WO2014072736A1 - Method for characterising hydrocarbon fluids - Google Patents

Method for characterising hydrocarbon fluids Download PDF

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Publication number
WO2014072736A1
WO2014072736A1 PCT/GB2013/052958 GB2013052958W WO2014072736A1 WO 2014072736 A1 WO2014072736 A1 WO 2014072736A1 GB 2013052958 W GB2013052958 W GB 2013052958W WO 2014072736 A1 WO2014072736 A1 WO 2014072736A1
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Prior art keywords
hydrocarbon fluid
characterising
output field
hydrocarbon
fluid
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PCT/GB2013/052958
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French (fr)
Inventor
Graeme Peter Alexander MALCOLM
Gareth Thomas MAKER
John Nicholls
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M Squared Lasers Limited
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Publication of WO2014072736A1 publication Critical patent/WO2014072736A1/en

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    • 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
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • 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
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • 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
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
    • 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
    • G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
    • 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
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; viscous liquids; paints; inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2823—Oils, i.e. hydrocarbon liquids raw oil, drilling fluid or polyphasic mixtures

Definitions

  • the present invention relates to the field of hydrocarbon exploration. More specifically, the present invention concerns the provision of a laser spectroscopy method for characterising or "fingerprinting" a hydrocarbon fluid in order to provide a means for identifying the source of the hydrocarbon fluid or for monitoring a hydrocarbon fluid for contaminants or foreign fluids.
  • Crude oils comprise many different hydrocarbon compounds each of which contribute to its characteristic spectral profile or fingerprint. The composition of such oils is known to differ from country to country and even from different exploratory fields within a single country. For example refined oils may consist of both fuel oils and lubricating oils.
  • Gasoline, kerosene and dieseline are fuel oils that are derived from the refining process and separated according to their different boiling points. Heavier oils are used for lubricating purposes and generally exhibit higher boiling points. It is known that the differences in the composition of these oils can be used to distinguish one hydrocarbon fluid from another i.e. the characteristic spectral profile or fingerprint of the hydrocarbon fluid can be used to identify the source of the fluid or to monitor the hydrocarbon fluid so as to check for the presence of contaminants or degradation of the hydrocarbon fluid. This may be achieved without the operator being required to determine the actual chemical components and ratios of the components within the complex hydrocarbon fluid. What is important is the overall characteristic spectral profile or fingerprint produced by the combined contribution of all the chemical components present.
  • TRLI F Time-resolved Laser-Induced Fluorescence
  • hydrocarbon fluids such as kerosene, gasoline, and diesel fuel
  • hydrocarbon fluids are each composed of mixtures of different hydrocarbons that fall within certain boiling point ranges loosely coordinated with molecular weight ranges.
  • the type and distribution of hydrocarbons within each class of fuel may also vary according to the geographical source of the crude oil and the type of refining method (distillation, cracking, etc.).
  • These fluids are dense, contain mixtures of hydrocarbons having overlapping excitation-emission spectra, produce fluorescent emissions that may be reabsorbed, and also may be contaminated with quenching compounds. As a result the fluorescence signals are often not particularly strong and so require high sensitive detectors to be employed.
  • the method for characterising the hydrocarbon production flow further comprises comparing the produced characteristic spectral profile or fingerprint with one or more known characteristic spectral profiles or fingerprints.
  • the comparison of the produced characteristic spectral profile may provide a means for identifying a source of the hydrocarbon production flow.
  • the comparison of the produced characteristic spectral profile may provide a means for identifying one or more contaminants or foreign fluids entering the hydrocarbon production flow.
  • the output field is preferably exposed to the hydrocarbon production flow by scanning the output field over an area of the hydrocarbon production flow.
  • the measurement of the absorption may comprise the measurement of a back-scatter absorption signal produced by the scanned output field.
  • the measurement of the absorption may comprise the measurement of a transmission signal produced by the scanned output field propagating through the hydrocarbon production flow.
  • the mid-infrared light source comprises an optical parametric device and in particular an intracavity optical parametric device.
  • the output field may comprise a pulsed field having a pulse repetition frequency of more than 100kHz, and preferably more than 200kHz.
  • the output field generated by the mid-infrared light source preferably comprises a wavelength between 2 to 6 microns.
  • the output field generated by the mid-infrared light source comprises a wavelength between 3 to 4 microns.
  • the output field generated by the mid-infrared light source exhibits a spectral linewidth less than or equal to 5GHz.
  • a scanning and detection system that provides a means for exposing the output field to the hydrocarbon production flow, measuring an absorption of the scanned output field following its exposure to the hydrocarbon production flow, and producing a characteristic spectral profile or fingerprint of the hydrocarbon production flow from the measured absorption.
  • the system further comprises a database of hydrocarbon fluid
  • Embodiments of the second aspect of the invention may comprise features to implement the preferred or optional features of the first aspect of the invention or vice versa.
  • a third aspect of the present invention there is provided a method for characterising a hydrocarbon fluid comprising:
  • the exposure of the hydrocarbon fluid to the output field comprises exposing the output field to a hydrocarbon production flow.
  • the output field is preferably exposed to the hydrocarbon production flow by scanning the output field over an area of the hydrocarbon production flow.
  • the exposure of the hydrocarbon fluid to the output field comprises exposing the output field to a sample taken from a hydrocarbon fluid.
  • the output field is preferably exposed to the hydrocarbon fluid by scanning the output field over an area of the hydrocarbon fluid.
  • Embodiments of the third aspect of the invention may comprise features to implement the preferred or optional features of the first or second aspects of the invention or vice versa.
  • a scanning and detection system that provides a means for exposing the output field to the hydrocarbon fluid, measuring an absorption of the wavelength scanned output field following its exposure to the fluid, and producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption.
  • the system further comprises a database of hydrocarbon fluid
  • the hydrocarbon fluid may comprise a barrel of oil.
  • the hydrocarbon fluid may comprise a sample taken from an oil spillage.
  • Embodiments of the fourth aspect of the invention may comprise features to implement the preferred or optional features of the first, second or third aspects of the invention or vice versa.
  • a fifth aspect of the present invention there is provided a method for monitoring a hydrocarbon fluid for the presence of contaminants or foreign fluids entering the hydrocarbon fluid the method comprising:
  • the method for monitoring the hydrocarbon fluid further comprises comparing the produced characteristic spectral profile or fingerprint with one or more known characteristic spectral profiles or fingerprints.
  • Embodiments of the fifth aspect of the invention may comprise features to implement the preferred or optional features of the first to fourth aspects of the invention or vice versa.
  • Figure 1 presents a schematic representation of a system employed to characterise or fingerprint a hydrocarbon production flow
  • Figure 2 presents a flow chart of the methodology involved in characterising or fingerprinting a hydrocarbon production flow
  • Figure 3 presents a schematic representation of a mid-infrared laser source employed by the system of Figure 1
  • Figure 4 presents a schematic representation of a scanning and detection system employed by the system of Figure 1
  • Figure 5 presents a schematic representation of a system employed to characterise or fingerprint a sample of a hydrocarbon fluid.
  • Figure 1 presents a schematic representation of a system 1 employed to characterise or fingerprint a hydrocarbon production flow 2.
  • the system 1 can be seen to comprise a fluid conduit 3 that forms part of a hydrocarbon production system, a mid-infrared laser source 4 and a raster scanning and detection system 5.
  • the fluid conduit 3 of the hydrocarbon production system may be one of many conduits present in range of locations across the system. These include locations at or on the wellhead, including on a wellhead or mandrel cap, adjacent to the choke body, immediately adjacent the wellhead between a flowline connector or a jumper or as part of fluid intervention system. Alternatively the apparatus of the invention may be used in locations disposed further away from the wellhead.
  • An output field 6 from the mid-infrared laser source 4 is initially directed into the scanning and detection system 5 by two beam steering mirrors 7 and 8. The output field 6 is then directed towards the hydrocarbon production flow 2 located within the fluid conduit 3 by the raster scanning and detection system so as to generate a back-scatter absorption signal 9. The output field 6 may reach the hydrocarbon production flow 2 via a window 10 in the fluid conduit 3.
  • the back-scatter absorption signal 9 may return to the scanning and detection system 5 via the window 10. It will be appreciated by the skilled reader that separate windows may be employed for the output field 6 and the back-scatter absorption signal 9 Similarly an alternative embodiment (not shown) may comprise separating the components of the scanning and detection system 5 such that the detector component is located so as to measure a transmission signal (not shown) produced by output field 6 after it has propagated through the hydrocarbon production flow 2. This embodiment is less preferable since it increase the overall footprint of the system 1 thus making it less compact and so less portable.
  • Figure 2 presents a flow chart of the method employed by the system of Figure 1. In the first instance the method comprises exposing the hydrocarbon production flow 2 to the output field 6 generated by the mid-infrared laser source 4.
  • the mid-infrared laser source 4 is then scanned such that the wavelength of the output field 6 scans across the wavelength range between 2 to 6 microns. More preferably the output field 6 scans across the wavelength range between 3 to 4 microns
  • the scanning and detection system 5 is employed to scan the position of the output field 6 across the hydrocarbon production flow 2 and to then measuring the generated back scatter absorption signal 9. Finally, the scanning and detection system 5 is employed to produce a characteristic spectral profile or fingerprint of the hydrocarbon production flow 2 from the measured absorption signal 9.
  • a suitable mid-infrared laser source 4 is an intracavity Optical Parametric Oscillator (OPO) as presented schematically within Figure 3 and as described in detail within international patent publication number WO 2006/061567.
  • the intracavity OPO 4 comprises a first optical cavity (pump laser cavity) containing a laser gain medium 11 that serves to provide a pump wave source for the nonlinear parametric process.
  • the laser gain medium 11 comprises a Nd:YV0 4 crystal that provides a pump wave source at 1.064 microns.
  • the intracavity OPO 4 further comprises a semiconductor diode 12 that provides an excitation source at 808.5nm for the laser gain medium 11.
  • a further component of the intracavity OPO 4 is a second optical cavity (signal cavity) that is in part common to the first optical cavity and which contains in that common part a nonlinear crystal 13.
  • the non-linear crystal 13 may comprise a periodically poled nonlinear crystal (for example PPLN or PPRTA), which serves to generate the down converted waves.
  • the non-linear crystal 13 is triple-band antireflection coated for the pump, signal and idler fields.
  • the diode 12 is thermoelectrically cooled such that the wavelength of the radiation it emits is coincident with the peak absorption in the Nd:YV0 4 crystal 1 1.
  • the radiation emitted by the diode 12 is collimated and then focused down into the Nd:YV0 4 crystal by a focusing lens assembly 14. Radiation emitted from the crystal 1 1 is then directed onto an intracavity mirror 15.
  • a Q-switch element 16 On the same optical path as the intracavity mirror 15 are a Q-switch element 16, a pump cavity etalon 17, an anti-reflection (at the pump wavelength) coated intracavity lens 18, a beam splitter 19, the nonlinear crystal 13, and a curved pump/signal mirror 20.
  • a beam splitter 19 Opposite the beam splitter 19 is a signal cavity etalon 21 and a signal mirror 22.
  • the pump laser cavity is defined by the rear face of the Nd: YV0 4 crystal 1 1 , which is antireflection coated for 808.5nm light and highly reflecting at 1.064microns and the pump/signal mirror 20, which is highly reflecting at 1.064microns and broad-band highly reflecting centred at 1.550 microns.
  • An appropriate beam waist of the pump intracavity field is formed in the nonlinear crystal 13 by the antireflection coated intracavity lens 18 and the curved pump/signal mirror 20.
  • the beamsplitter 19 is coated on both sides to be antireflection at the pump wavelength but, on its lower face, highly reflecting at the signal wavelength.
  • the pump/signal mirror 20 and the signal mirror 22 act to form the signal cavity.
  • the (mid- infrared) idler radiation is not resonated and exits the cavity through the pump/signal mirror 20 after being generated in the nonlinear crystal 13 so as to form an output field 6 for the system.
  • the wavelength of this output field 6 can be tuned by simply temperature tuning the
  • the above arrangement thus provides a portable laser source that exhibits a pulsed output field having a pulse repetition frequency of more than 100kHz, a spectral linewidth of less than or equal to 5GHz and which can be wavelength tuned from 2 to 6 microns.
  • the intracavity OPO 4 is therefore an ideal source for carrying out absorption spectroscopy upon a hydrocarbon fluid.
  • a suitable scanning and detection system 5 is also described in detail within international patent publication number WO 2006/061567 and presented schematically within Figure 4.
  • the output field 6 enters the scanning and detection system 5 along an optical axis 23.
  • the output field 6 is then incident on a plane mirror 24 placed on-axis in front of a collimating lens 25, which is fabricated from a material which exhibits high transmission over the 3 to 4 micron range, for example calcium fluoride.
  • a collimating lens 25 which is fabricated from a material which exhibits high transmission over the 3 to 4 micron range, for example calcium fluoride.
  • the output field 6 is directed via a rotating polygon scanner 26 and tilting mirror 27 to the hydrocarbon production flow 2.
  • the back- scattered absorption signal 9 returning from the hydrocarbon production flow 2 is collected via the same tilting mirror 27 and polygon scanner 26 and is then focused by a collection lens 28 onto the single element detector 29 located in its image plane.
  • the area of the collection lens 28 is sufficient such that the effective limiting collection aperture for the back- scattered absorption signal 9 occurs at the polygon mirror facet.
  • This arrangement ensures that the detector 29 always views the area of the hydrocarbon production flow 2 currently being illuminated by the scanned output field 6, i.e. the viewing direction is scanned in spatial synchronism with the illuminating beam.
  • the lens 25 placed before the mirror 24 allows independent adjustment of the focusing of the illuminating output field 6 on the hydrocarbon production flow 2. In particular it allows the projection of a beam waist onto the target area so as to optimise the spatial resolution of the scanner in relation to the response time of the detector and the lateral extent of the area being scanned.
  • a band pass filter 30 may be placed in close proximity to the detector 29 in order to reject stray infrared radiation from hot objects, lights and pump and signal fields that are leaked through OPO mirror PSM.
  • the acquisition electronics 31 Connected to the detector 29 are the acquisition electronics 31 , which in turn are connected to a display 32 and a trigger detector 33.
  • a low power laser diode 34 Associated with the trigger detector 33 is a low power laser diode 34.
  • the low power laser diode 34 is positioned to direct light onto the rotating polygon 26. Radiation reflected from the polygon 26 falls on the detector 33 at a pre-determined trigger position.
  • Detection of light by the detector 33 is used to trigger the image acquisition electronics 31 at the correct point of the polygon rotation 26 when scanning a horizontal line.
  • the acquisition electronics 31 capture data from the detector 29, process that data and provide a real-time spectral profile or fingerprint of the hydrocarbon production flow 2.
  • the polygon scanner 26 provides line scanning of the output field 6 in a horizontal direction.
  • the tilting mirror 27 provides scanning in the orthogonal (vertical) direction, and is set up so as to provide beam deflection over an angle of similar to that of the polygon scanner 26.
  • the rotational speed of the polygonal scanner 26 is such that the maximum bandwidth of the detector 29 and the subsequent acquisition electronics 31 are not exceeded.
  • a trigger signal from the acquisition electronics 31 is fed to the Q-Switch 16 in order to emit a mid-infrared pulse for every pixel acquired. Therefore, the maximum rate at which the Q-switch 16 can be triggered determines the upper ceiling of the framing rate that can be obtained from the system.
  • the characteristic spectral profile or fingerprint of the hydrocarbon production flow 2 can then be compared with a database 35 of known characteristic spectral profiles or fingerprints. This database 35 may be stored within the acquisition electronics 31. As a result the identification and quality of the hydrocarbon production flow 2 can be monitored in real time so as to highlight the presence of any contaminants or similar foreign fluids that have entered into the hydrocarbon production flow 2.
  • FIG. 5 presents a schematic representation of a system 36 employed to characterise or fingerprint hydrocarbon fluid sample 37.
  • the system 36 can again be seen to comprise a fluid sample 37, a mid-infrared laser source 4 and a raster scanning and detection system 5.
  • the system operates in a similar manner to that described above in relation to the hydrocarbon production flow 2, and as presented by the flow diagram of Figure 2.
  • the system 36 is however suited for testing hydrocarbon samples 37 such as the contents of a barrel or an oil spillage. In this way a fingerprint of the sample 37 can be quickly obtained.
  • an identification of the original source of the fluid sample 37 may be made by comparing the characteristic spectral profile or fingerprint obtained with the database 35 of known spectral profiles or fingerprints. This process can be repeated at a later time so as to monitor for the effects of weathering of a hydrocarbon fluid spillage or degradation of the hydrocarbon fluid itself.
  • the above described systems and methods provide an alternative for fingerprinting hydrocarbon fluids.
  • the described techniques are based on absorption spectroscopy rather than fluorescence spectroscopy and as such do not require high sensitive detectors to be employed.
  • the extraction of the relevant data requires simpler signal processing techniques than those generally employed with fluorescence spectroscopy techniques.
  • the system and methods can be employed with a hydrocarbon production fluid so as to provide a means for real time analysis of a production fluid.
  • the described fingerprinting techniques can also be readily employed to determine what type of oil is being analysed, for example distinguishing it from a crude oil source or a refined oil source.
  • the source of the oil being analysed can also be determined by comparing the generated fingerprints with known fingerprints stored in a database.
  • the fingerprinting techniques can also be used to link samples taken from an oil spillage to a suspected oil source.
  • a method and system for characterising a hydrocarbon fluid is described. The method involves exposing the hydrocarbon fluid to an output field generated by a mid-infrared laser source.
  • the wavelength of the output field is then scanned and the field is scanned over an area of the hydrocarbon fluid so allowing for the absorption of the output field by the hydrocarbon fluid to be measured. From this measured data a characteristic spectral profile or fingerprint of the hydrocarbon fluid can be produced. This spectral profile or fingerprint of the hydrocarbon fluid can then be used to identify the source of the hydrocarbon fluid or monitor for the presence of contaminants or foreign fluids entering the hydrocarbon fluid.
  • the method and system finds particular application for real time monitoring of a hydrocarbon production flow.

Abstract

A method and system for characterising a hydrocarbon fluid (2) is described. The method involves exposing the hydrocarbon fluid to an output field generated by a mid-infrared laser source (4). The wavelength of the output field is then scanned and the field is scanned over an area of the hydrocarbon fluid so allowing for the absorption of the output field by the hydrocarbon fluid to be measured. From this measured data a spectral profile or fingerprint (9) of the hydrocarbon fluid can be produced. This spectral profile or fingerprint of the hydrocarbon fluid can then be used to identify the source of the hydrocarbon fluid or monitor for the presence of contaminants or foreign fluids entering the hydrocarbon fluid. The method and system finds particular application for real time monitoring of a hydrocarbon production flow.

Description

Method for Characterising Hydrocarbon Fluids The present invention relates to the field of hydrocarbon exploration. More specifically, the present invention concerns the provision of a laser spectroscopy method for characterising or "fingerprinting" a hydrocarbon fluid in order to provide a means for identifying the source of the hydrocarbon fluid or for monitoring a hydrocarbon fluid for contaminants or foreign fluids. Crude oils comprise many different hydrocarbon compounds each of which contribute to its characteristic spectral profile or fingerprint. The composition of such oils is known to differ from country to country and even from different exploratory fields within a single country. For example refined oils may consist of both fuel oils and lubricating oils.
Gasoline, kerosene and dieseline are fuel oils that are derived from the refining process and separated according to their different boiling points. Heavier oils are used for lubricating purposes and generally exhibit higher boiling points. It is known that the differences in the composition of these oils can be used to distinguish one hydrocarbon fluid from another i.e. the characteristic spectral profile or fingerprint of the hydrocarbon fluid can be used to identify the source of the fluid or to monitor the hydrocarbon fluid so as to check for the presence of contaminants or degradation of the hydrocarbon fluid. This may be achieved without the operator being required to determine the actual chemical components and ratios of the components within the complex hydrocarbon fluid. What is important is the overall characteristic spectral profile or fingerprint produced by the combined contribution of all the chemical components present. Traditional fingerprinting methods have involved the collection of a sample of the hydrocarbon fluid and then separating this sample into various fractions that are then analysed using lab based equipment e.g. Gas Chromatography-Mass Spectrometers to give information regarding their chemical compositions. However, since these methods require large scale laboratory based equipment they cannot normally be used in situations where instant and or remote characterisation is required. In order to address these issues a number of UV induced fluorescence spectroscopy techniques have been developed. This is primarily due to these techniques being able to exploit broadband UV light sources, the wide tuning ability in terms of available excitation wavelengths (typically in the range of 200nm to 400nm), and the multiple ways known in the art for detecting and measuring the resulting fluorescence. Some fluorescence methods that have been applied for fingerprinting hydrocarbon fluids include: (a) Synchronous Scan Spectroscopy in which the oil spectra are produced by scanning the excitation wavelength and the emission wavelength, simultaneously, at a fixed wavelength separation;
(b) Contour (Total Luminescence) Spectroscopy in which contour diagrams for the oils are constructed out of several emission spectra that are excited at different excitation wavelengths; and
(c) Time-resolved Laser-Induced Fluorescence (TRLI F) spectroscopy in which the characterisation of the oils is done by monitoring the spectral as well as the temporal characteristics of the emitted fluorescence in either the excitation or in the detection stages, or in both. The most attractive of the above techniques is TRLIF spectroscopy since a laser source rather than a UV lamp can be employed. This make such systems portable and so more suited for remote sensing applications, see for example US patent publication numbers 2003/0141459, 2008/035858 and international patent publication number WO2012027059. As discussed above, hydrocarbon fluids, such as kerosene, gasoline, and diesel fuel, are each composed of mixtures of different hydrocarbons that fall within certain boiling point ranges loosely coordinated with molecular weight ranges. The type and distribution of hydrocarbons within each class of fuel may also vary according to the geographical source of the crude oil and the type of refining method (distillation, cracking, etc.). These fluids are dense, contain mixtures of hydrocarbons having overlapping excitation-emission spectra, produce fluorescent emissions that may be reabsorbed, and also may be contaminated with quenching compounds. As a result the fluorescence signals are often not particularly strong and so require high sensitive detectors to be employed.
Furthermore, extraction of the relevant data generally requires complex signal processing techniques in order to remove background signals and to separate overlapping excitation- emission spectra. Therefore, fluorescent spectroscopy has certain practical limitations when employed for characterising, or "fingerprinting" hydrocarbon fluids. It is recognised in the present invention that considerable advantage is to be gained in the provision of an alternative method for characterising, or fingerprinting hydrocarbon fluids and in particular one that can be employed in situ and or within remote locations. It is therefore an object of an aspect of the present invention to obviate or at least mitigate the foregoing disadvantages of the methods of characterising, or fingerprinting
hydrocarbon fluids known in the art. Summary of Invention According to a first aspect of the present invention there is provided a method for characterising a hydrocarbon production flow comprising:
-exposing the hydrocarbon production flow to an output field generated by a mid-infrared laser source;
-scanning a wavelength of the output field;
-measuring an absorption of the scanned output field following its exposure to the hydrocarbon production flow; and -producing a characteristic spectral profile or fingerprint of the hydrocarbon production flow from the measured absorption. Most preferably the method for characterising the hydrocarbon production flow further comprises comparing the produced characteristic spectral profile or fingerprint with one or more known characteristic spectral profiles or fingerprints. The comparison of the produced characteristic spectral profile may provide a means for identifying a source of the hydrocarbon production flow. The comparison of the produced characteristic spectral profile may provide a means for identifying one or more contaminants or foreign fluids entering the hydrocarbon production flow. The output field is preferably exposed to the hydrocarbon production flow by scanning the output field over an area of the hydrocarbon production flow. It is preferable for the measurement of the absorption to comprise the measurement of a back-scatter absorption signal produced by the scanned output field. Alternatively, the measurement of the absorption may comprise the measurement of a transmission signal produced by the scanned output field propagating through the hydrocarbon production flow. Most preferably the mid-infrared light source comprises an optical parametric device and in particular an intracavity optical parametric device. The output field may comprise a pulsed field having a pulse repetition frequency of more than 100kHz, and preferably more than 200kHz. The output field generated by the mid-infrared light source preferably comprises a wavelength between 2 to 6 microns. Most preferably the output field generated by the mid-infrared light source comprises a wavelength between 3 to 4 microns. Preferably the output field generated by the mid-infrared light source exhibits a spectral linewidth less than or equal to 5GHz. According to a second aspect of the present invention there is provided a system for characterising a hydrocarbon production flow comprising:
- a mid-infrared laser source that provides a means for producing a wavelength scanning output field;
- a scanning and detection system that provides a means for exposing the output field to the hydrocarbon production flow, measuring an absorption of the scanned output field following its exposure to the hydrocarbon production flow, and producing a characteristic spectral profile or fingerprint of the hydrocarbon production flow from the measured absorption. Most preferably the system further comprises a database of hydrocarbon fluid
characteristic spectral profiles or fingerprints. Embodiments of the second aspect of the invention may comprise features to implement the preferred or optional features of the first aspect of the invention or vice versa. According to a third aspect of the present invention there is provided a method for characterising a hydrocarbon fluid comprising:
-exposing a hydrocarbon fluid to an output field generated by a mid-infrared laser source; -scanning a wavelength of the output field;
-measuring an absorption of the wavelength scanned output field following its exposure to the hydrocarbon fluid; and
-producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption. Most preferably the exposure of the hydrocarbon fluid to the output field comprises exposing the output field to a hydrocarbon production flow. The output field is preferably exposed to the hydrocarbon production flow by scanning the output field over an area of the hydrocarbon production flow. Alternatively the exposure of the hydrocarbon fluid to the output field comprises exposing the output field to a sample taken from a hydrocarbon fluid. The output field is preferably exposed to the hydrocarbon fluid by scanning the output field over an area of the hydrocarbon fluid. Embodiments of the third aspect of the invention may comprise features to implement the preferred or optional features of the first or second aspects of the invention or vice versa. According to a fourth aspect of the present invention there is provided a system for characterising a hydrocarbon fluid comprising:
- a mid-infrared laser source that provides a means for producing a wavelength scanning output field;
- a scanning and detection system that provides a means for exposing the output field to the hydrocarbon fluid, measuring an absorption of the wavelength scanned output field following its exposure to the fluid, and producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption. Most preferably the system further comprises a database of hydrocarbon fluid
characteristic spectral profiles or fingerprints. The hydrocarbon fluid may comprise a barrel of oil. Alternatively the hydrocarbon fluid may comprise a sample taken from an oil spillage. Embodiments of the fourth aspect of the invention may comprise features to implement the preferred or optional features of the first, second or third aspects of the invention or vice versa. According to a fifth aspect of the present invention there is provided a method for monitoring a hydrocarbon fluid for the presence of contaminants or foreign fluids entering the hydrocarbon fluid the method comprising:
-exposing a hydrocarbon fluid to an output field generated by a mid-infrared laser source; -scanning a wavelength of the output field;
-measuring an absorption of the wavelength scanned output field following its exposure to the hydrocarbon fluid; and
-producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption. Most preferably the method for monitoring the hydrocarbon fluid further comprises comparing the produced characteristic spectral profile or fingerprint with one or more known characteristic spectral profiles or fingerprints. Embodiments of the fifth aspect of the invention may comprise features to implement the preferred or optional features of the first to fourth aspects of the invention or vice versa. Brief Description of Drawings Aspects and advantages of the present invention will become apparent upon reading the following detailed description and upon reference to the following drawings in which: Figure 1 presents a schematic representation of a system employed to characterise or fingerprint a hydrocarbon production flow; Figure 2 presents a flow chart of the methodology involved in characterising or fingerprinting a hydrocarbon production flow; Figure 3 presents a schematic representation of a mid-infrared laser source employed by the system of Figure 1 ; Figure 4 presents a schematic representation of a scanning and detection system employed by the system of Figure 1 ; and Figure 5 presents a schematic representation of a system employed to characterise or fingerprint a sample of a hydrocarbon fluid. Detailed Description A method for characterising or "fingerprinting" a hydrocarbon production flow will now be described with reference to Figures 1 to 4. In the context of this specification the term "mid-infrared" is taken to comprise a wavelength range between 2 to 6 microns. In particular, hydrocarbon molecules found within petroleum products exhibit a large number of absorption lines in the mid-infrared range between 3 to 4 microns. Figure 1 presents a schematic representation of a system 1 employed to characterise or fingerprint a hydrocarbon production flow 2. The system 1 can be seen to comprise a fluid conduit 3 that forms part of a hydrocarbon production system, a mid-infrared laser source 4 and a raster scanning and detection system 5. It will be appreciated by the skilled reader that the fluid conduit 3 of the hydrocarbon production system may be one of many conduits present in range of locations across the system. These include locations at or on the wellhead, including on a wellhead or mandrel cap, adjacent to the choke body, immediately adjacent the wellhead between a flowline connector or a jumper or as part of fluid intervention system. Alternatively the apparatus of the invention may be used in locations disposed further away from the wellhead. These include (but are not limited to) downstream of a jumper flowline or a section of a jumper flowline; a subsea collection manifold system; a subsea Pipe Line End Manifold (PLEM); a subsea Pipe Line End Termination (PLET); and/or a subsea Flow Line End Termination (FLET). An output field 6 from the mid-infrared laser source 4 is initially directed into the scanning and detection system 5 by two beam steering mirrors 7 and 8. The output field 6 is then directed towards the hydrocarbon production flow 2 located within the fluid conduit 3 by the raster scanning and detection system so as to generate a back-scatter absorption signal 9. The output field 6 may reach the hydrocarbon production flow 2 via a window 10 in the fluid conduit 3. Similarly the back-scatter absorption signal 9 may return to the scanning and detection system 5 via the window 10. It will be appreciated by the skilled reader that separate windows may be employed for the output field 6 and the back-scatter absorption signal 9 Similarly an alternative embodiment (not shown) may comprise separating the components of the scanning and detection system 5 such that the detector component is located so as to measure a transmission signal (not shown) produced by output field 6 after it has propagated through the hydrocarbon production flow 2. This embodiment is less preferable since it increase the overall footprint of the system 1 thus making it less compact and so less portable. Figure 2 presents a flow chart of the method employed by the system of Figure 1. In the first instance the method comprises exposing the hydrocarbon production flow 2 to the output field 6 generated by the mid-infrared laser source 4. The mid-infrared laser source 4 is then scanned such that the wavelength of the output field 6 scans across the wavelength range between 2 to 6 microns. More preferably the output field 6 scans across the wavelength range between 3 to 4 microns The scanning and detection system 5 is employed to scan the position of the output field 6 across the hydrocarbon production flow 2 and to then measuring the generated back scatter absorption signal 9. Finally, the scanning and detection system 5 is employed to produce a characteristic spectral profile or fingerprint of the hydrocarbon production flow 2 from the measured absorption signal 9. A suitable mid-infrared laser source 4 is an intracavity Optical Parametric Oscillator (OPO) as presented schematically within Figure 3 and as described in detail within international patent publication number WO 2006/061567. The intracavity OPO 4 comprises a first optical cavity (pump laser cavity) containing a laser gain medium 11 that serves to provide a pump wave source for the nonlinear parametric process. The laser gain medium 11 comprises a Nd:YV04 crystal that provides a pump wave source at 1.064 microns. The intracavity OPO 4 further comprises a semiconductor diode 12 that provides an excitation source at 808.5nm for the laser gain medium 11. A further component of the intracavity OPO 4 is a second optical cavity (signal cavity) that is in part common to the first optical cavity and which contains in that common part a nonlinear crystal 13. The non-linear crystal 13 may comprise a periodically poled nonlinear crystal (for example PPLN or PPRTA), which serves to generate the down converted waves. The non-linear crystal 13 is triple-band antireflection coated for the pump, signal and idler fields. The diode 12 is thermoelectrically cooled such that the wavelength of the radiation it emits is coincident with the peak absorption in the Nd:YV04 crystal 1 1. The radiation emitted by the diode 12 is collimated and then focused down into the Nd:YV04 crystal by a focusing lens assembly 14. Radiation emitted from the crystal 1 1 is then directed onto an intracavity mirror 15. On the same optical path as the intracavity mirror 15 are a Q-switch element 16, a pump cavity etalon 17, an anti-reflection (at the pump wavelength) coated intracavity lens 18, a beam splitter 19, the nonlinear crystal 13, and a curved pump/signal mirror 20. Opposite the beam splitter 19 is a signal cavity etalon 21 and a signal mirror 22. The pump laser cavity is defined by the rear face of the Nd: YV04 crystal 1 1 , which is antireflection coated for 808.5nm light and highly reflecting at 1.064microns and the pump/signal mirror 20, which is highly reflecting at 1.064microns and broad-band highly reflecting centred at 1.550 microns. An appropriate beam waist of the pump intracavity field is formed in the nonlinear crystal 13 by the antireflection coated intracavity lens 18 and the curved pump/signal mirror 20. The beamsplitter 19 is coated on both sides to be antireflection at the pump wavelength but, on its lower face, highly reflecting at the signal wavelength. Thus, the pump/signal mirror 20 and the signal mirror 22 act to form the signal cavity. With this arrangement the (mid- infrared) idler radiation is not resonated and exits the cavity through the pump/signal mirror 20 after being generated in the nonlinear crystal 13 so as to form an output field 6 for the system. As is known to those skilled in the art the wavelength of this output field 6 can be tuned by simply temperature tuning the
(periodically poled) nonlinear crystal 13. The above arrangement thus provides a portable laser source that exhibits a pulsed output field having a pulse repetition frequency of more than 100kHz, a spectral linewidth of less than or equal to 5GHz and which can be wavelength tuned from 2 to 6 microns. The intracavity OPO 4 is therefore an ideal source for carrying out absorption spectroscopy upon a hydrocarbon fluid. A suitable scanning and detection system 5 is also described in detail within international patent publication number WO 2006/061567 and presented schematically within Figure 4. The output field 6 enters the scanning and detection system 5 along an optical axis 23. The output field 6 is then incident on a plane mirror 24 placed on-axis in front of a collimating lens 25, which is fabricated from a material which exhibits high transmission over the 3 to 4 micron range, for example calcium fluoride. From the mirror 24, the output field 6 is directed via a rotating polygon scanner 26 and tilting mirror 27 to the hydrocarbon production flow 2. The back- scattered absorption signal 9 returning from the hydrocarbon production flow 2 is collected via the same tilting mirror 27 and polygon scanner 26 and is then focused by a collection lens 28 onto the single element detector 29 located in its image plane. The area of the collection lens 28 is sufficient such that the effective limiting collection aperture for the back- scattered absorption signal 9 occurs at the polygon mirror facet. This arrangement ensures that the detector 29 always views the area of the hydrocarbon production flow 2 currently being illuminated by the scanned output field 6, i.e. the viewing direction is scanned in spatial synchronism with the illuminating beam. The lens 25 placed before the mirror 24 allows independent adjustment of the focusing of the illuminating output field 6 on the hydrocarbon production flow 2. In particular it allows the projection of a beam waist onto the target area so as to optimise the spatial resolution of the scanner in relation to the response time of the detector and the lateral extent of the area being scanned. Since the detector employed exhibits sensitivity over a broad range of wavelengths, a band pass filter 30 may be placed in close proximity to the detector 29 in order to reject stray infrared radiation from hot objects, lights and pump and signal fields that are leaked through OPO mirror PSM. Connected to the detector 29 are the acquisition electronics 31 , which in turn are connected to a display 32 and a trigger detector 33. Associated with the trigger detector 33 is a low power laser diode 34. The low power laser diode 34 is positioned to direct light onto the rotating polygon 26. Radiation reflected from the polygon 26 falls on the detector 33 at a pre-determined trigger position. Detection of light by the detector 33 is used to trigger the image acquisition electronics 31 at the correct point of the polygon rotation 26 when scanning a horizontal line. When the trigger signal is received, the acquisition electronics 31 capture data from the detector 29, process that data and provide a real-time spectral profile or fingerprint of the hydrocarbon production flow 2. The polygon scanner 26 provides line scanning of the output field 6 in a horizontal direction. The tilting mirror 27 provides scanning in the orthogonal (vertical) direction, and is set up so as to provide beam deflection over an angle of similar to that of the polygon scanner 26. The rotational speed of the polygonal scanner 26 is such that the maximum bandwidth of the detector 29 and the subsequent acquisition electronics 31 are not exceeded. In use, a trigger signal from the acquisition electronics 31 is fed to the Q-Switch 16 in order to emit a mid-infrared pulse for every pixel acquired. Therefore, the maximum rate at which the Q-switch 16 can be triggered determines the upper ceiling of the framing rate that can be obtained from the system. The characteristic spectral profile or fingerprint of the hydrocarbon production flow 2 can then be compared with a database 35 of known characteristic spectral profiles or fingerprints. This database 35 may be stored within the acquisition electronics 31. As a result the identification and quality of the hydrocarbon production flow 2 can be monitored in real time so as to highlight the presence of any contaminants or similar foreign fluids that have entered into the hydrocarbon production flow 2. The presence of these contaminants or foreign fluids would result in a change in the detected fingerprint of the hydrocarbon production flow 2. Figure 5 presents a schematic representation of a system 36 employed to characterise or fingerprint hydrocarbon fluid sample 37. The system 36 can again be seen to comprise a fluid sample 37, a mid-infrared laser source 4 and a raster scanning and detection system 5. The system operates in a similar manner to that described above in relation to the hydrocarbon production flow 2, and as presented by the flow diagram of Figure 2. The system 36 is however suited for testing hydrocarbon samples 37 such as the contents of a barrel or an oil spillage. In this way a fingerprint of the sample 37 can be quickly obtained. Thereafter, an identification of the original source of the fluid sample 37 may be made by comparing the characteristic spectral profile or fingerprint obtained with the database 35 of known spectral profiles or fingerprints. This process can be repeated at a later time so as to monitor for the effects of weathering of a hydrocarbon fluid spillage or degradation of the hydrocarbon fluid itself. The above described systems and methods provide an alternative for fingerprinting hydrocarbon fluids. The described techniques are based on absorption spectroscopy rather than fluorescence spectroscopy and as such do not require high sensitive detectors to be employed. Furthermore, the extraction of the relevant data requires simpler signal processing techniques than those generally employed with fluorescence spectroscopy techniques. As a result of the portability of the devices and the speed of data acquisition the system and methods can be employed with a hydrocarbon production fluid so as to provide a means for real time analysis of a production fluid. The described fingerprinting techniques can also be readily employed to determine what type of oil is being analysed, for example distinguishing it from a crude oil source or a refined oil source. The source of the oil being analysed can also be determined by comparing the generated fingerprints with known fingerprints stored in a database. As a result, the fingerprinting techniques can also be used to link samples taken from an oil spillage to a suspected oil source. A method and system for characterising a hydrocarbon fluid is described. The method involves exposing the hydrocarbon fluid to an output field generated by a mid-infrared laser source. The wavelength of the output field is then scanned and the field is scanned over an area of the hydrocarbon fluid so allowing for the absorption of the output field by the hydrocarbon fluid to be measured. From this measured data a characteristic spectral profile or fingerprint of the hydrocarbon fluid can be produced. This spectral profile or fingerprint of the hydrocarbon fluid can then be used to identify the source of the hydrocarbon fluid or monitor for the presence of contaminants or foreign fluids entering the hydrocarbon fluid. The method and system finds particular application for real time monitoring of a hydrocarbon production flow. The foregoing description of the invention has been presented for purposes of illustration and description and is not intended to be exhaustive or to limit the invention to the precise form disclosed. The described embodiments were chosen and described in order to best explain the principles of the invention and its practical application to thereby enable others skilled in the art to best utilise the invention in various embodiments and with various modifications as are suited to the particular use contemplated. Therefore, further modifications or improvements may be incorporated without departing from the scope of the invention as defined by the appended claims.

Claims

Claims 1) A method for characterising a hydrocarbon fluid comprising:
-exposing the hydrocarbon fluid to an output field generated by a mid-infrared laser source;
-scanning a wavelength of the output field;
-measuring an absorption of the scanned output field following its exposure to the hydrocarbon fluid;
-producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption; and
-comparing the produced characteristic spectral profile or fingerprint with those of one or more known characteristic spectral profiles or fingerprints. 2) A method for characterising the source of a hydrocarbon fluid as claimed in claim 1 wherein the comparison of the produced characteristic spectral profile provides a means for identifying a source of the hydrocarbon fluid. 3) A method for characterising the source of a hydrocarbon fluid as claimed in claim 1 wherein the comparison of the produced characteristic spectral profile provides a means for identifying one or more contaminants or foreign fluids entering the hydrocarbon fluid. 4) A method for characterising a hydrocarbon fluid as claimed in any of claims 1 to 3 wherein the output field is exposed to the hydrocarbon fluid by scanning the output field over an area of the hydrocarbon fluid. 5) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the measurement of the absorption comprises the measurement of a back-scatter absorption signal produced by the scanned output field. 6) A method for characterising a hydrocarbon fluid as claimed in any of claims 1 to 4 wherein the measurement of the absorption comprises the measurement of a transmission signal produced by the scanned output field propagating through the hydrocarbon fluid. 7) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the mid-infrared light source comprises an optical parametric device. 8) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the mid-infrared light source comprises an intracavity optical parametric device. 9) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the output field comprises a pulsed field having a pulse repetition frequency of more than 100kHz. 10) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the output field comprises a pulsed field having a pulse repetition frequency of more than 200kHz. 11) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the output field generated by the mid-infrared light source comprises a wavelength between 2 to 6 microns. 12) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the output field generated by the mid-infrared light source comprises a wavelength between 3 to 4 microns. 13) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the output field generated by the mid-infrared light source exhibits a spectral linewidth less than or equal to 5GHz. 14) A method for characterising a hydrocarbon fluid as claimed in any of the preceding claims wherein the hydrocarbon fluid comprises a hydrocarbon production flow. 15) A method for characterising a hydrocarbon fluid as claimed in any of claims 1 to 13 wherein the hydrocarbon fluid is contained within a barrel. 16) A method for characterising a hydrocarbon fluid as claimed in any of claims 1 to 13 wherein the hydrocarbon fluid comprises an hydrocarbon fluid spillage. 17) A system for characterising a hydrocarbon fluid comprising:
-a mid-infrared laser source that provides a means for producing a wavelength scanning output field;
-a scanning and detection system that provides a means for exposing the output field to the hydrocarbon, fluid measuring an absorption of the scanned output field following its exposure to the hydrocarbon, fluid and producing a characteristic spectral profile or fingerprint of the hydrocarbon fluid from the measured absorption -a database of hydrocarbon fluid characteristic spectral profiles or fingerprints. 18) A system for characterising a hydrocarbon fluid as claimed in claim 17 wherein the database provides a means for identifying the source of the hydrocarbon fluid. 19) A system for characterising a hydrocarbon fluid as claimed in claim 17 wherein the database provides a means for identifying one or more contaminants or foreign fluids entering the hydrocarbon fluid.
PCT/GB2013/052958 2012-11-09 2013-11-11 Method for characterising hydrocarbon fluids WO2014072736A1 (en)

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