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I.5.2. Apparatus and procedure Experimental Methods, Results and Discussion In this work, high pressure measurements for the CO2/perfluoroalkane mixtures were carried out using a visual synthetic method. The experimental apparatus used in this work has been described in detail elsewhere and a good agreement with literature data was obtained for phase equilibria for the system methane/hexadecane (Pauly et al., 2005). The experimental apparatus, shown in Figure II.15, is essentially made up of a variable volume high pressure cell. (6) (7) (5) (4) T P (3) mg mL (8) (9) (10) Figure II.15. Schematic diagram of the apparatus. (1) high-pressure variable-volume cell; (2) piezoresistive pressure transducers; (3) magnetic bar; (4) thermostat bath circulator; (5) thermometer connected to a platinium resistance; (6) endoscope plus a video camera; (7) screen; (8) perfluoroalkanes; (9) vacuum pump; (10) carbon dioxide (2) (1) It consists of a horizontal hollow stainless steel cylinder closed at one end by a movable piston. A sapphire window that allows visual observation of the entire fluid in study closes the other end. A second sapphire window is fixed on the cylinder wall in order - 69 -
Experimental Methods, Results and Discussion to light the fluid with an optical fiber. This orthogonal positioning of light and observation limits the parasitic reflections and thus improves the observation in comparison to an axial lighting. A video acquisition system made up of an endoscope plus a video camera is placed behind the sapphire windows in order to display on the screen of a computer what happens inside the measuring cell. A small magnetic bar is placed inside the cell to allow the homogenization of the mixture by means of an external magnetic stirrer. Due to the presence of this magnetic stirring bar as well as of the second window, the minimum internal volume is limited to 8 cm 3 whereas the maximum volume was fixed to 30 cm 3 to limit the size of the cell and thus to reduce thermal inertia and temperature gradients within the cell. The temperature of the cell is kept constant by circulating a heat-carrier fluid thought three flow lines directly managed in the cell. This heat-carrier fluid is thermoregulated with temperature stability of 0.01 K by means of a thermostat bath circulator (HAAKE). The temperature is measured with a high precision thermometer, Model PN 5207 with an accuracy of 0.01K connected to a calibrated platinum resistance inserted inside the cell close to the sample. The pressure is measured by a piezoresistive silicon pressure transducer (Kulite) fixed directly inside the cell to reduce dead volumes. However, as this pressure transducer is placed inside the cell, it is subjected to changes in temperature and it needs to be calibrated. This calibration was done in the temperature range 273-507 K, by means of dead weight gauge (Bundenberg) with accuracy better than 0.02 %. The accuracy of the transducer in the experimental range studied is 0.2 MPa. The binary mixtures are prepared directly in the measuring cell. The cell is first loaded with a known amount of liquid perfluoroalkane by vacuum extraction. The exact mass of liquid introduced is determined by weighting the cell during its introduction with a precision balance (Ohaus) with an accuracy of 0.1 mg. The carbon dioxide is then added under pressure. For this purpose, the gas is initially loaded at saturation pressure in an aluminium reservoir tank (Gerzat) fixed in the plate of high weight / high precision balance having a maximum weighting capacity of 2000 g with an accuracy of 1 mg (Sartorius) and connected to the measuring cell by means of a flexible high pressure capillary. The needed amount of gas is then transferred from the gas container to the measuring cell. The exact - 70 -
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Ana Maria Antunes Dias Universidade
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o júri presidente Prof. Dr. Joaqui
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palavras-chave resumo perfluoroalca
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Contents Notation List of Tables Li
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Notation Abbreviations AAD EoS LCST
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List of Tables Table I.1 Average Bo
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Table III.6 Adjusted Binary Paramet
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Figure II.9 Comparison between corr
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Figure III.8 Temperature-density di
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Figure III.25 Vapor-phase mole frac
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I.1. Fluorine Properties General In
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Table I.2. Physicochemical Properti
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General Introduction order to compa
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General Introduction the numerous a
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General Introduction carbon dioxide
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General Introduction animals. That
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General Introduction Table I.3. Lit
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References General Introduction Ban
Page 37 and 38: General Introduction Hildebrand, J.
Page 39 and 40: General Introduction Rowinsky EK. N
Page 41 and 42: II. Part EXPERIMENTAL METHODS, RESU
Page 43 and 44: Experimental Methods, Results and D
Page 49 and 50: Table II.3. (continued) T K ρexp g
Page 51 and 52: ρ / g.cm-3 1.750 1.730 1.710 1.690
Page 55 and 56: I. 3. Vapour pressure I.3.1. Biblio
Page 57 and 58: I.3.2. Apparatus and Procedure Expe
Page 59 and 60: I.3.3. Experimental Results and Dis
Page 63 and 64: Table II.8. (continued) T K Pexp kP
Page 67 and 68: ΔH vap = TΔS vap 2⎛ d ln P ⎞
Page 69 and 70: I.4. Solubility at atmospheric pres
Page 79 and 80: x2 (T,P2) 7.0E-03 6.0E-03 5.0E-03 4
Page 81 and 82: L 2,1 0.70 0.60 0.50 0.40 0.30 285
Page 87: Experimental Methods, Results and D
Page 93 and 94: P / MPa 6 5 4 3 2 1 0 P / MPa 14 12
Page 95 and 96: II.6. Liquid - Liquid Equilibrium I
Page 101 and 102: 0 τ β Δ1 2Δ1 [ 1+ B τ + B τ +
Page 103 and 104: References Experimental Methods, Re
Page 111 and 112: III.1. Introduction Modeling Most c
Page 113 and 114: Modeling The pioneering work of Wer
Page 115 and 116: III.2. Soft-SAFT Model Modeling A S
Page 117 and 118: Modeling The equation of state is w
Page 119 and 120: Chain Term Modeling Originally Wert
Page 121 and 122: Modeling The model is easily extend
Page 123 and 124: ( ) ( ) ∑∑∑ 3 2 2 2 2 qq 32π
Page 125 and 126: Modeling HRT is a promising theory,
Page 127 and 128: ( ρ) ρ , 0 ≤ ρ ( ρ) 2 Modelin
Page 129 and 130: III.3. Application to Pure Compound
Page 131 and 132: Modeling From the optimised paramet
Page 133 and 134: T / K 400 350 300 250 200 150 100 5
Page 135 and 136: ln Pvap 1.0E+01 1.0E+00 1.0E-01 1.0
Page 137 and 138: Modeling Table III.2. Absolute Aver
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Modeling The correlation coefficien
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Pvap (MPa) 4.00 3.50 3.00 2.50 2.00
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Modeling The mixture parameters a a
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Modeling the assumptions made by th
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Modeling between oxygen and perfluo
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xSolute 5.5E-03 5.0E-03 4.5E-03 4.0
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Modeling previous work, dealing wit
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Modeling These results confirm that
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Modeling CO2 binary mixtures using
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Modeling average deviation (AAD) be
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P / MPa 14 12 10 8 6 4 2 0 0 0.2 0.
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Modeling Figures III.16, III.17 and
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Modeling calculations from the orig
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Table III.9. References for VLE exp
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P / MPa 20 18 16 14 12 10 8 6 4 2 0
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Modeling Finally, Figure III.24 pre
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III.4.4. VLE and LLE of Alkane and
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Modeling number of perfluro-n-alkan
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y C6F14 1.0 0.8 0.6 0.4 0.2 0.0 0.0
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P / MPa 0.08 0.07 0.06 0.05 0.04 0.
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P / MPa 0.12 0.10 0.08 0.06 0.04 0.
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Modeling approach based on the meth
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Modeling Blas, F. J.; Vega, L. F.,
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DIPPR, Thermophysical Properties Da
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Modeling Hildebrand, J. H.; Fisher,
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Modeling McCabe, C.; Jackson, SAFT-
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Modeling Poling, B.; Prauznitz, J.;
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Modeling Wertheim, M. S., Fluids wi
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