Optics: measuring and testing – Sample – specimen – or standard holder or support – Fluid containers
Reexamination Certificate
2000-03-10
2002-09-17
Font, Frank G. (Department: 2877)
Optics: measuring and testing
Sample, specimen, or standard holder or support
Fluid containers
C356S244000, C137S237000
Reexamination Certificate
active
06452672
ABSTRACT:
PRIOR RELATED PATENTS AND APPLICATIONS
The present invention is directed to an optical flow cell design that can be cleaned automatically without invasive physical means. It is particularly useful when optical measurements are made following chromatographic separation since these are often associated with particulate material and air bubbles which tend to adhere to the optical surfaces themselves.
Expressly incorporated herein are the following patents and applications concerning flow cells and related structures whose performance would be improved with the new invention.
U.S. Pat. No. 4,616,927—“Sample Cell for Light Scattering Measurements,” (Oct. 14, 1996)
U.S. Pat. No. 4,907,884—“Sample Cell Monitoring System,” (Mar. 13, 1990)
U.S. Pat. No. 5,305,071—“Differential Refractometer” (Apr. 19, 1994)
U.S. Pat. No. 5,404,217—“Laser Liquid Flow Cell Manifold System and Method for Assembly,” (Apr. 4, 1995)
U.S. Pat. No. 5,530,540—“Light Scattering Measurement Cell for Very Small Volumes,” (Jun. 25, 1996)
Application Ser. No. 08/989,364 “A New Electrode Design for Electrical Field Flow Fractionation”, Steven P. Trainoff. (Filed Dec. 12, 1997)
Application Ser. No. 08/870,937 “Extended range interferometric refractometer”, Steven P. Trainoff, David T. Phillips, Gary R. Janik, and Douglas W. Shepard. (Filed Jun. 6, 1997)
BACKGROUND
In the field of light scattering, as applied to determine the molar mass and mean square radius of solvated molecules, measurements are made from solutions comprised of a solvent containing a dissolved sample. By measuring the scattered light variation with scattering angle and measuring the concentration of the solute, one may in principle determine the molar mass and mean square radius of such solvated molecules. Similarly, the light scattering properties of sub micrometer particles in liquid suspension may be used to determine their average size. Light scattering techniques may be applied as well for measurements involving inelastic light scattering such as photon correlation spectroscopy, Raman spectroscopy, fluorescence, etc. These measurements, usually performed at a fixed single angle, are used to determine the hydrodynamic size of the particles or molecules illuminated.
Light scattering measurements are often made with a light scattering photometer wherein the sample is introduced into an optical cell such as referenced above in U.S. Pat. Nos. 4,616,927 and 5,404,217. Interfering with such optical measurements are a variety of contaminants whose presence inside the flow cell often contribute to the recorded light scattering signals in such a manner as to distort or even mask them. Such contaminants arise from various sources, many of which cannot be avoided. Included among these are small air bubbles, fine particles shedding from chromatographic columns if such are being employed to separate the molecules or sub-micrometer particles prior to measurement, aggregates formed from the sample itself which may have a strong affinity for the internal optical surfaces, contaminants in the poorly prepared solvent, debris from previous measurements that build up on the optical surfaces, etc.
During the measurement process, the presence of these contaminants are often recognized indirectly through the effects they have on the scattering or are noticeably visible through physical examination of the scattering cell, or both. There are various means by which such contaminants are removed or dislodged from the internal optical surfaces such as flushing the optical cell with different solvents such as acids or detergents or introducing a large air bubble in the manner of the familiar Technicon AutoAnalyzer of the 1960s. Sometimes, no matter how much effort has been expended, the flow cell must be disassembled and each component cleaned manually. Once disassembled, one of the most useful means for cleaning surfaces is to use ultrasonic waves as created in an ultrasonic cleaning bath. The components are placed in a fluid such as water and ultrasonic waves whose fixed frequencies are of the order 50 kHz are propagated throughout the bath. These waves are generally generated by means of piezoelectric transducers well coupled to the bath chamber. At the frequencies and power levels traditionally applied, cavitation effects generally cause the generation of bubbles which, when driven against a surface, tend to assist in the cleaning and scrubbing of such surfaces.
Although the disassembly of an optical cell and the subsequent cleaning of its parts in an ultrasonic bath are effected, it is time consuming. Unfortunately, it is often the only means possible. When the optical cell is used in a high temperature environment, such as is the case for chromatographic separations requiring high temperature solvents, the traditional disassembly concept becomes even more time-consuming since the temperature of the chromatograph itself must often be reduced significantly to obtain access to the optical cell which is then removed and cleaned. High temperature chromatographs, and especially the columns used therein, can be damaged during temperature cycling which, therefore, must be carefully executed. The process of cleaning an internally mounted optical cell can, in such a case, require up to 24 hours to effect a removal, cleaning, and reinstallation.
It always has been thought desirable to have optical elements of the light scattering cells designed in such a manner as to prevent the deposition of extraneous materials on their surfaces or, at the very least, design them in such a manner as to permit the cleaning of their internal surfaces with minimal effort. To this end, many structures requiring clean, particulate-free surfaces have been designated as “self-cleaning” such that once internal precipitants are detected they may be removed without need for disassembling the structures themselves. A process by which the initial formation of such contaminants may be reduced is taught, for example, by Davidson in U.S. Pat. No. 5,442,437 wherein windows, through which optical measurements are to be made, are so positioned that they extend into the flowing solution which, thereby, continuously “ . . . scour said window to minimize contamination and clouding [thereof] . . . ” This, of course, is an old concept that was disclosed in U.S. Pat. No. 4,616,927, referenced above, and numerous other similar implementations whereby it is necessary to clean observation windows of various types. Although such cleaning may keep the observation windows clear of particulate debris for some time, eventually sufficient particles may accrete so as to interfere with light passing through some optical surface.
Another example of a self cleaning cell is U.S. Pat. No. 4,874,243 by Perren wherein the windows are at an angle to the direction of flow which results in a “ . . . self cleaning action . . . ” as the flowing stream passes over them. A similar example is U.S. Pat. No. 4,330,206 of Gausmann et al. wherein is shown a measurement chamber “ . . . inherently self-clearing of air or gas bubbles in liquid samples . . . [which provide] inherently efficient cleansing of the measurement chamber . . . ” This is achieved by outlet means lying above the optical region guiding thereby air bubbles up and out of the fluid enclosed. The fluid flowing into the measurement channel strikes the cell window obliquely, thus cleaning it and maintaining it free of contaminants.
Berger in his U.S. Pat. No. 4,496,454 describes another example of a self-cleaning mechanism for the case of electrochchemical cells used with certain forms of liquid chromatography. His invention attacks a similar problem for electrochemical detection that faces light scattering detection: the fouling of the electrode surfaces during measurement which, in turn, affects the detector response. In the light scattering case, the optical surfaces can become fouled with particulates and small air bubbles. Berger achieves his cleaning by using a capillary tube to generate a water jet perpendicular to the detector electrode surface.
In addi
Font Frank G.
Punnoose Roy M.
Wyatt Philip J.
Wyatt Technology Corporation
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