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Iranian Journal of Chemical Engineering Vol. 7, No. 4 (Autumn), 2010, IAChE Research note
Measurement and Correlation of Ibuprofen in Supercritical
Carbon Dioxide Using Stryjek and Vera EOS
M. Mirzajanzadeh1, F. Zabihi2, M. Ardjmand1 1- Islamic Azad University, Tehran South Branch, Faculty of Graduate Studies, Department of Chemical 2- Islamic Azad University, Ayatollah Amoli Branch, Department of Chemical Engineering, Amol-Iran. Abstract
Ibuprofen solubility in supercritical carbon dioxide was measured using a dynamic
apparatus at a pressure between 80 and 140 bars at three different temperatures,
308.15, 313.15 and 318.15 K. The mole fraction of Ibuprofen in fluid phase was in the
range of 0.015 × 10-3 - 3.261 × 10-3 at the mentioned operational condition. Modified
Mendez-Santiago and Teja equation were used to check the consistency of the
experimental data. Results were correlated using the Stryjek and Vera equation of state
with the van der Waals 1-parameter (vdW1) and 2-parameters (vdW2) mixing and
combining rules. Interaction parameters along with the percentage of the average
absolute relative deviation (%AARD) were displayed. Also, the Lydersen group
contribution methods were used for predicting the physicochemical and critical
properties of the Ibuprofen.
Keywords: Ibuprofen Solubility, Supercritical Carbon Dioxide, Stryjek and Vera EOS,
Mendez-Santiago and Teja Equation

1- Introduction
Solubility data are essential for an accurate promoting high mass transfer, at least an design of the operational conditions and to calculate the concentration of supercritical liquids. In other words, a small change of solution, in order to investigate the feasibility of SCF based processes. Supercritical fluids temperature) gives rise to a large change in a are useful in a variety of applications as food supercritical fluid density, in spite of a dense and pharmaceutical industries. Supercritical liquid character. Therefore, the solvent fluids have been established as powerful properties of a fluid change significantly, solvents for many non volatile and thermal supercritical area has gas-like diffusivity, ∗ Corresponding author: Elyze_125@hotmail.com Measurement and Correlation of Ibuprofen in Supercritical Carbon Dioxide Using Stryjek and Vera EOS Based on the supercritical fluids 2.2- Solubility measurements
characteristics, the solubility of a solid
dynamic technique for the pressure between To predict the solubility of a solute in supercritical fluids, EOS models are widely used. Cubic EOSs are the simplest equations capable of predicting and representing fluid phase equilibrium. Mixing rules are necessary when equations of state are applied to calculate the fluid mixtures thermodynamic properties. Although cubic EOS’s are the simplest mathematical models, capable of predicting fluid phase equilibrium, semi-empirical models are often utilized because of their relative ease of application Figure 1. Schematic diagram of the experimental
commonly based on providing a correlation apparatus:1) gas tank, 2 ) ball valve, 3,11) pressure gauge indicator, 4,8,12,14,15,18) needle valve, 5) Current investigation has been organized to pump, 6) filter 7) pre-heater, 9,10) equilibrium-sell 16) throttling valve , 17) constant temperature bath supercritical CO2 in low pressure range (80-140 bars). Results have been drawn as three isotherms ( in 308.15, 313.15 and 318.15K). through a 0.5μm filter, to reach the desired Stryjek and Vera equation of state was used pressure. The compressed fluid entered into to correlate the experimental data within the a preheating coil contained in a temperature- controlled electronic oven to achieve thermal equilibrium and passed into a solubility cell that was packed with pure Ibuprofen powder. The solute laden purged to the atmosphere in order to ensure the operational condition consistency. The sampling part was a ,
2- Experimental method
2.1- Materials
Ibuprofen (Sina Daru, 99.99% purity) was unilateral needle valves. This pass was kept (Roham Gaz, 99.95%) was also used as the minutes the purge valve was closed and the solvent. Ethanol (99.8%, Sigma Aldrich) was needle valves were opened orderly. A sample of supercritical solution was trapped into the Iranian Journal of Chemical Engineering, Vol.7, No. 4
sampling pass by closing the needle valves. The sampling equipment (coil and valves) affected by the supercritical solvent pressure marinated in the pure ethanol. The valves out and all the solute was washed out by solvent power to increase. In addition, the ethanol. The ethanol-Ibuprofen solution was prepared for GC test to determine the solute Table 1. Experimental molar fraction solubility of
T(K) P(MPa) y ×
operational pressure and temperature in all performed in triplicate in each operational 3- Results and discussion
3.1- Experimental results
shown in Fig. 2 and are supported by data in Figure 2. Experimental solubility data obtained in
308.15, 313.15 and 318.15 K and the pressure range
According to the experimental results, the mole fraction of ibuprofen in the fluid phase was in the range from 0.015 × 10-3 - 3.261 × Iranian Journal of Chemical Engineering, Vol. 7, No. 4
Measurement and Correlation of Ibuprofen in Supercritical Carbon Dioxide Using Stryjek and Vera EOS more effective factor. Because although the solubility power in a constant pressure, changes with the temperature increasingly in temperature, the E factor impression by the in the higher pressure ranges. This result can be interpreted by the iso-fugacity criteria 3.2- Correlation of solubility using Stryjek and
If the solid phase does not dissolve the SC- 2, solute solubility in the CO2-riched fluid phase at equilibrium can be calculated using ⎛ v (P P ) ⎞ the equation (1). The Stryjek and Vera EOS has been selected to calculate SCF At a constant pressure, both the E and sub value affect the solubility. At pressures higher than the crossover point (about 120 mixing rules may be used to calculate the bar), the effect of E is relative to the solid mixture parameter 'a' and 'b' in SV-EOS.
component sublimation pressure intensively. In low pressure ranges, molecular with the mixing and combining rules and the interactions between Ibuprofen and carbon dioxide become severely weak by increasing the temperature. On the other hand, in higher pressure ranges, sublimation pressure is the Table 2. Summary of the cubic EOS, mixing and combining rules and fugacity coefficient
v(v + b) + b(v b) ⎡ 2a y + 2 a a 1(− k 1 − a (b l (b + b 1 Iranian Journal of Chemical Engineering, Vol.7, No. 4
The Correlation is performed by minimizing the objective function of Average Absolute also used to predict the physicochemical and critical properties of the Ibuprofen that are interaction parameters (k12 and l12) showed the best fitting between the experimental data and the calculated values (by SV-EOS and van der Waals mixing rules) (Table 4). A A trial and error algorithm was provided and comparison between the correlation results optimized values computation. The loop was different mixing rules is illustrated in Fig. 3. Table 3. Physicochemical and critical properties of the ibuprofen and CO2
Ibuprofen 749.7a 2.33a 0.819a 182.1b 4.95c 8.97c 16.0c b Estimated by Immirzi and Perini method Table 4. Optimized interaction parameter for the modeling of Ibuprofen solubility in CO2
with the SV-EOS and the van der Waals mixing rules Parameter
Iranian Journal of Chemical Engineering, Vol. 7, No. 4
Measurement and Correlation of Ibuprofen in Supercritical Carbon Dioxide Using Stryjek and Vera EOS Table 5. Modified Mendez-Santiago-Teja modeling
results
Figure 3. Experimental solubility of Ibuprofen in SC-
CO2 at 308.15(+), 313.15(o) and 318.15K(∗) and
correlation results obtained with SV EOS using the
vdW1 and vdW2
Figure 4. Experimental solubility data for Ibuprofen
and values correlated by modified M-S-T model
3.3- Modeling with a density-based correlation
4- Conclusions
Ibuprofen in SC carbon dioxide as a function mathematical models using Stryjek and Vera of absolute temperature and solvent density, we used the semi-empirical Mendez-Santiago supercritical carbon dioxide. Solubility values were measured in a 308.15, 313.15 and 318.15K and 80-120 pressure range. The experimental data correlate well with the SV EOS model with an average absolute relative T ln yP = A + Bρ + CT deviation (AARD%) of 10–23% along with the vdW1 mixing rule and 6-14% along with values are presented in Table 5 in the three results than vdW1, which is probably due to The experimental results were plotted in the the two available adjustable parameters, form of T ln y P CT against the supercritical which can offer a higher flexibility to the CO2 density, to test the M-S-T model self- consistency (Fig. 4). The linear behavior solubility data. These data are also well shown in Fig. 4 confirms that the measured correlated by the semi-empirical model of solid solubility data are consistent at all modified Mendez–Santiago–Teja with an AARD% of 9–11%. The correlated parameters in the semi-empirical models are Iranian Journal of Chemical Engineering, Vol.7, No. 4
5- Nomenelature
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Iranian Journal of Chemical Engineering, Vol.7, No. 4

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