MEASUREMENT OF PROPERTIES OF FLUIDS USING MRI
20170052100 ยท 2017-02-23
Inventors
Cpc classification
G01R33/5608
PHYSICS
G01F1/716
PHYSICS
International classification
G01F1/716
PHYSICS
Abstract
A method of determining rheological properties of a fluid. The method includes: providing an open-bore tube and defining within the bore a three dimensional grid (3DG) of voxels; defining at least an inlet cross section (ICS) and an outlet cross section (OCS); defining a volume of interest within the bore between the ICS and the OCS; obtaining rheological properties of the fluid; applying a pressure gradient to the bore between the ICS and the OCS; and nuclear magnetic resonance imaging the fluid within the volume of interest to determine various aspects of the fluid.
Claims
1. A method for determining rheological properties of a fluid, comprising the steps of: a. providing an open-bore tube and defining within said bore a three dimensional grid (3DG) of voxels, with each voxel Vox.sub.i having a position (x.sub.i, y.sub.i, z.sub.i) in said 3DG; defining at least two different cross sections, namely inlet cross section (ICS) and outlet cross section (OCS); and defining a volume of interest (VOI) within said bore between said ICS and said OCS; b. obtaining a database of rheological properties of said fluid; c. applying a pressure gradient to said bore between said ICS and said OCS, thereby flowing said fluid through said tube; d. NMR imaging said fluid within said VOI, said image having a plurality p of slices, each slice comprising a plane within said 3DG; e. from said image, for each of said voxels Vox.sub.i, determining a velocity for said fluid v.sub.i, f. for each of said voxels Vox.sub.i, from said velocity v.sub.i, calculating shear rate values (SRV); whilst, before or after determining a pressure gradient between said at least one ICS and said at least one OCS and thereby calculating shear stress values (SSV) for each voxel Vox.sub.i, from said SRV and said SSV determining at least one rheological property RP.sub.i, for each voxel Vox.sub.i; g. comparing, for said at least one rheological property, RP.sub.i calculated for voxel Vox.sub.i to stored RP.sub.i for voxel Vox.sub.i from said database, thereby determining the difference in rheological property DRPi for voxel Vox.sub.i; and h. from the set of said DRP, calculating 3D variations in said rheological property, therefrom determining the difference in rheological property DRPi as a function of position (x,yi,z.sub.i) in said grid; wherein the resolution of said difference in rheological property DRP.sub.i is multiplied by about p compared to the per-slice resolution.
2. The method of claim 1, comprising an additional step of selecting said rheological properties from a group consisting of fluid type, fluid density, fluid viscosity, fluid yield stress, and any combination thereof.
3. The method of claim 1, comprising an additional step of selecting said fluid type from a group consisting of Newtonian fluid, pseudoplastic fluid, dilatant fluid, Bingham plastic fluid, and Herschel-Bulkley fluid.
4. The method of claim 1, comprising an additional step of identifying inhomogeneous regions in said fluid.
5. The method of claim 4, wherein said inhomogeneous regions in said fluid are selected from a group consisting of gas bubbles, liquid bubbles, regions of stratification, regions of settlement, regions of broken-down emulsion, and regions of incomplete mixing.
6. The method of claim 1, comprising an additional step of identifying regions of turbulence by irregularities in the shape of the flow front.
7. The method of claim 1, comprising an additional step of identifying regions of turbulence by the presence of eddies in the velocity field.
8. The method of claim 1, further comprising a step of displaying said 3D velocity image on a display device.
9. A method for determining rheological properties of a fluid flowing through a tube, comprising the steps of: a. providing an open-bore tube and defining within said bore a three dimensional grid (3DG) of voxels, with each voxel Vox.sub.i having a position (x.sub.i, y.sub.i z.sub.i) in said 3DG; defining at least two different cross sections, namely inlet cross section (ICS) and outlet cross section (OCS); and defining a volume of interest (VOI) within said bore between said ICS and said OCS); b. applying a pressure gradient to said bore between said ICS and said OCS, thereby flowing said fluid through said tube; c. NMR imaging said fluid within said VOI, said NMR image having a plurality p of slices, each slice comprising a plane within said 3DG; d. from said image, for each of said voxels Vox.sub.i, determining a velocity for said fluid v.sub.i, e. for each of said voxels Vox.sub.i, from said velocity v.sub.i, calculating shear rate values (SRV); whilst, before or after determining a pressure gradient between said at least one ICS and said at least one OCS and thereby calculating shear stress values (SSV) for each voxel Vox.sub.i, from said SRV and said SSV determining at least one rheological property RP.sub.i for each voxel Vox.sub.i; f. creating at least two sets of voxels, set {Vox.sub.A} comprising at least one voxel Vox.sub.A,i and set {Vox.sub.B} comprising at least one voxel Vox.sub.B,i, locations of voxels in set (Vox.sub.A) differing from locations of voxels in set {Vox.sub.B} in a systematic way, each voxel Vox.sub.A,i in set {Vox.sub.A} having a corresponding voxel Vox.sub.B,i in set {Vox.sub.B}; g. comparing, for said at least one rheological property, for said at least two sets of voxels, rheological property RP.sub.A,i for each voxel Vox.sub.A,i in set {Vox.sub.A} to rheological parameter RP.sub.B,i for corresponding voxel Vox.sub.b,j in set {Vox.sub.B} thereby determining differences in rheological property DRP.sub.ij at relative position (x.sub.k, y.sub.k, Z.sub.k); and h. from the set of said DRP.sub.ij, calculating 3D variations in said rheological property, therefrom determining the relative difference in rheological property DRP.sub.ij as a function of relative position (x.sub.k, y.sub.k, Z.sub.k) in said grid wherein the resolution of said difference in rheological property DRP.sub.ij is multiplied by about p compared to the per-slice resolution.
10. The method of claim 9, comprising an additional step of selecting said rheological properties from a group consisting of fluid type, fluid density, fluid viscosity, fluid yield stress, and any combination thereof.
11. The method of claim 9, comprising an additional step of selecting said fluid type from a group consisting of Newtonian fluid, pseudoplastic fluid, dilatant fluid, Bingham plastic fluid, and Herschel-Bulkley fluid.
12. The method of claim 9, comprising an additional step of identifying inhomogeneous regions in said fluid.
13. The method of claim 12, wherein said inhomogeneous regions in said fluid are selected from a group consisting of gas bubbles, liquid bubbles, regions of stratification, regions of settlement, regions of broken-down emulsion, and regions of incomplete mixing.
14. The method of claim 9, comprising an additional step of identifying regions of turbulence by irregularities in the shape of the flow front.
15. The method of claim 9, comprising an additional step of identifying regions of turbulence by the presence of eddies in the velocity field.
16. The method of claim 9, further comprising a step of displaying said 3D velocity image on a display device.
Description
BRIEF DESCRIPTION OF THE FIGURES
[0030] In order to better understand the invention and its implementation in practice, a plurality of embodiments will now be described, by way of non-limiting example only, with reference to the accompanying drawings, wherein
[0031]
[0032]
[0033]
[0034]
[0035]
[0036]
[0037]
[0038]
[0039]
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0040] The following description is provided, alongside all chapters of the present invention, so as to enable any person skilled in the art to make use of the invention and sets forth the best modes contemplated by the inventor of carrying out this invention. Various modifications, however, will remain apparent to those skilled in the art, since the generic principles of the present invention have been defined specifically to provide a means and method for measurement of properties of fluids using MRI.
[0041] The term bubble hereinafter refers to a region substantially filled with a fluid of with characteristics which differ significantly from those of the main body of the flowing fluid. Bubbles need not be substantially spherical or ovoid, but the fluid therein should be of relatively uniform quality. A non-limiting example of a bubble is a region of air larger than approximately a millimeter within an emulsion or a liquid. Other non-limiting examples of bubbles are a region of oil within an emulsion or a liquid, or a region of liquid within a gas.
[0042] The terms about and approximately hereinafter refer to + or 25% of a value.
[0043] The system of the present invention uses 3D NMR to determine 3D velocity profiles of a flowing fluid and to determine rheological parameters from the 3D velocity profiles.
[0044] There are several advantages to 3D velocity profiles over 2 D profiles. 2D profiles, because of their two dimensional nature, can only give a velocity profile through one slice of the flowing fluid. For example, if the slice is perpendicular to the predominant direction of flow of the fluid (such as a slice parallel to the cross-section of a pipe through which the fluid is flowing), the velocity profile can be determined for that cross-section of the pipe. Such a velocity profile can determine asymmetries in the velocity profile for locations in that cross section. Such asymmetries can indicate, for example, as discussed hereinbelow, bubbles in the fluid. However, such a two-dimensional slice can not distinguish between a small, local bubble and the permanent presence of gas in the pipe. A vertical, longitudinal section could determine whether there was a layer of gas overlying other fluids in the pipe, for example if the pipe were underfilled, but could not identify bubbles away from the central, vertical diameter of the slice, bubbles which would be identifiable in a horizontal longitudinal slice. A series of cross-sectional slices at a fixed location could identify such an overlying layer of gas, but the time to identify the problem would be limited by the flow velocity of the fluid. In contrast, a 3D velocity profile can be used to identify rheological parameters and variations in them at any position within the 3D volume of interest and identification of both longitudinal and cross-sectional variation is not limited by the flow velocity of the fluid.
[0045] In an embodiment of the invention, the flowing fluid is in a plug reactor; the NMR device at least partially surrounds at least a portion of the plug reactor. The velocity profile measured by the NMR device is used to characterize the flowing material. The results of the characterization can be used to control the reaction, including such aspects as altering the composition of the fluid, altering the temperature profile of the fluid, altering mixing of the fluid or any of its components, by any of stirrers, shakers or rotators, irradiating the fluid (visible light sources, sources of IR electromagnetic radiation, sources of UV electromagnetic radiation, x-ray sources, sources of microwave radiation and ultrasound sources) and stopping, starting or aborting at least a portion of the reaction. The reaction control mechanism can be upstream, in conjunction with, or downstream of the NMR device.
[0046] Fluids can be characterized by the shape of the flow profile.
[0047]
[0048]
[0049] Measuring velocity profiles directly from NMR images suffers badly from the effects of noise in the NMR signal. However, the extraction of velocity profiles can be made more robust by the use of velocity resealing techniques. In one embodiment of a resealing technique, a resealed velocity dependent on the shear stress is used. The shear stress in the fluid inside a circular pipe, (r), as a function of radius r is
[0050] Where P is the pressure drop in the pipe and L is the length of the pipe. Since
[0051] This function is zero at the center of the tube, where v(
[0052] And since
[0053] The derivative dV.sub./d is the shear rate
[0054] The function V(x) can therefore also be found by integrating equation (4),
[0055] From equation (6), it is clear that the function V() depends only on the shear strain rate {dot over ()}, so that no fitting or smoothing of the data is required in order to find the velocity profile. The shear stress can be written as a function of the shear strain rate as {dot over ()}
=.sub.y+K|{dot over ()}|.sup.n >.sub.(6)
where .sub.y is the yield stress, and K and n are constants characterizing the fluid. Values of .sub., K and n for different types of fluid are shown in Table 1, where is the viscosity of the fluid.
TABLE-US-00001 TABLE 1 Type of Fluid Yield stress .sub. Exponent n Constant K Newtonian 0 1 Power law (pseudoplastic) 0 <1 Power law (dilatant) 0 >1 Bingham >0 1 K Herschel-Bulkley >0 1 K
[0056] Solving eq. (6) for {dot over ()}
[0057] Inserting eq. (7) into eq. (5), the resealed velocity V() is
[0058]
[0059] Eq. 9 will be a straight line if
[0060] Fluids with non-zero yield stress will have a linear region where >>.sub., but the slope will rapidly approach infinity as x approaches .sub..
For the Newtonian case, where n=1, solving equation (8) for the viscosity and equation (7) for the strain rate give
And
[0061] The function k()=.sup.2/(2V())=P.sup.2/(2F|v.sub.0v|) is also useful for non-Newtonian fluids. If equation (8) is inserted into equation (10), the function f() becomes
[0062] Taking the log of both sides of eq. (11),
[0063] And, if the yield stress .sub.y=0,
[0064] Taking the log of both sides of eq. (13),
[0065] Which is a straight line of slope (2n1)/n and intercept In
[0066] Since the viscosity as a function of shear stress for the abovementioned fluids takes the form
[0067] The ratio of f()/
[0068] So that f(r) can be easily determined from (), as n can be found from plots of ln(f()) versus ln() or of ln(V()) versus ln().
[0069] In NMR imaging systems, the velocity of material flowing through an envelope such as a tube or conduit can be found using either time of flight techniques or using phase encoding techniques. In either case, the flowing fluid is exposed to a constant magnetic field of a known strength, with a known spatial variation. After the spin systems have aligned with the imposed magnetic field, they are disturbed by a radio-frequency pulse that tags a region in the flow. Time of flight techniques involve building a velocity image by successively exciting a particular cross-section of the flow and detecting the arrival of the excited spins downstream from where they were excited. By knowing the downstream location where the spins were detected and the time between excitation and detection, the velocity profile can be constructed for laminar, unidirectional flow. Phase encode imaging produces direct images of velocity profile distributions for both unidirectional and more complex flows. In the case of unidirectional, steady flow, if the position of a nucleus with spin at time t is z(t), then z(t)=z.sub.0+wt where z.sub.0 is the position of the nucleus with spin at time zero and w is the velocity of the nucleus with spin. The applied magnetic field gradient in the flow direction has magnitude g.sub.z and the Bloch equations show that the phase of the magnetization is given by
=.sub.g.sub.0.sup.tz(s)g.sub.z(s)ds=(z.sub.0m.sub.0+wm.sub.1)(17)
where .sub.g is the gyromagnetic ratio of the nucleus and
m.sub.0=.sub.0.sup.tg.sub.z(s)ds
m.sub.1=.sub.0.sup.tsg.sub.z(s)ds(18)
[0070] In phase encode imaging, the applied gradient is designed such that m.sub.0=0 but m.sub.10. Then the phase angle is proportional to the velocity of the nucleus with spin; a properly designed gradient allows the phase to measure the distribution of velocities in the sample.
[0071] In an embodiment of the system of the present invention, gradients are chosen such that a three-dimensional map of the fluid front is generated from the velocity as a function of position in the sample.
[0072] In another embodiment of the system of the present invention, three 2D images of the flow front are created, each image perpendicular to the other two, and a 3D image of the flow front is recreated from the three images.
[0073] In other embodiments, more than three 2D images are created, and the angles between at least some of them differ from 90. For a non-limiting example, an image is created perpendicular to the direction of the flow, and three further images are made, all three perpendicular to the first one and each of the further images at 60 to the other two further images.
[0074] From the velocity distribution and the pressure drop across the sample, the resealed velocity V() (eq. (8)) is found. Using either eq. (9) or eq. (12), the type of flow can be found from the slope and the constant K from the intercept. From these, the viscosity, , of the fluid can be found.
[0075]
[0076]
The velocity is determined as a function of shear stress and the resealed velocity is calculated (632) and a log-log plot of the resealed velocity as a function of shear stress is created (636). The linear portion of the curve can be determined (640), using any of the methods known in the art, and the slope of the linear portion, n, calculated, using any of the methods known in the art. Once the slope n has been found, the constant K can be calculated (644) from the intercept of the linear portion with the shear stress =0 axis, where
If the curve remains linear even for the lowest shear stresses, (652), then the yield stress is zero (648). Otherwise, the yield stress (656) is found from the value of r where the resealed velocity decreases rapidly.
[0077] With the yield stress, n, and K, the type of fluid can be determined. If the yield stress is zero (664) and n=1 (660), then the flow is Newtonian (676) and K is the viscosity, . If the yield stress is zero (664) and n<1 (668), then the flow is pseudoplastic (684). Otherwise, n>1 and the flow is dilatant (680). If the yield stress is nonzero (664) and n=1 (672) then there is Bingham flow. Otherwise, the flow is Herschel-Bulkley flow (692). Since all the parameters for the flow have been determined, the flow is completely rheologically characterized. This characterization can be done in 3D, so that rheological differences between different regions in the flow can be determined. From the data, the flow front can be plotted. In some embodiments, the shape of the flow front is used to characterize the fluid. For non-limiting example, asymmetries in the flow front can indicate the presence of gas bubbles in the fluid, incomplete mixing of the components, unstable flow, or breakdown of an emulsion. The shape of the flow front can also be used to distinguish between laminar and turbulent flow, with turbulent flow having a flatter profile than laminar flow.
[0078] In one embodiment, the reaction is occurring during the time that the fluid is within the NMR device. The shape of the flow front, as described hereinabove, will characterize the maturity of the reaction so that corrective feedback can be applied, for example by altering the temperature of the tube walls, to bring the maturity within the desired parameters.
[0079] In another embodiment, the product is an emulsion such as mayonnaise. Emulsions normally exhibit Herschel-Bulkley type flow, with a sharply-pointed flow profile. If air bubbles are present or if the emulsion is breaking down, the flow profile becomes less pointed. Air bubbles or bubbles of unemulsified fluid will also cause asymmetries in the flow front, as will settlement of one or more components out of the emulsion.
[0080] In other embodiments, the system incorporates feedback mechanisms such that, if at least one rheological property of the fluid does not satisfy at least one desired criterion, at least one production parameter for the process is altered so as to cause the at least one rheological parameter of the fluid to satisfy the at least one desired criterion.
[0081] In yet another embodiment, the NMR system incorporates both high magnetic field NMR and low magnetic field NMR, such that a high resolution image of the velocities is acquired with the high-field system, a high-contrast image of the velocities is acquired with the low-field system, and the two images are fused to provide a high-contrast, high resolution image of the flow front of the fluid.
Example I
Comparison Between Power Law Exponent in a Flowing Fluid and Power Law Exponent Stored in a Database
[0082]
[0083]
Example II
Comparison Between Viscosity in a Flowing Fluid and Viscosity Stored in a Database
[0084]
[0085]