You are on page 1of 10

Particulate Science and Technology, 32: 544553

Copyright # 2014 Taylor & Francis Group, LLC


ISSN: 0272-6351 print=1548-0046 online
DOI: 10.1080/02726351.2014.930942

Effect of Particle Size on Direct Compaction of Urea


Fertilizer
INTAN SORAYA SHAMSUDIN,1 MOHD. SHAMSUL ANUAR,1 YUS ANIZA YUSOF,1
AHMAD HUSNI MOHD. HANIF,2 and SURAYA MOHD. TAHIR3
1
Department of Process and Food Engineering, Faculty of Engineering, Universiti Putra Malaysia, Serdang, Selangor, Malaysia
2
Department of Land Management, Faculty of Agriculture, Universiti Putra Malaysia, Serdang, Selangor, Malaysia
3
Department of Mechanical and Manufacturing Engineering, Faculty of Engineering, Universiti Putra Malaysia, Serdang,
Selangor, Malaysia

The effect of particle size on compaction properties and characteristics of urea tablets manufactured from available urea granules
(TG tablets) and ground urea powders (TP tablets) was investigated. The compaction properties, namely, plastic work, elastic
work, friction work, and maximum ejection pressure were analyzed from the force-displacement prole of the compaction process.
Five applied pressures ranging between 37.67 MPa and 188.35 MPa were used to compact the materials using a universal testing
machine. Characteristics of the tablets tested were mechanical strength and the release of ammonium ion through dissolution test.
The results demonstrated that TG tablets underwent high plastic work and elastic work but low friction work compared to the TP
tablets. TG tablets released lower amount of ammonium ion compared to the TP tablets at almost all applied pressures, except at
75.34 MPa. This study provides a valuable data for evaluating the behavior of urea in the form of granules and powders during the
compaction process as well as the suitability in choosing the form of raw material for the production of urea tablets.
Keywords: Ammonium ion release, compaction properties, tensile strength, universal testing machine, urea

1. Introduction particle size, for example, the materials apparently


underwent fragmentation under pressure. This evidence
Earlier studies by Adolfsson and Nystrom (1996), Shotton demonstrates that the strength of the tablets is less affected
and Ganderton (1961), Hersey et al., (1967), Riepma et al. by the change in particle size when the material undergoes
(1993), and Zuurman et al. (1994) have shown that decreas- fragmentation rather than plastic deformation (Roberts
ing size of the particles of materials could positively affect and Rowe 1987; Gustafsson 2000). On the other hand, few
the mechanical strength of the tablets. These studies are sup- studies reported the tablet strength was positively affected
ported by Alderborn (1996) and Mattsson (2000), who stated by an increase in particle size of the material (Wikberg and
that an increase in the tensile strength of a tablet depends on Alderborn 1990; Johansson et al. 1998).
the reduction of the particle size. Compaction of smaller par- In the fertilizer industry, the improvement of urea fertilizer
ticles tends to form stronger tablets due to the large surface through mechanically compressing and pelletizing the fertili-
area of the particles for excellent interparticles bonding com- zer has been shown to increase the strength, minimize
pared to larger particles (Nikolakakis and Pilpel 1988; Wong ammonia volatilization, total N loss, reducing the rate of
and Pilpel 1990; Sun and Grant 2001; Kaerger et al. 2004). the urea hydrolysis, and improve the rate of plant growth
Although it is generally accepted that tablet strength and retain the nitrogen in the soil (De Datta et al. 1983;
increases with decreasing particle size, the effect of the initial Mikkelsen et al. 1978; Othman 2011; Rahman et al. 1996;
particle size on the tablet strength depends on the mechanical Purakayastha and Katyal 1998; Savant and Stangel 1990,
properties of the materials, as well as on the mechanism 1998; Yadvinder-Singh et al. 1994). To date, little information
where the materials undergo deformation (Alderborn and is known on the effect of particle size in direct compaction of
Nystrom 1982; Vromans et al. 1985; Alderborn et al. 1988). urea fertilizer. Moreover, no reports are available in the
Previous studies by McKenna and McCafferty (1982) and literature about the properties of urea fertilizer under the
Patel et al. (2006) have reported that the tablet strength of inuence of an applied pressure such as elasticity, plasticity,
dicalcium phosphate and sucrose was not dependent on the bonding, and brittleness (Amidon et al. 2009; Antikainen
and Yliruusi 2003), and also the effect of the ejection process
Address correspondence to: Intan Soraya Shamsudin, Depart- on the characteristics of the urea tablet. Such information is
ment of Process and Food Engineering, Faculty of Engineering, essential for predicting any failure occurrence of urea tablet,
Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, and the way the tablet may manifest or its tablet-forming abil-
Malaysia. E-mail: soraya7787@gmail.com ity (Han et al. 2008; Alderborn 2007; Ragnarsson and Sjogren
Effect of Particle Size on Urea Tablets 545

1983). Therefore, in this study, tablets made of urea granules force-displacement prole (Ragnarsson and Sjogren 1983;
(TG tablets) and ground urea powder (TP tablets) have been Oates and Mitchell 1989; Ragnarsson 1996; Antikainen
developed in order to investigate the effect of particle size on 2003; Antikainen and Yliruusi 2003; Mohammed et al. 2005;
compaction properties and characteristics of the tablets. Viana et al. 2005; Alderborn 2007; Patel et al. 2007). Figure 2
shows a typical compaction curve obtained from the
2. Materials and Methods force-displacement prole of the loading and unloading stages
of the compaction process. Area A is the friction work, where
2.1 Materials work was expended to overcome the interparticles and die-
wall frictions (Paronen 1983; Velasco et al. 1997). The friction
Urea in the form of granules and ground powders was used in
phenomenon often occurs between the powder particles or
this study (Figures 1a and 1b). Available urea granules were
between the tablet and the die wall during the compaction by
purchased from Petronas Fertilizer (Kedah) Sdn. Bhd.,
the laboratory-scale uniaxial die compaction method (Moody
Malaysia. The characteristics of the urea granules included
et al. 1981; Alderborn 2007). Area B is the plastic work, where
particle size of 2 mm (diameter), included 46% nitrogen, 1%
work was expended by the tablet to undergo plastic defor-
biuret, 0.5% moisture by its maximum weight.
mation (permanent deformation), bonding, and the formation
of a rm tablet (Velasco et al. 1997). Area C refers to elastic
2.2 Methods work, where work was expended to deform the particles by
2.2.1 Sample Preparation temporary deformation (Ragnarsson 1996). The stored elastic
Ground urea powders were obtained by milling the urea component in the tablet will be recovered or expended in the
granules for 60 sec for every repetition using an electric expansion of the tablet, which takes place during the unloading
grinder (model RT-02A grinder, Taiwan). The process stage when the pressure on the tablet is relieved (Velasco et al.
resulted in particle sizes of 90% < 855.03 mm, 50% < 226. 1997; Antikainen 2003; Anuar and Briscoe 2009, 2010; Haware
20 mm, 10% < 10.62, bulk density of 471 kg=m3, tapped den- et al. 2010; Govedarica et al. 2012), and also after ejection of
sity of 765 kg=m3, and true density of 1380 kg=m3. the tablet (Baily and York 1976). The maximum ejection press-
ure during ejection of the tablet can be obtained from the ejec-
2.2.2 Uniaxial Die Compaction Method tion force-displacement prole. According to Garr and
Compaction by laboratory scale uniaxial die compaction Rubinstein (1991) and Cutt et al. (1989), the plastic and elastic
method was performed using Instron Universal Testing works during loading and unloading stages are associated with
5566 machine (USA). Five applied pressures ranges from the tablet strength, by which the area A and C should be as
37.67 to 188.35 MPa, were used to compact 1.0 0.02 g of small as possible in order to form a large degree of plasticity
the materials inside a 13 mm stainless steel cylindrical uniaxial (area B) and to improve the tablet strength.
die (Specac, UK). The die and punches were cleaned with
ethanol prior to each compaction to remove any sticking pow- 2.4 Tablet Characteristics
der. The urea tablet was formed without lubricant in a con-
trolled temperature (2025 C). The loading and unloading 2.4.1 Mechanical Strength of Urea Tablets
processes were conducted at constant speed of 0.1 mm=s and The physical testing of the urea tablet was performed 24 h
0.0167 mm=s (Mohammed et al. 2005). The tablet was then after ejection, allowing for full elastic recovery of the tablet
ejected from the die with a constant speed of 0.083 mm=s.
The applied force-displacement prole and ejection
force-displacement prole were recorded automatically using
a computer program from Bluehill Software (USA).

2.3 Compaction Properties


The analysis of plastic work, elastic work, and friction work
were estimated by integrating the area under the curve of the

Fig. 2. Schematic diagram of the force versus displacement


prole during uniaxial die compaction experiment (Ragnarsson
Fig. 1. Urea in forms of a) granules and b) powders. 1996).
546 Shamsudin et al.

(Krycer et al. 1982; Mollan and Celik 1996). Physical mea- tablets and conventional urea granules were studied based
surements and tests performed were weighed by electronic on their percentage of ammonium ion release in triplicate.
mass balance (A&D, Japan), while tablet thickness and
2.4.3 Particle Shape and Surface Characteristic
diameter was measured using a Vernier calliper (Mitutoyo,
Japan). The strength of the urea tablet was determined by The particle shape of urea powder and urea tablets side
Brazilian test using the Instron Universal Testing 5566 surfaces were examined using variable pressure scanning
machine (USA) to estimate its tensile strength (Fell and electron microscope (LEO 1455 VPSEM, Germany) at an
Newton 1970). The tablet was fractured diametrically in four accelerating voltage of 20 kV. The sample was mounted on
replicates at a constant speed of 0.0116 mm=s (Mohammed a 13 mm diameter sample stub using a double-sided adhesive
et al. 2005). The tensile strength (rt) was calculated using tape and sputter coated (BAL-TEC SCD 005, Germany)
the equation by Fell and Newton (1970): with gold for 180 sec under reduced pressure.

2P 2.5 Data Analysis


rt ; 1
pDT
2.5.1 Statistical Analysis
where The experimental data for the TG and TP tablets were pre-
rt tensile strength, sented as mean of 3 or 4 replicates, and statistical analysis
P tensile force or tensile failure, was performed using Minitab 16 Statistical Software. The
D tablet diameter, and data were analyzed using analysis of variance (ANOVA)
T tablet thickness. and dened as signicantly different at p < 0.05. Whenever
a signicant difference was found from the ANOVA results,
2.4.2 Ammonium Ion Release Through Dissolution Test the data were compared using a t test.
When urea is applied to irrigated rice soil, the urea is hydro-
lyzed by water to form ammonium carbonate, an unstable
3. Results and Discussion
compound that can decompose to produce ammonium
(NH 4 ion, bicarbonate anion or hydrogen carbonate ion, 3.1 Compaction Properties
and release ammonia (NH3) gas (Mikkelsen 2009). In this
3.1.1 Plastic Work
study, the hydrolysis of the urea tablets was determined by
conducting a dissolution test as a method for ammonium The work for the TG and TP tablets to deform plastically at
 various applied pressures is shown in Figure 3. The plastic
NH 4 ion analysis of the urea tablets made with different
work of the tablets increased with a logarithmic trend
particle sizes and applied pressures. The ammonium ion
as the applied pressure increase, which indicated that the
release reects the amount of nitrogen recovered, which is
deformation of the tablets was dependent on the applied
dissolved in a liquid medium during the dissolution test.
pressure. Apparently, the increase in plastic work with
Decreasing ammonium ion released indicates that the urea
applied pressure was more rapid in the low applied pressures
tablets possess a relatively higher tensile strength and mini-
range of 37.67 to 113 MPa and became moderate when using
mum loss of nitrogen content throughout the dissolution
high applied pressures of 150.68188.35 MPa. The increase
test. The test was conducted using a semi-automatic dissol-
in plastic work with applied pressure can be attributed to
ution tester (Pharma Test D-63512, Germany) using the
the predominant deformation at those applied pressure
paddle method. Three urea tablets weighed 3 g were placed
ranges.
in a covered beaker containing medium solution; 200 mL
In the early stage of compaction at low applied pressures,
distilled water (Purakayastha and Katyal 1998) of pH 6.8
the TG and TP tablets underwent particle rearrangement
at average ambient temperature of 30 C. The pH of distilled
water is always in the acidic range to avoid high emission of
ammonia gas and ensure the measurement of ammonium
ion content is correct (Mikkelsen 2009). The paddle was
rotated at 20 rpm (lowest paddle speed) to decelerate tablet
dissolving and promoting gradual homogeneous solution.
An amount of 4 mL of the sample was withdrawn from
the dissolution beaker over a period of 10 min and ltered
through fast ow lter 55 mm No. 111 (615 mm) (Filtres
Fioroni, France) for removal of any undissolved particles.
The values of ammonium ion concentration in the covered
beaker were measured photometrically using HI 96715
ammonia photometer high range (Hanna Instruments,
Inc., USA). The test was continued until 100% dissolution
or maximum reading of the ammonia photometer, for
example, 50 mg=L was achieved. For comparison purpose,
the ammonium ion released from conventional urea granules Fig. 3. Plastic work for TG and TP tablets at various applied
was also studied. The ammonium ion released from the urea pressures. Error bars are standard error of the mean, n 4.
Effect of Particle Size on Urea Tablets 547

and low elastic deformation, which caused a large volume


reduction. For that reason, the rate of plastic work with
pressure is rapid and the magnitude of plastic work at
applied pressures of 37.67113 MPa is high. At higher
applied pressures, the deformation becomes dominant,
which requires more energy input than required for particle
rearrangement and the rate of volume reduction with
pressure is less for the TG and TP tablets. This explains
the lower increase in plastic work with applied pressure,
where the deformation is dominant at applied pressures of
150.68188.35 MPa.
In Figure 3, the TG tablets have a higher level of plastic
work compared to the TP tablets at all applied pressures
except at 188.35 MPa. Zuurman et al. (1999) reported a high
plastic work related with difcult compaction of the parti-
cles. This might be due to the large and spherical shape of
the TG particles (Rahman et al. 1996).
It is assumed that the sequence of the deformation of TG
tablets can be divided into three modes and described
according to the deformation of pellets (Nicklasson and
Alderborn 1999; Tunon 2003). During compaction, the TG
particles possibly undergo: a) mode 1 deformation, where
the surfaces of the TG particles are attened under applied
pressure; b) extended mode 1 deformation, where the sur-
faces of the TG particles undergo indentations at certain
points of contact; and c) mode 2 deformation, where the
dimensions of the TG particles are attened due to the
change in the dimensions of the particles.
A further increase in the applied pressure results in
attening of the TG particles against the other adjacent
TG particles to a greater extent (Nicklasson et al. 1999a,
1999b) and thus, fragmented by brittle fracture into smaller
and discrete particles. This repetition of deformation and
breaking increases the surface area of the TG particles and
also the area for forming the bonding (Duberg and Nystrom
1982; Alderborn et al. 1985; Alderborn 2007). This work is
supported by Nicklasson and Alderborn (1999) who studied
Fig. 4. SEM images of TG tablets at a) 37.67 MPa and b) 188.35
the deformation of MCC=PEG pellets. They stated that the
MPa.
degree of permanent deformation which the pellets undergo
during compaction is controlled by the area of contact
formed between the pellets.
Increasing the applied pressure from 150.68 to 188.35 MPa strated a tendency to move very slowly to each other and
does not show any signicant (p > 0.05) difference for the have time to deform during the compaction (Sun and Grant
TG tablets, showing that the high degree of permanent 2001). After an applied pressure of 150.68 MPa, signicant
deformation had reached at the applied pressures of 150.68 (p < 0.05) differences in the plastic work for the TP tablets
and 188.35 MPa. Referring to Figures 4a and 4b, the SEM are observed by which the TP tablets exhibit higher plastic
images of tablets side surfaces for TG tablets at lowest work than TG tablets. This means that more energy is
and highest applied pressures; 37.67 and 188.35 MPa, required to form the TP tablets at a high applied pressure
respectively, shows new smooth surfaces. This indicated that of 188.35 MPa. This may be due to the utilization of more
the TG tablets are mainly consolidated by fragmentation as energy to overcome the increased cohesiveness of the TP
the deformed particles in the TG tablets depend on the particles that occur at high applied pressure. In addition, it
compaction pressure (Antikainen and Yliruusi is expected that the applied pressure for deformation of
2003). the TP particles may be higher than the applied pressure
In Figure 3, TP tablets have less plastic work compared to of 188.35 MPa in order to achieve constant plastic defor-
TG tablets at low applied pressures of 37.67113 MPa. This mation and consequently, form a large surface area for
is because TP particles consisted of an aggregate of very bonding. This is in agreement with the SEM images of TP
small particles with irregular angular shape and rough sur- tablets in Figures 6a and 6b by which the applied pressures
faces (Figures 5a and 5b). These small TP particles demon- used in this study have not successfully deform the particles
548 Shamsudin et al.

Fig. 5. SEM images of urea powders at a) 1000 and b) 100 Fig. 6. SEM images of TP tablets at a) 37.67 MPa and b) 188.35
magnication. MPa.

In Figure 7, the elastic work for both tablets does not


of TP tablets. This observation was possibly due to the small show any signicant (p > 0.05) difference from applied pres-
and irregular angular shape of TP particles possessed which sures of 37.67113 MPa. However, the values of the elastic
required relatively higher applied pressure than 188.35 MPa work for the TP tablets are signicantly (p < 0.05) lower
to undergo full plastic deformation. than that of the TG tablets at high applied pressures
(150.68 and 188.35 MPa). The result indicates a favorable
3.1.2 Elastic Work low tablet relaxation for the TP tablets as compared to the
In Figure 7, the elastic work for TG and TP tablets TG tablets due to its low elastic work. Moreover, it shows
increased as the applied pressure increased. During comp- that a high applied pressure can inuence the elastic defor-
action, elastic energy is stored in the tablet under applied mation for both tablets, but to a greater extent for the TG
pressure for elastic deformation. The restoration of this tablets as compared to the TP tablets. The lower elastic
energy takes place during the unloading stage of the com- deformation at higher pressures also conrms that the TP
paction process (Akande et al. 1997). Therefore, the appli- tablets undergo higher plastic deformation as the applied
cation of applied pressure during the compaction process pressure is increased (Figure 3). That is, greater inter-
greatly inuenced the amount of stored elastic energy in particulate contact and particle adhesivity (Sebhatu and
the tablet. An increase of the applied pressure leads to an Alderborn 1999) reduced the time available for the TP
increased in the stored elastic energy (Patel et al. 2007). tablets to relieve the elastic energy. In addition, Patel et al.
This explained the increase in elastic work as the applied (2007) pointed out that a smaller particle size undergoes less
pressure is increased. elastic deformation than a larger particle size. Meanwhile,
Effect of Particle Size on Urea Tablets 549

3.1.4 Maximum Ejection Pressure


The maximum ejection pressure for the TG and TP tablets
as shown in Figure 9 is nonlinear with applied pressure. In
Figure 9, the maximum ejection pressure for the TG tablets
is high for the low applied pressures (37.67113 MPa) and it
does not show any effect when the applied pressure is
further increased (188.35 MPa). This can be attributed to
the deformation of the TG particles during the compaction
process. At low applied pressures of 37.67113 MPa, the
plastic work is high for the TG tablets, which require a high
maximum ejection pressure in order to overcome the friction
between the die wall and the tablet. As the pressure
increases, the deformation of the TG tablets becomes
relatively low and constant. For that reason, a relatively
Fig. 7. Elastic work for TG and TP tablets at various applied constant maximum ejection pressure is necessary to eject
pressures. Error bars are standard error of the mean, n 4. the TG tablets when formed at applied pressures of 113
188.35 MPa. This is because a high applied pressure does
not further affect the friction of ejection. On the other hand,
the high elastic work of the TG tablets shows its high level of the increase of maximum ejection pressure for the TP tablets
tablet relaxation as the result of low interparticulate bond- is apparently seen from applied pressures of 37.67
ing. This is in agreement with Zuurman et al. (1999) who sta- 150.68 MPa and undergoes a high descent from applied
ted that tablet relaxation increases as the interparticle pressures of 150.68188.35 MPa, suggesting a reduction in
bonding is decreased. resistance to friction at that applied pressure. It can be
3.1.3 Friction Work observed that the TG tablets have a lower maximum ejec-
In Figure 8, the work to overcome the friction for the TG tion pressure than the TP tablets as a result of a higher elas-
and TP tablets increases with increasing applied pressure. tic relaxation in the TG tablets which corresponded to a
This is because during the compaction, some energy was also high elastic work (Figure 7). This observation gives an
lost in the form of heat due to friction encountered between advantage during the ejection process by which a plastic
the particles and the die-wall and interparticles friction. As junction cannot form between the tablet and the die wall
the applied pressure increases, the work used to deform (Mohammed et al. 2006). This effect points to facilitating
the particles plastically increases. Thus, the friction work is the ejection process which in turn requires a low maximum
also increased. In Figure 8, there is no signicant (p > 0.05) ejection pressure.
difference of friction work with the applied pressure between
the TG and TP tablets at applied pressures of 37.67 3.2 Tablet Characteristics
150.68 MPa. A high friction work is observed for the TP
tablets when formed at an applied pressure of 188.35 MPa 3.2.1 Mechanical Strength of Tablet
which corresponding to domination by the large plastic A logarithmic trend relating to the tensile strength and
deformation that the tablets suffered (Figure 3). Therefore, applied pressure for the TG and TP tablets is observed in
more energy was required to overcome the friction in the Figure 10. The initial tensile strength for the TG tablets is
TP tablets than the TG tablets. signicantly (p < 0.05) different in comparison to the TP

Fig. 9. Maximum ejection pressure for TG and TP tablets at


Fig. 8. Friction work for TG and TP tablets at various applied various applied pressures. Error bars are standard error of the
pressures. Error bars are standard error of the mean, n 4. mean, n 4.
550 Shamsudin et al.

almost double than that of the TG tablets. The irregular


shape and rough surfaces of the TP particles may contribute
to the increase in the interparticulate bonding and the tablet
strength (Wong and Pilpel 1990; Nikolakakis and Pilpel
1988). This is supported by the data shown earlier in
Figure 3, where an increase in the plastic work is observed
with the increase in the applied pressure. Therefore, a high
pressure failure during the mechanical strength test is
expected for the TP tablets due to the increase in the inter-
particulate bonding within the tablets. This explains the
higher tensile strength of the TP tablets compared to the
TG tablets, showing their higher mechanical strength.
Moreover, it can be deduced that the reduction in particle
size of the urea (urea powder) causes the material to suffer
Fig. 10. Tensile strength for TG and TP tablets at various greater deformation. In this case, the TP tablets consolidate
applied pressures. Error bars are standard error of the mean, more by plastic deformation due to their high plastic work
n 4. and tensile strength. On the other hand, the TG tablets are
susceptible to deform by fragmentation as a result of the
relatively high plastic work but low tensile strength.
tablets at a low applied pressure of 37.67 MPa. A higher
tensile strength is observed for the TP tablets over the TG 3.2.2 Dissolution Test
tablets at applied pressures of 75.34188.35 MPa. For the The ammonium ion release from the urea granules, TG and
TP tablets, this increase in tensile strength may continue to TP tablets is shown in Figure 11. The ammonium ion release
increase and exceed the pressure range used in this study. for the urea granules is 35.73% after 10 min of the dissol-
In contrast, the tensile strength for the TG tablets increases ution test. TG tablets give lower ammonium ion release as
over applied pressures of 37.6775.34 MPa and then decreases compared to the urea granules at all applied pressures while
by a small value beyond an applied pressure of 75.34 MPa. the TP tablets give lower ammonium ion release than the
In Figure 10, the TG tablets produced are low strength urea granules when the tablets are formed at low applied
tablets due to the low tensile strength. Thus, it can be pressures of 37.67 and 75.34 MPa.
deduced that the TG tablet was unable to maintain its Among the applied pressures used to form TG tablets,
inter-particulate bonding due to its weak deformation dur- applied pressure of 150.68 MPa gives the lowest ammonium
ing compaction. That is, the TG tablets were deformed by ion release (24.13%) compared to other applied pressures.
both plastic and fragmenting deformation, but to a greater This is contrary with the nding from mechanical strength
extent by fragmentation. This is explained by the relatively test by which the tensile strength for TG tablets formed at
high plastic work (Figure 3) of the TG tablets which causes applied pressure of 37.67 MPa gives the lowest tensile
the tablets to possess the lowest tensile strength (Figure 10) strength. Therefore, the ammonium ion release for TG
in comparison to the TP tablets. tablets at applied pressure of 37.67 MPa should be high in
On the other hand, the TP tablets produced are strong comparison to other applied pressures. Meanwhile, the
tablets, referring to their higher tensile strength which is applied pressure of 188.35 MPa give the highest ammonium

Fig. 11. Ammonium ion release for urea granules, TG, and TP tablets at various applied pressures. Error bars are standard error of
the mean, n 3.
Effect of Particle Size on Urea Tablets 551

ion release. This is expected as the tensile strength for TG References


tablets formed at applied pressure of 188.35 MPa gives Adolfsson, A., and C. Nystrom. 1996. Tablet strength, porosity,
relatively low tensile strength (Figure 10). From this obser- elasticity and solid state structure of tablets compressed at high
vation, it shows that all applied pressures used to deform loads. International Journal of Pharmaceutics 143:95106.
the TG tablets except 188.35 MPa do not have much inu- Akande, O. F., M. H. Rubinstein, and J. L. Ford. 1997. The compac-
tion properties of a 1:1 acetaminophen: microcrystalline cellulose
ence on the release of ammonium ion.
micture using pre-compression and main compression. Journal of
Comparing the applied pressures used for TP tablets, it is Pharmaceutical Sciences 86:900907.
clearly seen that applied pressure of 75.34 MPa gives the Alderborn, G. 1996. Particle dimensions. In Pharmaceutical
lowest ammonium ion release (29.2%) in comparison to powder compaction technology, eds. G. Alderborn and C. Nystrom,
other applied pressures. Referring to Figure 10, the tensile 245283. New York: Marcel Dekker.
strength for TP tablets increased with increasing of the Alderborn, G. 2007. Tablets and compaction. In Aultons pharma-
applied pressures. Thus, it is expected that the ammonium ceutics: The design and manufacture of medicines, ed. M. E. Aulton,
443481. Philadelphia: Elsevier.
ion release decreased as the applied pressure increase for Alderborn, G., E. Borjesson, M. Glazer, and C. Nystrom. 1988. Studies
the TP tablets. However, this is not the case as observed at on direct compression of tablets. XIX. The effect of particle size and
applied pressures of 113188.35 MPa by which the release shape on the mechanical strength of sodium bicarbonate tablets.
of ammonium ion is higher than the other applied pressures. Acta Pharmaceutica Suecica 25:31 40.
This is most probably because of the rough surfaces of the Alderborn, G., and C. Nystrom. 1982. Studies on direct compression of
TP tablets and common defects such as cracks that are tablets. IV. The effect of particle size on the mechanical strength of
produced during the compaction and ejection process. This tablets. Acta Pharmaceutica Suecica 19:381390.
Alderborn, G., K. Pasanen, and C. Nystrom. 1985. Studies on direct
is supported by SEM images of the TP tablets side surfaces compression of tablets. XI. Characterization of particle fragmen-
at applied pressure of 188.35 MPa (Figure 6b). Figure 6b tation during compaction by permeametry measurements of tablets.
shows that the irregular TP particles and rough surfaces International Journal of Pharmaceutics 23:7986.
are not fully deformed. For that reason, these kinds of sur- Amidon, G. E., P. J. Secreast, and D. Mudie. 2009. Particle, powder
faces may allow the easy penetration of water and release the and compact characterization. In Developing solid oral dosage
ammonium ion more rapidly. forms: Pharmaceutical theory and practice, ed. Y. Qiu, Y. Chen,
G. G. Z. Zhang, L. Liu, and W. R. Porter, 163183. New York:
At all applied pressures except 75.34 MPa, TG tablets
Elsevier.
give lower ammonium ion release than TP tablets. This Antikainen, O. 2003. New method to evaluate applicability of powders
observation may be due to the deformation they possessed and granules for tablet compression. University of Helsinki, Finland,
during compaction. SEM images of tablets side surfaces at Helsinki.
applied pressures of 37.67 and 188.35 MPa in Figures 4a, Antikainen, O., and J. Yliruusi. 2003. Determining the compression
4b, 6a, and 6b revealed that TG tablets are well deformed behaviour of pharmaceutical powders from force-distance
than TP tablets. The surfaces of TG tablets are smooth compression prole. International Journal of Pharmaceutics 252:
253261.
and have fewer pores compared to TP tablets. Anuar, M. S., and B. J. Briscoe. 2009. The elastic relaxation of starch
tablets during ejection. Powder Technology 195:96104.
4. Conclusion Anuar, M. S., and B. J. Briscoe. 2010. Interfacial elastic relaxation
during the ejection of bilayered tablets. International Journal of
The compaction study shows that TG tablets consume more Pharmaceutics 387:4247.
energy for plastic work, dissipated large elastic energy (elas- Baily, E. D., and P. York. 1976. An apparatus for the study of strain
tic work) in the expansion of the tablet and required lower recovery in compacts. Journal of Material Science 11:14701474.
maximum ejection pressure as compared to the TP tablets. Cutt, T., J. T. Fell, P. J. Rue, and M. S. Spring. 1989. Granulation
and compaction of a model system. III. Compaction properties of
The mechanical strength demonstrated by the TP tablets granules. International Journal of Pharmaceutics 49(2):157161.
has a higher tensile strength than the TG tablets. The De Datta, S. K., I. R. P. Fillery, and E. T. Craswell. 1983. Results
dissolution test shows that the use of larger particles (TG from recent studies on nitrogen fertilizer efciency in wetland rice.
tablets) give a lower ammonium ion release compared to Outlook on Agriculture 12:125134.
the smaller particles (TP tablets) at all applied pressures Duberg, M., and C. Nystrom. 1982. Studies on direct compression of
except 75.34 MPa. tablets. VI. Evaluation of methods for the estimation of particle
fragmentation during compaction. Acta Pharmaceutica Suecica
19:421436.
Funding Fell, J. T., and J. M. Newton. 1970. Determination of tablet strength by
diametral compression test. Journal of Pharmaceutical Sciences
The authors wish to thank Universiti Putra Malaysia 59:688691.
Research University Grant project number 05-02-12- Garr, J. S. M., and M. H. Rubinstein. 1991. Effect of rate of force
1921RU, Ministry of Higher Education Malaysia project application on the properties of microcrystalline cellulose and
no. 03-04-10-815FR, and Graduate Research Fellowship of dibasic calcium phosphate mixtures. International Journal of
Universiti Putra Malaysia for the funding. Pharmaceutics 73:7580.
Gustafsson, C. 2000. Solid state characterisation and compaction behav-
iour of pharmaceutical materials. Doctoral dissertation, Uppsala
NOMENCLATURE University, Uppsala, Sweden.
NH3 (gas) ammonia gas Govedarica, B., I. Ilic, R. Sibanc, R. Dreu, and S. Srcic. 2012. The
NH4 ammonium ion use of single particle mechanical properties for predicting the
552 Shamsudin et al.

compressibility of pharmaceutical materials. Powder Technology Oates, R. J., and A. G. Mitchell. 1989. Calculation of punch displace-
225:4351. ment and work of powder compaction on a rotary tablet press.
Han, L. H., J. A. Elliott, A. C. Bentham, A. Mills, G. E. Amidon, and Journal of Pharmacy and Pharmacology 41:517523.
B. C. Hancock. 2008. A modied Drucker-Prager cap model for die Othman, S. S. 2011. Mechanical strength and dissolution characteristics
compaction simulation of pharmaceutical powders. International of compacted urea fertilizer. Bachelor dissertation, Universiti Putra
Journal of Solids and Structures 45:30883106. Malaysia, Selango, Malaysia.
Haware, R. V., I. Tho, and A. Bauer-Brandl. 2010. Evaluation of a Paronen, P. 1983. Xylan as a direct compression adjuvant for tablets.
rapid approximation method for the elastic recovery of tablets. Doctoral dissertation, University of Kuopio, Kuopio.
Powder Technology 202:7177. Patel, S., A. M. Kaushal, and A. K. Bansal. 2007. Lubrication potential
Hersey, J. A., G. Bayraktar, and E. Shotton. (1967). The effect of of magnesium stearate studied on intrumented rotary tablet press.
particle size on the strength of sodium chloride tablets. Journal of AAPS PharmSciTech 8:18.
Pharmacy and Pharmacology. 19:24S30S. Purakayastha, T. J., and J. C. Katyal. 1998. Evaluation of compacted
Johansson, B., F. Nicklasson, and G. Alderborn. 1998. Effect of pellet size urea fertilizers prepared with acid and non-acid producing chemical
on degree of deformation and densication during compression and additives in three soils varying in pH and cation exchange capacity
on compactability of microcrystalline cellulose pellets. International I. NH3 volatilization. Nutrient Cycling in Agroecosystems 51:
Journal of Pharmaceutics 163:3548. 107115.
Kaerger, J. S., S. Edge, and R. Price. 2004. Inuence of particle size Ragnarsson, G. 1996. Force-displacement and network measurements.
and shape on owability and compactibility of binary mixtures of In Pharmaceutical powder compaction technology, eds. G. Alderborn
paracetamol and microcrystalline cellulose. European Journal of and C. Nystrom, 77132. New York: Marcel Dekker.
Pharmaceutical Science 22:173179. Ragnarsson, G., and J. Sjogren. 1983. Work of friction and net work
Krycer, I., D. G. Pope, and J. A. Hersey. 1982. An evaluation of the during compaction. Journal of pharmacy and pharmacology
techniques employed to investigate powder compaction behavior. 35:201204.
International Journal of Pharmaceutics 12:113134. Rahman, M., Y. Pelovski, S. Stefanova, and P. Bozadjiev. 1996. Study
Maganti, L., and M. Celik. 1993. Compaction studies on pellets I. of the properties of urea-ammonium sulphate (UAS) pellets.
Uncoated pellets. International Journal of Pharmaceutics 95: Fertilizer Research 44:189194.
2942. Riepma, K. A., H. Vromans, K. Zuurman, and C. F. Lerk. 1993. The
Mattsson, S. 2000. Pharmaceutical binders and their function in directly effect of dry granulation on the consolidation and compaction of
compressed tablets. Doctoral dissertation, Uppsala Universitet, crystalline lactose. International Journal of Pharmaceutics 97:2938.
Uppsala, Sweden. Roberts, R. J., and R. C. Rowe. 1987. The Youngs modulus of
McKenna, A., and D. F. McCafferty. 1982. Effect of particle size on pharmaceutical materials. International Journal of Pharmaceutics
the compaction mechanism and tensile strength of tablets. Journal 37:1518.
of Pharmacy and Pharmacology 34:347351. Savant, N. K., and P. J. Stangel. 1990. Deep placement of urea super-
Mikkelsen, R. 2009. Ammonia emissions from agricultural operations: granules in transplanted rice: Principles and practices. Fertilizer
Fertilizer. Better Crops 93:911. Research 25:183.
Mikkelsen, D. S., S. K. De Datta, and W. N. Obcemea. 1978. Savant, N. K., and P. J. Stangel. 1998. Urea briquettes containing dia-
Ammonia volatilization losses from ooded rice soils. Soil Science mmonium phosphate: A potential NP fertilizer for transplanted
Society of America Journal 42:725730. rice. Fertilizer Research 51:8594.
Mohammed, H., B. J. Briscoe, and K. G. Pitt. 2005. The interrelation- Sebhatu, T., and G. Alderborn. 1999. Relationships between the
ship between the compaction behavior and the mechanical strength effective interparticulate contact area and the tensile strength of
of pure pharmaceutical tablets. Chemical Engineering Science tablets of amorphous and crystalline lactose of varying particle size.
60:39413947. European Journal of Pharmaceutical Sciences 8:235242.
Mohammed, H., B. J. Briscoe, and K. G. Pitt. 2006. The intrinsic Shotton, E., and D. Ganderton. 1961. The strength of compressed
nature and the coherence of compacted pure pharmaceutical tablets. tablets. III. The relation of particle size, bonding and capping
Powder Technology 165:1121. in tablets of sodium chloride, aspirin and hexamine. Journal of
Mollan, Jr., M. J., and M. Celik. 1996. The effects of lubrication on Pharmacy and Pharmacology 13:144152.
the compaction and post-compaction properties of directly com- Sun, C., and D. J. W. Grant. 2001. Effect of initial particle size on
pressible maltodextrins. International Journal of Pharmaceutics the tableting properties of L-lysine monohydrochloride dihydrate
144:19. powder. International Journal of Pharmaceutics 215:221228.
Moody, G., M. H. Rubinstein, R. A. FitzSimmons. 1981. Tablet Tunon, A. 2003. Preparation of tablets from reservoir pellets with
lubricants I. Theory and modes of action. International Journal of emphasis on compression behaviour and drug release. Uppsala
Pharmaceutics 9:7580. University, Uppsala.
Nicklasson, F., and G. Alderborn. 1999. Modulation of the tabletting Velasco, V., A. Munoz-Ruiz, C. Monedero, and R. Jimenez-
behaviour of microcrystalline cellulose pellets by the incorporation Castellanos. 1997. Force-displacement parameters of maltodextrins
of polyethylene glycol. European Journal of Pharmaceutical Sciences after the addition of lubricants. International Journal of
9:5765. Pharmaceutics 152:111120.
Nicklasson, F., B. Johansson, and G. Alderborn. 1999a. Occurrence Viana, M., J. Ribet, F. Rodriguez, and D. Chulia. 2005. Powder
of fragmentation during compression of pellets prepared from a functionality test: a methodology for rheological and mechanical
4 to 1 mixture of dicalcium phosphate dihydrate and microcrystal- characterization. Pharmaceutical Development and Technology
line cellulose. European Journal of Pharmaceutical Sciences 7: 10:327338.
221229. Wikberg, M., and G. Alderborn. 1990. Compression characteristics of
Nicklasson, F., B. Johansson, and G. Alderborn. 1999b. Tabletting granulated materials. II. Evaluation of granule fragmentation dur-
behaviour of pellets of a series of porositiesA comparison between ing compression by tablet permeability and porosity measurements.
pellets of two different compositions. European Journal of Pharma- International Journal of Pharmaceutics 62(23):229241.
ceutical Sciences 8:1117. Wong, L. W., and N. Pilpel. 1990. The effect of particle shape on mech-
Nikolakakis, I., and N. Pilpel. 1988. Effects of particle shape and size anical properties of powders. International Journal of Pharmaceutics
on the tensile strengths of powders. Powder Technology 56:95103. 59:145154.
Effect of Particle Size on Urea Tablets 553
Yadvinder-Singh, M., S. S., M. Nyborg, and E. G. Beauchamp. 1994. compactibility of lactose granulations. International Journal of
Large granules, nests or bands: Methods of increasing efciency of Pharmaceutics 102:19.
fall-applied urea for small cereal grains in North America. Fertilizer Zuurman, K., K. Van der Voort Maarschalk, and G. K. Bolhuis.
Research 38:6187. 1999. Effect of magnesium stearate on bonding and porosity
Zuurman, K., K. A. Riepma, G. K. Bolhuis, H. Vromans, and expansion of tablets produced from materials with different consoli-
C. F. Lerk. 1994. The relationship between bulk density and dation properties. International Journal of Pharmaceutics 179:107115.

You might also like