CA1256713A - Method for determining the size and/or concentration of materials in suspension - Google Patents

Abstract

ABSTRACT

A fiber optic probe having a sealed, cylindrical housing closed at one end by a transparent window and at the opposite end by a wall through which a plurality of optical fibers extend toward the window.
Adjacent the window the fibers are radially and cir-cumferentially spaced about the axis of the housing and converge along lines which intersect one another at a common point on the housing axis that is adjacent or beyond the outer surface of the window. At least one of the fibers transmits light from a source through the window to illuminate a zone of a fluid sample or medium, whereby particles present in such zone scatter light therefrom to the remaining fibers for transmission through the probe housing to light detecting and measuring apparatus The fiber optic probe is adapted for determining the size and/or concentration of moving, light reflective particles in suspension in the fluid medium.

Description

~2~ 3 FIBER OPTIC PROBE AND METHOD FOR
DETERMINING THE SIZE AND/OR
CONCENTRATION OF MATERIALS IN SUSPENSION

This invention relates to a fiber op-tic probe that is particularly useful for in-situ detec-tion and measurement of the intensity of light scat--tered by particles sus~ended in a -transparent or translucent fluid medium. This invention also relates to the in-situ measurement of the size and/or concen-tration of solid particles, immiscible li~uid droplets, or gas bubbles in suspension in the fluid medium.

In the practice of many chemical processes proper control of the process requires detection of the presence of a suspended phase in the reaction medium and determination of its concentration, particle size, or both. An example of such a process is one in which crystals are to be formed in a reaction li~uid.
Detection of the onset of crystallization usually is necessary to control the process in such manner as to yield crystals of the desired size and purity.
Detection of the onset o~ crystallization currently is accomplished by visual monitoring of the reaction medium, detection of the exotherm resultin~ from the heat of crystallization, or detection of an increase 34,420-F -1-

-2- ~5~7~3 of the -turbidity of the reaction medium as a result of the presence therein of crystals. These known methods often lack sufficient sensitivity and dynamic range for proper process control.

Numerous other methods exist for measuring the size and concentration of solid particles in suspension, but nearly all require removal of a sample of the suspension for examination and thus are not generally applicable to the measurement of li~uid droplets or gas bubbles. These known methods also are unsuitable for the measuremen-t of solid par-ticles in those instances in which the size and/or concentration undergoes changes unless the caus~ of the changes can be terminated abruptly on removal of the sample from the suspension.

A fiber optic probe constructed in accor-dance with the invention makes use of the phenomenon -that light traversing a transparent or translucent fluid medium containing particles whose refractive index differs from that of the medium results in the scattering of some of the light. This effect is known as Tyndall scattering. The fraction of the light scattered per unit of light path length depends on the surface area of the particles, the refractive indices of the medium and the particles (or, if the particles are opaque, on the reflectivity of the particle surface), and upon the relative sizes of the particles with respect to the wavelength of the illuminating ligh-t. At relatively low particle concentrations, the scattered light fraction is sub-stantially linear with the concentration, assuming the 34,420-F -2-~25 Ei7~3 other factors to be relatively constant. At rela--tively high concentrations, however, both the illu-minating light and the scat-tered light are attenua-ted by secondary scat-tering, resulting in non-linearity of the collected sca-ttered light with concentration.

A probe according to -the invention employs one or more optical fibers for transmitting light from a source to a continuous phase reac-tion medium so as to illuminate a predetermined area or zone thereof. The probe also employs one or more op-tical fibers to collect light scattered by particles in the illuminated zone and transmit such collected light to a detector. The use of optical fibers enables the illuminating light source and the collected light detec-tor to be located at safe distances from the medium being monitored.

Both sets of fibers, i.e., the illuminating light fibers and the scattered light collecting fibers, are enclosed in a single fluid tight probe housing having a transparent window at one end which confronts the medium to be examined. The material from which the housing is made is one which can withstand the heat and constituency of the medium so as to be capable of immersion in the medium itself and at any desired area and depth thereof. The optical fibers are so oriented to the longitudinal axis of the probe housing that -the longitudinal axes of the illuminating light fibers intersect -the longitudinal axes of the collected light fibers at a common point on the longitudinal axis of the housing. This arrangement provides an ade~uate ~one of illumination and an adequate illu-minated field of view.

34,420-F -3-~5~7~3 6469~-3722 More particularly, the invention resides in a .~ethod for determinin~ in situ the size and concentration of moving, light reflective particles present in a fluid medium, said method comprising:
(a) illuminating a zone of said medium with light capable of being transmitted by said medium and reflected by said particles;
(b) collecting light reflect by said particles and measuring the intensity of such collected light;
(c) determining both the average intensity value and the variation in intensity value of the collected light;
(d) using both of the values obtained in step (c) to compute a first value indicative of particle size and a second value indicative of particle concentration;
and (e) comparing the values obtained in step d with corresponding values obtained by the in situ application of steps (a), ~b), (c) and (d) to at least one other like medium containing like particles.
Probes constructed in accordance with the invention are illustrated in the accompanying drawings, wherein:
Figure l is a fragmentary sectional view of one embodiment and taken on the line l-l of Figure 2;
Figure 2 is an end elevation view of the embodiment of Figure l;
Figure 3 is a view similar to Figure l, but taken on the ~ine 3-3 of Figure 4 and illustrating another embodiment;

34,420-F -4-- ~256~3 64693-3722 .~

-4a-Figure 4 is an end elevational view of the embodiment of Figure 3;
Figure 5 is a view similar to Figure 3, but illustrating a further embodiment; and Figure 6 is a diagrammatic illustration of the manner in which a probe according to the invention may be used.

34,420~F -4a-~2S~7~3 A probe constructed in accordance with the embodiment of Figure 1 is generally designated by reference number 1 and comprises a hollow, cylindri-cal, elongate housing 2 formed of a metal ox some other suitable material capable of immersion in a fluid medium that is to be monitored. Hereinafter the fluid medium sometimes will be referred to as the sample. The housing 2 has external threads 3 at one end thereof. Fitted into the threaded end of the housing 2 is a support 4 having a flange 5 which is seated on the free end of the housing. Adjacent the flange is a groove 6 in which is accommodated a sealing ring 7 so as to provide a fluid -tight joint between the support and the interior of the housing.
The support 4 also is provided with an annular sroove 8 on which is seated another seal 9.

Seated upon the support 4 and the annular seal 9 is a transparent window 10 of suitable thickness, such as 2 mm, and formed of a suitable material, such as glass, quartz, sapphire, and the like. The support 4 and the window 10 are maintained in an assembled relationship by means of a cap 11 having an internally threaded bore 12 in which the threaded end of the housing 2 is accommodated. The cap has a flange 13 which overlies and seats upon the marginal edge of the window 10.

The opposite end of the housing 2 is exteriorly threaded as at 14 for accommodation in a correspondingly threaded skirt 15 of a cap 16. A
suitable seal 1~ is interposed between the end of the housing 2 and the cap 16.

34,420 F -5-5L~5~7~3 The cap 16 is provided with three axially extending openings 18 which are radially and cir-cumferentially spaced at uniform distances about the longitudinal axis 19 of the housing 2. The circum-ferential spacing between each opening 18 is preferably120 although it will be obvious that other spacings for the openings are practical.

Extending through each of the openings 18 is an optical fiber 20 o~ preferably uniform diameter.
Suitable seals 21 provide a fluid tight connection between the cap 16 and the fibers 20. The fibers extend through the housing and have corresponding ends fixed in openings 22 formed in the support ~. The openings 22 also are preferably radially and cir-cumferentially spaced uniformly about the axis 19 ofthe housing, but unlike the openings 18, the axes of the openings 22 converge in a direction toward the adjacent end of the housing. The angle of conver-gence may vary, as will be explained. The fibers 20 extend through the openings 22 and abut the inner surface of the window 10. Preferably, a thin coat-ing 23 of an optical coupling gel or oil having a refractive index similar to -that of the fibers and the window is in-terposed between the window and the confronting ends of the fibers to reduce reflection losses at the fiber/window interface.

At least one of the fibers 20 has its free end located in a position to receive light from a source and transmit such light through the window 10 to illuminate a zone of a fluid sample.
The remaining fibers may be coupled to one or more light detectors as will be explained in more 34,420-F -6-~567~

de-tail hereinafter. For the time being, however, it is sufficient to state that the longitudinal axes of all of the fibers 20 intersect one another and the longitudinal axis 19 of the probe 1 at a common point 24 which lies on the longitudinal axis of the probe beyond the outer surface of the window 10. The diameter of the illumina-ting fiber is such that a substantially cylindrical beam of light 25 passes through the window into the sample. The diameter of -the collec-ting light fibers preferably corresponds to that of the illumina-ting fiber so that, when an imaginary cylinder along the extended axes of the light collecting fibers 25a intersect with the light beam 25, there is formed a field of view 2~ having the configuration of two back-to-back cones. The significance of this will be explained hereinafter.

Figure 3 discloses a probe la which cor-responds to the probe 1 excep-t that the probe la has a window lOa having a convex outer surface lOb and the flange 13a at the free end of the cap 11 is configured to accommodate and seat upon the con-cave surface. The greatest thickness of the window lOa is at the longitudinal axis 19 of the probe and may be about 3 mm in thickness. Ano-ther dif-ference between the probes 1 and la is that thesupport 4a of the latter has four openings 22a therein instead of three. The openings 22a are uniformly radially and circumferentially spaced about the longi-tudinal axis 19 of the probe la and the longitudinal axes of the fibers converge and intersect one another and the axis 19 at a common point 24a. The angle of convergence with respect to the axis 19 is about 20. The intersection point 24a does not 34,420-F -7-~256~3 extend beyond the convex outer surface lOb of the window lOa, but instead coincides therewith.

Accomm~dated in each of the openings 22a is one of the optical fibers 20. Two diametrically opposed fibers are coupled to one or more li~ht sources for transmitting ligh-t beams 25a through the window lOa into the sample, whereas the other two fibers are associated with one or more light detectors for transmitting thereto light scattered by particles in that zone of the sample ad~acent the point 24a.

As is apparent from Figure 3, the resulting field of view 26a at the intersec-tion of the fiber axes and the housing axis is su~stantially conical in configura-tion with the base of the cone coinciding with the convex outer surface of the window lOa.
The field of view 26a, therefore, is less than the field of view 26 produced in the embodiment of Figure 1.

It is not necessary to use a window having a convex external surface to obtain a conical field of view like that indicated at 26a.

In the embodiment shown in Figure 5, the window lOa has a flat outer surface and a peripheral flange 27 which underlies a flange 13b at the free end of a cap llb. Between the flanges 13b and 27 is an annular seal 28. A support 4b is similar to the supports 4 and 4a and underlies the inner surface of the window lOb and is provided with openings 22b for either three or four optical fibers 20 whose 34,420-F -8-~2567~3 g longitudinal axes converge and intersect one another and the longitudinal axis l9b at a common point 24b located at the outer surface of the window lOb, as a conse~uence of which the field of view 26b is conical and has its base at the outer surface of the window.

In the application of any of the disclosed probes for use, optical fibers which are to transmit light into the sample have those ends which are remote from the sample optically connected to a suitable light source 29 as shown in Figure 6. Such fiber or fibers hereinafter will be referred to as the illu-minating fiber or fibers. The remote ends of the remaining fibers are connected to one or more suitable light detecting and intensity measuring devices 30 1~ and 31, respectively. Such remaining fibers herein-after will be referred to as the light collecting fibers. For convenience of illustration only one illuminating fiber and one light collecting fibex are shown in Figure 6.

A suitable source of light is a light emitting diode (LED), a laser diode, a continuous wave (CW) gas laser, an incandescent lamp, and a spectral lamp. Suitable detectors 30 include photodiodes and photomultipliers. A suitable inten-sity measuring device 31 is a photometer. The preferred detection and measuring devices comprise a photodiode and a transimpendance amplifier the output from which is coupled to a suitable control computer 32 or the like which is operable to control the process.

34,420-F -g_ 67~

More particularly, a sui-table source 29 of light is a Honeywell Model SPX 4689-04 GaAl~s light emitting diode ~LED) which emits light at a wavelength of about 0.8 micron and -this is suitable for use in suspensions of particles of about one micron or greater in diameter. The light source may be ener-gized by a Hewlett-Packard Model 6181C DC power source.
A suitable detector 30 is a Math Associates Model E-5100 silicon PIN photodiode. A suitable measuring device/amplifier 31 is a UDT model lOlA amplifier manufactured by United Detector Technology. A suitable control/computer 32 is an Intel single board computer Model SBC-80/24. Each optical fiber may be a plastic clad silica fiber having a core diameter of 0.6 mm. A
source of such fibers is Quartz Products Corporation.

If light other than that intentionally transmitted to the sample is present, an optical filter 33 can be interposed between the collecting fiber end and the detector 30 so as to exclude from -the latter light having wavelengths o-ther than those emitted by the light source.

If a high degree of ambient light exclusion is required, the light source 29 may be a monochro-matic CW gas laser, a laser diode, or a spectLal lamp, and the filter 33, 29 may be a narrow band pass filter or a monochromator.

In ~se, the probe l may be inserted via conventional tube fittings into a vessel 34 containing the sample 35 to be examined for the presence of particles or the probe may b~ immersed in the medium at any desired location within the latter.

34,420-F -10-2567~,3 Although the term "particles" is used herein, such term is intended to encompass all forms of materials present in discontinuous form in a reaction medium. Thus, the term "particles" is intended to apply to materials such as liquid dropl~ts in a gas or in an immiscible liquid, gas bubbles in a liquid, or solid particulate in a gas or liquid.

The embodiment shown in Figure 1 is pre-ferred for use in the monitoring of samples containing low concentrations o~ particles. This is because a sample containing a low concentration is less turbid than one having a greater concentration, as a conse-quence of which there is less obstruction to penetra-tion to penetration of the sample by the illuminating light beam. Thus, the light beam 25 is capable of illuminating a relatively large volumn of the sample as compared to the probe design 43 e.g. Figure 3 or 5.

The field of view 26 is determined by pro-jecting the imaginary cylinder 25a of the lightcollecting fiber 20 beyond the outer surface of the window 10 so that it intersects the light beam 25.
Any particles in the field of view 26 will reflect or scatter some of the light and some of the scattered light will be collected by the light collecting fiber and will be transmitted by the latter to the detector and intensity measuring devices.

In those instances in which the co~centration of particles in the sample is relatively high, the probe la of ~igure 3 or 4 is preferred. In such case the light beams 25a emitted by the illuminating fibers 34,420-F -11-12 ~5~7~

have a relatively shallow penetration into the sample, but the field of view 26a commences at the exterior surface of the window, thereby enabling light scattered by par-ticles in the field of view to be collected by the light collecting fibers.

The sensitivity of probes constructed accor-ding -to the invention is dependent upon (1) the amount of light conducted to the field of view, (2) the efficiency with which the light scattered by the particles in the sample is collected and transmitted to the detector, and (3) the efficiency with which light other than that scattered by the particles (extraneous light) is excluded.

For detection of very small concentrations of particles (in the parts per million to parts per billion range) exclusion of extraneous light is the most important consideration. A major source of extraneous light results from reflection of the illu-minating light at the in-terface between -the sample and the window. Typically 10 5 to 10 2 Watts (W) of light are used to illuminate the sample. The reflection at the window-sample interface is typically about 0.1 to 1 percent, or 10 4 to 10 8 W, and varies with the refractive index of the sample. The scattered light collected from very low concentrations of particles may be as low as 10 13 W, Accordingly it is necessary to exclude virtually all of the reflected light.

The geometry of the probes disclosed herein has been selected to yield maximum exclusion of reflected light consistent with otherwise acceptable performance.

34,420-F -12--13- ~2567~3 This is accomplished by choosing the angle be-tween the longitudinal axes of the fibers and the longi-tudinal axis of the probe, the radial spacing of the fibers from the longitudinal axis of -the probe, the circumferential spacing between the fibers, and the window thickness so that light reflected from the window does not fall on any of the collecting fiber ends. Typically, these factors are so selected that such reflected light falls either along the probe axis or on that side of the probe axis opposite the illuminating fiber and bet.ween adjacent collecting fibers. By positioning the illuminating fibers diametrically opposite one another, light reflected from one such fiber is least likely to fall on a light collecting fiber.

The amount of light collected and trans-mitted by the collecting fibers is approximately proportional to (1) their total cross-sectional area (i.e., the product of the number of collecting fibers and the cross-sectional area of each), (2) the inverse of the square of the distance between the ends of the fibers and the intersection of their axes, and

(3) the angle between the illuminating fiber(s) and the collecting fibers(s). The optimum angle was found experimentally to be between about 20 to 25~ for particles with diameters between 0.2 and 200 microns, but angles between about 10 and 30 yielded sensi-tivities within about 30 percent of the maximum.

A radial distance from the fiber to -the longitudinal axis of the probe of two to three times the fiber diameter was found to yield satisfactory results for three and our fiber probes in which the 34,420-F -13-~2S6~3 angle be-tween the longitudinal axes of the fibers and the longitudinal axis of the probe is between 10 and 25. The choice of the circumferential spacing between the illuminating fibers and the collecting fibers also represents a compromise between sensitivity and extra-neous light reflection, with relatively small spacing (less than 90) yielding better extraneous light rejec-tion, but poorer sensitivity than larger spacing ~over 90). In practice, a circumferential spacing of the fibers of from 60 to 120 performs well.

Assuming that the circumferential spacing between the fibers and the ratio between the fiber diameter and the distance to the longitudinal axis of the probe is constant, the sensitivity is approximately proportional to the fiber diameter. This results from the fact that both -the cross-sectional area of the fibers and -the sguare of the distance to the inter-section are proportional to the square of the fiber diameter, while the depth of field (i.e., the length of the region in which the fields of view of the illu-minating fibers and the collecting fibers overlap) increases with the fiber diameter. Plastic clad silica fibers having a core diameter of from 200 to 600 microns are most suitable. The larger diameters (about 600 microns) perform slightly better and are easiest to handle and are thus preferred. Fibers with larger core diameters are more expensive however and require probes of a larger diameter, due to their large bending radii, and are thus less desirable.

The diameter o~ the illuminating fibers may be identical to each other and to that of the collec-ting fib~rs. When used in conjunction with LEDs or 34,420-F -14-~2567~

extended light sources, such as incandescent lamps or spectral lamps, smaller fibers will generally transmit less light to the sample and larger fibers increase the extraneous light more than they increase the illumina-tion of the region viewed by the collection fibers.
When focused beams from CW lasers or laser diodes are used for illumination, fibers with core diame-ters smaller than those of the collection fibers are pre-ferred because their use results in less extraneous light due to the smaller diameter of the reflection from the window sample interface. Further, the depth of field of the probe is reduced, due to the smaller diameter of the illuminating light beam, which results in increased dynamic range. Illuminating fibers with core diameters of from 100 to 300 microns perform well in conjunction with laser light sources and 600 micron diameter collecting fibers.

The number of collecting fibers employed represents a compromise between sensitivity and expense. One collecting fiber is sufficent for most applications, but more are advantageous for appli-cations requiring high sensitivity.

One illuminating fiber is sufficient to collect the light from a light emitting diode, laser, or laser diode, whereas two or more are advantageous for collecting light from extended sources.

Probes with more than the minimum number of fibers required for the measurement provide redundancy which is advantageous in case of fiber breakage.

34,420-F -15--16- ~2S6~13 The present invention also relates to a method for measuring either the size or concentration, or both simultaneously, of particles, immiscible liquid droplets, or gas bubbles suspended in a fluid medium employing the apparatus hereinbefore described. For convenience, the term "particle~s)" as used hereinafter in the description and claims means solid particulate material, gas bubbles, or liquid droplets. The measurements can be performed in-situ within closed reactors, pipes, or other process equipment. It thus is suitable for process control applications.

The method is applicable to suspensions which are stirred, agitated, or flowing, or in which the particles otherwise are set in motion as, for example, suspensions in which the particles are moving under the influence of gravity.

The method comprises illuminating a zone of a fluid medium containing moving, light reflective particles with light of a constant intensity and collecting and measuring a portion of the light reflected by the particles. The average intensity and the variance of the intensity of the collected reflected light are computed. The size and con-centration of the particles are determined by comparison of the computed values with values resulting from identical measurements of a like medium containing like particles of known size and concentrations.

Upon illumination of a zone of a trans parent or translucent medium containing particles which are at least as large as the wavelength of the 34,420-F -16--17- ~6~3 illuminating ligh-t, and which have a refractive index different from that of the medium, a fraction of the light is reflected. The fraction of the incident light reflected from an illuminated zone of fixed volume within the medium depends on the size and number of particles present in that zone and on the refractive indices o~ the particles and the medium.
If the intensity of the illuminating light is not constant throughout -the illuminated zone, or if the efficiency of collection of the reflec-ted light is not constant throughout, the intensity of the detected light (i,e., the collected, reflected light) from a par-ticle will depend on the position of the particle within the zone. If the particles are in motion, rather than stationary, the number and positions of particles in -the illuminated zone will vary with time, thereby resulting in random fluc-tuations in the intensity of the detected light. The magnitude of these fluctuations will depend on the size and number of particles present.

In a case in which a dilute suspension of monosized particles is illuminated by light of constant intensity, the fraction of light reflected from each par-ticle may be considered a constant.
Thus, fluctuations in the intensity of the detected light will be due to the statistical variations in the number and positions of particles in the illu-minated zone. In this ins-tance, the average (mean) intensity of the detected light (X) and the variance (V) of the intensity of the detected light are given by:
X = A* (C/D) Equation 1 V = B* (CD) Equation 2 34,420-F -17-~L256';7~3 where D is the particle diameter, C is the particle concentration, and A* and B* are quantities whose values depend on the refractive index or reflectivity of the particles, the intensity of -the illuminating light, the size of the illuminated zone, and the geometry of the illuminating and light collecting optics. A* and B* thus are constants for a par-ticular combination of particle material, sus-pendin~ medium, and optical system.

Equations 1 and 2 can be solved simultaneously for the concentra-tion i~C) and diameter (D) to yield:
C = A (XV)1/2 Equation 3 D = B X Equation 4 where A and B are constants which are related to A* and B* by the equations:

A = A*B* Equation 5 A* 1/2 20B = B* Equation 6 If a suspension of particles o known size and concentration is obtained, the size and concen-tration of like particles of unknown size and concen-tration suspended in a like medium can be determined by measuring the mean and variance of the intensity of light reflected by the known and unknown sus-pensions, respectively, usin~ the same measuring apparatus for both suspensions, and applying Equation 3 and Equation 4.

34,420-F -18--19~ 567~3 Because Equation 3 is independent of the particle size and Equa-tion 4 is independent of con-centration, it is possible to determine either the size or the concentration independently.

The determination of particle size in a medium does not necessarily require that the average concentration of the particles in the illuminated zone be the same as that of the entire medium. It is only necessary tha-t the particles in that zone be representative. Thus, the invention is applicable to particle size determination in processes in which the particle concentration is not constant throughout the medium.

If s-table samples of known particle size and concentration are no-t available, as always is the case for gas bubbles, and often for liquid droplets, the calibration must be performed external to the process equipment. This sometimes can be accom-plished by making light reflection measurements simultaneously with other measurements, such as photography-image analysis, which yields measures of the concentration and particle size.

If a suspension of known particle size and concentration is not available, the relative sizes and concentrations of the particles in two suspensions of the same material in the same medium still can be determined. If Xi and Vi represent the average intensity and variance, respectively, of the detected light from one sample, and Ci and Di represent the concen-tration and average particle si7.e of the particles inthat suspension, and if Xj, Vj, Cj, and Dj represent 34,420-F -19--20- ~2S~3 the same variables in a second suspension of the same material in the same medium, then:
Ci XiVi 1/2 Cj XjVj Equation 7 Di X~ l/2 Dj XiVj Equation 8 The direction, i.e., smaller or larger, and the relative magnitude of changes in the concentration and of the average size of particles, in a single suspension, also can be determined by repeatedly measuring the average intensity and variance of the collected liyht and applying Equations 7 and 8.

In some instances not all of the conditions stated above will be met. For example, in some industrial processes the size or concentration of the particles may not fall within the range for which Equation 1 and Equation 2 are valid. In these cases the relationships among the size, concentration, mean, and variance are complex and exact expressions relating the variables cannot easily be derived. In such cases multiple known suspensions, having particle sizes and concentrations throughout the ranges of interest, may be employed to determine empirical relationships which will have the general form of nonlinear simultaneous equations. If the average in-tensity and variance of the detected light are monotonic functions of the average particle size and concentration throughout the range of interest, unique values for the concentration and average particle size of an unknown suspension can be obtained by inserting the measured values of -the average intensity and the variance of the detected light from the unknown samples into the empirical equation thus obtained.

34,420-F -20--21- ~2S67~3 The concentrations and average diameters of samples of polystyrene beads were determined by the following procedure:
I. Calibration Samples A plurality of samples o~ polystyrene beads of known size were suspended in an aqueous sodium chloride solution. Three different samples of beads, having average diameters of 0.222 mm, 0.458 mm, and 0.621 mm, .respectively, were suspended in the solution at concentrations of between 1.5 percent and 15 percent by volume. The beads were set in motion by agitation of the suspensions. Using the apparatus described above, the intensity of the reflected light was measured ten -thousand times at three millisecond intervals for each suspension and the average (mean) and variance of these measurements computed. This was done thre~ times for each of the suspensions. Average values for the mean and variance of each suspension were then used to compute, by the method of least squares, the cons-tants for the regression equations:
C = K1 (XV)1/2 + K2 Equation 9 D = K3 X + K~ Equation 10 II. Unknown Samples Twenty-seven suspensions then were prepared like the calibration samples, except that the diameters of the beads were not known. The values of the mean and variance of the intensity of the detected light from each suspension were determined in a manner identical to that used in the calibration procedure.
Measured values for the concentrations and average diameters then were obtained by inserting the detected 34,420-F -21-~256713 mean and variance values in-to the linear regression Equations 9 and 10. The true average diameters of the three samples were then determined by micropho-tography. The measured and true values for the par-ticle diameter and concentration of each unknownsuspension are set forth in the following Table:

TABLE
(Resul-ts from Illustrative Example) Diameter Rel Concentration Rel (microns) Error (Vol. %) Error Sample Meas. True % Meas. True %
1 324 301 7.6 2.24 2.30 2.6 2 318 301 5.6 3.19 3.03 5.3 3 310 301 3.0 4.44 4.12 7.8

4 302 301 0.3 5.32 5.00 6.4 318 301 5.6 6.44 5.73 12.4 6 324 301 7.6 7.56 6.60 14.5 7 315 301 4.7 8.14 7.42 9.7 8 324 301 7.6 9.20 8.19 12.3 9 323 301 7.3 10.44 9.11 14.6 360 374 3.7 2.19 2.74 20.0 11 407 374 8.8 3.87 3.89 0.5 12 396 374 5.9 4.94 4.94 0.0 13 399 374 6.7 6.33 6.17 2.6 14 404 374 8.0 7.63 7.41 3.0 383 374 2.4 8.59 8.82 2.6 16 389 374 4.0 9.81 9.23 6.3 17 395 374 5.6 11.29 11.44 1.3 18 398 374 6.4 12.56 12.89 2.6 19 450 4~7 0.7 2.85 3.35 14.9 459 447 2.7 4.19 ~.50 6.9 21 436 447 2.5 5.33 5.91 9.8 22 430 447 3.8 6.43 7.15 10.1 23 450 447 0.7 7.66 8.19 6.5 24 439 447 1.8 8.59 9.51 9.7 448 447 0.2 7.86 10.74 8.2 26 444 447 0.7 10.75 11.96 10.1 27 456 447 2.0 12.06 13.22 8.8 34,420-F -22--23 ~25~7~

The disclosed embodiments are represent-ative of presently preferred embodiments of the inven tion, but are intended to be illustrative rather definitive thereof.

34,420-F -23-

Claims (15)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS
FOLLOWS:

1. A method for determining in situ the size and concentration of moving, light reflective particles present in a fluid medium, said method comprising:
(a) illuminating a zone of said medium with light capable of being transmitted by said medium and reflected by said particles;
(b) collecting light reflect by said particles and measuring the intensity of such collected light;
(c) determining both the average intensity value and the variation in intensity value of the collected light;
(d) using both of the values obtained in step (c) to compute a first value indicative of particle size and a second value indicative of particle concentration; and (e) comparing the values obtained in step (d) with corresponding values obtained by the in situ application of steps (a), (b), (c) and (d) to at least one other like medium containing like particles.

2. The method of Claim 1, wherein the size and concentration of the particles in aid other medium are known.

3. The method of Claim 1, wherein said particles have a diameter at least as great as the wavelength of the illuminating light.

4. The method of Claim 1, wherein said illuminating light has a constant intensity.

5. The method of Claim 1, wherein said illuminating light is introduced to said medium from a remote source via at least one optical fiber.

6. The method of Claim 1, wherein the collected reflected light is transmitted from said medium via at least one optical fiber.

7. The method of Claim 1, wherein said illuminating light is introduced to said medium from a remote source via a single optical fiber and the collected reflected light is transmitted from said medium by a single optical fiber.

8. The method of Claim 1, wherein said particles are solid.

9. The method of Claim 1, wherein said particles are gas bubbles.

10. The method of Claim 1, wherein said particles are immiscible liquid droplets.

11. A method for determining in situ the size of moving, light reflective particles present in a fluid medium, said method comprising:

(a) illuminating a zone of said medium with light capable of being transmitted by said medium and reflected by said particles;
(b) collecting light reflected by said particles and measuring the intensity of such collected light;
(c) determining both the average intensity value and the variation in intensity value of the collected light;
(d) using both of the values obtained in step (c) to compute a value indicative of particle size; and (e) comparing the value obtained in step (d) with a corresponding value obtained by the in situ application of steps (a), (b), (c) and (d) to at least one other like medium containing like particles.

12. The method of Claim 11, wherein the size of said like particles is known.

13. A method for determining in situ the concentration of moving, light reflective particles present in a fluid medium, said method comprising:
(a) illuminating a zone of said medium with light capable of being transmitted by said medium and reflected by said particles;
(b) collecting light reflected by said particles and measuring the intensity of such collected light;
(c) determining both the average intensity value and the variation in intensity value of the collected light;
(d) using both of the values obtained in step (c) to compute a value indicative of particle concentration; and (e) comparing the value obtained in step (d) with a corresponding value obtained by the in situ application of steps (a), (b), (c) and (d) to at least one other like medium.

14. The method of Claim 13, wherein the concentration of said like particles is known.

15. The method of Claim 1, 11 or 13, wherein said medium contains a plurality of said particles, and wherein the light is reflected by said particles.