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WO1995026018A1 - Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur - Google Patents

Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur

Info

Publication number
WO1995026018A1
WO1995026018A1 PCT/US1994/003006 US9403006W WO9526018A1 WO 1995026018 A1 WO1995026018 A1 WO 1995026018A1 US 9403006 W US9403006 W US 9403006W WO 9526018 A1 WO9526018 A1 WO 9526018A1
Authority
WO
WIPO (PCT)
Prior art keywords
light
fluid
vapor
gas
light sources
Prior art date
Application number
PCT/US1994/003006
Other languages
English (en)
Inventor
Scott D. Wohlstein
Emil W. Ciurczak
Original Assignee
Sd Laboratories, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to US07/677,643 priority Critical patent/US5296843A/en
Priority claimed from US07/677,643 external-priority patent/US5296843A/en
Application filed by Sd Laboratories, Inc. filed Critical Sd Laboratories, Inc.
Priority to AU65891/94A priority patent/AU6589194A/en
Priority to PCT/US1994/003006 priority patent/WO1995026018A1/fr
Publication of WO1995026018A1 publication Critical patent/WO1995026018A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
    • G01N21/3151—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths using two sources of radiation of different wavelengths

Definitions

  • the invention relates to a fluid or vapor diagnostic device and more particularly to a device which non-destructively determines the quality of a fluid or vapor tested by passing light of different wavelengths through the fluid or vapor and then comparing the ratio of the resulting detected light strengths to a predetermined ratio indicating whether the operating parameters of the fluid or vapor are within acceptable limits.
  • fluids refers to both fluids, gases and vapors unless stated otherwise. It has been found that when many fluids are exposed to a variety of environmental conditions, their physical properties change.
  • the light absorbing properties of a fluid is altered by the breakdown of the fluid itself, or by the introduction of contaminants or additives into the fluid. It was also discovered that breakdown or contamination of the fluid affects the light absorbing characteristics of the fluid by different amounts for different wavelengths of light.
  • a ratio established by passing light of various wavelengths through the fluid to be tested and then detecting and comparing the strength of the light after passing through the fluid indicates the condition of the fluid related to the above mentioned detrimental characteristics or indicates the presence of an additive.
  • the ratio for the preselected wavelengths reaches a certain ratio, the fluid is no longer within acceptable standards set for the fluid or contains certain amount of an identifiable additive.
  • the fluid In the case where the fluid is changing due to use or contamination, because the change in fluid takes place within the environment where the fluid is found and because change in the fluid is a continuous process, the fluid should be tested continuously while it is being used in order to immediately detect detrimental changes. In this context, it is preferable to non-destructively, continuously test the fluid so that the testing process itself does not contribute to the breakdown and contamination problems of the fluid. Therefore, the light of various wavelengths should be introduced to the fluid in such a way that it can continuously and non-destructively interact with the fluid while helping to determine the condition of the fluid.
  • Light of preselected wavelengths is passed through a fluid to be tested.
  • the light is detected after passing through the fluid.
  • a voltage is created for each wavelength of light, proportional in amplitude to the detected light strength of each wavelength.
  • These proportional voltages are compared to produce a ratio which represents the condition of the fluid.
  • control signals which may trigger alarms or other warning devices, are triggered.
  • the light of the selected wavelengths is created preferable by appropriate photodiodes.
  • the light is introduced into the fluid to be tested by transmitting the light of the various frequencies through respective fiber optic cables into a reservoir of the fluid. There the light is emitted across a gap through which the fluid may travel. The emitted light is then received through a corresponding fiber optic cable on the other side of the gap. The received light is transmitted through a fiber optic cable out of the reservoir where its strength may be determined.
  • the signal strength of the light received across the gap is determined by having the light impinge on a detector which produces a voltage output proportional to the impinging light strength.
  • the resulting electronic analog signal may be processed to amplify it and filter noise present with the signal. Thereafter, the electronic signals corresponding to the detected light strengths from the different wavelengths are electronically combined to from a ratio. This ratio has been found to represent the quality of the fluid that is being tested.
  • the ratio is analyzed to determine whether it lies within preselected boundaries representing acceptable qualities of the fluid. If the ratio is found to be outside of these boundaries, control signals are generated to draw attention to the unacceptable quality of the fluid.
  • a probe containing the light emitting and receiving fibers, as well as the gap between them is mounted in the wall of a reservoir of a fluid to be tested.
  • the light creating devices, the light detectors, ratio determining and analyzing circuitry, control signal generator circuitry, and alarm means are all located outside the fluid reservoir.
  • control signals are sent out of the reservoir by appropriate means.
  • a handheld unit having a probe comprising respective input and output fiber optics separated by a gap is provided.
  • the probe may be immersed into a selected fluid for testing.
  • the operation of the device is exactly the same as that described above except that the gap and fiber optic cords are not continuously present within the fluid reservoir to be tested, but are instead inserted into the fluid at the discretion of the user. It is an object of the invention to provide a device for non-destructive testing of fluids in real time in the environment where the fluids are found under work conditions.
  • Fig. 1 is a block diagram of the invention.
  • Fig. 2A is a side view of the probe.
  • Fig. 2B is a plan view of the probe.
  • Fig. 3 is a block diagram of the electronics of the invention.
  • Fig. 4 is a block diagram of the preferred embodiment of the signaling system.
  • FIG. 1 shows a block diagram of the invention generally labeled 10.
  • a probe 12 (Fig. 2A, B) is placed in contact with the fluid or vapor to be tested.
  • First and second light sources 14, 16, (Fig. 3) respectively, each provide light of a preselected wavelength to probe 12 through first and second input cables 24, 26 respectively.
  • first and second light source 14, 16 are photo-diodes while first and second input cable 24, 26 are fiber optic cables.
  • the photo-diodes are chosen to have specific emission frequencies for the particular fluid to be analyzed. These preselected wavelengths have been experimentally determined to yield optimum results in determining the quality of the fluid that is tested. Experience has shown that for most fluids, the wavelength of light used ranges from .4 micrometers, which is in the visible range, to 5 micrometers which is in the midinfrared range.
  • wavelengths of 450 nm and 550 nm yield the most 9 accurate determination of the quality of the motor oil.
  • the wavelength of 1500 nm has been found to be particularly effective.
  • photo diodes are the preferred light source 14,16 for the invention, any other source of light which is able to produce selected wavelengths such as standard LEDs, SRLEDs, or laser diodes are within the scope of the invention. Additionally, lasers at the preselected wavelengths, monochromatic incandescent light sources, or filtered light which produces light at the preselected wavelengths may also be used.
  • the important thing is that light, including possibly modulated light, of preselected wavelengths is made available.
  • the preselected wavelengths may be either fixed wavelengths or preselected bands of wavelengths which may be scanned.
  • First and second input cables 24, 26 are attached on their opposite ends to probe 12 as shown in detail in Fig. 2A.
  • Cables 24, 26 are fiber optic cables.
  • the first and second input cables 24, 26, enter probe 12 through a connector 48.
  • Connector 48 is in turn attached to bulk head 49.
  • the fiber optic cables of first and second input cables 24 and 26 extend through connector 48 and bulk head 49 and exit bulk head 49 through first and second emission fibers 36, 46, respectively which are also fiber optic cables.
  • first and second detection fibers 32, 42 also comprised of fiber optic cables.
  • each light source has its own fiber optic cable carrying that light to and from the fluid reservoir.
  • a first and second gap 34, 44 separates the emission fibers 36, 46 and detection fibers 32, 42 respectively.
  • First and second gaps 34, 44 allow the fluid or vapor of interest to move between the respective emission fibers 36, 46 and detection fibers 32, 42.
  • the gap 34,44 between respective emission and detection fibers 36,32 and 46,42 may be quite small, possibly even being as small as a millimeter.
  • Table 1 shows the length of the gap 34, 44 found to be most effective in analyzing the corresponding fluid or vapor with the respective wavelength of light. Also shown is the type of analysis possible and whether the analysis is qualitative or quantitative.
  • First and second detection fibers 32, 42 extend through bulk head 49 and connector 48 to exit probe 12 through first and second output cables 25, 27 respectively.
  • Output cables 25, 27 are also made of fiber optics, and are connected to spectrometer 18.
  • a screen 35 surrounds first and second emission fibers 36,46 and first and second detection fibers 32,42. This screen 35 prevents debris from entering first and second gaps 34,44 and disrupting the light path between the respective emission and detection fibers.
  • a wall 37 shown in side view in Fig. 2A and in top view in Fig. 2B, is placed between the respective pairs of emission and detection fibers 36,32 and 46,42. This wall 37 prevents stray light from one of the emission fibers 36,46 from being diffracted into the other pair's detectors 42,32 and thereby affecting the light signal detected across respective first and second gaps 34,44.
  • Spectrometer 18 comprises detectors 15, 17 and analyzes the absolute strength or intensity of the light received from first and second detection fibers 32, 34 which has been passed on to spectrometer 18 through first and second output cables 25, 27. Spectrometer 18 determines this absolute light strength for each frequency of light received from the respective first and second detection fibers 32,34. In essence, spectrometer_ light signals of varying amplitude into a proportional electric signal of varying electrical amplitude. Cadmium sulfide (CdS) or Lead Sulfide/Lead Selenium (PbS/PbSe) detectors 15, 17 have been found to be particularly adapted to perform this conversion.
  • CdS Cadmium sulfide
  • PbS/PbSe Lead Sulfide/Lead Selenium
  • modulator 28 which is a timer connected to a switch which alternately activates and deactivates the respective light emitters 14, 16 and corresponding detectors 15, 17.
  • modulator 28 An RCALM555CN timer and GE-CD4066 Quad-Bilateral Switch have been found to produce an excellent modulator 28.
  • Filter 19 may be any analog or digital voltage filter which suppresses spurious noise in the voltage signal from the detectors.
  • filter 19 may include an A to D converter followed by a digital filter followed in turn by a D to A converter.
  • filter 19 may include a phase locked loop. Such filters are well known in the art. The resulting filtered signal is now a "clean" signal free of spurious noise.
  • This "clean" signal may be amplified by amplifiers 23 A,B to produce an appropriate signal strength as needed.
  • the amplifiers 23 may be standard OP-AMPs.
  • the outputs of amplifiers 23, A, B are passed to Log converters 55A, B which determine the Log of each wavelength's signal strength.
  • Log converters 55A, B are diode feedback type Log converters or Log/Antilog Amps such as GE-1CL8048 which are well known in the art.
  • the outputs from Log converters 55A, B are then divided by Analog Divider 57 to produce a voltage based on the ratio of the outputs of amplifiers 23A, B. This voltage is indicative of the fluid quality.
  • Analog divider 57 may be an analog divider/Multiplier such as the Burr-Brown MPYIOOAG. This establishes the ratio of the determined Logs according to the formula:
  • a central processing unit may be appropriately connected to the outputs of amplifiers 23A, B to calculate, according to preprogrammed instructions, the ratio of voltages and produce a voltage or digital signal indicative of the ratio.
  • a voltage representative of the ratio is produced, when the ratio and consequently voltage moves outside of preselected values, control signals are generated.
  • the determination that the ratio is outside the preselected values is done by a comparator stage generally labeled 56.
  • Comparator 56 may be a dual OPAMP or part of as standard Quad OP AMP configured to operate in a window.
  • the determination that the ratio is outside of the preselected values and the generation of control signals may be done by the central processing unit in response to preprogrammed instructions.
  • control signals in turn activate signaling means 60 for alerting the operator that the fluid has moved outside the range of acceptable operating parameters.
  • signaling means 60 include, in the preferred embodiment (Fig. 4), LED's 62, activated through a multiplexer 64 connected to comparator 56, which visually indicate that the fluid is outside the acceptable operating parameters.
  • an audio alarm, or additional visual alarm means such as flashing lights, as well as the possibility of interacting with a computerized control system may also be used.
  • bulk head 49 also includes threads 39 which allow probe 12 to be inserted into the wall of a container containing a reservoir of the fluid or vapor to be tested.
  • O-ring 38 is seated in bulk head 49 so that probe 12 will be in sealing contact with the wall of the container containing the fluid or vapor to be tested.
  • Fiber optic input cables 24, 26 from the light sources 14, 16 themselves may then be attached to the appropriate fiber optic cables of the probe 12, or the light sources 14, 16 may themselves be attached to the ends of fiber optic cables of the probe 12.
  • a power supply 66 (Fig. 4) is provided which is connected to an alternating current source 68 such as a wall socket. Power supply 66 converts alternating current to direct current for powering the electronic components of the device 10 by means well known in the art.
  • a handle may be attached to bulkhead 49 to allow for manual placement of the probe 12 directly into a fluid or vapor to be tested.
  • This embodiment of the invention will be particularly suited for testing samples of fluid in a spotcheck fashion.
  • the spectrometer 18, filter 19, log converters 55, comparator 56, analog divider 57 and signaling means 60, as well as first and second light source 14, 16 may all be contained in a single portable unit which is connected to probe 12 by first and second input and output cables 24, 26 and 25, 27, respectively.
  • power supply 66 is preferably a battery to render the device 10 more portable.
  • the power supply of the preferred embodiment may also be used in this embodiment.
  • an analyte is present in a matrix.
  • the invention detects the analyte in the minimum concentrations listed in the Tables corresponding to each example.
  • the Tables also list the corresponding percentage of the analyte to the matrix.
  • the Tables also list the preferred wavelengths of the first and second light sources for each matrix.
  • the gases or vapors are any gas or vapor including but not limited to ambient air and hydrocarbon fuel vapors.
  • the wavelengths given for the first and second light sources are the preferred wavelengths.
  • a range of wavelengths is given, it is to be understood that the range given corresponds to a preferred range of wavelengths for the first and second light sources. In either case, wavelengths other than those described may be used with the invention.
  • the optimum wavelengths for operation of the invention may vary from the wavelengths disclosed due to factors related to the condition of the analyte and the fluid or vapor to be detected. Consequently, it may be desirable to vary the wavelengths of the first and second light sources from the values disclosed to obtain optimum detection of the fluid or vapor under the particular condition of the fluid or vapor and the analyte.
  • the wavelength of the first and second light sources may be varied by filtering the light output of the light sources or by shifting the electronic parameters of the light sources. For example, varying the voltage, current or temperature of the light sources will affect the wavelength of light emitted by the light sources.
  • the gap length of gaps 34, 44 for the examples below are preferably about 1 - 20 mm for fluids and about 10 - 20 cm for gases or vapors. Once again, these values are given as the preferable values for the gap lengths. Due to the considerable variation in optical characteristics of the varied fluids, gases and vapors, optimal gap lengths are best determined by varying the gap length, preferably within the ranges given above, while the gaps 34, 44 are in place within the analyte and the device 10 is in operation.
  • Example 1 - Analyte Water Water is detected in the matrixes listed in Table 2.
  • Creams (Face, etc- 100 0.010 Beauty/ cosmetic , 1440/2000 containing emulsifiers, lipids, collagens, fragrances, surfactants, preservatives, etc.)
  • Example 2 Analyte: Protein Protein, such as amide bonds and CO-N-H, is detected in the matrixes listed in Table 3.
  • Fat Fat such as ester linkages, combinations and overtones, is detected in the matrixes listed in Table 4.
  • Example 4 - Analyte Detergent Detergent is detected in the matrixes listed in Table 5.
  • Example 5 Sugar Sugar, including sugars having OH bonds, is detected in the matrixes listed in Table 6.
  • Example 6 Analyte: Artificial Sweetener Artificial sweeteners, including saccarin, are detected in the matrixes listed in Table 7. TABLE 7
  • Example 7 - Analyte Colorants Colorants are detected in the matrixes listed in Table 8.
  • Example 8 - Analyte Organic Preservatives
  • Organic preservatives such as benzoates, parabens and ascorbic acids, are detected in the matrixes listed in Table 9.
  • Example 9 Analyte: Salt Salt is detected in the matrixes listed in Table 10.
  • Example 10 - Analyte Alcohol Alcohol, such as ethanol and methanol, is detected in the matrixes listed in Table 11.
  • Mouthwash 100 0.0100 2310/1440
  • Example 11 - Analyte Nutrients Nutrients, such as proteins and starches, are detected in the matrixes listed in Table 12.
  • Example 12 - Analyte Particulates .
  • Light scattering particulates such as Ti0 2 , are detected in the matrixes listed in Table 13.
  • Example 13 - Analyte Bacterial Growth Light scattering bacterial growths, such as E-coli, are detected in the matrixes listed in Table 14.
  • Example 14 Analyte: Adulterants
  • Adulterants such as denaturants and organic trace materials, are detected in the matrix listed in Table 15. TABLE 15
  • Aromatics such as polyaromatic hydrocarbons and benzene, are detected in the matrix listed in Table 16.
  • Example 16 - Analyte Carbon Dioxide Carbon dioxide is detected in the matrixes listed in Table 17.
  • Example 17 - Analyte CO bonds CO (carbon monoxide) is detected in the matrix listed in Table 18.
  • Example 18 - Analyte Fuel Vapors Fuel vapors, such as C-H bonds, Methylene (CH 2 ) and Methyl (CH 3 ), are detected in the matrixes listed in Table 19.
  • Example 19 - Analyte Anesthesia Gases Anesthesia gases are detected in the matrix listed in Table 20. TABLE 20
  • Dopant mixes such as PH 3 and B 2 H 6 , are detected in gases and vapors according to the parameters listed in Table 21.
  • Carbon based gases such as CO (Carbon Monoxide) and C0 2 (Carbon Dioxide), are detected in gases or vapors according to the parameters listed in Table 22.
  • Silicon precursors such as SiH 4 , SiH 2 Cl 2 and SiClH 3 , are detected in gases and vapors according to the parameters listed in Table 23. TABLE 23
  • the invention has been described primarily in relation to fluids. However, it works equally well when addressed to the analysis of vapors. When used in this context, vapors instead of fluid is present in the gap 34,44 between the fiber optic cables.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

L'invention concerne un dispositif (12) permettant de faire passer une lumière ayant des longueurs d'onde présélectionnées dans un fluide, un gaz ou une vapeur à surveiller. La lumière est détectée après son passage dans le fluide, le gaz ou la vapeur. Cette détection produit une tension électrique qui est proportionnelle en amplitude à l'intensité lumineuse détectée pour chaque longueur d'onde. Ces tensions sont comparées pour calculer un rapport qui représente l'état du fluide, du gaz ou de la vapeur qui est examiné, ou la présence d'un analyte à étudier. Lorsque le rapport est en dehors des limites présélectionnées, des signaux de commande sont émis, qui peuvent déclencher des alarmes (60) ou provoquer une autre réponse appropriée. Dans une forme d'exécution préférée de l'invention, on détecte dans les gaz ou les vapeurs, la présence de gaz contenant du carbone, tel que l'oxyde de carbone et le gaz carbonique.
PCT/US1994/003006 1991-03-28 1994-03-22 Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur WO1995026018A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US07/677,643 US5296843A (en) 1991-03-28 1991-03-28 Fluid or vapor diagnostic device
AU65891/94A AU6589194A (en) 1991-03-28 1994-03-22 Fluid, gas or vapor diagnostic device
PCT/US1994/003006 WO1995026018A1 (fr) 1991-03-28 1994-03-22 Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US07/677,643 US5296843A (en) 1991-03-28 1991-03-28 Fluid or vapor diagnostic device
PCT/US1994/003006 WO1995026018A1 (fr) 1991-03-28 1994-03-22 Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur

Publications (1)

Publication Number Publication Date
WO1995026018A1 true WO1995026018A1 (fr) 1995-09-28

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1994/003006 WO1995026018A1 (fr) 1991-03-28 1994-03-22 Dispositif d'analyse diagnostique d'un fluide, d'un gaz ou d'une vapeur

Country Status (1)

Country Link
WO (1) WO1995026018A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2195637A4 (fr) * 2007-10-11 2011-04-13 Ecolab Inc Détecteur de produit optique
WO2012049666A2 (fr) 2010-10-15 2012-04-19 Verrana, Llc Analyse de mots de données par spectroscopie
CN109415868A (zh) * 2016-07-05 2019-03-01 艺康美国股份有限公司 液体产品耗尽报警系统和方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4699509A (en) * 1984-04-21 1987-10-13 Nippon Soken, Inc. Device for measuring contamination of lubricant
US4707133A (en) * 1986-03-06 1987-11-17 The United States Of America As Represented By The Secretary Of The Army Apparatus for plasma diagnostics
US4911549A (en) * 1988-04-05 1990-03-27 Baxter International Inc. Heparin monitoring system and methodology
US4929847A (en) * 1988-05-09 1990-05-29 Cosmo Oil Co., Ltd. Rapid determination of sludge content and device therefor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4699509A (en) * 1984-04-21 1987-10-13 Nippon Soken, Inc. Device for measuring contamination of lubricant
US4707133A (en) * 1986-03-06 1987-11-17 The United States Of America As Represented By The Secretary Of The Army Apparatus for plasma diagnostics
US4911549A (en) * 1988-04-05 1990-03-27 Baxter International Inc. Heparin monitoring system and methodology
US4929847A (en) * 1988-05-09 1990-05-29 Cosmo Oil Co., Ltd. Rapid determination of sludge content and device therefor

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2195637A4 (fr) * 2007-10-11 2011-04-13 Ecolab Inc Détecteur de produit optique
AU2008309192B2 (en) * 2007-10-11 2013-06-27 Ecolab Inc. Optical product detection sensor
WO2012049666A2 (fr) 2010-10-15 2012-04-19 Verrana, Llc Analyse de mots de données par spectroscopie
US8517274B2 (en) 2010-10-15 2013-08-27 Verrana Llc Data word analysis by spectroscopy
CN109415868A (zh) * 2016-07-05 2019-03-01 艺康美国股份有限公司 液体产品耗尽报警系统和方法
CN109415868B (zh) * 2016-07-05 2021-09-24 艺康美国股份有限公司 液体产品耗尽报警系统和方法

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