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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
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).
(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.
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.
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
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