CA2968623A1 - A multifunctional apparatus for measuring induction time, surface and interfacial properties - Google Patents
A multifunctional apparatus for measuring induction time, surface and interfacial properties Download PDFInfo
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Abstract
A method and apparatus for measuring induction time, surface and interfacial properties of flotation separation systems is provided, the induction time is the minimum time required for establishing attachment between any two phases of gas, liquid and solid or between two different liquid phases; the surface and interfacial properties include, but not limited to, contact angle between a liquid and a solid phase, surface tension/energy of a liquid-air interface, interfacial tension/energy of two liquid interface, surface energy of a solid-air or solid-liquid interface.
The method of measuring induction time comprises (a) moving a gas bubble, preferably an air bubble to a solid particle bed or a flat surface of a solid substrate in a testing liquid and then holding for a specified time period of contacting prior to moving it away from the solid particle bed or the solid substrate, and observing whether attachment is established or not; (b) moving a drop of the testing liquid to a solid particle bed or a flat surface of a solid substrate exposing in the air environment directly and observing whether attachment is established or not. The method of measuring surface and interfacial properties of flotation separation systems comprises (a) both static and dynamic sessile drop and pendent drop methods, (b) Du Noüy ring, Du Noüy-Padday rod and Wilhelmy plate methods. The method also includes a simultaneous estimation of air bubble impact force for each induction time measurement.
The apparatus comprises an advanced video system that includes a high speed CMOS or CCD camera with 200-2000 frames per second (fps), a lens (preferably a telecentric lens with adjustable focus, zoom and iris) and a LED or optical telecentric backlight illuminator, a sample stage with three-way translation and a heater, a main motorized vertical stage holding a voice coil motor or a speaker, a precision micro (preferably submicron)-displacement sensor and a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements.
The method of measuring induction time comprises (a) moving a gas bubble, preferably an air bubble to a solid particle bed or a flat surface of a solid substrate in a testing liquid and then holding for a specified time period of contacting prior to moving it away from the solid particle bed or the solid substrate, and observing whether attachment is established or not; (b) moving a drop of the testing liquid to a solid particle bed or a flat surface of a solid substrate exposing in the air environment directly and observing whether attachment is established or not. The method of measuring surface and interfacial properties of flotation separation systems comprises (a) both static and dynamic sessile drop and pendent drop methods, (b) Du Noüy ring, Du Noüy-Padday rod and Wilhelmy plate methods. The method also includes a simultaneous estimation of air bubble impact force for each induction time measurement.
The apparatus comprises an advanced video system that includes a high speed CMOS or CCD camera with 200-2000 frames per second (fps), a lens (preferably a telecentric lens with adjustable focus, zoom and iris) and a LED or optical telecentric backlight illuminator, a sample stage with three-way translation and a heater, a main motorized vertical stage holding a voice coil motor or a speaker, a precision micro (preferably submicron)-displacement sensor and a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements.
Description
A Method And Apparatus For Measuring Induction Time, Surface And Interfacial Properties Inventor: Guoxing Gu (Edmonton, CA) Field of the Invention 100011 This invention relates to a method and apparatus for measuring induction time, surface and interfacial properties of flotation separation systems.
Background 100021 Flotation is an important separation technique which has been used for a century in the mining industry for recovery of valuable minerals. Flotation has also been adapted by other industries, e.g. the pulp and paper industry for separation of ink, toner, and other unwanted contaminants from wood fibers during waste paper recycle operations. In Canadian oil sands operation, flotation has been used to recover bitumen from oil sands. Air-particle or air-bitumen attachment is an essential step for a successful flotation and is strongly dependent on the chemistry of a flotation system. The attachment process involves thinning and rupture of the intervening film between the two interacting phases. In a broad sense, the minimum time required for the film to thin to a critical thickness and rupture spontaneously to form a stable two-phase attachment in a liquid is defined as the induction time. The induction time plays a critical role in flotation. Under a given hydrodynamic condition, the shorter the induction time is, the higher is the flotation recovery (Jowett, A., 1980. Formation and disruption of particle-bubble aggregates in flotation. In: Somasundaran, P. (Ed.), Fine Particle Processing.
Proceedings of the International Symposium, Las Vegas, Nevada, February 1980, vol. 1.
AIME, New York, pp. 720-754.; Yoon, R.H. and Yordan, J.L., 1991. Induction time measurements for the quartz¨amine flotation system. J. Colloid Interface Sci.
141 (2), 374-383.). The thinning and rupture process consists of three fundamental stages:
(1) film thinning from an original thickness to a critical thickness; (2) film rupture from the critical thickness to the formation of a nuclei hole with a critical radius forming a three-phase contact (TPC) line;
and (3) the TPC line expansion from the critical radius to a minimum radius (r5) required for a stable attachment. The measured induction time (t) as such consists of three components: the time required for film thinning (1t), film rupture (4) and TPC line expansion (te), i.e.
t = t, +t. +t (1) Since it is fairly difficult to accurately measure these times separately, in practice, they have been measured collectively and referred to as the induction time.
[0003] The concept of induction time was first introduced by Sven-Nilsson, I., (1934. Effect of contact time between mineral and air bubbles on flotation. Kolloid-Z. 69
Background 100021 Flotation is an important separation technique which has been used for a century in the mining industry for recovery of valuable minerals. Flotation has also been adapted by other industries, e.g. the pulp and paper industry for separation of ink, toner, and other unwanted contaminants from wood fibers during waste paper recycle operations. In Canadian oil sands operation, flotation has been used to recover bitumen from oil sands. Air-particle or air-bitumen attachment is an essential step for a successful flotation and is strongly dependent on the chemistry of a flotation system. The attachment process involves thinning and rupture of the intervening film between the two interacting phases. In a broad sense, the minimum time required for the film to thin to a critical thickness and rupture spontaneously to form a stable two-phase attachment in a liquid is defined as the induction time. The induction time plays a critical role in flotation. Under a given hydrodynamic condition, the shorter the induction time is, the higher is the flotation recovery (Jowett, A., 1980. Formation and disruption of particle-bubble aggregates in flotation. In: Somasundaran, P. (Ed.), Fine Particle Processing.
Proceedings of the International Symposium, Las Vegas, Nevada, February 1980, vol. 1.
AIME, New York, pp. 720-754.; Yoon, R.H. and Yordan, J.L., 1991. Induction time measurements for the quartz¨amine flotation system. J. Colloid Interface Sci.
141 (2), 374-383.). The thinning and rupture process consists of three fundamental stages:
(1) film thinning from an original thickness to a critical thickness; (2) film rupture from the critical thickness to the formation of a nuclei hole with a critical radius forming a three-phase contact (TPC) line;
and (3) the TPC line expansion from the critical radius to a minimum radius (r5) required for a stable attachment. The measured induction time (t) as such consists of three components: the time required for film thinning (1t), film rupture (4) and TPC line expansion (te), i.e.
t = t, +t. +t (1) Since it is fairly difficult to accurately measure these times separately, in practice, they have been measured collectively and referred to as the induction time.
[0003] The concept of induction time was first introduced by Sven-Nilsson, I., (1934. Effect of contact time between mineral and air bubbles on flotation. Kolloid-Z. 69
(2) 230-232) who measured induction time by moving a captive bubble toward and then away from a flat mineral surface. fie considered induction time to be the minimum contact time for successful thinning of the intervening liquid film to critical thickness where film rupture occurs. The induction time was subsequently measured by moving a mineral surface or a bed of small mineral particles in a solution toward and then away from a fixed captive bubble (Eigeles, M.A., Volova, M.L., 1960. Kinetic investigation of effect of contact time, temperature and surface condition on the adhesion of bubble to mineral surfaces. Proc. 5th Int. Mineral Processing Congr. (London). Inst. Min. Metall., London, 271-284.) Glembotsky, V.A., (1953. The time of attachment of air bubble to minerals in flotation and its measurement (in Russian). Izv. Akad. Nauk SSSR 11, 1524-1531.) also developed a technique to determine the induction time. This method was adopted by Yoon and Yordan (1991) and Ye et al. (1989.
Induction time measurements at a particle bed. Int. J. Miner. Process. 25, 221-240).
[0004] Gu, et al (2003. Effects of physical environment on induction time of air-bitumen attachment. Int. J. Miner. Process. 69, 235-250), refined the induction timer by using a video-assisted system to monitor the contact process and a high speed data processing system to accurately control the contact time to determine the induction time. A
schematic of the induction timer is shown in Chart 1.
____________________ DA __ Amplifier Speaker PC¨
AD Capillary _________________________________________ 77 tube Micro-___________________________ displacement ¨ Water sensor jacket = \
) ___________________________ CCD __ II
Monitor Sample Work station .1"
Chart 1. A schematic of the setup used for measuring induction time.
[0005] With this refined induction timer, it was found that the measured induction time is highly dependent on the physical and mechanical parameters involved in the measurement.
The parameters examined include the initial gap (170) between the air bubble and the particle bed, the displacement (Ho) of the air bubble holder, the diameter (db) of the air bubble and the velocities of the air bubble approaching (ua) to and retracting (u,.) from the particle bed as shown in Chart 2.
Induction time measurements at a particle bed. Int. J. Miner. Process. 25, 221-240).
[0004] Gu, et al (2003. Effects of physical environment on induction time of air-bitumen attachment. Int. J. Miner. Process. 69, 235-250), refined the induction timer by using a video-assisted system to monitor the contact process and a high speed data processing system to accurately control the contact time to determine the induction time. A
schematic of the induction timer is shown in Chart 1.
____________________ DA __ Amplifier Speaker PC¨
AD Capillary _________________________________________ 77 tube Micro-___________________________ displacement ¨ Water sensor jacket = \
) ___________________________ CCD __ II
Monitor Sample Work station .1"
Chart 1. A schematic of the setup used for measuring induction time.
[0005] With this refined induction timer, it was found that the measured induction time is highly dependent on the physical and mechanical parameters involved in the measurement.
The parameters examined include the initial gap (170) between the air bubble and the particle bed, the displacement (Ho) of the air bubble holder, the diameter (db) of the air bubble and the velocities of the air bubble approaching (ua) to and retracting (u,.) from the particle bed as shown in Chart 2.
- 3 -Ur U. HO
ho -)1c51:1õ
00 = = 11111110 00 ---------- 00 Chart 2. An air bubble attaching surface of solid particles in a testing solution.
[0006] Theoretical studies on film thinning (Jowett, 1980; Scheludko, 1967.
Thin liquid films. Adv. Colloid Interface Sci. 1, 391-464.; Malhotra and Wasan, 1986.
Stability of foam and emulsion films: effects of the drainage and film size on critical thickness of rupture.
Chem. Eng. Commun. 48, 35-56.), film rupture (Taylor and Michael, 1973. On making holes in a sheet of fluid. J. Fluid Mech. 58 (4), 625-639.; Prokhorov and Derjaguin, 1988. On the generalized theory of bilayer film rupture. J. Colloid Interface Sci. 125 (1), 111-121.) and TPC line expansion (Ye et al., 1989) also showed that the induction time measured by moving an air bubble toward and then away from a mineral bed in a liquid is a function of particle size (dp), density and contact angle of the particles, air bubble diameter (db), velocities of the air bubble approaching (ua) to and retracting (Ur) from the mineral bed, the initial gap (h0) between the bubble and the particle bed, viscosity, density and surface tension of the liquid and the three-phase contact line tension. Eigeles and Volova (1960) recognized a stronger effect of particle size on measured induction time than that predicted. The measured induction time was reported to increase with increasing particle size. Yoon and Yordan (1991) and Ye et at. (1989) reported a power law dependence between measured induction time and particle size, which is consistent with theoretical analysis (Jowett, 1980; Li et al., 1990. Rate of
ho -)1c51:1õ
00 = = 11111110 00 ---------- 00 Chart 2. An air bubble attaching surface of solid particles in a testing solution.
[0006] Theoretical studies on film thinning (Jowett, 1980; Scheludko, 1967.
Thin liquid films. Adv. Colloid Interface Sci. 1, 391-464.; Malhotra and Wasan, 1986.
Stability of foam and emulsion films: effects of the drainage and film size on critical thickness of rupture.
Chem. Eng. Commun. 48, 35-56.), film rupture (Taylor and Michael, 1973. On making holes in a sheet of fluid. J. Fluid Mech. 58 (4), 625-639.; Prokhorov and Derjaguin, 1988. On the generalized theory of bilayer film rupture. J. Colloid Interface Sci. 125 (1), 111-121.) and TPC line expansion (Ye et al., 1989) also showed that the induction time measured by moving an air bubble toward and then away from a mineral bed in a liquid is a function of particle size (dp), density and contact angle of the particles, air bubble diameter (db), velocities of the air bubble approaching (ua) to and retracting (Ur) from the mineral bed, the initial gap (h0) between the bubble and the particle bed, viscosity, density and surface tension of the liquid and the three-phase contact line tension. Eigeles and Volova (1960) recognized a stronger effect of particle size on measured induction time than that predicted. The measured induction time was reported to increase with increasing particle size. Yoon and Yordan (1991) and Ye et at. (1989) reported a power law dependence between measured induction time and particle size, which is consistent with theoretical analysis (Jowett, 1980; Li et al., 1990. Rate of
- 4 -collection of particles by flotation. Ind. Eng. Chem. Res. 29 (6), 955-967.).
Dobby and Finch (1987. Particle size dependence in flotation derived from a fundamental model of the capture process. Int. J. Miner. Process. 21, 241¨ 260.) proposed an indirect method to assess the induction time. When attachment is achieved, induction time is considered equal to the time for a particle to slide around a bubble from the point of contact to the point where it stops moving (Schulze and Gottschalk, 1981. Investigations of the hydrodynamic interaction between a gas bubble and mineral particles in flotation. In: Laskowski, J.
(Ed.), Proceedings, 13th Int. Min. Proc. Congr., Warsaw, June 1979. Elsevier, New York, pp. 63-84.
Part A).
100071 Gu et al (2004. A novel experimental technique to study single bubble¨bitumen attachment in flotation Int. J. Miner. Process. 74, 15-29) built another setup for studying small single bubble-bitumen attachment. This unique apparatus is capable of generating individual hydrogen bubbles with a desired size larger than 10 [im. Once a hydrogen bubble of a desired diameter is produced via electrodes and a bubble collection mechanism, it is released to contact a suspended bitumen droplet. The entire process of bubble sliding and attachment is recorded with a high speed digital imaging system for subsequent playback and analysis. A
number of factors that affect bitumen flotation were studied with this technique, including process temperature, bubble size and aqueous phase chemistry. The results showed that higher process temperature and smaller bubble size are favorable to bitumen flotation. It was found that the maximum (critical) bubble size required for effective bitumen flotation is highly dependent on dissolved air content and ionic composition in the aqueous phase.
For experiments where the aqueous phase chemistry resembled that typically found in the oil sands industry, only very small bubbles were found to attach to the bitumen droplet.
Dobby and Finch (1987. Particle size dependence in flotation derived from a fundamental model of the capture process. Int. J. Miner. Process. 21, 241¨ 260.) proposed an indirect method to assess the induction time. When attachment is achieved, induction time is considered equal to the time for a particle to slide around a bubble from the point of contact to the point where it stops moving (Schulze and Gottschalk, 1981. Investigations of the hydrodynamic interaction between a gas bubble and mineral particles in flotation. In: Laskowski, J.
(Ed.), Proceedings, 13th Int. Min. Proc. Congr., Warsaw, June 1979. Elsevier, New York, pp. 63-84.
Part A).
100071 Gu et al (2004. A novel experimental technique to study single bubble¨bitumen attachment in flotation Int. J. Miner. Process. 74, 15-29) built another setup for studying small single bubble-bitumen attachment. This unique apparatus is capable of generating individual hydrogen bubbles with a desired size larger than 10 [im. Once a hydrogen bubble of a desired diameter is produced via electrodes and a bubble collection mechanism, it is released to contact a suspended bitumen droplet. The entire process of bubble sliding and attachment is recorded with a high speed digital imaging system for subsequent playback and analysis. A
number of factors that affect bitumen flotation were studied with this technique, including process temperature, bubble size and aqueous phase chemistry. The results showed that higher process temperature and smaller bubble size are favorable to bitumen flotation. It was found that the maximum (critical) bubble size required for effective bitumen flotation is highly dependent on dissolved air content and ionic composition in the aqueous phase.
For experiments where the aqueous phase chemistry resembled that typically found in the oil sands industry, only very small bubbles were found to attach to the bitumen droplet.
- 5 -[0008] Wang et al (2013. Measurement of interactions between solid particles, liquid droplets, and/or gas bubbles in a liquid using an integrated thin film drainage apparatus, Langmuir 2013, 29, 3594- 3603.) upgraded Gu et al's setup by integrating a piezoelectric bimorph force sensor and two CCD cameras to achieve direct and simultaneous measurements of force barrier, true film drainage time, and bubble/droplet deformation under a well-controlled external force, receding and advancing contact angles, capillary force, and adhesion (detachment) force between an air bubble or oil droplet and a solid, a liquid, or an air bubble in an immiscible liquid.
[0009] The induction time setup (Gu, et al, 2003.) and its upgraded version (Wang et al, 2013) with a piezoelectric bimorph force sensor and two CCD cameras are both in the shape of prototypes, which have not been optimized to be a professional apparatus that can provide a higher performance in all aspects. e.g. higher image quality at high frame rate for both online static and dynamics image processing rather than playback processing.
[0010] One object of present invention is to provide an optimized apparatus for induction time measurement.
[0011] Another object of present invention is to simplify the upgraded version of induction time setup (Wang et al, 2013) to reduce overall cost.
[0012] Another object of present invention is to provide a multifunctional apparatus to measure impact force of an air bubble or a liquid drop toward a surface of a particle bed or a substrate, surface and interfacial properties, e.g. contact angle of a liquid contacting a solid
[0009] The induction time setup (Gu, et al, 2003.) and its upgraded version (Wang et al, 2013) with a piezoelectric bimorph force sensor and two CCD cameras are both in the shape of prototypes, which have not been optimized to be a professional apparatus that can provide a higher performance in all aspects. e.g. higher image quality at high frame rate for both online static and dynamics image processing rather than playback processing.
[0010] One object of present invention is to provide an optimized apparatus for induction time measurement.
[0011] Another object of present invention is to simplify the upgraded version of induction time setup (Wang et al, 2013) to reduce overall cost.
[0012] Another object of present invention is to provide a multifunctional apparatus to measure impact force of an air bubble or a liquid drop toward a surface of a particle bed or a substrate, surface and interfacial properties, e.g. contact angle of a liquid contacting a solid
- 6 -surface, surface tension of a liquid exposing in the air, interfacial tension of two intervening liquids.
[0013] Another object of present invention is to provide a multifunctional apparatus to measure surface and interfacial properties using sessile drop method and pendant drop method in conjunction with drop shape profile digitization and analysis.
[0014] The sessile drop method is used for the characterization of solid surface energies, and in some cases, aspects of liquid surface energies as shown in Chart 3a. The main premise of the method is that by placing a droplet of liquid with a known surface energy, the shape of the droplet, specifically the contact angle, and the known surface energy of the liquid are the parameters which can be used to calculate the surface energy of the solid sample. The liquid used for such experiments is referred to as the probe liquid, and the use of several different probe liquids is required.
hg Ysg (a) (b) Chart 3. An illustration of (a) the sessile drop and (b) the pendent drop methods, where 0 is the contact angle, and 7,g , 71g , 7,1 represent the solid-gas, gas-liquid, and liquid-solid interfaces, respectively, d is the tube diameter, m is the weight of the pendent drop.
[0013] Another object of present invention is to provide a multifunctional apparatus to measure surface and interfacial properties using sessile drop method and pendant drop method in conjunction with drop shape profile digitization and analysis.
[0014] The sessile drop method is used for the characterization of solid surface energies, and in some cases, aspects of liquid surface energies as shown in Chart 3a. The main premise of the method is that by placing a droplet of liquid with a known surface energy, the shape of the droplet, specifically the contact angle, and the known surface energy of the liquid are the parameters which can be used to calculate the surface energy of the solid sample. The liquid used for such experiments is referred to as the probe liquid, and the use of several different probe liquids is required.
hg Ysg (a) (b) Chart 3. An illustration of (a) the sessile drop and (b) the pendent drop methods, where 0 is the contact angle, and 7,g , 71g , 7,1 represent the solid-gas, gas-liquid, and liquid-solid interfaces, respectively, d is the tube diameter, m is the weight of the pendent drop.
- 7 -The shape of a liquid-vapor interface is determined by the Young-Laplace equation, with the contact angle playing the role of a boundary condition via Young's Equation.
The shape profile of the sessile drop is digitized and analyized using Young-Laplace equation for contact angle calculation. The theoretical description of contact arises from the consideration of a thermodynamic equilibrium between the three phases: the liquid phase (L), the solid phase (S), and the gas or vapor phase (G) (which could be a mixture of ambient atmosphere and an equilibrium concentration of the liquid vapor). (The "gaseous" phase could be replaced by another immiscible liquid phase.) If the solid-vapor interfacial energy is denoted by 7,,, the solid-liquid interfacial energy by and the liquid¨vapor interfacial energy (i.e. the surface tension) by ygi , then the equilibrium contact angle 0 is determined from these quantities by Young's Equation:
ysg=ylg= cos + y,1 (2) The contact angle can also be related to the work of adhesion via the Young¨Dupre equation:
A Wsõ = y(1 + cos 0) (3) where A W,õ is the solid-liquid adhesion energy per unit area when in the medium V.
[0015] The pendant drop method is a technique by which a drop of liquid is suspended from a tube (capillary or needle) in a bulk liquid or gaseous phase. The shape of the drop results from the relationship between the surface tension or interfacial tension and gravity. In the pendant drop method, the surface tension or interfacial tension is calculated from the shadow image of a pendant drop using drop shape analysis in accordence with Young-Laplace equation as shown in Chart 3b. The force due to surface tension is proportional to the length of the boundary between the liquid and the tube, with the proportionality constant usually
The shape profile of the sessile drop is digitized and analyized using Young-Laplace equation for contact angle calculation. The theoretical description of contact arises from the consideration of a thermodynamic equilibrium between the three phases: the liquid phase (L), the solid phase (S), and the gas or vapor phase (G) (which could be a mixture of ambient atmosphere and an equilibrium concentration of the liquid vapor). (The "gaseous" phase could be replaced by another immiscible liquid phase.) If the solid-vapor interfacial energy is denoted by 7,,, the solid-liquid interfacial energy by and the liquid¨vapor interfacial energy (i.e. the surface tension) by ygi , then the equilibrium contact angle 0 is determined from these quantities by Young's Equation:
ysg=ylg= cos + y,1 (2) The contact angle can also be related to the work of adhesion via the Young¨Dupre equation:
A Wsõ = y(1 + cos 0) (3) where A W,õ is the solid-liquid adhesion energy per unit area when in the medium V.
[0015] The pendant drop method is a technique by which a drop of liquid is suspended from a tube (capillary or needle) in a bulk liquid or gaseous phase. The shape of the drop results from the relationship between the surface tension or interfacial tension and gravity. In the pendant drop method, the surface tension or interfacial tension is calculated from the shadow image of a pendant drop using drop shape analysis in accordence with Young-Laplace equation as shown in Chart 3b. The force due to surface tension is proportional to the length of the boundary between the liquid and the tube, with the proportionality constant usually
- 8 denoted, y. Since the length of this boundary is the circumference of the tube, the force due to surface tension is given by F = 71- = d = 7 , (4) where d is the tube diameter.
The mass, m, of the drop hanging from the end of the tube can be found by equating the force due to gravity with the component of the surface tension in the vertical direction giving the formula m = g 7z- = d = 7 = sin , (5) where 0 is the contact angle with the tube, and g is the acceleration due to gravity. The limit of this formula, as 0 goes to 900, gives the maximum weight of a pendant drop for a liquid with a given surface tension, 7.
m=g=71-=d=7, (6) This relationship is the basis of a convenient method of measuring surface tension, commonly used in the petroleum industry. More sophisticated methods are available to take account of the developing shape of the pendant as the drop grows. These methods are used if the surface tension is unknown.
100161 Another object of present invention is to provide a multifunctional apparatus to measure surface and interfacial properties using Du Noiiy ring method, Du Noiiy-Padday rod method and Wilhelmy plate method.
100171 The du Noily ring method is one technique by which the surface tension (SFT) of a liquid or the interfacial tension (IFT) between two liquids can be measured as shown in Chart 4(a). The method involves slowly lifting a ring, often made of platinum or platinum-iridium,
The mass, m, of the drop hanging from the end of the tube can be found by equating the force due to gravity with the component of the surface tension in the vertical direction giving the formula m = g 7z- = d = 7 = sin , (5) where 0 is the contact angle with the tube, and g is the acceleration due to gravity. The limit of this formula, as 0 goes to 900, gives the maximum weight of a pendant drop for a liquid with a given surface tension, 7.
m=g=71-=d=7, (6) This relationship is the basis of a convenient method of measuring surface tension, commonly used in the petroleum industry. More sophisticated methods are available to take account of the developing shape of the pendant as the drop grows. These methods are used if the surface tension is unknown.
100161 Another object of present invention is to provide a multifunctional apparatus to measure surface and interfacial properties using Du Noiiy ring method, Du Noiiy-Padday rod method and Wilhelmy plate method.
100171 The du Noily ring method is one technique by which the surface tension (SFT) of a liquid or the interfacial tension (IFT) between two liquids can be measured as shown in Chart 4(a). The method involves slowly lifting a ring, often made of platinum or platinum-iridium,
- 9 -from the surface of a liquid. Using platinum or platinum-iridium as the material for the ring is that this alloy is optimally wettable due to its very high surface free energy and therefore generally forms a contact angle 0 of 00 with liquids. The material is also chemically inert and easy to clean., The force, F, required to rise the ring from the liquid's surface is measured and related to the liquid's surface tension, y:
F = 27r = (r, + rõ) = y , (7) where r, is the radius of the inner ring of the liquid film pulled and r, is the radius of the outer ring of the liquid film.
Png Air F
IF Air 1 Meniscus d F (force) A
Air ,,t):
gglhIMIINliall Liquid Liquid (a) (b) (c) Chart 4. A schematic diagram of (a) the Du Nay ring method, (b) the Du Notiy-Padday rod method and (c) the Wilhelmy plate method.
[0018] The Du Nofiy-Padday rod method is a minimized version of the Du Noily ring method replacing the large platinum ring with a thin rod (probe) that is used to measure equilibrium surface tension or dynamic surface tension at an air-liquid interface. In this method, the rod is oriented perpendicular to the interface, and the force exerted on it is measured as shown in Chart 4(b). The Du Nay Padday rod consists of a rod usually on the
F = 27r = (r, + rõ) = y , (7) where r, is the radius of the inner ring of the liquid film pulled and r, is the radius of the outer ring of the liquid film.
Png Air F
IF Air 1 Meniscus d F (force) A
Air ,,t):
gglhIMIINliall Liquid Liquid (a) (b) (c) Chart 4. A schematic diagram of (a) the Du Nay ring method, (b) the Du Notiy-Padday rod method and (c) the Wilhelmy plate method.
[0018] The Du Nofiy-Padday rod method is a minimized version of the Du Noily ring method replacing the large platinum ring with a thin rod (probe) that is used to measure equilibrium surface tension or dynamic surface tension at an air-liquid interface. In this method, the rod is oriented perpendicular to the interface, and the force exerted on it is measured as shown in Chart 4(b). The Du Nay Padday rod consists of a rod usually on the
- 10 -order of a few millimeters square making a small ring. The rod is often made from a composite metal material that may be roughened to ensure complete wetting at the interface.
The rod is attached to a scale or balance via a thin metal hook. The Padday method uses the maximum pull force method, i.e. the maximum force due to the surface tension is recorded as the probe is first immersed approxmately one mm into the liquid and then slowly withdrawn from the interface. The main forces acting on the probe are the buoyancy stemming from the volume displaced by the probe and the mass of the meniscus of the liquid adhering to the probe, the two forces are in equilibrium, 2D = 71- = y =cos0 = mõ, = g, (8) where D is diameter of the probe, y is the surface tension of the liquid, 19 is the contact angle between the probe and the liquid that is measured, and is negligible for the majority of liquids, mm is the surface tension and the weight of the meniscus under the probe. In the situation considered here the volume displaced by the probe is included in the meniscus, g is the accelaration. Thus, the force measured by the balance is given by Fp = nen, = g Fbuovancy, (9) where Fp is the force acting on the probe, Fmmyamy is the buyancy force. At the point of detachment the volume of the probe immersed in the liquid vanishes, and thus, also the buoyancy term. This is observed as a maximum in the force curve, which relates to the surface tension through ax = (10) 27-/- = D
The maximum pull force Fmax is obtained when the buoyancy force reaches its minimum.
The rod is attached to a scale or balance via a thin metal hook. The Padday method uses the maximum pull force method, i.e. the maximum force due to the surface tension is recorded as the probe is first immersed approxmately one mm into the liquid and then slowly withdrawn from the interface. The main forces acting on the probe are the buoyancy stemming from the volume displaced by the probe and the mass of the meniscus of the liquid adhering to the probe, the two forces are in equilibrium, 2D = 71- = y =cos0 = mõ, = g, (8) where D is diameter of the probe, y is the surface tension of the liquid, 19 is the contact angle between the probe and the liquid that is measured, and is negligible for the majority of liquids, mm is the surface tension and the weight of the meniscus under the probe. In the situation considered here the volume displaced by the probe is included in the meniscus, g is the accelaration. Thus, the force measured by the balance is given by Fp = nen, = g Fbuovancy, (9) where Fp is the force acting on the probe, Fmmyamy is the buyancy force. At the point of detachment the volume of the probe immersed in the liquid vanishes, and thus, also the buoyancy term. This is observed as a maximum in the force curve, which relates to the surface tension through ax = (10) 27-/- = D
The maximum pull force Fmax is obtained when the buoyancy force reaches its minimum.
- 11 -[0019] Wilhelmy plate method is used to measure equilibrium surface and interfacial tension at an air¨liquid or liquid¨liquid interface as shown in Chart 4(c). In this method, the plate is oriented perpendicular to the interface, and the force exerted on it is measured. The Wilhelmy plate is often made from filter paper, glass or platinum which may be roughened to ensure complete wetting. In fact, the results of the experiment do not depend on the material used, as long as the material is wetted by the liquid. The plate is cleaned thoroughly and attached to a balance with a thin metal wire. The force on the plate due to wetting is measured using a tensiometer or microbalance and used to calculate the surface tension, y, using the Wilhelmy equation:
= ______________________________________ (11) 1 = cos 0 where / is the wetted perimeter (2w + 2d, w is the plate width and d is the plate thickness) of the Wilhelmy plate and 0 is the contact angle between the liquid phase and the plate. In practice the contact angle is rarely measured, instead either literature values are used, or complete wetting (0 = 0) is assumed.
[0020] Another object of present invention is to provide a multifunctional apparatus to measure induction time, surface and interfacial properties, where the surface and interfacial properties are measured using both drop methods (sessile drop and pendant drop) and probe methods (Du Notiy ring, Du Noily-Padday rod and Wilhelmy plate).
Summary of the Invention [0021] A method and apparatus for measuring induction time, surface and interfacial properties of flotation separation systems is provided, the induction time is the minimum time
= ______________________________________ (11) 1 = cos 0 where / is the wetted perimeter (2w + 2d, w is the plate width and d is the plate thickness) of the Wilhelmy plate and 0 is the contact angle between the liquid phase and the plate. In practice the contact angle is rarely measured, instead either literature values are used, or complete wetting (0 = 0) is assumed.
[0020] Another object of present invention is to provide a multifunctional apparatus to measure induction time, surface and interfacial properties, where the surface and interfacial properties are measured using both drop methods (sessile drop and pendant drop) and probe methods (Du Notiy ring, Du Noily-Padday rod and Wilhelmy plate).
Summary of the Invention [0021] A method and apparatus for measuring induction time, surface and interfacial properties of flotation separation systems is provided, the induction time is the minimum time
- 12 -required for establishing attachment between a gas phase and a solid phase, a liquid phase and a solid phase, a gas phase and a liquid phase, or between two different liquid phases; the surface and interfacial properties include, but not limited to, contact angle of a liquid-vapor interface meeting a solid surface that quantifys the wettability of the solid surface by the liquid via the Young's equation, surface tension/energy of a liquid-air interface, interfical tension/energy of two-liquid interface, surface nenergy of a solid-air interface, and surface energy of a solid-liquid interface.
100221 The method of measuring induction time comprises a) moving a gas bubble, preferably an air bubble to a solid particle bed or a flat surface of a solid substrate in a testing liquid and then holding for a specified time period of contacting prior to moving it away from the solid particle bed or the solid substrate, and observing whether attachment is established or not; b) moving a drop of the testing liquid to a solid particle bed or a flat surface of a solid substrate exposing in the air environment directly and observing whether attachment is established or not.
100231 The apparatus comprises an advanced video system that includes a high speed CMOS
or CCD camera with 200-2000 frames per second (fps), a lens (preferably a telecentric lens with adjustable focus, zoom and iris) and a LED or optical telecentric backlight illuminator, a sample stage with three-way translation and a heater, a main motorized vertical stage holding a voice coil motor or a speaker, a precision micro (preferably submicron)-displacement sensor and a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements.
100221 The method of measuring induction time comprises a) moving a gas bubble, preferably an air bubble to a solid particle bed or a flat surface of a solid substrate in a testing liquid and then holding for a specified time period of contacting prior to moving it away from the solid particle bed or the solid substrate, and observing whether attachment is established or not; b) moving a drop of the testing liquid to a solid particle bed or a flat surface of a solid substrate exposing in the air environment directly and observing whether attachment is established or not.
100231 The apparatus comprises an advanced video system that includes a high speed CMOS
or CCD camera with 200-2000 frames per second (fps), a lens (preferably a telecentric lens with adjustable focus, zoom and iris) and a LED or optical telecentric backlight illuminator, a sample stage with three-way translation and a heater, a main motorized vertical stage holding a voice coil motor or a speaker, a precision micro (preferably submicron)-displacement sensor and a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements.
- 13 -[0024] A given static system of solid, liquid, and vapor at a given temperature and pressure has a unique equilibrium contact angle. The equilibrium contact angle reflects the relative strength of the liquid, solid, and vapor molecular interaction. However, in practice contact angle hysteresis is observed, ranging from the so-called advancing (maximal) contact angle to the receding (minimal) contact angle. The equilibrium contact is within those values, and can be calculated from them. While for a given system of solid, liquid, and vapor at a given temperature and pressure with the liquid moving quickly over the solid surface, the contact angle can be altered from its value at rest. The advancing contact angle will increase with speed, and the receding contact angle will decrease.
[0025] The equilibrium contact angle reflects the relative strength of the liquid, solid, and vapor molecular interaction. However, in practice contact angle hysteresis is observed, ranging from the so-called advancing (maximal) contact angle to the receding (minimal) contact angle. The equilibrium contact is within those values, and can be calculated from them.
100261 The method of measuring surface and interfacial properties comprises both static and dynamic drop methods (sessile drop and pendant drop) and probe methods (Du Notiy ring, Du Noily-Padday rod and Wilhelmy plate).
Brief Description of the Drawings [0027] Fig. 1 is a schematic diagram of the method and apparatus for measuring induction time, surface and interfacial properties.
[0028] Fig. 2 is a front-3D view of the apparatus.
[0025] The equilibrium contact angle reflects the relative strength of the liquid, solid, and vapor molecular interaction. However, in practice contact angle hysteresis is observed, ranging from the so-called advancing (maximal) contact angle to the receding (minimal) contact angle. The equilibrium contact is within those values, and can be calculated from them.
100261 The method of measuring surface and interfacial properties comprises both static and dynamic drop methods (sessile drop and pendant drop) and probe methods (Du Notiy ring, Du Noily-Padday rod and Wilhelmy plate).
Brief Description of the Drawings [0027] Fig. 1 is a schematic diagram of the method and apparatus for measuring induction time, surface and interfacial properties.
[0028] Fig. 2 is a front-3D view of the apparatus.
- 14 -[0029] Fig. 3 is a back-3D view of the apparatus.
[0030] Fig. 4 is a front-3D zoom-in view of the apparatus.
[0031] Fig. 5 is a back-3D zoom-in view of the apparatus.
[0032] Fig. 6 is an illustration of induction time measurement in four different situations: (a) an air bubble attaching surface of solid particles in a testing liquid; (b) a drop of testing liquid attaching surface of solid particles exposing in the air; (c) an air bubble attaching surface of a solid substrate in a testing liquid; (d) a drop of testing liquid attaching surface of a solid substrate exposing in the air.
[0033] Fig. 7 is an illustration of induction time measurement in other two situations: (a) an air bubble attaching bitumen-coated surface of a solid substrate in a testing liquid; (b) a drop of testing liquid attaching bitumen-coated surface of a solid substrate exposing in the air.
[0034] Fig. 8 is a schematic diagram of the apparatus for measuring surface and interfacial properties using the sessile drop method.
[0035] Fig. 9 is a schematic diagram of the apparatus for measuring surface and interfacial properties using the pendant drop method.
[0036] Fig. 10 is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Notly ring method.
[0037] Fig. 11 is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Notiy-Padday rod method.
[0030] Fig. 4 is a front-3D zoom-in view of the apparatus.
[0031] Fig. 5 is a back-3D zoom-in view of the apparatus.
[0032] Fig. 6 is an illustration of induction time measurement in four different situations: (a) an air bubble attaching surface of solid particles in a testing liquid; (b) a drop of testing liquid attaching surface of solid particles exposing in the air; (c) an air bubble attaching surface of a solid substrate in a testing liquid; (d) a drop of testing liquid attaching surface of a solid substrate exposing in the air.
[0033] Fig. 7 is an illustration of induction time measurement in other two situations: (a) an air bubble attaching bitumen-coated surface of a solid substrate in a testing liquid; (b) a drop of testing liquid attaching bitumen-coated surface of a solid substrate exposing in the air.
[0034] Fig. 8 is a schematic diagram of the apparatus for measuring surface and interfacial properties using the sessile drop method.
[0035] Fig. 9 is a schematic diagram of the apparatus for measuring surface and interfacial properties using the pendant drop method.
[0036] Fig. 10 is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Notly ring method.
[0037] Fig. 11 is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Notiy-Padday rod method.
- 15 -[0038] Fig. 12 is a schematic diagram of the apparatus for measuring surface and interfacial properties using Wilhelmy plate method.
Detailed Description of Preferred Embodiments [0039] One embodiment of the present invention is described below with reference to Fig. 1, which is a schematic diagram of the method and apparatus for measuring induction time, surface and interfacial properties, including a main motorized vertical stage holding a voice coil motor or a speaker 1, a gas bubble or liquid drop generation system, an advanced image system, a sample stage with a three-way translation, a precision micro displacement sensor, a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements, and a control box enclosing all required electronics.
[0040] As shown in Fig. 1, the voice coil motor or the speaker 1 comprises a magnet 2, a voice coil 3, a diaphragm 4 attaching to the coil 3, and a pair of electric wire terminals 5 for DC input; the gas bubble or liquid drop generation system comprises a capillary tube holder 6, a disk plate 7, a locking nut 8, a capillary tube 9 and a micro-syringe 11.
The capillary tube holder 6 as shown in the sectional view has its large tube side attaching to the center of the diaphragm 4 and another threaded tube side for mounting the disk plate 7 and the locking nut 8 as well as the capillary tube 9. It is very critical to make the capillary tube holder as less weight as possible, aluminum is the preferred material, multiple holes and slots are symmetrically cut on the wall of the capillary tube holder and its thickness is made minimal.
There is an o-ring between the capillary tube 9 and the nut 8 (not shown in the diagram) holding the capillary tube when the nut is screwed tight. The micro syringe 11 is connected to
Detailed Description of Preferred Embodiments [0039] One embodiment of the present invention is described below with reference to Fig. 1, which is a schematic diagram of the method and apparatus for measuring induction time, surface and interfacial properties, including a main motorized vertical stage holding a voice coil motor or a speaker 1, a gas bubble or liquid drop generation system, an advanced image system, a sample stage with a three-way translation, a precision micro displacement sensor, a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements, and a control box enclosing all required electronics.
[0040] As shown in Fig. 1, the voice coil motor or the speaker 1 comprises a magnet 2, a voice coil 3, a diaphragm 4 attaching to the coil 3, and a pair of electric wire terminals 5 for DC input; the gas bubble or liquid drop generation system comprises a capillary tube holder 6, a disk plate 7, a locking nut 8, a capillary tube 9 and a micro-syringe 11.
The capillary tube holder 6 as shown in the sectional view has its large tube side attaching to the center of the diaphragm 4 and another threaded tube side for mounting the disk plate 7 and the locking nut 8 as well as the capillary tube 9. It is very critical to make the capillary tube holder as less weight as possible, aluminum is the preferred material, multiple holes and slots are symmetrically cut on the wall of the capillary tube holder and its thickness is made minimal.
There is an o-ring between the capillary tube 9 and the nut 8 (not shown in the diagram) holding the capillary tube when the nut is screwed tight. The micro syringe 11 is connected to
- 16-the tip of the capillary tube via a Teflon tube 12 through one of the holes or slots on the wall of the capillary tube holder 6. The syringe cylinder, the Teflon tube and the top part of the capillary tube can be filled with either pure water or a testing liquid, leaving only the bottom part of the capillary tube for the air (empty), an air bubble 13 can be generated at the tip of the capillary tube that is dipped in a testing liquid holding in a square glass cell 21. The precision micro displacement sensor 14, preferably a submicron displacement sensor, is mounted close to the disk plate for measuring the disk's displacement when the diaphragm is moved upward or downward. The voice coil motor or the speaker is mounted on a main stage 10 (not shown in Fig. 1 to avid overlap, but shown in subsequent Figures.) that is motorized to move the voice coil motor or the speaker 1 up and down, carrying all associated components (capillary tube holder 6, disk plate 7, nut 8, capillary tube 9 and displacement sensor 14) to move up or down accordingly.
[0041] Referring to Fig.1, the sample stage 20 with the three-way translation comprises a heater 22 at its top and a precision 3-way translation stage, which consisting of two linear translation stages 23 and 24 and a vertical translation stage 25. The glass cell 21 having a layer of mineral particles 26 in the testing liquid shall be transparent square-shaped for clear images. The advanced image system comprises a camera stage 30 with a high speed CMOS
or CCD camera 32 and an attached lens 31, an illuminator stage 40 with a telecentric backlight illuminator 41 connecting via a fiber gooseneck 42 to an optical or a LED light source 43. The high speed CMOS or CCD camera has a frame rate in the range of fps, and the camera interface can be either GigE, Camera Link, IEEE 1394 or USB3, preferably USB3. It is desirable to have a lens with a magnification within 0.5-3.0X range and
[0041] Referring to Fig.1, the sample stage 20 with the three-way translation comprises a heater 22 at its top and a precision 3-way translation stage, which consisting of two linear translation stages 23 and 24 and a vertical translation stage 25. The glass cell 21 having a layer of mineral particles 26 in the testing liquid shall be transparent square-shaped for clear images. The advanced image system comprises a camera stage 30 with a high speed CMOS
or CCD camera 32 and an attached lens 31, an illuminator stage 40 with a telecentric backlight illuminator 41 connecting via a fiber gooseneck 42 to an optical or a LED light source 43. The high speed CMOS or CCD camera has a frame rate in the range of fps, and the camera interface can be either GigE, Camera Link, IEEE 1394 or USB3, preferably USB3. It is desirable to have a lens with a magnification within 0.5-3.0X range and
- 17-a adjustable focus, preferably to have a telecentric lens with adjustable zoom, focus and Iris.
Both the telecentric lens and the telecentric backlight illuminator are to improve image quality significantly compared with the setups disclosed previously, where a regular fixed focal lens and a regular optical gooseneck illuminator were used. The improved image quality makes the image shape profile digitization precisely and the interfacial property measurements accurately. Both the induction time and the interfacial property measurements are performed using a computer 70 through a control box 60. All four stages (main, sample, camera and illuminator) are mounted on a breadboard 50.
[0042] Referring to Figs. 2 and 3, they are a front-3D and a back-3D views of the apparatus, the main stage 10 holding the voice coil motor or the speaker whereby holding the capillary tube 9 and the air bubble 13, the sample stage 20 holding the testing sample 26 (shown in Fig.
1) and testing liquid in the glass cell 21, the camera stage 30 holding the camera 32 and the attached lens 31, and the illuminator stage 40 holding the illuminator 41, are all well positioned on the breadboard 50 so that the air bubble is located not only at the lens focal plane but also on a centerline of the lens and the illuminator.
[0043] Referring to Figs. 4 and 5, they are a front-3D and a back-3D zoom-in views of the apparatus, excluding the light source 43, the control box 60 and the computer 70. The 3D
zoom-in views show the main body of the induction timer.
[0044] Referring to Figs. 3, 4 and 5, the main stage 10 is for supporting the voice coil motor or the speaker 1 that is held by a speaker holder 39; the speaker holder 39 is mounted on a motorized linear translation stage 15 that is attached to two mounting claps 16 clamping on a mounting post 17; the mounting post 17 is screwed on a mounting base 18 having two sliding
Both the telecentric lens and the telecentric backlight illuminator are to improve image quality significantly compared with the setups disclosed previously, where a regular fixed focal lens and a regular optical gooseneck illuminator were used. The improved image quality makes the image shape profile digitization precisely and the interfacial property measurements accurately. Both the induction time and the interfacial property measurements are performed using a computer 70 through a control box 60. All four stages (main, sample, camera and illuminator) are mounted on a breadboard 50.
[0042] Referring to Figs. 2 and 3, they are a front-3D and a back-3D views of the apparatus, the main stage 10 holding the voice coil motor or the speaker whereby holding the capillary tube 9 and the air bubble 13, the sample stage 20 holding the testing sample 26 (shown in Fig.
1) and testing liquid in the glass cell 21, the camera stage 30 holding the camera 32 and the attached lens 31, and the illuminator stage 40 holding the illuminator 41, are all well positioned on the breadboard 50 so that the air bubble is located not only at the lens focal plane but also on a centerline of the lens and the illuminator.
[0043] Referring to Figs. 4 and 5, they are a front-3D and a back-3D zoom-in views of the apparatus, excluding the light source 43, the control box 60 and the computer 70. The 3D
zoom-in views show the main body of the induction timer.
[0044] Referring to Figs. 3, 4 and 5, the main stage 10 is for supporting the voice coil motor or the speaker 1 that is held by a speaker holder 39; the speaker holder 39 is mounted on a motorized linear translation stage 15 that is attached to two mounting claps 16 clamping on a mounting post 17; the mounting post 17 is screwed on a mounting base 18 having two sliding
- 18 -slots 19, allowing the mounting post to be adjusted close to or far from the sample stage 20 so that the capillary tip (or the air bubble 13) is in the centerline of the lens and the illuminator, which is determined when the capillary tip is observed in the center of an image showing on the computer's screen. The micro syringe 11 is also mounted at a corner of the speaker holder 39. The sample stage 20 holds sample cell 21 that is placed on the heater 22 having two heat cartridges 27 and a thermocouple 28. There is a reflection plate 29 in conjunction with the heater 22 attached to the three-way translation stage that is mounted directly on the breadboard 50.
[0045] Referring further to Figs. 3, 4 and 5, the camera stage holds the lens 31 and the high speed CMOS or CCD camera 32. The lens is directly attached to the camera via C-mount connection thread. The camera can be directly screwed on a mounting plate 33 with two sliding slots 34 when the lens is light, allowing the camera to hold the lens;
however, the lens needs to be mounted on the mounting plate 33 with two sliding slots when the lens is heavy, using the lens to hold the camera. The mounting plate 33 is mounted on an adjustable height platform 35 then on an adjustable height collar 36, which are mounted on a mounting post 37 screwed on a mounting base 38, which is firmly bolted on the breadboard 50.
The two sliding slots 34 allow the lens to be moved close to or far from the capillary tube 9 holding the air bubble 13. The adjustable height platform and collar allow the camera and lens to be moved upward or downward so that the air bubble can be in the center of the image's field of view.
The illuminator stage 40 holds the illuminator 41 using a clamp 44 that is mounted on an adjustable height platform 45, which is then mounted on a mounting post 46 screwed on a mounting plate 47, which is firmly bolted on the breadboard 50. The adjustable height
[0045] Referring further to Figs. 3, 4 and 5, the camera stage holds the lens 31 and the high speed CMOS or CCD camera 32. The lens is directly attached to the camera via C-mount connection thread. The camera can be directly screwed on a mounting plate 33 with two sliding slots 34 when the lens is light, allowing the camera to hold the lens;
however, the lens needs to be mounted on the mounting plate 33 with two sliding slots when the lens is heavy, using the lens to hold the camera. The mounting plate 33 is mounted on an adjustable height platform 35 then on an adjustable height collar 36, which are mounted on a mounting post 37 screwed on a mounting base 38, which is firmly bolted on the breadboard 50.
The two sliding slots 34 allow the lens to be moved close to or far from the capillary tube 9 holding the air bubble 13. The adjustable height platform and collar allow the camera and lens to be moved upward or downward so that the air bubble can be in the center of the image's field of view.
The illuminator stage 40 holds the illuminator 41 using a clamp 44 that is mounted on an adjustable height platform 45, which is then mounted on a mounting post 46 screwed on a mounting plate 47, which is firmly bolted on the breadboard 50. The adjustable height
- 19 -platform allows the illuminator to be moved upward and downward so that its centerline is well aligned with the lens's centerline. This is critical to ensure high quality images when both telecentric lens and telecentric illuminator are used.
[0046] Referring to Fig. 2, the light source 43 connecting to the illuminator 41 via the optical gooseneck 42 can be either an optical or a LED light source with an intensity control 48 and power switch 49, preferably also to have an iris control and replaceable filters.
[0047] Referring to Figs. 2, 3 and 5, the electric control box 60 has a temperature controller 61, an power switch 62 and a heater switch 63 in the front panel, and a power inlet 64, a fuse holder 65, a CPC connector 66 for AC power wires from the box to the heater cartridges 27, a CPC connector 67 for variety of signal wires and a USB port on the back. The temperature controller 61 monitors and controls the temperature of the heater 22 via the thermocouple 28, the heater 22 is AC powered from the control box via the CPC connector 66 to the two heat cartridges 27. The CPC connector 67 for variety of signal wires include the wires from the control box to the DC power terminal 5, the wires between the control box and the motorized vertical stage 15, the wires between the control box and the displacement sensor 14, the wires from the thermocouple 28 to the control box. The USB port is for connecting the control box 60 to the computer 70 for data communications.
[0048] Referring to Figs. 1 and 6, the method of induction time measurement comprises using a controller to send a square (or a ladder) wave instruction with preset wave half width, in, and amplitude from the computer 70 to an transconductance amplifier enclosed in the control box 60 and observing whether attachment can be established between the air bubble and the solid particles in a testing liquid, the amplifier then applies a current /out, that is
[0046] Referring to Fig. 2, the light source 43 connecting to the illuminator 41 via the optical gooseneck 42 can be either an optical or a LED light source with an intensity control 48 and power switch 49, preferably also to have an iris control and replaceable filters.
[0047] Referring to Figs. 2, 3 and 5, the electric control box 60 has a temperature controller 61, an power switch 62 and a heater switch 63 in the front panel, and a power inlet 64, a fuse holder 65, a CPC connector 66 for AC power wires from the box to the heater cartridges 27, a CPC connector 67 for variety of signal wires and a USB port on the back. The temperature controller 61 monitors and controls the temperature of the heater 22 via the thermocouple 28, the heater 22 is AC powered from the control box via the CPC connector 66 to the two heat cartridges 27. The CPC connector 67 for variety of signal wires include the wires from the control box to the DC power terminal 5, the wires between the control box and the motorized vertical stage 15, the wires between the control box and the displacement sensor 14, the wires from the thermocouple 28 to the control box. The USB port is for connecting the control box 60 to the computer 70 for data communications.
[0048] Referring to Figs. 1 and 6, the method of induction time measurement comprises using a controller to send a square (or a ladder) wave instruction with preset wave half width, in, and amplitude from the computer 70 to an transconductance amplifier enclosed in the control box 60 and observing whether attachment can be established between the air bubble and the solid particles in a testing liquid, the amplifier then applies a current /out, that is
- 20 -proportional to the Vmn, to the terminal 5 and drives the diaphragm 4 to move downward, carrying the capillary tube holder 6 and the air bubble 13 down to and make contact with the particle bed 26 for the preset time period tn, then retract to its original place as shown in Fig.
6(a). Induction time tmd is defined as the minimum contact time required to establish attachment between the air bubble and the solid particles. When a few solid particles are observed at the bottom of the air bubble after the air bubble retracts to its original place, the attachment is believed having been established, the preset contact time iõ is considered longer than the induction time tind, a shorter time tõ_1 shall be preset and do another try. Contrarily, when no solid particle is observed at the bottom of the air bubble after the air bubble retracts to its original place, the attachment is believed having not been established, the preset contact time tn is considered shorter than the induction time trnd, a longer time t,j shall be preset and another try shall be carried out. This testing procedure shall be performed as many times as possible till the incremental value (tõ+1 - tn) is close or equal to the decremental value (tõ -and falls an acceptable error range, then the tn is considered as its induction time t/nd 100491 Referring further to Fig. 6, the induction time of solid-air bubble can be measured either using an air bubble 13 to attach a solid particle bed 26 in a testing liquid as shown in Fig. 6(a) or using a drop of the testing liquid 13' to attach the solid particles bed 26 exposing in the air directly as shown in Fig. 6(b). The method 6(a) involves the liquid receding process (solid-air interface replacing solid-liquid interface), hence provides a receding induction time irecechnp while the method 6(b) involves the liquid advancing process (solid-liquid interface replacing solid-air interface), hence provides an advancing induction time tadõncing.
6(a). Induction time tmd is defined as the minimum contact time required to establish attachment between the air bubble and the solid particles. When a few solid particles are observed at the bottom of the air bubble after the air bubble retracts to its original place, the attachment is believed having been established, the preset contact time iõ is considered longer than the induction time tind, a shorter time tõ_1 shall be preset and do another try. Contrarily, when no solid particle is observed at the bottom of the air bubble after the air bubble retracts to its original place, the attachment is believed having not been established, the preset contact time tn is considered shorter than the induction time trnd, a longer time t,j shall be preset and another try shall be carried out. This testing procedure shall be performed as many times as possible till the incremental value (tõ+1 - tn) is close or equal to the decremental value (tõ -and falls an acceptable error range, then the tn is considered as its induction time t/nd 100491 Referring further to Fig. 6, the induction time of solid-air bubble can be measured either using an air bubble 13 to attach a solid particle bed 26 in a testing liquid as shown in Fig. 6(a) or using a drop of the testing liquid 13' to attach the solid particles bed 26 exposing in the air directly as shown in Fig. 6(b). The method 6(a) involves the liquid receding process (solid-air interface replacing solid-liquid interface), hence provides a receding induction time irecechnp while the method 6(b) involves the liquid advancing process (solid-liquid interface replacing solid-air interface), hence provides an advancing induction time tadõncing.
-21-[0050] Referring further to Fig. 6, the induction time of solid-air bubble in the testing liquid can also be measured using a solid substrate with a flat surface as shown in Fig. 6(c), attachment between the solid surface 26' and the air bubble 13 is believed to have been established when the air bubble is sticking on the solid surface after the capillary tube retracts to its original place. The induction time of solid-air bubble in the testing liquid can also be measured using a drop of the testing liquid 13' to contact the solid substrate 26' in the air environment as shown in Fig. 6(d), attachment between the solid surface 26' and the testing liquid drop 13' is believed to have been established when the drop of the testing liquid is sticking on the solid surface after the capillary tube retracts to its original place. The method shown in Fig. 6(c) provides a receding induction time, while the method shown in Fig. 6(d) provides an advancing induction time.
[0051] Referring to Fig. 7, in the oil sands processing industry, bitumen is floated, the induction time of bitumen-air bubble in the testing liquid can also be measured using a bitumen-coated solid substrate 26' as shown in Fig. 7(a) an air bubble attaching bitumen-coated surface of a solid substrate, and Fig. 7(b) a drop of testing liquid attaching bitumen-coated surface of a solid substrate exposing in the air. The method shown in Fig. 7(a) provides a receding induction time, while the method shown in Fig. 7(b) provides an advancing induction time.
[0052] Referring to Figs. 1, 6 and 7, the air bubble shape is deformed while being pushed downward to contact either the solids particle bed or a substrate for each induction time measurement. With the advanced high speed image system and the multifunctional software,
[0051] Referring to Fig. 7, in the oil sands processing industry, bitumen is floated, the induction time of bitumen-air bubble in the testing liquid can also be measured using a bitumen-coated solid substrate 26' as shown in Fig. 7(a) an air bubble attaching bitumen-coated surface of a solid substrate, and Fig. 7(b) a drop of testing liquid attaching bitumen-coated surface of a solid substrate exposing in the air. The method shown in Fig. 7(a) provides a receding induction time, while the method shown in Fig. 7(b) provides an advancing induction time.
[0052] Referring to Figs. 1, 6 and 7, the air bubble shape is deformed while being pushed downward to contact either the solids particle bed or a substrate for each induction time measurement. With the advanced high speed image system and the multifunctional software,
- 22 -the air bubble impact force can be derived using the digitized air bubble's shape profile and Young-Laplace analysis.
[0053] Referring to Fig. 8, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using the sessile drop method. A drop of testing liquid 51 is released from the capillary tube 9 onto the surface of the solid substrate 26', the wetting process is recorded using the high speed camera system and displayed on the computer screen, the images are analyized using Young-Laplace equation for the solid-liquid dynamic contact angle and/or the liquid's surface tension calculation.
[0054] Referring to Fig. 9, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using the pendent drop method. A drop of testing liquid 52 is generated at the tip of the capillary tube 9 carefully, the liquid drop generation process is recorded using the high speed camera system and displayed on the computer screen, the images are analyized using Young-Laplace equation for the liquid's surface tension calculation.
[0055] Referring to Fig. 10, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Nay ring method. The capillary tube 13 in Fig. 1 is replaced with the ring's arm 53. The Du Noily ring 54 is dipped into a liquid holding in the glass cell 21, then it is lifted slowly by rising the capillary holder 6 and associated metal disk 7, the displacement sensor 14 as well as the speaker holder 39 via the motorized vertical stage 15 (shown in Fig. 5). The gap, G, between the disk 7 and the displacement sensor 14 is measured using the displacement sensor. There are two ways of deriving surface force, one
[0053] Referring to Fig. 8, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using the sessile drop method. A drop of testing liquid 51 is released from the capillary tube 9 onto the surface of the solid substrate 26', the wetting process is recorded using the high speed camera system and displayed on the computer screen, the images are analyized using Young-Laplace equation for the solid-liquid dynamic contact angle and/or the liquid's surface tension calculation.
[0054] Referring to Fig. 9, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using the pendent drop method. A drop of testing liquid 52 is generated at the tip of the capillary tube 9 carefully, the liquid drop generation process is recorded using the high speed camera system and displayed on the computer screen, the images are analyized using Young-Laplace equation for the liquid's surface tension calculation.
[0055] Referring to Fig. 10, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Nay ring method. The capillary tube 13 in Fig. 1 is replaced with the ring's arm 53. The Du Noily ring 54 is dipped into a liquid holding in the glass cell 21, then it is lifted slowly by rising the capillary holder 6 and associated metal disk 7, the displacement sensor 14 as well as the speaker holder 39 via the motorized vertical stage 15 (shown in Fig. 5). The gap, G, between the disk 7 and the displacement sensor 14 is measured using the displacement sensor. There are two ways of deriving surface force, one
- 23 -way is to consider the diaphragm of the speaker working as a spring balance, which can be expressed using Hooke's law, F = k = AG (12) where k is a constant factor characteristic of the spring, AG is the gap variation. The constant k can be obtained by a calibration, which uses a few standard masses hanging on the Du Notly ring so that gap variations can be obtained respectively. The constant k is then obtained via linear correlation. The surface force of the testing liquid F can be calculated once the gap variation is measured. Another way is to consider the diaphragm of the speaker working as an electronic balance, the gap variation AG is a feedback signal, which can be used by a controller to generate a square wave instruction with preset wave width, tõ
and amplitude 171, to the transconductance amplifier, the amplifier then applies a current I, that is proportional to the Võ to the terminal 5 and drives the diaphragm 4 to move upward counterbalancing the downward force proportional to the gap variation AG. The Force can be expressed as F =kõ=V, = k = AG, (13) where k, is a constant voltage factor of the speaker's controller. Similar to the spring balance consideration, a calibration is also used to determine the constant voltage factor lc.
[0056] Referring to Fig. 11, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Noily-Padday rod method. The capillary tube 13 in Fig. 1 is replaced with the Du Noiiy-Padday rod 55. All measurement procedures are similar to the Du Notiy ring method except that different calculations are used.
and amplitude 171, to the transconductance amplifier, the amplifier then applies a current I, that is proportional to the Võ to the terminal 5 and drives the diaphragm 4 to move upward counterbalancing the downward force proportional to the gap variation AG. The Force can be expressed as F =kõ=V, = k = AG, (13) where k, is a constant voltage factor of the speaker's controller. Similar to the spring balance consideration, a calibration is also used to determine the constant voltage factor lc.
[0056] Referring to Fig. 11, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using Du Noily-Padday rod method. The capillary tube 13 in Fig. 1 is replaced with the Du Noiiy-Padday rod 55. All measurement procedures are similar to the Du Notiy ring method except that different calculations are used.
- 24 -100571 Referring to Fig. 12, which is a schematic diagram of the apparatus for measuring surface and interfacial properties using Wilhelmy plate method. The capillary tube 13 in Fig. 1 is replaced with the Wilhelmy plate 56. All measurement procedures are similar to the Du Nay ring method except that different calculations are used.
100581 The apparatus showing in Figs. 2 through 5 is one example of the present invention.
Other variations, e.g. making the apparatus more compact with similar components but different shapes, are the scope of the present invention. Figs. 1, 6 and 7 shows the method of measuring induction time using the apparatus, air bubble impact force can also be estimated simultaneously. Figs. 8 and 9 shows the method of measuring surface and interfacial properties using both static and dynamic drop methods (sessile drop and pendant drop). Figs.
10, 11 and 12 shows the method of measuring surface and interfacial properties using the probe methods (Du Nay ring, Du Noily-Padday rod and Wilhelmy plate). Combining the induction time measurement with any one of or any combinations of the methods for measuring surface and interfacial properties belongs to the present invention.
100581 The apparatus showing in Figs. 2 through 5 is one example of the present invention.
Other variations, e.g. making the apparatus more compact with similar components but different shapes, are the scope of the present invention. Figs. 1, 6 and 7 shows the method of measuring induction time using the apparatus, air bubble impact force can also be estimated simultaneously. Figs. 8 and 9 shows the method of measuring surface and interfacial properties using both static and dynamic drop methods (sessile drop and pendant drop). Figs.
10, 11 and 12 shows the method of measuring surface and interfacial properties using the probe methods (Du Nay ring, Du Noily-Padday rod and Wilhelmy plate). Combining the induction time measurement with any one of or any combinations of the methods for measuring surface and interfacial properties belongs to the present invention.
- 25 -
Claims (23)
1. A multifunctional apparatus for measuring induction time, surface and interfacial properties of various flotation separation systems.
2. The apparatus of claim 1 comprises a motorized vertical main stage holding a voice coil motor or a speaker, a gas bubble or liquid drop generation system, a sample stage with a three-way translation, a precision micro displacement sensor, an advanced image system, a multifunctional software that controls all motors, monitors the displacement sensor's feedback, records and analyzes images to make multifunctional measurements, and a electric control box enclosing all required electronics.
3. The apparatus of claims 1 and 2 wherein the motorized vertical main stage is for supporting the voice coil motor or the speaker that is held by a speaker holder; the speaker holder is mounted on a motorized linear translation stage that is attached to one or two mounting claps clamping on a mounting post; the mounting post is screwed on a mounting base having two sliding slots, allowing the mounting post to be adjusted close to or away from the sample stage. The voice coil motor or the speaker carries all associated components (capillary tube holder, disk plate, nut, capillary tube and displacement sensor ) to move up or down accordingly when the motorized vertical main stage moves the voice coil motor or the speaker up and down.
4. The apparatus of claims 1, 2 and 3 wherein the voice coil motor or the speaker comprises a magnet, a voice coil, a diaphragm attaching to the coil, and a pair of electric wire terminals for DC input;
5. The apparatus of claims 1, 2 and 3 wherein the gas bubble or liquid drop generation system comprises a capillary tube holder, a disk plate, a locking nut, a capillary tube and a micro-syringe.
6. The apparatus of claims 1 and 5 wherein the capillary tube holder shall be as less weight as possible, aluminum is a preferred material, multiple holes and slots are symmetrically cut on the wall of the capillary tube holder and its thickness is made minimal.
7. The apparatus of claims 1, 3, 4, 5 and 6 wherein the capillary tube holder has its large tube side attaching to the center of the diaphragm and another threaded tube side for mounting the disk plate and the locking nut as well as the capillary tube. There is an o-ring between the capillary tube and the locking nut holding the capillary tube when the locking nut is screwed tight. The micro syringe is connected to the tip of the capillary tube via a Teflon tube through one of the holes or slots on the wall of the capillary tube holder. The micro syringe's body is mounted at a corner of the speaker holder.
8. The apparatus of claims 1 and 2 wherein the sample stage with the three-way translation comprises a heater at its top, a precision 3-way translation stage consisting of two linear translation stages and a vertical translation stage and a sample cell having a layer of mineral particles in the testing liquid and sitting on the 3-way translation stage. The sample stage holds the sample cell that is placed on a heater having two heat cartridges and a thermocouple. There is a reflection plate in conjunction with the heater attached to the three-way translation stage. The sample cell is a square-shaped transparent glass cell
9.The apparatus of claims 1, 5 and 7 wherein the syringe's cylinder, the Teflon tube and the top part of the capillary tube can be filled with either pure water or a testing liquid, leaving only the bottom part of the capillary tube for the air (empty), an air bubble can be generated at the tip of the capillary tube that is dipped in a testing liquid holding in the sample cell.
10. The apparatus of claims 1, 2, 3, 4 and 5 wherein the precision micro displacement sensor preferably being a submicron displacement sensor, is attached to the speaker holder and its sensor head is perpendicularly mounted within its measuring range to the disk plate for measuring the disk's displacement when the diaphragm moves upward or downward.
11. The apparatus of claims 1 and 2 wherein the advanced image system comprises a camera stage with a high speed CMOS or CCD camera and an attached lens, an illuminator stage with a telecentric backlight illuminator connecting via a fiber gooseneck to an optical or a LED light source. The high speed CMOS or CCD camera has a frame rate in the range of 200-2000 fps, and the camera interface can be either GigE, Camera Link, IEEE
1394 or USB3, preferably USB3. It is desirable to have a lens with a magnification within 0.5-3.0X range and a adjustable focus, preferably to have a telecentric lens with adjustable zoom, focus and Iris.
1394 or USB3, preferably USB3. It is desirable to have a lens with a magnification within 0.5-3.0X range and a adjustable focus, preferably to have a telecentric lens with adjustable zoom, focus and Iris.
12. The apparatus of claims 1, 2 and 11 wherein the camera stage holds the lens and the high speed CMOS or CCD camera. The lens is directly attached to the camera via C-mount connection thread. The camera can be directly screwed on a mounting plate with two sliding slots when the lens is light, allowing the camera to hold the lens;
however, the lens needs to be mounted on a mounting plate with two sliding slots when the lens is heavy, using the lens to hold the camera. The mounting plate is mounted on an adjustable height platform then on an adjustable height collar, which are mounted on a mounting post screwed on a mounting base that is firmly bolted on a breadboard. The two sliding slots allow the lens to be moved close to or away from the capillary tube holding the air bubble.
The adjustable height platform and collar allow the camera and lens to be moved upward or downward so that the air bubble can be in the center of the image's field of view. The illuminator stage holds the illuminator using a clamp that is mounted on an adjustable height platform, which is then mounted on a mounting post screwed on a mounting plate that is firmly bolted on the breadboard. The adjustable height platform allows the illuminator to be moved upward and downward so that its centerline is well aligned with the lens's centerline.
however, the lens needs to be mounted on a mounting plate with two sliding slots when the lens is heavy, using the lens to hold the camera. The mounting plate is mounted on an adjustable height platform then on an adjustable height collar, which are mounted on a mounting post screwed on a mounting base that is firmly bolted on a breadboard. The two sliding slots allow the lens to be moved close to or away from the capillary tube holding the air bubble.
The adjustable height platform and collar allow the camera and lens to be moved upward or downward so that the air bubble can be in the center of the image's field of view. The illuminator stage holds the illuminator using a clamp that is mounted on an adjustable height platform, which is then mounted on a mounting post screwed on a mounting plate that is firmly bolted on the breadboard. The adjustable height platform allows the illuminator to be moved upward and downward so that its centerline is well aligned with the lens's centerline.
13. The apparatus of claims 1, 2 and 11 wherein the motorized vertical main stage holds the voice coil motor or the speaker whereby holds the capillary tube and the air bubble; the sample stage holds the testing sample and testing liquid in the sample cell;
the camera stage holds the camera and the attached lens; and the illuminator stage holds the illuminator. The four stages are all well positioned on the breadboard so that the air bubble is located not only at the lens focal plane but also on a centerline of the lens and the illuminator.
the camera stage holds the camera and the attached lens; and the illuminator stage holds the illuminator. The four stages are all well positioned on the breadboard so that the air bubble is located not only at the lens focal plane but also on a centerline of the lens and the illuminator.
14. The apparatus of claims 1, 2 and 11 wherein the light source connecting to the illuminator via the optical gooseneck can be either an optical or a LED light source with an intensity control and power switch, preferably also to have an iris control and replaceable filters.
15. The apparatus of claims 1 and 2 wherein the electric control box has a temperature controller, an power switch and a heater switch in the front panel, and a power inlet, a fuse holder, a CPC connector for AC power wires from the box to the heater cartridges, a CPC
connector for variety of signal wires and a USB port on the back. The temperature controller monitors and controls the temperature of the heater via the thermocouple, the heater is AC powered from the control box via the CPC connector to the two heat cartridges. The CPC connector for variety of signal wires include the wires from the control box to the DC power terminal, the wires between the control box and the motorized vertical stage, the wires between the control box and the displacement sensor, the wires from the thermocouple to the control box. The USB port is for connecting the electric control box to the computer for data communications.
connector for variety of signal wires and a USB port on the back. The temperature controller monitors and controls the temperature of the heater via the thermocouple, the heater is AC powered from the control box via the CPC connector to the two heat cartridges. The CPC connector for variety of signal wires include the wires from the control box to the DC power terminal, the wires between the control box and the motorized vertical stage, the wires between the control box and the displacement sensor, the wires from the thermocouple to the control box. The USB port is for connecting the electric control box to the computer for data communications.
16. The apparatus of claims 1 wherein the induction time of solid-air bubble can be measured either using an air bubble to attach a solid particle bed in a testing liquid (namely receding induction time) or using a drop of the testing liquid to attach the solid particles bed exposing in the air directly (namely advancing induction time).
17. The apparatus of claims I wherein the induction time of solid-air bubble in the testing liquid can also be measured using a solid substrate with a flat surface (receding induction time), attachment between the solid surface and the air bubble is believed to have been established when the air bubble is sticking on the solid surface after the capillary tube retracts to its original place. The induction time of solid-air bubble in the testing liquid can also be measured using a drop of the testing liquid to contact the solid substrate in the air environment (advancing induction time), attachment between the solid surface and the testing liquid drop is believed to have been established when the drop of the testing liquid is sticking on the solid surface after the capillary tube retracts to its original place.
18. The apparatus of claims 1 wherein the induction time of bitumen-air bubble in the testing liquid can be measured using a bitumen-coated solid substrate either via an air bubble attaching bitumen-coated surface of a solid substrate (receding induction time) or a drop of testing liquid attaching bitumen-coated surface of a solid substrate exposing in the air (advancing induction time).
19. The apparatus of claims 1 wherein surface and interfacial properties are measured using the sessile drop method.
20. The apparatus of claims 1 wherein surface and interfacial properties are measured using the pendent drop method.
21. The apparatus of claims 1 wherein surface and interfacial properties are measured using Du Nouy ring method.
22. The apparatus of claims 1 wherein surface and interfacial properties are measured using Du Nouy-Padday rod method.
23. The apparatus of claims 1 wherein surface and interfacial properties are measured using Wilhelmy plate method.
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| Application Number | Priority Date | Filing Date | Title |
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| US201662353498P | 2016-06-22 | 2016-06-22 | |
| US62353498 | 2016-06-22 |
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| CA2968623A1 true CA2968623A1 (en) | 2017-12-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CA2968623A Abandoned CA2968623A1 (en) | 2016-06-22 | 2017-05-30 | A multifunctional apparatus for measuring induction time, surface and interfacial properties |
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