WO2010120603A2 - A high pressure and high temperature optical spectroscopy cell - Google Patents

A high pressure and high temperature optical spectroscopy cell Download PDF

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Publication number
WO2010120603A2
WO2010120603A2 PCT/US2010/030165 US2010030165W WO2010120603A2 WO 2010120603 A2 WO2010120603 A2 WO 2010120603A2 US 2010030165 W US2010030165 W US 2010030165W WO 2010120603 A2 WO2010120603 A2 WO 2010120603A2
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WO
WIPO (PCT)
Prior art keywords
light
lens
fluid
pathway
source
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PCT/US2010/030165
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French (fr)
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WO2010120603A3 (en
Inventor
Robert Schroeder
Bill Grant
Dan Angelescu
Original Assignee
Services Petroliers Schlumberger
Schlumberger Canada Limited
Schlumberger Holdings Limited
Schlumberger Technology B.V.
Prad Research And Development Limited
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Application filed by Services Petroliers Schlumberger, Schlumberger Canada Limited, Schlumberger Holdings Limited, Schlumberger Technology B.V., Prad Research And Development Limited filed Critical Services Petroliers Schlumberger
Priority to JP2012503782A priority Critical patent/JP5470447B2/en
Priority to CA2753392A priority patent/CA2753392A1/en
Priority to EP10764924A priority patent/EP2419711A4/en
Publication of WO2010120603A2 publication Critical patent/WO2010120603A2/en
Publication of WO2010120603A3 publication Critical patent/WO2010120603A3/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0291Housings; Spectrometer accessories; Spatial arrangement of elements, e.g. folded path arrangements
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0205Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • G01J3/0208Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using focussing or collimating elements, e.g. lenses or mirrors; performing aberration correction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0205Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows
    • G01J3/0218Optical elements not provided otherwise, e.g. optical manifolds, diffusers, windows using optical fibers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02Details
    • G01J3/0286Constructional arrangements for compensating for fluctuations caused by temperature, humidity or pressure, or using cooling or temperature stabilization of parts of the device; Controlling the atmosphere inside a spectrometer, e.g. vacuum
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/0303Optical path conditioning in cuvettes, e.g. windows; adapted optical elements or systems; path modifying or adjustment
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/0317High pressure cuvettes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/05Flow-through cuvettes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26Oils; Viscous liquids; Paints; Inks
    • G01N33/28Oils, i.e. hydrocarbon liquids
    • G01N33/2823Raw oil, drilling fluid or polyphasic mixtures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0346Capillary cells; Microcells
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0389Windows
    • G01N2021/0392Nonplanar windows
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/06Illumination; Optics
    • G01N2201/063Illuminating optical parts
    • G01N2201/0638Refractive parts
    • G01N2201/0639Sphere lens

Definitions

  • the subject matter disclosed in the application generally relates to devices and methods for integration of optical sensors with microfluidic systems.
  • a microfluidic cell such as a high pressure and/or high temperature microfluidic cell, that provides optical signal throughput, a collimated light path for spectroscopy and provides for minimum sized fluid dead volumes for microfluidic applications.
  • a cell designed for the optical spectroscopic measurements of fluids or gas is provided. It is noted that some embodiments of the subject matter disclosed in the application can provide for a cell that can be used from ultra violet (UV) to far infrared wavelengths, among other wavelengths. According to some embodiments, devices capable of measurements made similar to Schlumberger's DFA suite (LFA, CFA, pH). According to some embodiments, a cell is provided that is well suited for applications using very small fluid volumes, on the order of micro liters, such as micro fiuidic systems. Some embodiments are suited to larger volumes. At least some embodiments are particularly useful in very high pressure and temperature environments (for example, 20kpsi or greater at 175 degree C or greater).
  • Such conditions may be found in oilfield downhole environments. However, it is conceived that some embodiments may be used for surface and subterranean environments. It is noted that some embodiments of the subject matter disclosed in the application can be used for H2S and C 02 environments.
  • the design is simple, of very small size, by non-limiting example, less than 1 inch x 1 inch x 0.5 inch, uses inexpensive, replaceable lenses that provide the pressure barrier and collimation of the optical beam path for spectroscopic measurements.
  • some embodiments can provide for modularity in design, allowing single fiber ports on either side, or a combination of optical single fiber and/or photodiodes, light emitting diodes, small tungsten halogen lamps. Further still, some embodiments can be used as a replacement for the DFA optical cell presently in use, thereby using a small physical space even in non- microfiuidic applications.
  • a cell is provided that operates at up to 20Kpsi at 175C, with excellent optical performance over that of known similar devices.
  • a design is provided that retains up to 40kpsi of pressure and greater.
  • a metal is grown around one or more lens or windows so as to replace sealing devices such as O-rings, or the like.
  • a method of brazing may be utilized to braze Sapphire metal parts to an O-ring.
  • materials such as Sapphire and/or diamonds are used.
  • Quartz is a material used, which can result in a larger sized device due to reduced pressure strength properties.
  • the lens may be adjustable when positioned in the device.
  • the lens shape may be non-uniformly or uniformly spherical shaped, having at least one side that is non-uniformly or uniformly spherical shaped.
  • Figs Ia, Ib and Ic are schematics illustrating high pressure and/or high temperature microfluidic optical cell, according to some embodiments.
  • Fig. 2a shows a modularly designed high pressure high temperature microfluidic optical cell, according to some embodiments
  • FIG. 2b shows a simplified view of the fluid path, according to some embodiments.
  • Figs. 3a and 3b show examples of results an optical ray trace model of an arrangement according to some embodiments.
  • Fig. 4 shows a high pressure high temperature optical cell, according to some embodiments.
  • At least one optical sensor is integrated with a microfiuidic system.
  • Current systems for downhole optical spectroscopy for example with Schlumberger's MDT product line, can be performed with two large diameter (approximately 5mm) fiber bundles.
  • the fiber bundles are positioned on opposing sides of two, 7mm thick, 6mm diameter sapphire pressure windows. Each fiber bundle consists hundreds of single multimode fibers.
  • the gap between the two sapphire windows, the optical path length, is about 2mm.
  • One fiber bundle provides illumination from a tungsten halogen lamp.
  • the second fiber bundle collects light after it has transverse the multiphase fluids in the MDT flowline.
  • n.a. n m sin( ⁇ ), where ⁇ is the half angle of light emission/collection from the fiber and n m is the medium (fluid or air) that the fiber's distal end is immersed in.
  • is the half angle of light emission/collection from the fiber
  • n m is the medium (fluid or air) that the fiber's distal end is immersed in.
  • microfiuidic means a system having a flowpath having a cross section less than about 1 mm.
  • the common range for cross sectional dimensions in micro fluidic pathways is about a few 10s of microns to several 100s of microns.
  • the integration of optics into microfluidic flow systems was first developed as a pH Diver Tool for Schlumberger Water Services. See, US Patent Application Publication No. 2006/0008382, which is incorporated herein by reference.
  • the pH Diver was a complete Lab-on-Chip tool for low temperature and pressure service (less than 5OC and a lOOOpsi of pressure).
  • the pH chip had an optical cell channel that measured 10 mm long by 130 micron square.
  • Single optical fibers where integrated into the plastic (COC) chip of approximately the same dimension (125 micron diameter fiber).
  • the fibers where glued into a COC pocket and behind a transparent COC window that kept fluids out of contact with the fiber surface.
  • optical fibers can epoxied within a metal (e.g. stainless steel) tube and the tube sealed with HIP pressure fittings into either end of a microfluidic flow system.
  • the shear strength of the epoxy provides the pressure barrier between the fiber and the stainless steel tube.
  • problems can arise with the use of epoxy when operating at high temperatures.
  • optical fibers e.g.
  • quartz or sapphire could be mounted or sealed via metal (e.g. nickel) vapor deposition growth around the fibers directly or tube containing the fibers.
  • metal e.g. nickel
  • vapor deposition growth around the fibers directly or tube containing the fibers.
  • a lens that acts as a pressure window is provided that results in improved optical signal throughput, gives a collimated light path for spectroscopy and maintains very small fluid dead volumes for microfluidic applications.
  • a separate pressure window and lens are provided.
  • Figs. Ia, Ib and Ic are schematics illustrating high pressure and/or high temperature microfluidic optical cell, according to some embodiments.
  • high pressure and/or high temperature means above lkpsi and above 5OC, although some embodiments described herein are capable of safely operating at 20kpsi at 185C. Further, some embodiments described herein are further capable of operating at 40kpsi at 225C.
  • microfluidic optical cell 110 is made from metal (nickel, SS, etc).
  • a microfluidic pathway 112 is formed within the body of cell 110. Note that although the pathway is shown parallel to the optical measurement path, other arrangements are possible according to other embodiments.
  • Optical lenses 122 and 132 are sealed in place along the pathway 112 so as to maintain a high pressure seal in pathway 112.
  • the lenses 122 and 132 provide a collimated light path for spectroscopy though pathway 112, thereby providing improved optical signal throughput.
  • Optical fibers 120 and 130 are optically coupled to lenses 122 and 132 respectively. Fiber 120 carries light from light source 124 to lens 122, and fiber 130 carries light from lens 130 to optical detector 134. Note that although only a single fibers 120 and 130 are shown on either side of cell 110, according to other embodiments, other numbers of fibers can be used.
  • Figs. Ib and Ic show an arrangement according to some other embodiments.
  • the lens 122 is coupled directly with a light source 126, which is preferably a point source of light such as an LED.
  • lens 132 is coupled directly with a photodetector 136 such as a photodiode. Electrical signals are carried to the source 126 and from the detector 136 via wires 128 and 138 respectively.
  • separate pressure windows 116 and 118 provide high pressure sealing along pathway 112. Note that according to different embodiments, different combinations of optical fibers, direct couplings of sources and detectors, and separate pressure windows are provided using the arrangements shown in Figs. la-c.
  • Fig. 2a shows a modularly designed high pressure high temperature microfiuidic optical cell, according to some embodiments.
  • Fig. 2a shows the main cell block 210 that is made from titanium and measures about 1 inch x 0.6 inch x 0.5 inch in dimension.
  • the two 2mm sapphire ball lenses 222 and 232 are shown, along with the sealing Viton o-rings 224 and 234.
  • the lenses 222 and 232 are held in place with lens retainers 242 and 252 respectively.
  • On the right side is shown a retaining nut 240 for a small sized (mu type) fiber ferrule holding a 100 micron core fiber.
  • the left side retaining nut 250 holds a second mu fiber ferrule.
  • a photodiode 236 is mounted instead.
  • the unit 236 is an LED light source. It will be recognized that other options are also possible according to other embodiments.
  • novel methods and devices are provided that transfer light from a single optical fiber, through a high pressure and high temperature (e.g. 20kpsi at 175C) fluid or gas to a receiving single optical fiber or photodiode.
  • a high pressure and high temperature fluid or gas e.g. 20kpsi at 175C
  • some embodiments are particularly suited for small volume microfiuidic systems that require optical integration.
  • arrangements for larger volume sample systems are also provided.
  • a small planar sapphire window is used for pressure retention, behind which was placed a lens (of any material, like fused silica) for beam collimation from an optical fiber or other source, such as a light emitting diode (LED).
  • a receiving window and lens combination provide the same function on the opposing end of the cell, but instead focuses the collimated light into a fiber or photodiode.
  • Sapphire being robust to chemical attack and with a material strength of approximately 400 MPa has been found to be a good choice for the pressure windows, or the lenses, where not separate pressure window is provided.
  • other materials having similar properties as Sapphire are be used.
  • SiO 2 or fused silica windows have only a strength of 60MPa and could be used with sufficient thickness for a given application.
  • a 1 mm thick sapphire window can be sufficient to hold off 20kpsi of pressure with a safety factor of approximately 4 included. It has been found that minimizing the window diameter and still providing a seal (via an o-ring or metal sapphire brazing) will minimize the fluid dead volume.
  • FIG. 2b shows a simplified view of the fluid path, according to some embodiments.
  • the fluid takes a Z-shaped path along fluid pathway 212.
  • a predetermined optical path length may be highly desirable, the Z-path is a useful way to obtain such path lengths for microfluidic systems.
  • the standard optical cell path length is approximately 2mm.
  • the cell design directs the light path in line with the fluid flow. This is different than the current DFA design, but has been found to be of little optical significance.
  • the complication of mounting the window can be compounded by the need to also mount an additional focusing lens and the small optical fiber behind it. Given the small maximum optical beam diameter required ( ⁇ 0.6mm), the off-the- shelf availability of sapphire lenses (in particular spherical or ball designs), combining the functionality of the lens and window has been found to be advantageous. [0030] Figs.
  • 3a and 3b show examples of results an optical ray trace model of an arrangement according to some embodiments, made with commercial software (TracePro® from Lambda Research Corp.) 2 mm ball lens 322 and 332 are immersed on one side with oil or water is shown.
  • Talbot® from Lambda Research Corp.
  • 2 mm ball lens 322 and 332 are immersed on one side with oil or water is shown.
  • optical beam collimation can be achieved within pathway 312 of defined by wall 310.
  • Collimation of the interrogation light source is ideal for spectroscopic measurements. It has been found that the arrangement shown makes for a very simple robust design. According to some embodiments, other sizes and shapes of lenses are used, depending on the optical design, the anticipated pressures, and the sealing technology. For example, according to one embodiment, two lmm ball lenses are used.
  • the ball lenses 322 and 332 can be sealed with small o-rings or brazed into retaining pockets (not shown). To make the mechanical sealing easier, 2mm diameter ball lenses (cost: $12 each) are used, according to some embodiments. It has been found that with an exposed diameter of only 0.6mm, the strength of sapphire will retain up to 40kpsi of pressure.
  • Fig. 4 shows a high pressure high temperature optical cell, according to some embodiments.
  • the cell shown in Fig. 4 is designed to operate at high pressures and high temperatures of extreme environments, such as in subterranean locations.
  • the single lens/window design described herein is used in non-microfludic applications as well. While many of the embodiments described herein are particularly well suited for downhole deployment due to their small size, robust design and HPHT capabilities, many of the embodiments are also suitable for analysis on the surface where HPHT cells are used, such as measurement of dew point, bubble point, spectroscopy and other optical measurements. Additionally some of the non-micro fluidic embodiments are well suited to multiphase flow analysis as well.
  • Two ball lenses 422 and 432 approximately 6 mm diameter each, and a single fiber on either end is used instead of a pressure window and large bundles of fibers as in conventional cells.
  • the ball lenses 422 and 432 are sealed onto the flow line 412 within body 410 using o-rings 424 and 434 respectively.
  • the flow line 412 is approximately 2mm in diameter and the flow is transverse to the optical path as shown.
  • the lenses 422 and 432 are held in place using lens retainers 442 and 452 respectively. Fiber ferrules are held on either side of the cell with retainers 440 and 450. Note that according to some embodiments, two or more fibers are used.
  • the lens is mounted on the flowline of a tool such as Schlumberger's MDT tool line, like a ball filling the holes of a flute.
  • a tool such as Schlumberger's MDT tool line
  • Advantages of embodiments such as shown in Fig. 4 include the small size of the parts and mounting hardware, and the smaller bend radius of the single fiber vs. the stiffer fiber bundle. Additionally, with the use of collimating lenses 422 and 432, all the light from the single fiber is imaged through the flow line, whereas in conventional arrangements without lenses not all fibers 'see' the same flow regime per unit of time measurement.
  • the arrangements described herein a may be used in accordance with the '908 patent application, which describes methods for fabricating devices having embedded features such as optical devices. It is noted that some embodiments may include one or more topographical patterns of a base substrate, along with other devices such as: an optical element, an optical device, a portion of a channel, an enclosed channel, an optical feedthrough, an electrical feedthrough, a sensor device, a wire shaped device or some combination thereof. [0035] According to some embodiments, the arrangements described herein may be used in accordance with U.S. Patent Application Publication US 2006/0008382 to Salamitou et al, incorporated by reference herein in its entirety, which discloses the use of self-supporting micro fluidic systems for chemical analysis of water or mixtures of water and oil.
  • a small ball lens is used that holds off enough pressure for a microfluidic device, wherein a material such as nickel is grown around the lens.
  • This material growing technique on the lens or window has been found to be effective in reducing the fluid dead volume in some embodiments.
  • the microchannel having a cross section of about 140 microns is exposed to pressures of up to 20kpsi.
  • the thickness sapphire is about 80 micron, and if fused silica is used instead of sapphire the thickness is about 200 microns. It is noted these dimensions include a safety margin of approximately 4.
  • a 300 micron ball lens has been found to be adequate to provide an adequate pressure barrier up to at least 20Kpsi and some degree of collimation of light to improve throughput.
  • the strength S of materials used is 60MPa for fused silica and 400MPa for sapphire.
  • the following formula can be used:
  • d/L 0.5 sqrt ⁇ k * f * P/S ⁇
  • f 4 is the safety factor
  • P is pressure in MPa
  • k varies between 0.75 and 1.125 depending on whether the window is secured on one or both sides to pressure
  • d/L is the ratio of window thickness/exposed window diameter

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Abstract

Devices, methods and systems for making optical measurements of a fluid at elevated pressures and temperatures are disclosed. A cell is designed for the optical spectroscopic measurements of fluids or gas using light from ultra violet (UV) to far infrared wavelengths, among other wavelengths. A cell is described that is well suited for applications using very small fluid volumes, on the order of micro liters, such as microfluidic systems. Some described embodiments are suited for very high pressure and temperature environments (for example, 20kpsi or greater at 175 degree C or greater). Such conditions, for example, may be found in oilfield downhole environments. Some embodiments provide are inexpensive, and make use of replaceable lenses that are used as a pressure barrier and for collimation of the optical beam path for spectroscopic measurements.

Description

A HIGH PRESSURE AND HIGH TEMPERATURE OPTICAL SPECTROSCOPY
CELL
CROSS REFERENCE TO RELATED APPLICATION
[0001] This patent application claims benefit of United States Provisional Patent Application Serial Number 61/170,488, filed April 17, 2009 which is incorporated by reference herein.
BACKGROUND
1. Field of the Subject Matter Disclosed
[0002] The subject matter disclosed in the application generally relates to devices and methods for integration of optical sensors with microfluidic systems. In particular, the integration of one or more fiber as a feed through into a microfluidic cell such as a high pressure and/or high temperature microfluidic cell, that provides optical signal throughput, a collimated light path for spectroscopy and provides for minimum sized fluid dead volumes for microfluidic applications.
2. Background of the Subject Matter Disclosed
[0003] Often in many applications there is a need for transmitting optical signal from one side of a metallic part to the other, for example, measuring fluid and gas analysis. Often, such transmission needs to occur while there is a significant pressure difference between the two sides of the metallic part. Several solutions exist to this problem, including but not limited to the use of optical windows sealed with elastomeric o-rings or brazed to the metallic part.
[0004] In many applications there is also a need for a metallic part with very intricate details machined in it, such as small channels and holes, at length scales and resolutions down to the micron level, which are not easily achievable using conventional machining techniques. One example of a situation where such a need exists is in the manufacturing of metallic microfluidic devices.
[0005] Accordingly, there is a need for improved methods and systems capable of providing devices worthy of use in demanding environments so as to withstand, by non-limiting example, high pressures, high temperatures and harsh environments. There is also the need for versatile fabrication methods for integrating optical sensors with micro fiuidic systems capable of manufacturing and/or processing of parts having characteristics, such as: high structural strength and excellent chemical resistance.
SUMMARY OF THE SUBJECT MATTER DISCLOSED
[0006] According to some embodiments, a cell designed for the optical spectroscopic measurements of fluids or gas is provided. It is noted that some embodiments of the subject matter disclosed in the application can provide for a cell that can be used from ultra violet (UV) to far infrared wavelengths, among other wavelengths. According to some embodiments, devices capable of measurements made similar to Schlumberger's DFA suite (LFA, CFA, pH). According to some embodiments, a cell is provided that is well suited for applications using very small fluid volumes, on the order of micro liters, such as micro fiuidic systems. Some embodiments are suited to larger volumes. At least some embodiments are particularly useful in very high pressure and temperature environments (for example, 20kpsi or greater at 175 degree C or greater). Such conditions, for example, may be found in oilfield downhole environments. However, it is conceived that some embodiments may be used for surface and subterranean environments. It is noted that some embodiments of the subject matter disclosed in the application can be used for H2S and C 02 environments.
[0007] According to some embodiments, the design is simple, of very small size, by non-limiting example, less than 1 inch x 1 inch x 0.5 inch, uses inexpensive, replaceable lenses that provide the pressure barrier and collimation of the optical beam path for spectroscopic measurements. Further, some embodiments can provide for modularity in design, allowing single fiber ports on either side, or a combination of optical single fiber and/or photodiodes, light emitting diodes, small tungsten halogen lamps. Further still, some embodiments can be used as a replacement for the DFA optical cell presently in use, thereby using a small physical space even in non- microfiuidic applications. According to some embodiments, a cell is provided that operates at up to 20Kpsi at 175C, with excellent optical performance over that of known similar devices. According to at least one embodiment, a design is provided that retains up to 40kpsi of pressure and greater. [0008] According to at least one embodiment, a metal is grown around one or more lens or windows so as to replace sealing devices such as O-rings, or the like. According to some embodiments a method of brazing may be utilized to braze Sapphire metal parts to an O-ring. According to some embodiments, materials such as Sapphire and/or diamonds are used. According to some embodiments, Quartz is a material used, which can result in a larger sized device due to reduced pressure strength properties.
[0009] According to some embodiments, the lens may be adjustable when positioned in the device. Further, the lens shape may be non-uniformly or uniformly spherical shaped, having at least one side that is non-uniformly or uniformly spherical shaped.
[0010] Further features and advantages of the subject matter disclosed in the application will become more readily apparent from the following detailed description when taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The subject matter disclosed in the application is further described in the detailed description which follows, in reference to the noted plurality of drawings by way of non- limiting examples of exemplary embodiments of the subject matter disclosed in the application, in which like reference numerals represent similar parts throughout the several views of the drawings, and wherein:
[0012] Figs Ia, Ib and Ic are schematics illustrating high pressure and/or high temperature microfluidic optical cell, according to some embodiments;
[0013] Fig. 2a shows a modularly designed high pressure high temperature microfluidic optical cell, according to some embodiments;
[0014] Fig. 2b shows a simplified view of the fluid path, according to some embodiments;
[0015] Figs. 3a and 3b show examples of results an optical ray trace model of an arrangement according to some embodiments; and
[0016] Fig. 4 shows a high pressure high temperature optical cell, according to some embodiments. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] The particulars shown herein are by way of example and for purposes of illustrative discussion of the embodiments of the subject matter disclosed in the application only and are presented in the cause of providing what is believed to be the most useful and readily understood description of the principles and conceptual aspects of the subject matter disclosed in the application. In this regard, no attempt is made to show structural details of the subject matter disclosed in the application in more detail than is necessary for the fundamental understanding of the subject matter disclosed in the application, the description taken with the drawings making apparent to those skilled in the art how the several forms of the subject matter disclosed in the application may be embodied in practice. Further, like reference numbers and designations in the various drawings indicated like elements.
[0018] According to some embodiments, at least one optical sensor is integrated with a microfiuidic system. Current systems for downhole optical spectroscopy, for example with Schlumberger's MDT product line, can be performed with two large diameter (approximately 5mm) fiber bundles. In the case of the MDT product line, the fiber bundles are positioned on opposing sides of two, 7mm thick, 6mm diameter sapphire pressure windows. Each fiber bundle consists hundreds of single multimode fibers. The gap between the two sapphire windows, the optical path length, is about 2mm. One fiber bundle provides illumination from a tungsten halogen lamp. The second fiber bundle collects light after it has transverse the multiphase fluids in the MDT flowline. Note that in current system, the light path from the fibers is commonly transverse to the flow direction. Each individual fiber in the fiber bundle expands or collects light within it numerical aperture (n.a.). Numerical aperture is defined as n.a. = nm sin(θ), where θ is the half angle of light emission/collection from the fiber and nm is the medium (fluid or air) that the fiber's distal end is immersed in. [0019] Currently available systems, such as with Schlumberger's MDT product line, typically use relatively large flow volumes and cross sections. Cross sections are measured in millimeters. In contrast, in microfluidics applications, the flow volumes are measured in micro liters and cross sections of microfiuidic flow systems are 10 to several hundreds of microns. As used herein the term "microfiuidic" means a system having a flowpath having a cross section less than about 1 mm. The common range for cross sectional dimensions in micro fluidic pathways is about a few 10s of microns to several 100s of microns.
[0020] The integration of optics into microfluidic flow systems was first developed as a pH Diver Tool for Schlumberger Water Services. See, US Patent Application Publication No. 2006/0008382, which is incorporated herein by reference. The pH Diver was a complete Lab-on-Chip tool for low temperature and pressure service (less than 5OC and a lOOOpsi of pressure). The pH chip had an optical cell channel that measured 10 mm long by 130 micron square. Single optical fibers where integrated into the plastic (COC) chip of approximately the same dimension (125 micron diameter fiber). The fibers where glued into a COC pocket and behind a transparent COC window that kept fluids out of contact with the fiber surface. Since no focusing optics were integrated with the pH chip, light expanded within the n.a. of the single fiber before reaching the collection fiber 10 mm away. This simple, low cost designed works very well for the intended applications, but the light loss was approximately 18dB or a factor of 60 due to the lack of light collimation. [0021] Optical fibers can epoxied within a metal (e.g. stainless steel) tube and the tube sealed with HIP pressure fittings into either end of a microfluidic flow system. The shear strength of the epoxy provides the pressure barrier between the fiber and the stainless steel tube. However, problems can arise with the use of epoxy when operating at high temperatures. According to some embodiments, optical fibers (e.g. quartz or sapphire) could be mounted or sealed via metal (e.g. nickel) vapor deposition growth around the fibers directly or tube containing the fibers. For further details on such growth techniques, see Angelescu and Schroeder, 'Fabrication Technique for Metallic Devices with Embedded Optical Elements, Optical devices, or Optical and Electrical Feedthroughs', 12/191,908, filed on August 14, 2008, hereinafter referred to as the '"908 patent application", which is hereby incorporated by reference herein. In systems within out a lens or a pressure window, the HPHT fluid contact with the epoxy or the fibers themselves can be a failure point. Also, in systems without lenses, even though the light emitted by the fibers will reflect off of the metal walls inside the fluidic device (unlike the pH transparent COC chip), there is no real optical gain from that process, due to the large reflection losses in the metal. Thus, according to some embodiments, a lens that acts as a pressure window is provided that results in improved optical signal throughput, gives a collimated light path for spectroscopy and maintains very small fluid dead volumes for microfluidic applications. According to some other embodiments a separate pressure window and lens are provided.
[0022] Figs. Ia, Ib and Ic are schematics illustrating high pressure and/or high temperature microfluidic optical cell, according to some embodiments. As used herein the term high pressure and/or high temperature (HPHT) means above lkpsi and above 5OC, although some embodiments described herein are capable of safely operating at 20kpsi at 185C. Further, some embodiments described herein are further capable of operating at 40kpsi at 225C. In Fig. Ia, microfluidic optical cell 110 is made from metal (nickel, SS, etc). A microfluidic pathway 112 is formed within the body of cell 110. Note that although the pathway is shown parallel to the optical measurement path, other arrangements are possible according to other embodiments. Also, although liquids such as oilfield liquids may be discussed in connection with various embodiments, the pathway 112 and similar pathways described herein can be used to carry and optically analyze gases as well. Optical lenses 122 and 132 are sealed in place along the pathway 112 so as to maintain a high pressure seal in pathway 112. The lenses 122 and 132 provide a collimated light path for spectroscopy though pathway 112, thereby providing improved optical signal throughput. Optical fibers 120 and 130 are optically coupled to lenses 122 and 132 respectively. Fiber 120 carries light from light source 124 to lens 122, and fiber 130 carries light from lens 130 to optical detector 134. Note that although only a single fibers 120 and 130 are shown on either side of cell 110, according to other embodiments, other numbers of fibers can be used.
[0023] Figs. Ib and Ic show an arrangement according to some other embodiments. In Fig. Ib, the lens 122 is coupled directly with a light source 126, which is preferably a point source of light such as an LED. Likewise, lens 132 is coupled directly with a photodetector 136 such as a photodiode. Electrical signals are carried to the source 126 and from the detector 136 via wires 128 and 138 respectively. In Fig. Ic, separate pressure windows 116 and 118 provide high pressure sealing along pathway 112. Note that according to different embodiments, different combinations of optical fibers, direct couplings of sources and detectors, and separate pressure windows are provided using the arrangements shown in Figs. la-c. Note that with the use of collimating lenses, the light sources used are preferably point light sources such as LEDs. As used herein the term "point source" of light refers to a light source whose light emitting portion has a physical extent on the order of 10s to 100s of microns, and when placed at the focal point of a lens, tends to produce collimated light essentially parallel to the optical axis of the lens system. [0024] Fig. 2a shows a modularly designed high pressure high temperature microfiuidic optical cell, according to some embodiments. In particular, Fig. 2a shows the main cell block 210 that is made from titanium and measures about 1 inch x 0.6 inch x 0.5 inch in dimension. The two 2mm sapphire ball lenses 222 and 232 are shown, along with the sealing Viton o-rings 224 and 234. The lenses 222 and 232 are held in place with lens retainers 242 and 252 respectively. On the right side is shown a retaining nut 240 for a small sized (mu type) fiber ferrule holding a 100 micron core fiber. The left side retaining nut 250, according to some embodiments, holds a second mu fiber ferrule. However, in the embodiment shown in Fig. 2a, a photodiode 236 is mounted instead. According to some other embodiments, the unit 236 is an LED light source. It will be recognized that other options are also possible according to other embodiments.
[0025] It has been found that, arrangements such as shown in Fig. 2a are able to operate at pressures of up to 20kpsi at 175C with no fluid leaks. It has also been found that the optical spectrum of such arrangements compare well with a baseline laboratory spectrometer. Other metrological tests have been performed indicating that embodiments of the subject matter disclosed in the application are able to handle even higher pressures than 20 kpsi and at higher temperatures than 175 C without fluid leaks.
[0026] According to some embodiments, novel methods and devices are provided that transfer light from a single optical fiber, through a high pressure and high temperature (e.g. 20kpsi at 175C) fluid or gas to a receiving single optical fiber or photodiode. Among other things, some embodiments are particularly suited for small volume microfiuidic systems that require optical integration. However, according to some embodiments, arrangements for larger volume sample systems are also provided.
[0027] Because microfiuidic environments involve very small cross sectional channels, the combination of the material strength of sapphire, among other materials, and the small exposed area allows for very thin pressure windows. According to some embodiment such as shown in Fig. Ic, a small planar sapphire window is used for pressure retention, behind which was placed a lens (of any material, like fused silica) for beam collimation from an optical fiber or other source, such as a light emitting diode (LED). A receiving window and lens combination provide the same function on the opposing end of the cell, but instead focuses the collimated light into a fiber or photodiode.
[0028] Sapphire, being robust to chemical attack and with a material strength of approximately 400 MPa has been found to be a good choice for the pressure windows, or the lenses, where not separate pressure window is provided. However, according to other embodiments, other materials having similar properties as Sapphire are be used. For example, SiO2 or fused silica windows have only a strength of 60MPa and could be used with sufficient thickness for a given application. In a planar window design, with only 600 microns diameter channel, a 1 mm thick sapphire window can be sufficient to hold off 20kpsi of pressure with a safety factor of approximately 4 included. It has been found that minimizing the window diameter and still providing a seal (via an o-ring or metal sapphire brazing) will minimize the fluid dead volume. A larger diameter window is easy to seal, but will give larger dead volumes between the window and the o-ring. Further, by integrating the window and the lens in to a single part, it has been found that the fluid dead volumes can be reduced. Smaller fluid dead volumes are preferred for many microfluidic measurements. Fig. 2b shows a simplified view of the fluid path, according to some embodiments. The fluid takes a Z-shaped path along fluid pathway 212. To conform to measurement standard for existing tool systems, a predetermined optical path length may be highly desirable, the Z-path is a useful way to obtain such path lengths for microfluidic systems. For example, for Schlumberger's MDT tools using DFA, the standard optical cell path length is approximately 2mm. To achieve this with a 600 micron diameter fluid path, the cell design directs the light path in line with the fluid flow. This is different than the current DFA design, but has been found to be of little optical significance. [0029] The complication of mounting the window can be compounded by the need to also mount an additional focusing lens and the small optical fiber behind it. Given the small maximum optical beam diameter required (< 0.6mm), the off-the- shelf availability of sapphire lenses (in particular spherical or ball designs), combining the functionality of the lens and window has been found to be advantageous. [0030] Figs. 3a and 3b show examples of results an optical ray trace model of an arrangement according to some embodiments, made with commercial software (TracePro® from Lambda Research Corp.) 2 mm ball lens 322 and 332 are immersed on one side with oil or water is shown. By adjustment of the locations of the emitting source 336 and the receiving fiber 326 to compensate for fluid immersion of the two ball lenses 322 and 332, optical beam collimation can be achieved within pathway 312 of defined by wall 310. Collimation of the interrogation light source is ideal for spectroscopic measurements. It has been found that the arrangement shown makes for a very simple robust design. According to some embodiments, other sizes and shapes of lenses are used, depending on the optical design, the anticipated pressures, and the sealing technology. For example, according to one embodiment, two lmm ball lenses are used.
[0031] The ball lenses 322 and 332 can be sealed with small o-rings or brazed into retaining pockets (not shown). To make the mechanical sealing easier, 2mm diameter ball lenses (cost: $12 each) are used, according to some embodiments. It has been found that with an exposed diameter of only 0.6mm, the strength of sapphire will retain up to 40kpsi of pressure.
[0032] Fig. 4 shows a high pressure high temperature optical cell, according to some embodiments. The cell shown in Fig. 4 is designed to operate at high pressures and high temperatures of extreme environments, such as in subterranean locations. According to some embodiments, the single lens/window design described herein is used in non-microfludic applications as well. While many of the embodiments described herein are particularly well suited for downhole deployment due to their small size, robust design and HPHT capabilities, many of the embodiments are also suitable for analysis on the surface where HPHT cells are used, such as measurement of dew point, bubble point, spectroscopy and other optical measurements. Additionally some of the non-micro fluidic embodiments are well suited to multiphase flow analysis as well. Two ball lenses 422 and 432, approximately 6 mm diameter each, and a single fiber on either end is used instead of a pressure window and large bundles of fibers as in conventional cells. The ball lenses 422 and 432 are sealed onto the flow line 412 within body 410 using o-rings 424 and 434 respectively. The flow line 412 is approximately 2mm in diameter and the flow is transverse to the optical path as shown. The lenses 422 and 432 are held in place using lens retainers 442 and 452 respectively. Fiber ferrules are held on either side of the cell with retainers 440 and 450. Note that according to some embodiments, two or more fibers are used. Further, according to some embodiments of the subject matter disclosed in the application, the lens is mounted on the flowline of a tool such as Schlumberger's MDT tool line, like a ball filling the holes of a flute. [0033] Advantages of embodiments such as shown in Fig. 4 include the small size of the parts and mounting hardware, and the smaller bend radius of the single fiber vs. the stiffer fiber bundle. Additionally, with the use of collimating lenses 422 and 432, all the light from the single fiber is imaged through the flow line, whereas in conventional arrangements without lenses not all fibers 'see' the same flow regime per unit of time measurement.
[0034] According to some embodiments, the arrangements described herein a may be used in accordance with the '908 patent application, which describes methods for fabricating devices having embedded features such as optical devices. It is noted that some embodiments may include one or more topographical patterns of a base substrate, along with other devices such as: an optical element, an optical device, a portion of a channel, an enclosed channel, an optical feedthrough, an electrical feedthrough, a sensor device, a wire shaped device or some combination thereof. [0035] According to some embodiments, the arrangements described herein may be used in accordance with U.S. Patent Application Publication US 2006/0008382 to Salamitou et al, incorporated by reference herein in its entirety, which discloses the use of self-supporting micro fluidic systems for chemical analysis of water or mixtures of water and oil.
[0036] According to some embodiments, a small ball lens is used that holds off enough pressure for a microfluidic device, wherein a material such as nickel is grown around the lens. This material growing technique on the lens or window has been found to be effective in reducing the fluid dead volume in some embodiments. According to some embodiments, the microchannel having a cross section of about 140 microns is exposed to pressures of up to 20kpsi. The thickness sapphire is about 80 micron, and if fused silica is used instead of sapphire the thickness is about 200 microns. It is noted these dimensions include a safety margin of approximately 4. According to some embodiments a 300 micron ball lens has been found to be adequate to provide an adequate pressure barrier up to at least 20Kpsi and some degree of collimation of light to improve throughput.
[0037] The strength S of materials used is 60MPa for fused silica and 400MPa for sapphire. The following formula can be used:
d/L = 0.5 sqrt{ k * f * P/S} where f = 4 is the safety factor, P is pressure in MPa, k varies between 0.75 and 1.125 depending on whether the window is secured on one or both sides to pressure, and d/L is the ratio of window thickness/exposed window diameter, (see data and formula from: Infrared Window and Dome Materials, Daniel C. Harris, Tutorial Texts in Optical Engineering, Vol. TTlO, SPIE Optical Engineering Press, 1992, which is incorporated by reference herein.)
[0038] Although the techniques described herein can be used for optical measurements in multiphase flow, it has been found that many of the microfiuidic embodiments are particularly well suited for optical measurements for single phases. [0039] Several embodiments of the subject matter disclosed in the application have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the subject matter disclosed in the application. For example, embodiments of the subject matter disclosed in the application as disclosed above have many further applications in both surface and subterranean environments, such as reducing the size of spectroscopic measurements and/or being a part of new optical measurements under HPHT conditions. It is noted that the foregoing examples have been provided merely for the purpose of explanation and are in no way to be construed as limiting of the subject matter disclosed in the application. While the subject matter disclosed in the application has been described with reference to an exemplary embodiment, it is understood that the words, which have been used herein, are words of description and illustration, rather than words of limitation. Changes may be made, within the purview of the appended claims, as presently stated and as amended, without departing from the scope and spirit of the subject matter disclosed in the application in its aspects. Although the subject matter disclosed in the application has been described herein with reference to particular means, materials and embodiments, the subject matter disclosed in the application is not intended to be limited to the particulars disclosed herein; rather, the subject matter disclosed in the application extends to all functionally equivalent structures, methods and uses, such as are within the scope of the appended claims.

Claims

What is claimed is:
1. A device for making optical measurements of a fluid at elevated pressures and temperatures, the device comprising: a fluid pathway; a source of light; a light detector; a first lens in optical in communication with the source of light, the first lens positioned and dimensioned to as to direct light from the source through the fluid pathway; and a second lens in optical communication with a light detector, the second lens positioned and dimensioned to so as to direct light from the source in the fluid pathway towards the light detector.
2. The device according to claim 1, wherein the pathway is a micro fluidic pathway.
3. The device according to claim 1, further comprising a first pressure window and a second pressure window having each a surface exposed to fluid in the pathway, and each sealed to an opening in the fluid pathway.
4. The device according to claim 3, wherein the first and second pressure windows are made from a material selected from the group consisting of: sapphire, diamond or quartz.
5. The device according to claim 3, wherein the first pressure window and the first lens form a single piece of material, and the second pressure window and the second lens form a single piece of material.
6. The device according to claim 5, wherein the first and second lenses are made from sapphire.
7. The device according to claim 3, wherein the first and second pressure windows are sealed using one or more techniques selected from the group consisting of o-rings, brazing, or a material grown on a window surface.
8. The device according to claim 2, wherein the light from the first lens toward the second lens travels in a direction approximately parallel to the fluid flowing in the fluid pathway.
9. The device according to claim 1, wherein the first and second lenses are one of uniformly, non-uniformly or some combination thereof spherical shaped.
10. The device according to claim 1, wherein the source of light is a point source of light.
11. The device according to claim 10, wherein the light emitting area of the point source of light has a largest physical dimension of less than 500 microns.
12. The device according to claim 1, further comprising a first optical fiber adapted and positioned so as to transmit light from the source of light to the first lens.
13. The device according to claim 12, wherein predominantly all of the light that the first lens receives from the source of light is transmitted through the first optical fiber.
14. The device according to claim 1, further comprising a second optical fiber adapted and positioned so as to transmit light from the second lens to the light detector.
15. The device according to claim 14, wherein predominantly all of the light that the light detector receives from the second lens is transmitted through the second optical fiber.
16. The device according to claim 1, wherein the light source is either a light emitting diode or a tungsten halogen lamp.
17. The device according to claim 16, wherein the light source is a light emitting diode and is positioned so as to directly emit light into the first lens.
18. The device according to claim 1, wherein the light detector is a photodiode.
19. The device according to claim 18, wherein the photodiode is positioned proximately to the second lens so as to receive light directly from the second lens.
20. The device according to claim 1, wherein the first lens dimensioned, shaped and positioned such that the light directed through the fluid pathway is predominantly travels parallel to a main axis of the first lens.
21. The device according to claim 1, wherein the device is designed so as to operate at pressures within the pathway of at least 5kpsi.
22. The device according to claim 21, wherein the device is designed so as to operate at pressures within the pathway of at least lOkpsi.
23. The device according to claim 22, wherein the device is designed so as to operate at pressures within the pathway of at least 20kpsi.
24. The device according to claim 1, wherein the device is designed so as to operate at temperatures of at least 5OC.
25. The device according to claim 24, wherein the device is designed so as to operate at temperatures of at least 175 C.
26. The device according to claim 1, wherein the light from the first lens toward the second lens travels in a direction approximately orthogonal to fluid flowing in the fluid pathway.
27. The device according to claim 1, wherein light emitted from the source and detected by the detector includes wavelengths predominantly with a range including ultraviolet and far infrared wavelengths.
28. The device according to claim 1, wherein the device is adapted to be deployed downhole in a borehole.
29. The device according to claim 1, wherein the optical measurements are spectroscopic measurements.
30. A method for making optical measurements of a fluid at elevated pressures and temperatures, the method comprising: flowing a fluid in a fluid pathway; generating light from a source of light; directing light from the source with a first lens through the fluid pathway; directing light from the fluid pathway with a second lens towards a light detector; and detecting light so to make optical measurements of the fluid.
31. The method according to claim 30, wherein the pathway is a microfiuidic pathway.
32. The method according to claim 30, wherein the pathway includes first and second pressure windows having each a surface exposed to fluid in the pathway, and each sealed to an opening in the fluid pathway.
33. The method according to claim 32, wherein the first pressure window and the first lens form a single piece of material, and the second pressure window and the second lens form a single piece of material.
34. The method according to claim 33, wherein the first and second lenses are made from sapphire.
35. The method according to claim 32, wherein the first and second pressure windows are sealed using one or more techniques selected from the group consisting of o-rings, brazing, or a material grown on a window surface.
36. The method according to claim 31 , wherein the light from the first lens toward the second lens travels in a direction approximately parallel to fluid flowing in the fluid pathway.
37. The method according to claim 30, wherein the first and second lenses are one of uniformly, non-uniformly or some combination thereof spherical shaped.
38. The method according to claim 30, wherein the source of light is a point source of light having a light emitting area with a largest physical dimension of less than 500 microns.
39. The method according to claim 30, further comprising a first optical fiber adapted and positioned so as to transmit light from the source of light to the first lens.
40. The method according to claim 39, wherein predominantly all of the light that the first lens receives from the source of light is transmitted through the first optical fiber.
41. The method according to claim 30, further comprising a second optical fiber adapted and positioned so as to transmit light from the second lens to the light detector.
42. The method according to claim 41, wherein predominantly all of the light that the light detector receives from the second lens is transmitted through the second optical fiber.
43. The method according to claim 30, wherein the light source is either a light emitting diode or a tungsten halogen lamp.
44. The method according to claim 43, wherein the light source is a light emitting diode and is positioned so as to directly emit light into the first lens.
45. The method according to claim 30, wherein the light detector is a photodiode.
46. The method according to claim 45, wherein the photodiode is positioned proximately to the second lens so as to receive light directly from the second lens.
47. The method according to claim 30, wherein the first lens dimensioned, shaped and positioned such that the light directed through the fluid pathway is predominantly travels parallel to a main axis of the first lens.
48. The method according to claim 30, wherein the fluid pathway is designed to maintain pressures of at least 5kpsi.
49. The method according to claim 48, wherein the fluid pathway is designed to maintain pressures of at least lOkpsi.
50. The method according to claim 49, wherein the fluid pathway is designed to maintain pressures of at least 20kpsi.
51. The method according to claim 30, wherein measurements are made while the fluid temperature is at least 5OC.
52. The method according to claim 51 , wherein measurements are made while the fluid temperature is at least 175 C.
53. The method according to claim 30, wherein the light from the first lens toward the second lens travels in a direction approximately orthogonal to fluid flowing in the fluid pathway.
54. The method according to claim 30, wherein the generated light and the detected light includes wavelengths predominantly with a range including ultraviolet and far infrared wavelengths.
55. The method according to claim 30, further comprising deploying the fluid pathway, the source, the detector and the first and second lenses downhole and wherein the optical fluid measurements are made downhole.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2479555B1 (en) * 2010-12-21 2013-03-13 Sick Ag Optical analyser with a holder for installation in a gas-bearing cavity

Families Citing this family (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2011294831B2 (en) 2010-08-26 2014-10-02 Schlumberger Technology B.V. Apparatus and method for phase equilibrium with in-situ sensing
AT510765B1 (en) * 2010-12-15 2012-09-15 Wolfgang Dipl Ing Vogl DEVICE FOR PHOTOMETRIC OR BZW. SPECTROMETRIC STUDY OF A LIQUID SAMPLE
EP2508869B1 (en) * 2011-04-05 2015-10-14 Sick Ag Concentration measurement device, concentration measurement assembly and concentration measurement method
US9249661B2 (en) 2012-01-20 2016-02-02 Schlumberger Technology Corporation Apparatus and methods for determining commingling compatibility of fluids from different formation zones
US8910514B2 (en) * 2012-02-24 2014-12-16 Schlumberger Technology Corporation Systems and methods of determining fluid properties
US20150022807A1 (en) * 2012-03-12 2015-01-22 Ecole Polytechnique Federale De Lausanne (Epfl) Universal sample holder
US9816915B2 (en) 2013-10-11 2017-11-14 Fireye, Inc. Couplings for flame observation devices
DE102013018080B3 (en) * 2013-11-27 2015-02-12 Festo Ag & Co. Kg Analysis device for performing spectrometric analyzes
AU2015286862B2 (en) * 2014-07-07 2018-01-04 Shell Internationale Research Maatschappij B.V. Interconnecting optical fibers at a hydrocarbon fluid production facility
KR102235612B1 (en) 2015-01-29 2021-04-02 삼성전자주식회사 Semiconductor device having work-function metal and method of forming the same
US10215604B2 (en) 2015-11-20 2019-02-26 Schlumberger Technology Corporation Fluid analysis system with densitometer having electrically isolated vibrating tube
US10132164B2 (en) 2015-12-18 2018-11-20 Schlumberger Technology Corporation Systems and methods for in-situ measurements of mixed formation fluids
US10344592B2 (en) 2015-12-21 2019-07-09 Schlumberger Technology Corporation Flushing microfluidic sensor systems
US10208591B2 (en) 2015-12-21 2019-02-19 Schlumberger Technology Corporation Flushing microfluidic sensor systems
US11105198B2 (en) 2016-03-31 2021-08-31 Schlumberger Technology Corporation Methods for in-situ multi-temperature measurements using downhole acquisition tool
US10684152B2 (en) 2016-04-20 2020-06-16 Schlumberger Technology Corporation Fluid analysis with Coriolis effect flowmeter
JP6551609B2 (en) 2016-08-25 2019-07-31 株式会社島津製作所 Flow cell
CA3054803A1 (en) * 2017-02-28 2018-09-07 MarqMetrix Inc. Fluid flow cell including a spherical lens
WO2019084766A1 (en) * 2017-10-31 2019-05-09 深圳大学 Hybrid optical fiber coupler and preparation method thereof
AR114207A1 (en) 2018-01-15 2020-08-05 Baker Hughes A Ge Co Llc USE OF MICROFLUIDS AS A RAPID EVALUATION TECHNOLOGY FOR ENHANCED OIL RECOVERY
CN109030373A (en) * 2018-08-31 2018-12-18 四川永祥新能源有限公司 A kind of liquid sampling analysis cell
WO2020154601A1 (en) * 2019-01-24 2020-07-30 Nirrin Technologies, Inc. Flow cell device, system and method for optical interrogation using the flow cell device
EP3792673A1 (en) * 2019-09-16 2021-03-17 ASML Netherlands B.V. Assembly for collimating broadband radiation
WO2021043516A1 (en) * 2019-09-03 2021-03-11 Asml Netherlands B.V. Assembly for collimating broadband radiation
DE102020124916B4 (en) 2020-09-24 2022-07-28 Rheinische Friedrich-Wilhelms-Universität Bonn Attachment of an optically transparent window to a metal work piece

Family Cites Families (38)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1982002952A1 (en) * 1981-02-17 1982-09-02 Instruments Inc Beckman Double beam photometer for measuring fluid samples
US4747687A (en) * 1984-06-08 1988-05-31 Milton Roy Company Ball cell windows for spectrophotometers
US4802761A (en) * 1987-08-31 1989-02-07 Western Research Institute Optical-fiber raman spectroscopy used for remote in-situ environmental analysis
JPH07109313B2 (en) 1987-09-17 1995-11-22 株式会社日立製作所 Air conditioner
JPH0175851U (en) * 1987-11-11 1989-05-23
US4886356A (en) 1988-04-01 1989-12-12 The Perkin-Elmer Corporation Detector cell for liquid chromatography
US5054919A (en) * 1989-02-07 1991-10-08 Linear Instruments Corporation Seal for high pressure and small volume sample cells
US5046854A (en) * 1990-02-01 1991-09-10 The Dow Chemical Company Photometric cell and probe having windows fusion sealed to a metallic body
US5310526A (en) * 1990-10-30 1994-05-10 The Dow Chemical Company Chemical sensor
US5124555A (en) * 1991-01-03 1992-06-23 Hewlett-Packard Company High pressure window assembly
DE69230863T2 (en) * 1991-12-03 2000-07-27 Applied Biosystems CAPILLARY FLOW CELL FOR DETECTING SEVERAL WAVELENGTHS
US5274227A (en) * 1992-10-23 1993-12-28 Applied Biosystems, Inc. Capillary detector cell having imaging elements positioned to optimize sensitivity
EP0597552A1 (en) 1992-11-13 1994-05-18 Lc Packings Nederland B.V. An improved method of and a capillary flow cell for analysing fluid samples
JPH09264840A (en) 1996-03-29 1997-10-07 Tosoh Corp Absorbancy meter
JP3356044B2 (en) 1997-12-10 2002-12-09 株式会社島津製作所 UV-visible absorbance detector
US5923431A (en) * 1998-04-14 1999-07-13 Uop Llc Spectroscopic helical separator and fluid sample interface
EP1010975A1 (en) 1998-12-14 2000-06-21 SCITEX DIGITAL PRINTING, Inc. Liquid concentration optical sensor
US6281975B1 (en) * 2000-03-07 2001-08-28 Eldex Laboratories, Inc. Capillary flow cell with bulbous ends
US6638668B2 (en) * 2000-05-12 2003-10-28 Ocean Optics, Inc. Method for making monolithic patterned dichroic filter detector arrays for spectroscopic imaging
US6700690B1 (en) * 2000-10-02 2004-03-02 Ocean Optics, Inc. Tunable variable bandpass optical filter
US6474152B1 (en) * 2000-11-02 2002-11-05 Schlumberger Technology Corporation Methods and apparatus for optically measuring fluid compressibility downhole
US7670559B2 (en) * 2001-02-15 2010-03-02 Caliper Life Sciences, Inc. Microfluidic systems with enhanced detection systems
JP3726691B2 (en) 2001-03-09 2005-12-14 株式会社日本自動車部品総合研究所 Infrared gas analyzer
JP2003279471A (en) 2002-03-20 2003-10-02 Nippon Sheet Glass Co Ltd Chip for microchemical system and microchemical system
JP2004157043A (en) 2002-11-07 2004-06-03 Shimadzu Corp Optical measuring device
US6839176B2 (en) * 2002-12-16 2005-01-04 Ocean Optics, Inc. Composition and method of making high-reflection silver mirrors or thin-film optical filters
US20050063869A1 (en) 2003-09-24 2005-03-24 Stephane Follonier Device, system and method of detecting targets in a fluid sample
JP2005329330A (en) 2004-05-20 2005-12-02 Yokogawa Electric Corp Structure of window for high temperature and high pressure vessel
US8262909B2 (en) * 2004-07-06 2012-09-11 Schlumberger Technology Corporation Methods and devices for minimizing membrane fouling for microfluidic separators
US7575681B2 (en) * 2004-07-06 2009-08-18 Schlumberger Technology Corporation Microfluidic separator
US7799278B2 (en) * 2004-07-06 2010-09-21 Schlumberger Technology Corporation Microfluidic system for chemical analysis
EP1617202B1 (en) * 2004-07-13 2009-09-23 Services Petroliers Schlumberger Detector for distinguishing phases in a multiphase fluid mixture
US7149033B2 (en) * 2004-10-28 2006-12-12 Ocean Optics, Inc. UV visual light beam combiner
US7307717B2 (en) * 2005-09-16 2007-12-11 Lockheed Martin Corporation Optical flow cell capable of use in high temperature and high pressure environment
US7515259B2 (en) * 2006-03-10 2009-04-07 Dionex Corporation Flow cell for optical detector and method of forming same
US7687770B2 (en) * 2007-01-19 2010-03-30 Schlumberger Technology Corporation Methods and apparatus for multi dimension fluorescence spectrum measurement downhole
JP4712745B2 (en) 2007-03-06 2011-06-29 倉敷紡績株式会社 Flow cell for transmitted light measurement
US8389054B2 (en) * 2008-08-14 2013-03-05 Schlumberger Technology Corporation Fabrication technique for metallic devices with embedded optical elements, optical devices, or optical and electrical feedthroughs

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of EP2419711A4 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2479555B1 (en) * 2010-12-21 2013-03-13 Sick Ag Optical analyser with a holder for installation in a gas-bearing cavity

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EP2419711A4 (en) 2012-09-26
CA2753392A1 (en) 2010-10-21
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JP5470447B2 (en) 2014-04-16
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US8564768B2 (en) 2013-10-22
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