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Trong Dang-Vu*, Jan HUPKA∗

**CHARACTERIZATION OF POROUS MATERIALS BY CAPILLARY RISE METHOD
**

Received March 15, 2005; reviewed; accepted May 15, 2005 Capillary rise method is widely used for contact angle determination using Washburn equation. Penetration kinetics of porous media comprised from particles of varying size distribution was investigated. It was found that the penetration kinetics and the validation of Washburn’s theory depend not only on the particle size but also on the pore size distribution. The effect of particle size on contact angles was not observed. In case of bed consisting of wide size distribution particles, the smallest fraction plays a significant role creating the smallest capillaries and allowing for more even porous bed penetration. This increases precision of contact angle measurement. A difference of time between fluid flow through a porous bed and its complete saturation (∆tsf) was proposed as a new parameter describing capillary size distribution in porous media. It allows for fast estimation of both capillary size distribution in a porous bed and precision of contact angle determination. Key words: capillary rise, penetration kinetics, Washburn’s equation, porous media.

INTRODUCTION Capillary rise is a fundamental phenomenon existing in many natural processes and human activities [1]. Knowledge of capillarity laws is important in chemical, metallurgy, and ceramic industry, in oil recovery and civil engineering, in dyeing of textile fabrics, ink printing, and a variety of other fields. This explains the continuous interest in the subject from the side of industry and fundamental science. Experimental method based on capillary rise is widely used for porous media characterization (i.e. pore radius, contact angle, free surface energy). Among them measurement of height penetration and mass gain of wetting liquids in time are most commonly employed. In both approaches Washburn’s equation is a basic instrument for analysis of obtained results. For along time of using this equation, many modifications have been applied and although critics, Washburn’s equation presents useful model for evaluation of porous media observed in industrial practice.

∗

Department of Chemical Technology, Gdansk University of Technology, 80-952 Gdansk, Poland, jhupka@chem.pg.gda.pl

particles aggregation. the rate of liquid penetration is given as follows: dV = r 4 ∆Pπ dt 8ηh (1) The relationship between the liquid volume and height is given by: dV = r 2 πdh (2) The difference between capillary Pk (Eq. Measurements of penetration distance [12-16] and liquid mass gain [7.48 Trong Dang-Vu. which is very important in flotation. J. By assuming the steady-state flow and according to Poiseuille’s law expressing the balance between viscous forces and capillary and hydrostatics forces (neglecting inertial effects). It also enables to calculate the surface free energy. 3)) and hydrostatic pressure Ph (Eq. (1) the penetration rate is transformed into: dh r 2 ⎛ 2γ ⎞ = ⎜ cos θ − gρh ⎟ dt 8ηh ⎝ r ⎠ (6) .4)) allows calculating the pressure drop. However. 18] are two main experimental methods. 17. (2) and (5) to Eq. ∆P (Eq. Hupka Capillary rise method is used broadly for characterization of porous materials. 6-11]. The aim of this paper is to characterize the porous materials using capillary rise method and to study the effect of particle size on penetration kinetics and contact angles. it does not or not sufficiently study the effect of particle size of porous materials on the contact angles and penetration kinetics. in which Washburn equation is a basic instrument to analyze the obtained results. and stability of colloid system [4. 5)): Pk = 2γ cos θ r (3) (4) (5) Ph = gρh ∆P = 2γ cos θ − gρh r By substitution of Eq. WASHBURN’S EQUATION AND CAPILLARY RISE METHOD Capillary rise method allows determination of the radius of the porous media and contact angles of liquid on the solid surface [2-5].

Eq. However. 20-23]. (9): m = πRk2 hρε Substitution into Eq. Several restrictions are applied to this relationship: (a) steady-state laminar flow. (11)) present linear dependence of square of height penetration and square of liquid mass versus time. The relation between liquid mass and height in the column is linear as given by Eq.Characterization of porous materials by capillary rise method 49 Assuming that the hydrostatic pressure can be neglected in case of flow under capillary pressure. (8) gives: ⎡ r πR 2 2 ε 2 ⎤ ρ 2γ cos θ k ⎥ m2 = ⎢ t 2 η ⎢ ⎥ ⎣ ⎦ (9) ( ) (10) Which leads to m2 = where Cρ 2γ cos θ η 2 t (11) r πRk2 ε 2 C= 2 ( ) (12) Washburn’s equation (Eq. In case of porous media. the deviation from . (b) zero velocity of the liquid at solid/liquid interface. The modified Washburn’s equation is also used as dependence between wetting liquid mass and time [17]. which is observed by many researchers [2. Capillary radius r is equal to mean or equivalent pore radius. (7) with the initial condition (h = 0 at t = 0) [19]: h2 = rγ cos θ t 2η (8) Washburn’s equation presents linear dependence of square of height penetration of penetrating liquid in the tube versus time. (8)) and its modified form (Eq. and (d) negligible gravitation differences. (c) no external pressure. (6) can be rewritten as: h dh rγ cos θ = dt 4η (7) The Washburn’s equation is obtained after the integration of Eq. 5. Washburn’s theory assumes the model as a bundle of cylindrical capillaries. it means lack of slip (slip coefficient ε =0).

t)) [26] are proposed.0 21. non-uniform pore size distribution in porous media [1]. see Table 1.50 Trong Dang-Vu. It results that the influence of particle size on the penetration kinetics was observed. Hypothesis of non-uniform pore size distribution is cited in literature [1]. author did not study the bed with different pore size distribution. Table 1. Hupka linearity is also observed [1. or the change of start line of penetrating liquid into bed (the choice of the coordinate system (h. the effect of particle size is not observed. 17] [17] [28] [29] [13] [30] 0 – 123 0 – 123 < 106 106 – 300 300 – 425 37 46 5 – 10 44 – 53 204 – 208 105 – 125 125 – 149 149 – 177 250 – 297 297 – 350 100 – 120 450 – 520 0 – 500 7. However.8 15. As a reason the change of contact angles during capillary rise [27].5 28. THE EFFECT OF PARTICLE SIZE ON PENETRATION KINETICS AND CONTACT ANGLES The large number of particle size and type is used to study the effect of particle properties on the penetration kinetics and wettability by capillary rise method.22 9. J. In case of contact angles. so this shows lack of strong fundaments of hypothesis. Type and size of particle bed used for capillary rise investigation Type of bed Silica flour Alkyl-silane treated silica flour Glass Quartz particle Hydrophilic and hydrophobized quartz crystals Siliconized beads Particle size [µm] The effect of particles The larger particle size distribution the higher penetration rate The larger particle size distribution the higher penetration rate The effect of particle size on the contact angles is not observed The effect of particle size on the contact angles is not observed The effect of particle size on the contact angles is not observed The larger particle size distribution the higher penetration rate Literature [2. and this is not discussed in literature. 17. 24-26].6 38 – 75 75 – 150 Glass beads Limestone Sphalerite particles The larger particle size distribution the higher penetration rate [2] The larger particle size distribution the higher penetration rate The effect of particle size on the contact angles is not observed [18] [2] [17] [5] .

However.41 0.55 0.20 0. 0. The assumption of the present study is that packed beds with a comparable bulk density have similar spatial packing. and making up amorphous 2410 kg/m3 density glassy phase. penetration rate decreases with increasing in porous materials porosity.0 20. Table 2. see Table 3. for exfoliated graphite the situation is opposite. the packing procedure was run as follows: the particles with known mass were manually .92 Surface tension [mJ/m2] 72. [µm] 60 – 110 150 – 250 60 – 250 Porosity. For carbonized fir fibers and carbon fiber felts penetration rate of heavy oil increases with increasing in porous materials porosity. EXPERIMENTAL The investigation was carried out for glass beads containing: 70-73 % SiO2. The particles were manually placed in small. [m3/ m3] 0.3 21. [31]. 1. 7-11 % CaO and max.5 2. Characteristics of liquids used for capillary rise experiments (20°C) Wetting liquid Water Toluene Ethanol Heptane Octane Decane Density [kg/m3] 997 862 785 684 703 730 Viscosity [mPa⋅s] 1.9 Dielectric constant 78.30 Bulk density. Characteristics of bed of particles Symbol A B C Pore size. The time t = 0 approximately corresponded to the moment of column submersion in the wetting liquid.3 24 1. attached to a computer. The characteristics of particle bed are presented in Table 2. 13-15% Na2O. glass columns (0. Table 3.34 0.8 23. The procedure and repeatability of the packing play a key role in capillary rise method.7 cm inner diameter and 20 cm long) which were closed at the bottom by nonwoven fabric to support the bed.3 27. therefore a great care was taken when preparing the packed bed.0 The apparatus for the capillary rise experiments is shown in Fig.8 22.01 0. The decrease in mass of the container with the wetting liquid was recorded every second using an electronic balance.9 2.1 % Fe2O3.33 0.Characterization of porous materials by capillary rise method 51 Variable results were presented by Nishi et al.55 1. In order to obtain repeatable packing density. [kg/m3] 1589 1619 1678 Capillary rise experiments were carried out using liquids for which properties were readily available.9 1.

This leads to even packing of bed along the column. 1. The standard deviation of values of liquid mass for different bed packing is given by: s= ∑ (x n i =1 i −x ) 2 n −1 (13) where: xi . Porous materials with the same ratio of mass vs. Hupka introduced to the column.liquid mass in given time.52 Trong Dang-Vu.the number of values of liquid mass. In the procedure use in this work the whole particle mass is put to the column once. J. Fig. 6-camera. 7-micrometric screw Evaluation of repeatability of bed packing is based on the assertion that if the mass of liquid penetrating into different bed packing at the same interval time is comparable. which then was tapped many times from the height of 2 cm until the particle height reached the given value. height of packing in the column have the same bulk density. Adding particles as weight increments results in uneven packing because the lower layer has higher bulk density due to more tapping time. For this purpose the difference between the liquid mass for two bed packing after the same time is evaluated using FSnedecor and t-Student test.the arithmetic mean of liquid mass. 3-liquid front. not several times. Laboratory set-up used for measurements: 1-electronic balance. x . then the bed packing is repeatable. 4-particle bed. 5-column. n . . 2-covered container with wetting liquid.

05. the increase of liquid mass for packing height of 40 and 50 mm after 5. is put in the numerator and the smaller value in the denominator. .Characterization of porous materials by capillary rise method 53 Parameter F of F-Snedecor test is defined as follows: F= s12 2 s2 (14) 2 where s12 or s 2 .776. and 40 seconds. (14) and critical value Fcritic (from the table of F) with significance level α and number of degrees of freedom f1 and f2 (where f1 = n1 – 1 and f2 = n2 –1). so that F > 1. the bed packing for these three heights is not statistically different regarding precision and accuracy. otherwise the statistical difference is occurred. 50. From Table 4 it results that for bed heights of 40. The overlapping of curves in the plot indicates good repeatability of bed packing. The obtained results for penetration of heptane into bed A are presented in Table 4. Hence. otherwise the statistical difference is occurred. 30. the following conclusions can be drawn: if t < tcritic then values of standard deviation are not different regarding accuracy. 20. Parameter t of t-Student test is defined as follows: t= x1 − x2 2 s12 + s2 ⋅ n (15) From a comparison between t calculated using Eq. whichever is the larger. In order to evaluate the repeatability of bed packing. the following conclusions can be drawn: if F < Fcritic then values of standard deviation are not different regarding precision. For the remaining experimental system of wetting liquids and particle beds similar results are obtained. 15 and critical value tcritic (from the table of t) with significance level α and number of degrees of freedom f = n1 + n2 – 2. 50. critical values Fcritic = 19 and tcritic = 2. 20. RESULTS AND DISCUSSION REPEATABILITY OF BED PACKING The dependence of heptane mass increase vs. 10. The same procedure is repeated for packing height of 40 and 50 mm after 5. From a comparison between F calculated using Eq. With significance level of α = 0. and 60 mm packing height is shown in Fig. and 60 mm the conditions F < Fcritic and t < tcritic are satisfied. 10. 2. and 30 seconds are compared by means of the F-Snedecor and t-Student test. time for capillary tubes with 40.

0153 n=3 x = 0.279 s = 0.transition range 0 0 30 60 90 Time [s] Fig.379 s = 0.379 s = 0.56 2. Mass of liquid penetrating particle bed A vs.087 30 1. Hence.64 0.205 s = 0.246 0.25 1.360 0.324 40 1. F-test results of bed packing for heptane Time [s] 5 Height of bed [mm] 40 n=3 x = 0. J. penetration time .0098 n=3 x = 0.0119 n=3 x = 0.279 s = 0.454 s = 0. the proposed method satisfies the repeatable conditions of packed bed for the capillary rise method.28 0.0118 n=3 x = 0.411 0. Table 4.4 0.0096 n=3 x = 0.0131 n=3 x = 0.031 0.0123 n=3 x = 0.2 J . Hupka Similar results were obtained for other wetting liquids as well as remaining beds.67 1.457 s = 0.449 0.0101 60 n=3 x = 0.0070 n=3 x = 0.346 10 1.02 0.206 s = 0.8 Height of bed 40 mm 50 mm 60 mm J J J Mass of wetting liquid [g] 0.308 20 1.24 1.33 Calculated t for two heights of bed [mm] 40 i 50 50 i 60 0.6 0.0105 50 n=3 x = 0.210 s = 0. 2.0098 n=3 x = 0.0167 Calculated F for two heights of bed [mm] 40 i 50 50 i 60 1.276 s = 0.64 0.0116 n=3 x = 0.54 Trong Dang-Vu.456 s = 0.517 s = 0.523 s = 0.382 s = 0.0067 n=3 x = 0.

In order to better observation of liquid penetration into the bed. Particles of bed A are small and have narrow pore size distribution (see Table 2). 4. Particles of bed B are larger than A (see Table 2). through which the liquid flow is even. The liquid penetration into bed B was presented in Fig. therefore. and in the second one. When liquid rises to the top of the packed bed. they create the similar space in the column.Characterization of porous materials by capillary rise method KINETICS OF LIQUID PENETRATION. liquid penetrates capillaries in the bed at different . the spaces in the bed B are uneven. wetting liquid was dyed by potassium permanganate with concentration of 0. The liquid front rises uniformly until saturation. 3. t = t1 t = t2 t = t3 t = t4 Fig. t is penetration time. so liquid flow through the bed A is even. it is saturated immediately. the liquid mass increases gradually until it reaches a more or less constant value. In the first stage. In case of bed A.5 g/l. 3 shows stages of water penetration into bed A. the transition range (J) is short and clear due to even liquid penetration. 2) is distinguished two stages: penetration and saturation. It can be seen that penetration is uneven. Therefore. t4 > t3 > t2 > t1 The curve of dependence between liquid mass and penetration time (Fig. A DIFFERENCE OF TIME ∆TSF AS A NEW PARAMETER DESCRIBING CAPILLARY SIZE DISTRIBUTION IN POROUS MATERIALS 55 Fig. the liquid mass does not change due to saturation of the bed. Gradual penetration of wetting liquid into bed A.

so they create diversified capillaries.56 Trong Dang-Vu. so in Fig. i. while for bulk density of 6 kg/m3 transition range is not almost observable. so created capillaries in bed C are more homogeneous regarding the size than that in bed B. Despite of concluding larger particles. The transition range of bed B is long. When the kinetic of liquid penetration into bed A. 4. B. t is penetration time. [31]. In case of carbonized fir fibers for bulk density of 31 kg/m3 transition range is very sharp. transition range for bed C is clearer than that for bed B. then relatively fills quick somes and continues to penetrate remaining capillaries. 5 it can be seen the gentle section. the transition range is gentle and gradual. When all of capillaries are filled. and C is analyzed. It is in agreement with results of Nishi et al. penetration time for bed C is presented in Fig 6. At the beginning liquid penetrates all of capillaries. Hupka rates. the following conclusions are made: . It can be seen that transition range between penetration and saturation stages is long.e. In bed C the smaller pore size distribution of 60 – 110 µm fills the large space created by larger pore size distribution of 150 . 5 shows the dependence between heptane mass and penetration time for bed B. the saturation is taken place. Fig. The bed C is mixture of 50 % bed A and 50 % bed B. The difference between flow and penetration time ∆tsf is proposed as a new parameter characterizing porous materials. which prove that the transition range is clearer for higher bulk density of bed. J. Particles of bed B are large. as a consequence the difference between flow and saturation time is large (for heptane the difference of time ∆tsf for bed B for height of 60 mm is equal 25 s. It results that dependence have an intermediate character between the bed A and B. Gradual penetration of wetting liquid into bed B. but for bed A – 7 s).250 µm. t4 > t3 > t2 > t1 t =t4 The dependence of heptane mass vs. for smaller and more homogeneous. t =t1 t =t2 t =t3 Fig. and in case of height of 60 mm.

The bed with large and small particles characterizes small value of ∆tsf. so the pores in this bed are small. for example bed C. for example bed B. 3. 0. Coarse particles create the diversified capillaries regarding the size. For heptane penetration into bed A with height of 60 mm. Liquid penetrates these capillaries at different rates. the difference of time ∆tsf is small. ∆tsf is equal 7 s. 2. Mass of liquid penetrating particle bed B vs. the model of parallel capillaries with the same radius can be used. The model of parallel capillaries with different radii is used to describe the bed. the bed B at bed height of 60 mm. created by small particles. are small and homogeneous regarding the size. penetration time These observations can be interpreted using Washburn’s theory. Considering the liquid penetration into the bed with flow time tf and saturation time ts.Characterization of porous materials by capillary rise method 57 1. For example. the Washburn’s equation can be rewritten as follows: h 2 r f γ cos θ f = (16) η tf h 2 rsγ cos θ s = η ts (17) . To describe this bed. These pores are smaller than pores created by large particles only.6 Mass of wetting liquid [g] J J 0. In case of small particles. ∆tsf = 27 s. 5. This causes large ∆tsf.transition range Height of bed 0. Small particles fill large pores created by large particles. Capillaries.4 J .8 J 0. The large value of ∆tsf responses to large particles of bed.2 40 mm 50 mm 60 mm 0 0 40 80 120 160 Time [s] Fig.

4 J J Mass of wetting liquid [g] J 0.6 Height of bed 40 mm 50 mm 60 mm 0. 0. Eq. J. Mass of liquid penetrating particle bed C vs. . create small and homogeneous capillaries. Hupka where subscript f and s correspond to the liquid flow to the top of given bed height and its saturation. Combination of Eq. (16) and (17) leads to: ts − t f h 2 = ⎞ η ⎛ 1 1 ⎟ ⋅⎜ − γ ⎜ rs cos θ s r f cos θ f ⎟ ⎠ ⎝ (18) ∆t = h 2 ⋅ ⎞ η ⎛ 1 1 ⎟ ⋅⎜ − ⎜ rs cos θ s r f cos θ f ⎟ γ ⎝ ⎠ (19) Assumption of cos θ s = cos θ f = cos θ . (19) becomes: ∆t = h 2 ⋅ ⎛1 1⎞ ⋅⎜ − ⎟ γ cos θ ⎜ rs rf ⎟ ⎝ ⎠ η (20) where rf is radius of quick penetrating capillaries created in the bed. r f ≈ rs so t f ≈ t s . and time needed to fill these capillaries corresponds to flow time tf.transition range 0 0 15 30 45 60 Time [s] Fig. 6. as the consequence the difference of flow and saturation time is small. while rs is radius of slow penetrating capillaries and time needed to fill these capillaries corresponds to saturation time ts.58 Trong Dang-Vu. penetration time Particles of bed A are small with narrow pore size distribution.2 J .

ethanol – the slowest. Contact angles obtained for other liquids are presented in Table 5.(11).8 0. the smaller the ∆tsf and the clearer the transition range.998 Toluene 0.999 Octane 0. time. Contact angle values are calculated by means of Eq.999 Ethanol 0.2 Symbol Liquid R2 Water 0.4 0 0 30 60 90 120 Time [s] Fig. Although water faster penetrates than toluene. 7. Dependence of square of liquid mass vs. (11). created capillaries are heterogeneous and the value of ∆tsf is large.999 Square of liquid mass [g2] 0. This value allowed calculating of the contact angles for other liquids according to Eq.997 Heptane 0. 7 that water is the fastest penetrating liquid.Characterization of porous materials by capillary rise method 59 The lower the bed height. surface tension. and on plot of dependence of square of mass increasing vs. In case of bed B. 1. This means that the t ρ 2γ penetration rate is not proportional (correlational) with wettability of solid due to the complexity effect of viscosity. CONTACT ANGLES AND PORE RADIUS Wettability determination by capillary rise method is based on measurement of mass increasing of capillary tubes filled glass beads. The slope for toluene was calculated and used to determine C. time for bed A . particles are large. Fig. however toluene was assumed m2 η as the reference liquid according to its largest product ⋅ . It is seen from Fig. 7 shows the dependence between square of liquid mass and penetration time for bed A.999 Decane 0. and density of liquid. For all wetting liquids the dependences are linear and in agreement with Washburn’s equation.

The decreasing order of contact angles values: toluene > heptane > ethanol > water is in agreement with findings of Bruil and van Aartsen [12]. ra =3.5 µm THE EFFECT OF PARTICLE SIZE ON PENETRATION KINETICS AND WETTABILITY The relationship between liquid mass squared and time for beds B and C is presented in Fig. Eq. Slope and contact angles for bed A Wetting liquid Water Toluene Heptaen Octane Decane Ethanol Slope 0. 8 and Fig.0 2.60 Trong Dang-Vu. (12) can be rewritten: 2C r= (21) 2 πRk2 ε 2 ( ) hence.1x 3.0065 0. 9 . Table 5.8 2. [17]. respectively. In case of bed C (see Fig 9) the curves of relationship between square of liquid mass and time for all studied liquids are linear and in agreement with Washburn’s . The bed surface represents amphipatic (hydrophobic . therefore most researchers agree that the surface is hydrophilic. water contact angle on the surface of bed A is smaller than 90°. On the other hand.0036 0. 3.0152 0. In case of hydrocarbon. contact angles for strongly polar water are larger than that for the investigated hydrocarbons which are hydrophobic liquids. 32-34]. who studied wettability of aluminium powder. which contains coarser glass beads than bed A.916. it is shown that penetration rate increases and contact angle decreases as a function of the alkane length (number of carbon atoms). viscosity. This is in agreement with results obtained by other researchers [2. Hupka As show in Table 5. Such influence of the particle size on the kinetics of liquid flow was previously reported by Siebold et al. The values of C enables to determine the pore mean radius of bed A. J. This also can be clearly shown in Table 6: the coefficient of determination of heptane and decane for bed B is equal 0. It also results that the correlation between wettability.7 2. the function of heptane and decane is no longer linear.0110 0. Since hydrocarbons even better wet the bed than water. respectively. surface tension.0x10-16 θ [deg] 44 * 20 25 29 27 * Toluene was assumed as reference liquid.961 and 0.0030 C⋅cosθ x1016 2.0053 0.6 2.hydrophilic) properties. In case of bed B. and density of liquid are not observed.7 C 3.

It is shown that rb > ra > rc.9988 0. penetration time for bed B A mean radius of pore of bed B and C was calculated according to Eq (11).0096 0. coefficient of determination.0024 Bed C Coefficient of determination 0.0027 0.4 µm.9776 0.9938 0. and the results are rb =3.9 µm and rc =3. and contact angles for bed B and C Wetting liquid Water Toluene Heptane Octane Decane Ethanol Slope 0. .9972 0.4 0.9940 θ [deg] 54 * 21 25 28 23 * Toluene was assumed as reference liquid.0032 Bed B Coefficient of determination 0. 8.0117 0.6 Symbol Liquid Water Toluene Heptane Octane Decane Ethanol Square of liquid mass [g2] 0. Table 6. Slope.9990 0. so the pores in bed C are small.0047 0. Liquid penetrates bed C more uniformly than bed B.2 0 0 40 80 120 160 Time [s] Fig.9872 θ [deg] 38 * 50 26 52 27 Slope 0. Square of mass of wetting liquid vs.0085 0.9164 0. 0.0028 0.0056 0. because in bed C small particles of pore size distribution of 60 – 110 µm fill large pores created by larger particle of pore size distribution of 150 – 250 µm. and create small capillaries with comparable radii.9616 0.9765 0.0050 0.0178 0.Characterization of porous materials by capillary rise method 61 equation.9982 0.9989 0.0041 0.

It is seen from Table 5 and Table 6 that the contact angles are changed slightly with the particle size variation. This indicates that in case of mixing of two different pore size distributions of bed. This value allowed calculating of the contact angles of other liquids by means of Eq.2 0 0 40 80 120 Time [s] Fig. Water fastest penetrates and worst wets bed A and C. This is in agreement with data presented in literature [5.62 Trong Dang-Vu. which is mixture of bed A and B. 13. The slope for toluene was t ρ γ calculated and used to determine the constant C for bed B and C. 9. 28. The similar results are observed for bed B in spite of heptane and decane. . Except water. the slope for bed B is the largest. Therefore. The coefficient of determination of heptane and decane for bed B is very smaller than one. In comparing of three beds. the particle size does not influent on the contact angles. Hupka Analogously to case of bed A. for bed B and C toluene has largest product η m ⋅ 2 and was assumed as the reference wetting liquid. contact angle of liquids for all beds is comparable within measurement error limits. J. penetration time for bed C The radius of bed C. their curves are better described by parabolas.6 Symbol Liquid Water Toluene Heptane Octane Decane Ethanol Square of liquid mass [g2] 0. Square of mass of wetting liquid vs. and for bed C – smallest. 2 0. is comparable with radius of bed A. a smaller one plays a key role creating mean radius of the porous bed. (11) and obtained results are presented in Table 6. The slope of curves and contact angles regarding wetting liquid for bed A and C are identical. 29].4 0. see Table 5 and Table 6.

... J.. A simple procedure of preparing a packed bed was proposed for capillary rise method. REFERENCES 1. F... Effect of dynamic contact angles on capillary rise phenomena. 6 (1992) 413 – 428.t(0) is transferred to other one h’. t’. van Oss C. Determination of contact angles and pore sizes of porous media by column and thin layer wicking. When coordinate h(0). Walliser A. 2. Chaudhury M. these arguments are still discussed and were used only by author et al. A.. Raphaelides S. Contact angles of studied liquids are calculated basing on the contact angle of reference liquid and it depends on penetration rate.... J. Savopoulos T. Colloid Interface Sci. Siebold A. However. P. On the other hand. Colloid Surf.. by means of which the relationship between square of liquid mass and time will be linear. Oppliger M. Marmur A. including reference liquid. Schultz J. Technol. 39 (1992) 13 – 33.. [26. For the larger particles the application of Washburn’s equation is restricted due to uneven liquid rise in the bed and the deviation from linearity of dependence between square of liquid mass and penetration time is observed. D. Li Z. 35. 36]. It is the first time that the statistics test is used to evaluate the repeatability of packed bed and the obtained results confirm the accuracy of the proposed procedure. N. B. Adv.. Adhesion Sci. the particle size as well as pores size distribution do not influent on the values of contact angles due to the fundament (comparative) of capillary rise method using Washburn’s equation. Addition of fine particles to the bed increases the penetration rate of liquid and improves precision of the measurement. Therefore. and by the Gdansk University of Technology. A dynamic wicking technique for determining the effective pore radius of pregelatinized starch sheets. From present study it results that penetration kinetics as well as validation of Washburn’s equation depend not only on the particle size but also on the pore size distribution.. Karapantsios T. Murphy K. then the new equation rise will be obtained. Norris J.. CONCLUSIONS The Washburn’s equation is the useful tool for characterization of porous materials in case of small particles of bed... 35 (2004) 159 – 167. variation of particle size causes variation of penetration rate of all liquids. Colloid Surf. Labajos et al.Characterization of porous materials by capillary rise method 63 It can be seen that studied particle size influents on the penetration rate but not on contact angles. Giese R. K. [26] interpreted deviation from linearity by choice of coordinate system. Kalogianni E. 161 (2000) 81 – 87. J.. Capillary rise is a comparative method. . Penetration and displacement in capillary systems of limited size.. Nardin M. Good R.. 3. ACKNOWLEDGEMENTS The investigations were financed by the Polish Committee for Scientific Research within the framework of grant No. 4.

P.. 6. On the determination of the surface energetics of porous polymer materials. The influence of ultimate composition upon the wettability of carbon blacks.. 12 (1999) 1347 – 1357. J. Chibowski E. Heertjes P. Contact angles of quarts by capillary penetration of liquids and captive bubble techniques. Manas-Zloczower I. rough and porous solid surfaces. Neumann A. Part III: role of the contact angle..... 9 (1996) 727 – 741.. Colloid Polym.. Middea A. Colloid Surf.. Studebaker M. Int. V. Lins F. Eng... 19 (2002) 198 – 202. Rev. Adhesion Sci. B.. 18. J. van Aartsen J.. Hołysz L.. Colloid Polym. 17 (1921) 273 – 283. 33 (1998) 445 – 452. Lunkwitz K.. Grundke K.. 15. F. 14. Popovich L. Kwok D..4(1995) 185. Subrahmanyam T.. J. Snow C... Chibowski E.. Augsburg A. Sci.. Determination of surface free energy of interactive dry powder liposome formulations using capillary penetration technique. Hogg R.. Van Brakel J. W.. J. Prestidge C. Surface free energy components of α-alumina from thin layer wicking. Langmuir.. 16 (1977) 75 – 81. M. F. 22.. Langmuir. Progr. W. Colloids Surf. 59 (1955) 973 – 976. Mater. 11.. Contact angle and surface analysis studies of sphalerite particles.. Determination of the surface tension of microporous membranes using wetting kinetics measurements. Nardin M. Giese R. Capillary rise in porous media. Technol. L. Jacobasch H. L. 12. Burger W... Wetting measurements on smooth. 10. Eng. J.. W. Powder Technol. Colloid Surf. Oppliger M.64 Trong Dang-Vu. Li D. Hołysz L. Influence of physical and interfacial characteristics on the wetting and spreading of fluid on powders. Monte M. Varadaraj R. L. Part I: a problem.. M.... L. Grundke K.. Wawrzacz B. Heertjes P. Bogumil T. Subrahmanyam T. 8 (1992) 717 – 721. Sci.. Naim J... Ralston J. Feke D. Wettability studies of morphine sulfate powders. Surface free energy components of silica gel determined by the thin layer wicking method for different layer thicknesses of gel. 134 (1998) 299 – 304. Miner. Walliser A... Desai T.. Troger J. Bruil H. A. Wolfrom R. J. 13. 16. Solid surface free energy components determination by the thin-layer wicking technique.. Finlay W... 198 (2000) 201 – 212. J.. V. Capillary rise for thermodynamic characterization of solid particle surface.. Influence of surfactant structure on wettability modification of hydrophobic granular surfaces... J. B.. Capillary rise in porous media. Pharm.... Powder Technol. Miner. Powder Technol.. Wong J. 14 (2000) 765 – 775.. O. 6.. 186 (1997) 60 – 70.... M. 7. J. A. Wu W. . Heertjes P. 8. 23. rozprawa doktorska. 101 (1996) 58 – 68... A. Hupka 5. Politechnika Gdanska. Colloid Interface Sci. Powder Technol.. (1992) 1069 – 1090. 167 (1994) 207 – 210. 1998. Brons N. R. J. Schultz J. 8 (1992) 710 – 716... 24. Tsatouhas G. Washburn E. van Oss C. H. Adhesion Sci. The determination of contact angles of aqueous surfactant solutions on powders. 16 (1977) 91 – 96.. 252 (1974) 32 – 38.. 16 (1977) 83 – 90. Capillary rise in porous media. 9. The dynamics of capillary flow. Valdiviezo E.. Use of the Washburn equation for surface free energy determination... Siebold A. 19. Metallurg. Gietzelt T. 25.. 17. Prestidge C. Miner.. 104 (1999) 68 – 74. 20. Evaluation of capillary rise methods for determining wettability of powders. Van Brakel J. Bock J.. Chander S. Zushma S. J. Process. Part II: secondary phenomena. Chibowski E. Grundke K. 22 (2001) 107 – 113.. Colloid Interface Sci.. Sci... G. Interaction between proteins and inorganic oxides – adsorption of albumin and its desorption with a complexing agent.B. Van Brakel J. 21. Technol. Hołysz L.189. Wettability of Carbon Blacks. Phys. Y..

ang). ‘Functional Fillers and Nanoscale Minerals’.. Nishi Y. Zografi G.. 233 (2001) 356 – 360. J.. G. Różnica w czasie jaka wynika z przepływu cieczy przez ośrodek porowaty i je do całkowite nasyceniu cieczą (∆tsf) została zaproponowana jako mowy parametr opisujący rozkład wielkości porów w ciele porowatym. 30. 33. Brown S. że kinetyki penetracji i ważność prawa Washburna zalezą nie tylko od wielkości cząstek ale także od dystrybucji wielkości porów. Contact angles on particles and plates. Charakterystyka materiałów porowatych za pomocy metody wzniesienia kapilarnego.. M. 28. C.. 35. Iwashita N. Dang-Vu T.2002. K. Water Research. Inagaki M.. 27 (1987) 57-64. Inc. A... Comparison of the use of Washburn’s equation in the distancOn the use of Washburn’s equ-time and weighttime imbibition technique. Nie zaobserwowano wpływu wielkości dystrybucji cząstek na zmianę wielkości kąta zwilżania. J. Wersocki S. 122 (1988) 35 – 46. M.Characterization of porous materials by capillary rise method 65 26. To zjawisko ma wpływ na dokładność w dokładności mierzenia kąta zwilżania. Bruque J. Dang-Vu T. Yang Y.. 31. M. 240 (2001) 467 – 472.. Crawford. Miller E. Na podstawie przeprowadzonych badań okazało się. J. 2.. Colloid Interface Sci.. J. Sawada Y. L. Nalaskowski J. Gronzalez-Garcia C. 139 – 145.. Hupka J. Physicochemical Problems of Mineral Processing.. Gronzalez-Martin M. Oliveira R. II. B. Materiały The Third International Conference Environmental Technology for Oil Pollution. R. 211 (1999) 175 – 177. Parametr ten pozwala na szybkie określenie rozkładu wielkości porów oraz dokładne wyznaczenie kąta zwilżania. Labajos-Broncano L. Inżynieria Ekologiczna. Labajos-Broncano L. Moudgil. Colloid Interface Sci. J... Sorption kinetics of heavy oil into porous carbons.. Kellar. Washburn’a equation facing Galileo’s transformation: some remarks.. 36 (2002) 5029 – 5036... 36. Nylander T. M. Society for Mining. Herpefr. (2002) “Important of time evaluation in capillary rise method”. Bruque J.. A. Gronzalez-Martin M.. Colloid Interface Sci.. 34. część najdrobniejszych cząstek odgrywa istotna role w powstaniu najmniejszych kapilar. Capillary flow phenomena and wettability in porous media... Colloid Interface Sci. Janczuk B. M... 29. Bruque J. M. Hupka J. Badanie osadu czynnego jako sorbentu oleju. Hamraoui A. 253 (2002) 472 – 474.. M. Gonz C. J. Metallurgy and Exploration. 226 (2000) 199 – 204. Distance-time measurements in capillary penetration: choice of the coordinate system. Gonzalez-Martın M. Janczuk B. L... M.. 2003. Yaminski V... 39 (2005) 47-65 (w jęz. 27. Badane były kinetyki penetracji ciał porowatych złożonych z cząstek o różnych wymiarach. Ralston.. . L... M.. Dynamic flow studes. 08-11. Colloid Interface Sci... Moudgii B. Bruque J. 105 –112.. Colloid Interface Sci. Koopal.09. Gronzalez-Martin M. E. 9 (2003) 145 – 153. Dang-Vu T. Thuresson K. 32. Gronzalez-Garcia C.. Analysis of the Silica Surface Free Energy by the Imbibition.. Colloid Surf. M. Hupka J. Labajos-Broncano L. Can a dynamic contact angle be understood in terms of friction coefficient? J. Gdańsk. L.. Labajos-Broncano L. Metoda wzniesienia kapilarnego jest szeroko używana dla określenia kąta zwilżania przy wykorzystaniu równania Washburna. Colorado USA... ‘Method for characterizing the wettability of filler particles” in J. C. W.. J. które odgrywają istotną role w penetracji cieczy. W przypadku gdy placek składał się z cząstek o szerokiej dystrybucji wielkości.

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