Integrated, portable sample analysis system and method
11796486 · 2023-10-24
Assignee
Inventors
- Patrick F. Henning (Concord, MA)
- Thomas G. Barraclough (Maynard, MA, US)
- Eric J. Olson (Phillipston, MA)
- Stephen D. Lawrence (Ayer, MA, US)
- Robert J. Yurko (Chelmsford, MA, US)
Cpc classification
G01N23/2076
PHYSICS
International classification
G01N23/207
PHYSICS
G01N23/223
PHYSICS
Abstract
A flip top spectrometer sample cell including first and second members each includes a window aligned with each other when the first and second members are coupled together defining a predefined spacing between the windows when the first and second members are coupled together, the first and second members decoupled for manually placing a fluid sample on a the window. The flip top spectrometer sample cell is configured to be withdrawn out of a housing for cleaning of the windows.
Claims
1. A sample cell system for infrared spectroscopic analysis comprising: a sample cell including: a first member, a second member for coupling to the first member, a first window port associated with the first member when the first and second members are coupled together and closed and also when the first and second members are decoupled and opened, a second window port associated with the second member when the first and second members are coupled together and closed and also when the first and second members are decoupled and opened, at least one of the first and second window ports configured to accept a fluid sample manually deposited directly on at least one of the first and second window ports when the first and second members are decoupled and opened, and at least three mounts associated with the first member and/or second member contacting the other member when the first and second members are coupled together and closed and spacing the first and second window ports from each other by about 100 microns when the first and second members are coupled together and closed forming a sample chamber for the fluid sample between the first and second window ports; a housing for the sample cell, the housing slidably receiving the first and second members in a channel in the housing when the first and second members are coupled together and closed to direct radiation along a radiation path through the first window port, through the fluid sample, and through the second window port for spectral analysis; and the housing and sample cell configured such that the first and second members can be slidably withdrawn from the housing channel and decoupled and opened to manually wipe said window ports clean prior to spectral analysis of another fluid sample and such that the first member is prevented from full removal from the housing.
2. The sample cell system of claim 1 in which the first and second members are plates.
3. The sample cell system of claim 2 in which the plates are hinged together.
4. The sample cell system of claim 1 in which the first window port is made of ZnSe.
5. The sample cell system of claim 1 in which the second window port is made of ZnSe.
6. The sample cell system of claim 1 in which the sample cell is vertically disposed in said housing channel.
7. The sample cell system of claim 1 further including a source of radiation in the housing for directing radiation through said first window port, through said sample, and through said second window port.
8. The sample cell system of claim 1 further including a seal about said windows.
9. The sample cell system of claim 1 in which the mounts are kinematic mounts.
10. The sample cell system of claim 1 in which said kinematic mounts are adjustable.
11. The sample cell system of claim 1 further including a coupler for removably joining the housing to a spectral analyzer.
12. The sample cell system of claim 1 in which one said member includes at least one magnet for releasably coupling said first and second members together.
13. A sample cell for infrared spectroscopic analysis comprising: a sample cell including: a first member, a second member, a first window port associated with the first member, a second window port associated with the second member, at least one of the first and second window ports configured to accept a fluid sample manually deposited directly on at least one of the first and second window ports when the first and second members are decoupled and opened, and mounts associated with the first member and/or second member spacing the first and second window ports from each other when the first and second members are coupled together forming a sample chamber for the fluid sample between the first and second window ports; a housing for the sample cell, the housing receiving the first and second members when the first and second members are coupled together to direct radiation along a radiation path through the first window port, through the fluid sample, and through the second window port for spectral analysis; and the housing and sample cell configured such that the first and second members can be withdrawn from the housing and decoupled to manually wipe said window ports clean prior to spectral analysis of another fluid sample.
14. The sample cell system of claim 13 in which the first and second members are plates.
15. The sample cell system of claim 14 in which the plates are hinged together.
16. The sample cell system of claim 13 in which the first window port is made of ZnSe.
17. The sample cell system of claim 13 in which the second window port is made of ZnSe.
18. The sample cell system of claim 13 in which the sample cell is vertically disposed in said housing.
19. The sample cell system of claim 13 further including a source of radiation in the housing for directing radiation through said first window port, through said sample, and through said second window port.
20. The sample cell system of claim 13 in which the sample cell is configured, when the first and second members are coupled together, to slide into the housing.
21. The sample cell system of claim 13 in which at least one of the first and second members are prevented from full removal from of the housing.
22. The sample cell system of claim 13 in which the housing includes therein a channel receiving the sample cell therein when the first and second members are coupled together.
23. The sample cell system of claim 22 in which said channel is vertically disposed in the housing.
24. The sample cell system of claim 13 further including a coupler for removably joining the housing to a spectral analyzer.
25. The sample cell system of claim 13 further including a seal about said windows.
26. The sample cell system of claim 13 in which the mounts define a spacing of about 100 microns between the first and second window ports when the first and second members are coupled together.
27. The sample cell system of claim 13 in which there are at least three mounts associated with one of the first and second members.
28. The sample cell system of claim 27 in which the mounts are kinematic mounts.
29. The sample cell system of claim 13 in which one said member includes at least one magnet for releaseably coupling said first and second members together.
Description
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
(1) Other objects, features and advantages will occur to those skilled in the art from the following description of a preferred embodiment and the accompanying drawings, in which:
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DETAILED DESCRIPTION OF THE INVENTION
(20) Aside from the preferred embodiment or embodiments disclosed below, this invention is capable of other embodiments and of being practiced or being carried out in various ways. Thus, it is to be understood that the invention is not limited in its application to the details of construction and the arrangements of components set forth in the following description or illustrated in the drawings. If only one embodiment is described herein, the claims hereof are not to be limited to that embodiment. Moreover, the claims hereof are not to be read restrictively unless there is clear and convincing evidence manifesting a certain exclusion, restriction, or disclaimer.
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(22) Syringe pump subsystem 22 includes port 24 for receiving a third portion of the sample. Syringe pump subsystem 22 is configured to urge the third portion of the sample through a filter (described below) which collects particles in the sample thereon. In one example, this filter is a component of a specially designed particulate cartridge received in outlet port 25. This particulate cartridge serves two key initial purposes: One, it is designed to behave as a pore blockage particle counting system in and of itself, which enables the user to obtain particle count (which includes number and size distribution), information from the device. Two, by monitoring the particle counting while the syringe is dispensing the oil liquid through the cartridge, it serves as a feedback loop to ensure that a consistent particulate deposition (e.g. total number of particles) occurs on the patch itself. This second purpose allows for a highly calibrated sample which significantly increases the accuracy of subsequent x-ray analysis. The particulate cartridge may be inserted into port 30 associated with x-ray analysis subsystem 28 which is configured to x-ray the particles on the filter and to output signals corresponding to the composition of the particles. In one example, the amount of elements (e.g., metals) such as Ag, Al, Cr, Cu, Fe, Mo, Ni, and Pb in ppm is determined.
(23) A fourth liquid portion of the sample (unfiltered) may be deposited on a liquid sample cartridge which is also inserted into x-ray analysis subsystem 28 port 30 and the x-ray analysis subsystem then outputs signals corresponding to the composition and amount of any dissolved material (e.g., metals) in the sample. The total amount of particular metals (dissolved and undissolved) may be calculated and displayed.
(24) A processing subsystem is also included as shown at 32 (e.g., a microprocessor, controller, or the like) and is responsive to the signals output by the viscometer, the infrared spectrometer, and the x-ray analyzer. Processing subsystem 32 is configured to process the signals corresponding to the viscosity of the sample, the physical properties of the sample, the composition of any particles present in the sample, and the composition of any particulate or dissolved material in the sample. The processing subsystem provides a report (for example, on monitor 34) concerning the sample and its viscosity, physical properties, particulates, and dissolved material and the like. Software operating on processing subsystem 32 is also configured to highlight certain select information about the sample based on its viscosity, physical properties, particulates, and/or dissolved material, etc. In but one example, if a value such as viscosity, ppm Ni, and/or % Glycol exceeds a maximum threshold or is below a minimum threshold, then the value may be displayed in red or otherwise highlighted. Trends can be reported, for example, by depicting on the screen, for a particular asset like an engine, the viscosity level for several samples taken at different times to indicate trend information. Trend information like a large jump from one example to another regarding the amount of iron present can be highlighted automatically for the user. The processing subsystem can even be programmed to make recommendations based on the outputs of the various analyzers and/or data sets over time.
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(26) The analyzer of the JR spectrometer subsystem (located behind panel 12b,
(27) In this example, the spectrometer subsystem includes flip-top cell 40 with hinged plates 50a and 50b, each including a window 16a and 16b. When the plates are coupled together, there is a predefined spacing between windows 16a and 16b for the second portion of the sample deposited via a syringe. Kinematic mounts 52a, 52b, and 52c define the spacing. Magnets can be used to releasably couple the plates together.
(28) Viscometer subsystem 18 is also shown in
(29) Second plate 110b is typically hinged to plate 110a as shown at 120 and includes flat surface 122 to 116 RMS and +/1 degree over rail 112 separated there from by a predetermined gap (e.g., 100-200 μm) and thus constrains fluid to the rail by surface tension when rail 112 (and plate 10a) is inclined (e.g., positioned vertically) and gravity pulls fluid along the rail from proximal end 116a to distal end 116b. Typically, the gap is much less than 9 times the width of the rail.
(30) In this particular design, plate 110b includes spaced recessed positive face magnets 130a, 130b, and 130c and plate 110a includes corresponding negative face magnets 132a, 132b, and 132c received in raised flat lands 144c, 146b, and 146d, respectively. Lands 144c, 146b, and 146d may be the same height as rail 112. Magnets 130 and 132 releasably couple plate 110a to plate 110b in order for plates 110a and 110b to be used for viscosity measurements and then separated (via the hinge) for cleaning. Alternatively, items 130a-130c could be magnets and items 132a-132c could be ferromagnetic material. The relative position of the magnets and/or the ferromagnetic material in the respective plates could also be reversed.
(31) To properly space surface 122 of plate 10b over rail 112 by a specific (e.g., 100 μm) gap when the two plates are coupled together, kinematic mounts 136a-136c are disposed in plate 110b as shown and mate with disks 138a-138c, respectively. Disk 138a-138c are disposed flush in lands 144d, 144b, and 146c, respectively, which also typically have a height the same as the height of rail 112. The same is true for lands 144a and 146a. Other means for providing a predefined gap between the top surface of rail 112 and plate 110b, however, are within the scope of the subject invention. See also U.S. Patent Application Publication No. 2010/0182599 incorporated herein by this reference.
(32) As shown, lands 144a-144d are spaced from each other and they are also spaced from rail 112 on one side of rail 112 while lands 146a-146d are spaced from rail 112 on the opposite side of rail 112. This arrangement, in turn, defines cross wise channels 150a and 150b, 152a and 152b, and 154a and 154b. Electromagnetic energy (e.g., laser light or LED light) can be directed in these channels in order to measure the velocity of a fluid sample moving along rail 112 as discussed below.
(33) In this particular embodiment, rail 112 also has proximal end 160 defining a well with ramp 162 sloping upwards to the rail top surface. Rail 112 divides into split fingers 164a and 164b on opposite sides of ramp 162. Ramp 166 may also be provided in plate 110b as shown to further define the fluid sample well. Various materials may be used for plates 110a and 110b including aluminum and stainless steel and typically all the features shown are machined or otherwise formed on the surfaces of the respective plates.
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(36) This arrangement allows for a measurement of the time it takes fluid on the top surface of rail 112a to move along rail 112 in order to thus provide a calculation of the velocity of the fluid on rail 112.
(37) Sources 192 direct light through the gap between the rail and the surface spaced from the rail. A sample of a fluid is deposited at port 178 (defined by sloping ramp 62a in plate 110a and sloping ramp 166 in plate 110b,
(38) The processing subsystem microprocessor or controller 32,
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(40) The gap is known (e.g., 100 μm), as is the constant K
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and the acceleration due to gravity. Other means for determining the kinematic viscosity of the fluid as a function of the predefined gap between the rail and surface 122 of plate 110b and the time it takes the fluid to flow along the rail are also within the scope of the subject invention. Microprocessor 32 can be programmed as set forth above and may reside in a portable computer of the like. The plates are then separated, the rail wiped clean, and then the viscometer is ready again for use. Processor 32 provides the viscosity information as a report to monitor 34 and can then provide one or more recommendations based on the fluid's viscosity and other properties.
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(44) The technician then removes cartridge 300 from syringe pump subsystem port 25,
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(46) A portion of the sample is delivered to well 36 of liquid sample cartridge 330 using a syringe and liquid sample cartridge 330 is then placed in port 30,
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(50) A pressure differential between fluid above and below the cartridge membrane (306,
(51) By including a pressure sensor 303,
(52) In the laboratory, a determination of the solids in a sample would include acid digestion to transfer the solids in liquid form for an analysis by x-ray techniques and the like.
(53) In the subject invention, solids (particles) are analyzed two ways: 1) the filtered particles (above a predetermined size) are x-rayed at a lower power using the filter membrane cartridge discussed above placed in the x-ray port (30,
(54) The result is analysis and identification of particles below and above a certain size (e.g., below and above 10 microns). The processing subsystem is preferably programmed to automatically energize the x-ray source at a lower power (e.g., 0.5 Watts) when the particle cartridge of
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(56) The system software operating on processor 32 is preferably an asset-based system. In other words, each measurement suite is tied to a particular asset (for example, the main diesel engine of a dump truck). Information about that asset is stored in a SQL database 404 stored in RAM, for example. Once a measurement suite takes place, the system software retrieves information associated with that asset and compares it to the measured values. In a typical configuration, this will include high-and-low limit values for each property measured. The software performs the comparison to the high-and-low limit values and the measured values and reaches a conclusion at three levels: One, at the specific property level (e.g., viscosity or Fe content), two, at the instrument level (IR, viscosity, x-ray, particle count), and three, at the overall recommendation level. The conclusion reached is configured to be at 3 levels: all OK, warning, and alarm. If any specific property associated with an instrument is in an alarm or warning state, the worst state of all properties will be reflected at the instrument level recommendation. Similarly, the worst state of any particular instrument will be reflected at the overall recommendation level.
(57) The software is configured such that the overall recommendation is simply an “OK” check mark for good, a warning sign for warning and a red circle with a slash though it for an alarm state. This is shown in the sample report screens of
(58) The software works to feed information into this reporting structure by initiating and collecting measurements from each individual system instrument. The individual instrument information is gathered by the software and archived automatically in the on-device SQL database. In general, the raw information from each instrument is turned into measurement information (e.g. amount of water or Si in ppm) by the system software. This is the information which populates the reporting section and is also archived in the same on-device SQL database. The system software allows for the creation of a measurement suite for a particular asset in order to streamline the measurement process. This information is stored in the database as unique asset information. For example, the user may not be interested in the viscosity of certain very low viscosity fluids (e.g., hydraulic fluids), so an asset which employs hydraulic fluids may be set up such that its measurement suite only includes IR and x-ray measurements. The menus and measurement navigation are changed automatically to reflect the measurement suite of the particular asset under test.
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(60) The processing subsystem is preferably configured (e.g., programmed) to highlight data and report data above a predetermined threshold and/or below a predetermined threshold. In the example shown in
(61) The result is a portable and highly integrated sample analysis system and method wherein a sample is analyzed using several instruments and the analysis information is processed in order to note important information about the sample and/or the equipment from which the sample originated. The system of the subject invention can be operated by a less-skilled worker. The carrying case of the portable system is designed in such a way that four portions of the sample can be presented to different instruments and then the processing subsystem provides a report concerning, for example, the sample and its viscosity, its physical properties, particulates and dissolved material. One or more recommendations can even be made based on the sample's viscosity, physical properties, particulates and the composition of any dissolved materials in the sample. Further, the operator does not need to use chemicals, solvents or diluents of any kind in order to operate the system. He or she simply wipes the viscometer and IR subsystems clean with a shop rag, and the entire system is ready for its next measurement. This makes the device particularly useful for operation in remote locations or where chemicals are not readily available, and significantly enhances its portability.
(62) In use, a technician takes a sample from an apparatus on site (e.g., oil from an engine crankcase) and uses a syringe to place a first-portion of a sample in viscometer 18,
(63) Although specific features of the invention are shown in some drawings and not in others, this is for convenience only as each feature may be combined with any or all of the other features in accordance with the invention. The words “including”, “comprising”, “having”, and “with” as used herein are to be interpreted broadly and comprehensively and are not limited to any physical interconnection. Moreover, any embodiments disclosed in the subject application are not to be taken as the only possible embodiments.
(64) In addition, any amendment presented during the prosecution of the patent application for this patent is not a disclaimer of any claim element presented in the application as filed: those skilled in the art cannot reasonably be expected to draft a claim that would literally encompass all possible equivalents, many equivalents will be unforeseeable at the time of the amendment and are beyond a fair interpretation of what is to be surrendered (if anything), the rationale underlying the amendment may bear no more than a tangential relation to many equivalents, and/or there are many other reasons the applicant cannot be expected to describe certain insubstantial substitutes for any claim element amended.
(65) Other embodiments will occur to those skilled in the art and are within the following claims.