xm and other variables are obtained, if marble is excluded from regression analysis. Thus, it is
xm, mm

xm, mm

y = 14.69x -0.50
deduced that the optimum sizey x=m2.90xincreases
-0.16 with decreasing P-wave velocity, Schmidt rebound value,
R² = 0.35
uniaxial compressive
1 strength and tangent modulus of elasticity,
R² = 0.08 1 for all materials tested except for
marble. It is therefore obvious that as strength or stiffness of a material increases the optimum size at
which the breakage rate obtains its maximum value becomes finer.
0 0
0 5 10 10 30 50 70
Appl. Sci. 2018,
3 8, x P-wave
FOR PEER REVIEW
velocity Vp, km/s 3 Schmidt rebound values RL 13 of 18

(a) (b)
3 3
2 2
xm, mm xm, mm

xm, mm xm, mm

y = 14.69x-0.50
2 y = 2.90x-0.16 2 R² = 0.35
1 R² = 0.08 1
y = 13.15x-0.41
R² = 0.57 y = 4.28x-0.18
1 1 R² = 0.09
0 0
0 5 10 10 30 50 70

P-wave velocity Vp, km/s Schmidt rebound values RL

0 0
20 70 120 170
(a) 10 30 (b)50 70 90
Uniaxial compressive strength UCS, MPa Tangent modulus of elasticity Et, GPa

(c) (d)
Figure 14. Correlations between optimum size xm and (a) P-wave velocity Vp, (b) Schmidt rebound
Figure 14. Correlations between optimum size xm and (a) P-wave velocity Vp , (b) Schmidt rebound
values RL, (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et; horizontal
values RL , (c) uniaxial compressive strength UCS and (d) tangent modulus of elasticity Et ; horizontal
error bars show standard deviation of the measurements.
error bars show standard deviation of the measurements.
The results for marble are indeed peculiar. It is known that the behavior of a material during
breakage depends on several factors including mainly rock size, grain size and microstructure,
crystallinity, porosity, mixtures of grinding media, presence of secondary mineral phases and
microcracks [26,60,61]. In addition, breakage of mineral grains may be affected by the presence of
inter-granular cementations [62]. Furthermore, the energy required for plastic deformation is
different for each material and this affects breakage rate [63]. In a recent study, a spheroid model was
used to identify the role of shape in particle size analysis [64]. One major difference between marble
and the other three materials examined in our study is that the formation of marble is the result of
Appl. Sci. 2018, 8, 220 13 of 17

The results for marble are indeed peculiar. It is known that the behavior of a material during
breakage depends on several factors including mainly rock size, grain size and microstructure,
crystallinity, porosity, mixtures of grinding media, presence of secondary mineral phases and
microcracks [26,60,61]. In addition, breakage of mineral grains may be affected by the presence
of inter-granular cementations [62]. Furthermore, the energy required for plastic deformation is
different for each material and this affects breakage rate [63]. In a recent study, a spheroid model
was used to identify the role of shape in particle size analysis [64]. One major difference between
marble and the other three materials examined in our study is that the formation of marble is the
result of metamorphism of sedimentary carbonate rocks, mainly limestones or dolomites. Twinning
planes (planes along which two crystals meet) are also present in marbles. Furthermore, during
grinding of marble ultra-fine particles are generated and this may affect breakage rate and final
particle size distribution. In a recent study, it has been shown that the initial breakage rate of
coarse particles increases with increasing proportion of fines in the mixture; the presence of a big
proportion of fines indicates that they exhibit a much smaller collision cross-section compared to
coarser particles [65]. All these factors definitely affect the behavior of marble during breakage and
thus additional experimental studies are required to elucidate this aspect.

3.5.2. Multiple Regression Analysis

Multiple regression analysis is an extension of simple regression analysis and involves one
dependent and two or more independent variables [66]. In our study, multiple regression analysis
was performed, using two independent variables, to identify correlations between breakage rate
parameters and Vp , RL , UCS and Et . The correlation matrix for breakage rate parameters (Si , αT , α and
Sm ) and Vp , RL , UCS and Et is shown in Table 6. For each dependent variable the two independent
variables with the highest correlation coefficients, as shown in the correlation matrix, were used to
perform the analysis. Furthermore, because of the weak correlations between optimum size xm and
other variables for all tested materials (Figure 14), this dependent variable was not taken into account
in our study.

Table 6. Correlation matrix for study variables.

Property Si αT α Sm Vp Et RL UCS
Si 1
αT 0.982 1
α 0.856 0.938 1
Sm 0.950 0.983 0.947 1
Vp −0.922 −0.938 −0.886 −0.865 1
Et −0.923 −0.939 −0.886 −0.866 1.000 1
RL −0.990 −0.991 −0.896 −0.983 0.893 0.895 1
UCS −0.977 −0.923 −0.733 −0.888 0.842 0.843 0.956 1

The equations obtained for each dependent variable are the following:

Si = 1.440 − 0.007· R L − 0.002·UCS, R2 = 0.991 (7)

αT = 2.018 − 0.006·T − 0.011· R L , R2 = 0.995 (8)

α = 1.346 − 0.004· R L − 0.036·VP , R2 = 0.838 (9)

Sm = 3.977 − 0.054· R L − 0.012·UCS, R2 = 0.998 (10)

The results of multiple regression analysis indicate that when specific material properties are
considered the breakage rate parameters of silica rich materials, namely quartz, quartzite and
metasandstone, can be well determined. An exception is shown only for parameter xm for marble.
Appl. Sci. 2018, 8, 220 14 of 17

4. Conclusions
In this study, the correlation between the properties of four materials, namely quartz, marble,
quartzite and metasandstone, and breakage rate parameters have been established. The properties of
the materials that were taken into account were P-wave velocity, Schmidt rebound values, uniaxial
compressive strength and tangent modulus of elasticity. The breakage rate parameters that were
determined through batch grinding experiments were breakage rate Si , parameter αT , parameter α,
maximum breakage rate Sm and optimum particle size xm . The results can be summarized as follows:
Breakage rate Si or parameter αT increase with decreasing uniaxial compressive strength (UCS)
and tangent modulus of elasticity (Et ). Therefore, it is deduced that as the strength or stiffness of
a material is reduced this will be ground faster in a mill. Similar results can be obtained from the
P-wave velocity (Vp ) and Schmidt rebound values (RL ), which are widely considered for the indirect
estimation of material’s hardness and strength. The properties of the tested materials can be used for
an accurate prediction of Si or αT of the ground materials since the obtained correlation coefficients
are high.
Parameter α which is constant for the same material and independent of grinding conditions is
well correlated with Vp , RL and Et when inverse exponential functions are used. However, the results
showed that α has a moderate correlation with UCS (R2 = 0.67) and therefore the results of the functions
derived are not very reliable.
Maximum breakage rate Sm is strongly correlated with RL and UCS using inverse functions and
therefore either RL or UCS values can be used to predict the maximum breakage rate of each tested
material during grinding. However, the prediction of Sm from Vp or Et is not fully reliable due to the
moderate correlations between these parameters.
As far as optimum size xm is concerned, the results showed that optimum size xm increases
with decreasing P-wave velocity, Schmidt rebound value, uniaxial compressive strength and tangent
modulus of elasticity. However, marble seems to deviate from this tendency and further research is
required, by considering its properties and other aspects including the presence of twinning planes
and the production of ultra-fine material during grinding, to elucidate its behavior. It is mentioned
that the behavior of mixed materials and the effect of each material type on the overall breakage rate is
now under investigation.

Acknowledgments: The authors would like to thank the anonymous reviewers of this article for their constructive
comments and recommendations. The authors also gratefully acknowledge S. Mavrigiannakis, Mining Engineer,
Faculty of Rock Mechanics Laboratory, Technical University of Crete, for performing the UCS tests.
Author Contributions: Evangelos Petrakis conceived, designed and performed the experiments, analyzed the
data and wrote the paper; Konstantinos Komnitsas critically reviewed the experimental design, the analysis of the
results and wrote the paper.
Conflicts of Interest: The authors declare no conflict of interest.

Nomenclature
D internal diameter of the mill (m)
d ball diameter (mm)
Et tangent modulus of elasticity (GPa)
fc powder filling volume (%)
J ball filling volume (%)
i size class index
N rotational speed (rpm)
Qi correction factor (-)
RL Schmidt hammer rebound value (-)
R2 correlation coefficient (-)
Si breakage rate (min−1 )
Sm maximum breakage rate (min−1 )
t grinding time (min)
Appl. Sci. 2018, 8, 220 15 of 17

U interstitial filling (-)

UCS uniaxial compressive strength (MPa)
Vp P-wave velocity (km/s)
x0 standard size 1 mm
xi the upper size of size class i (mm)
xm optimum feed size (mm)
α parameter depending on material properties (-)
αT parameter depending on milling conditions (-)
ε bed porosity (%)
Λ parameter depending on material properties (-)
µ parameter depending on milling conditions (-)
ρb specific gravity of the balls (g/cm3 )

References
1. Palm, N.A.; Shackleton, N.J.; Malysiak, V.; O’Connor, C.T. The effect of using different comminution
procedures on the flotation of sphalerite. Miner. Eng. 2010, 23, 1053–1057. [CrossRef]
2. Ozkan, S.G. Further Investigations on Simultaneous Ultrasonic Coal Flotation. Minerals 2017, 7, 177. [CrossRef]
3. Batchelor, A.R.; Buttress, A.J.; Jones, D.A.; Katrib, J.; Way, D.; Chenje, T.; Stoll, D.; Dodds, C.; Kingman, S.W.
Towards large scale microwave treatment of ores: Part 2—Metallurgical testing. Miner. Eng. 2017, 111, 5–24.
[CrossRef]
4. Touil, D.; Belaadi, S.; Frances, C. Energy efficiency of cement finish grinding in a dry batch ball mill.
Cem. Concr. Res. 2006, 36, 416–421. [CrossRef]
5. Ipek, H.; Ucbas, Y.; Yekeler, M.; Hosten, Ç. Grinding of ceramic raw materials by a standard Bond mill:
Quartz, kaolin and K-feldspar. Miner. Process. Extr. Metall. 2005, 114, 213–218. [CrossRef]
6. Kutuk, S. Influence of milling parameters on particle size of ulexite material. Powder Technol. 2016, 301,
421–428. [CrossRef]
7. Djordjevic, N. Improvement of energy efficiency of rock comminution through reduction of thermal losses.
Miner. Eng. 2010, 23, 1237–1244. [CrossRef]
8. Petrakis, E.; Stamboliadis, E.; Komnitsas, K. Identification of optimal mill operating parameters during
grinding of quartz with the use of population balance modelling. KONA Powder Part. J. 2017, 34, 213–223.
[CrossRef]
9. Charles, R.J. Energy-size reduction relationships in comminution. Trans. AIME 1957, 208, 80–88.
10. Stamboliadis, E. A contribution to the relationship of energy and particle size in the comminution of brittle
particulate materials. Miner. Eng. 2002, 15, 707–713.
11. Fuerstenau, D.W.; Phatak, P.B.; Kapur, P.C.; Abouzeid, A.-Z.M. Simulation of the grinding of coarse/fine
(heterogeneous) systems in a ball mill. Int. J. Miner. Process. 2011, 99, 32–38. [CrossRef]
12. Shi, F.; Kojovic, T.; Brennan, M. Modelling of vertical spindle mills. Part 1: Sub-models for comminution and
classification. Fuel 2015, 143, 595–601. [CrossRef]
13. Petrakis, E.; Komnitsas, K. Improved modeling of the grinding process through the combined use of matrix
and population balance models. Minerals 2017, 7, 67. [CrossRef]
14. Herbst, J.A.; Fuerstenau, D.W. Scale-up procedure for continuous grinding mill design using population
balance models. Int. J. Miner. Process. 1980, 7, 1–31. [CrossRef]
15. Austin, L.G.; Klimpel, R.R.; Luckie, P.T. Process Engineering of Size Reduction: Ball Milling; SME-AIME:
New York, NY, USA, 1984.
16. Ipek, H.; Göktepe, F. Determination of grindability characteristics of zeolite. Physicochem. Probl. Miner. Process.
2011, 47, 183–192.
17. Gupta, V.K.; Sharma, S. Analysis of ball mill grinding operation using mill power specific kinetic parameters.
Adv. Powder Technol. 2014, 25, 625–634. [CrossRef]
18. Fuerstenau, D.W.; Kapur, P.C.; De, A. Modelling Breakage Kinetics in Various Dry Comminution Systems.
KONA Powder Part. J. 2003, 21, 121–132. [CrossRef]
19. Deniz, V. Comparisons of dry grinding kinetics of lignite, bituminous coal and petroleum coke.
Energy Source Part A 2013, 35, 913–920. [CrossRef]
Appl. Sci. 2018, 8, 220 16 of 17

20. Mulenga, F.K. Sensitivity analysis of Austin’s scale-up model for tumbling ball mills—Part 2. Effects of
full-scale milling parameters. Powder Technol. 2017, 317, 6–12. [CrossRef]
21. Mulenga, F.K. Sensitivity analysis of Austin’s scale-up model for tumbling ball mills—Part 3. A global study
using the Monte Carlo paradigm. Powder Technol. 2017, 322, 195–201. [CrossRef]
22. Mokokha, A.B.; Moys, M.H. Towards optimizing ball-milling capacity: Effect of lifter design. Miner. Eng.
2006, 19, 1439–1445. [CrossRef]
23. Samanli, S.; Cuhadaroglu, D.; Ipek, H.; Ucbas, Y. The investigation of grinding kinetics of power plant solid
fossil fuel in ball mill. Fuel 2010, 89, 703–707. [CrossRef]
24. Samanli, S. Breakage behavior of two different coal types in a grinding process and importance for thermal
power stations. Part. Sci. Technol. 2016. [CrossRef]
25. Katubilwa, F.M.; Moys, M.H. Effect of ball size distribution on milling rate. Miner. Eng. 2009, 22, 1283–1288.
[CrossRef]
26. Simba, K.P.; Moys, M.H. Effects of mixtures of grinding media of different shapes on milling kinetics.
Miner. Eng. 2014, 61, 40–46. [CrossRef]
27. Vogel, L.; Peukert, W. From single particle impact behaviour to modelling of impact mills. Chem. Eng. Sci.
2005, 60, 5164–5176. [CrossRef]
28. Sato, J.; Itoh, J.; Aydan, Ö.; Akagi, T. Prediction of time-dependent behaviour of a tunnel in squeezing rocks.
In Proceedings of the 4th International Symposium, Bergamo, Italy, 10–12 April 1995; pp. 47–54.
29. Kahraman, S. A correlation between P-wave velocity, number of joints and Schmidt hammer rebound
number. Int. J. Rock Mech. Min. Sci. 2001, 38, 729–733. [CrossRef]
30. Yasar, E.; Erdogan, Y. Estimation of rock physiomechanical properties using hardness methods. Eng. Geol.
2004, 71, 281–288. [CrossRef]
31. Karakus, M.; Tutmez, B. Fuzzy and multiple regressions modelling for evaluation of intact rock strength
based on point load, Schmidt hammer and sonic velocity. Rock Mech. Rock Eng. 2006, 39, 45–57. [CrossRef]
32. Kahraman, S.; Yeken, T. Determination of physical properties of carbonate rocks from P-wave velocity.
Bull. Eng. Geol. Environ. 2008, 67, 277–281. [CrossRef]
33. Cobanoglu, I.; Celik, S.B. Estimation of uniaxial compressive strength from point load strength, Schmidt
hardness and P-wave velocity. Bull. Eng. Geol. Environ. 2008, 67, 491–498. [CrossRef]
34. Khandelwal, M.; Singh, T.N. Correlating static properties of coal measures rocks with P-wave velocity.
Int. J. Coal Geol. 2009, 79, 55–60. [CrossRef]
35. Yagiz, S. P-wave Velocity Test for Assessment of Geotechnical Properties of some Rock Materials.
Bull. Mater. Sci. 2011, 34, 947–953. [CrossRef]
36. Sarkar, K.; Vishal, V.; Singh, T.N. An empirical correlation of index geomechanical parameters with the
compressional wave velocity. Geotech. Geol. Eng. 2012, 30, 469–479. [CrossRef]
37. Goktan, R.M.; Gunes, N. A comparative study of Schmidt hammer testing procedures with reference to rock
cutting machine performance prediction. Int. J. Rock Mech. Min. Sci. 2005, 42, 466–472. [CrossRef]
38. ISRM 1978. Suggested methods for determining hardness and abrasiveness of rocks. Int. J. Rock Mech. Min.
Sci. Geomech. Abstr. 1978, 15, 89–97.
39. International Society for Rock Mechanics. The Complete ISRM Suggested Methods for Rock Characterization,
Testing and Monitoring: 1974–2006; Hudson, U., Ed.; ISRM Turkish National Group: Ankara, Turkey, 2007.
40. ASTM. Standard Test Method for Determination of Rock Hardness by Rebound Hammer Method; ASTM D 5873-00;
ASTM International: West Conshohocken, PA, USA, 2001.
41. Buyuksagis, I.S.; Goktan, R.M. The effect of Schmidt hammer type on uniaxial compressive strength
prediction of rock. Int. J. Rock Mech. Min. Sci. 2007, 44, 299–307. [CrossRef]
42. Hucka, V. A rapid method for determining the strength of rocks in situ. Int. J. Rock Mech. Min. Sci. 1965, 2,
127–134. [CrossRef]
43. Poole, R.W.; Farmer, I.W. Consistency and repeatability of Schmidt hammer rebound data during field
testing. Int. J. Rock Mech. Min. Sci. Geomech. Abstr. 1980, 17, 167–171. [CrossRef]
44. Goktan, R.M.; Ayday, C.A. Suggested improvement to the Schmidt rebound hardness ISRM suggested method
with particular reference to rock machineability. Int. J. Rock Mech. Min. Sci. 1993, 30, 321–322. [CrossRef]
45. Deniz, V. Relationships between Bond’s grindability (Gbg) and breakage parameters of grinding kinetic on
limestone. Powder Technol. 2004, 139, 208–213. [CrossRef]
Appl. Sci. 2018, 8, 220 17 of 17

46. Aras, A.; Ozkan, A.; Aydogan, S. Correlations of Bond and Breakage Parameters of Some Ores with the
Corresponding Point Load Index. Part. Part. Syst. Charact. 2012, 29, 204–210. [CrossRef]
47. British Standards Institution. Natural Stone Test Methods. Determination of Real Density and Apparent Density,
and of Total and Open Porosity; BS EN 1936:2006; British Standard Institution (BSI): London, UK, 2017.
48. Shih, Y.-F.; Wang, Y.-R.; Lin, K.-L.; Chen, C.-W. Improving Non-Destructive Concrete Strength Tests Using
Support Vector Machines. Materials 2015, 8, 7169–7178. [CrossRef] [PubMed]
49. Khandelwal, M.; Ranjith, P.G. Correlating index properties of rocks with P-wave measurements. J. Appl. Geophys.
2010, 71, 1–5. [CrossRef]
50. Gupta, V.K.; Zouit, H.; Hodouin, D. The effect of ball and mill diameters on grinding rate parameters in dry
grinding operation. Powder Technol. 1985, 42, 199–208. [CrossRef]
51. Kılıç, A.; Teymen, A. Determination of mechanical properties of rocks using simple methods.
Bull. Eng. Geol. Environ. 2008, 67, 237–244. [CrossRef]
52. Kassab, M.A.; Weller, A. Study on P-wave and S-wave velocity in dry and wet sandstones of Tushka region.
Egypt. Egypt. J. Petrol. 2015, 24, 1–11. [CrossRef]
53. Rey, P.F.; Fountain, D.M.; Clement, W.P. P-wave velocity across a noncoaxial ductile shear zone and its
associated strain gradient: Consequences for upper crustal reflectivity. J. Geophys. Res. 1994, 99, 4533–4548.
[CrossRef]
54. Tandom, R.S.; Gupta, V. Estimation of strength characteristics of different Himalayan rocks from Schmidt
hammer rebound, point load index, and compressional wave velocity. Bull. Eng. Geol. Environ. 2015, 74,
521–533. [CrossRef]
55. Saptono, S.; Kramadibrata, S.; Sulistianto, B. Using the Schmidt hammer on rock mass characteristic in
sedimentary rock at Tutupan coal mine. Procedia Earth Planet. Sci. 2013, 6, 390–395. [CrossRef]
56. Kahraman, S.; Bilgin, N.; Feridunoglu, C. Dominant rock properties affecting the penetration rate of
percussive drills. Int. J. Rock Mech. Min. Sci. 2003, 40, 711–723. [CrossRef]
57. Behnia, D.; Behnia, M.; Shahriar, K.; Goshtasbi, K. A new predictive model for rock strength parameters
utilizing GEP method. Procedia Eng. 2017, 191, 591–599. [CrossRef]
58. Vishnu, C.S.; Mamtani, M.A.; Basu, A. AMS, ultrasonic P-wave velocity and rock strength analysis in
quartzites devoid of mesoscopic foliations—Implications for rock mechanics studies. Tectonophysics 2010,
494, 191–200. [CrossRef]
59. Zwiessler, R.; Kenkmann, T.; Poelchau, M.H.; Nau, S.; Hess, S. On the use of a split Hopkinson pressure
bar in structural geology: High strain rate deformation of Seeberger sandstone and Carrara marble under
uniaxial compression. J. Struct. Geol. 2017, 97, 225–236. [CrossRef]
60. Meng, Q.; Zhang, M.; Han, L.; Pu, H.; Li, H. Effects of size and strain rate on the mechanical behaviors of
rock specimens under uniaxial compression. Arab. J. Geosci. 2016, 9, 1–14. [CrossRef]
61. Aben, F.M.; Doan, M.-L.; Gratier, J.-P.; Renard, F. High strain rate deformation of porous sandstone and the
asymmetry of earthquake damage in shallow fault zones. Earth Planet. Sci. Lett. 2017, 463, 81–91. [CrossRef]
62. He, Z.; Li, G.; Tian, S.; Wang, H.; Shen, Z.; Li, J. SEM analysis on rock failure mechanism by supercritical CO2
jet impingement. J. Pet. Sci. Eng. 2016, 146, 111–120. [CrossRef]
63. Kanda, Y.; Sano, S.; Saito, F.; Yashima, S. Relationships between particle size and fracture energy for single
particle crushing. KONA Powder Part. J. 1985, 3, 26–31. [CrossRef]
64. Hogg, R. A spheroid model for the role of shape in particle size analysis. KONA Powder Part. J. 2015, 32,
227–235. [CrossRef]
65. Fuerstenau, D.W.; Abouzeid, A.-Z.M.; Phatak, P.B. Effect of particulate environment on the kinetics and
energetics of dry ball milling. Int. J. Miner. Process. 2010, 97, 52–58. [CrossRef]
66. Tumac, D. Predicting the performance of large diameter circular saws based on Schmidt hammer and other
properties for some Turkish carbonate rocks. Int. J. Rock Mech. Min. Sci. 2015, 75, 159–168. [CrossRef]

© 2018 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access
article distributed under the terms and conditions of the Creative Commons Attribution
(CC BY) license (http://creativecommons.org/licenses/by/4.0/).