US20160195507A1 - Characterization of crude oil and its fractions by fourier transform infrared spectroscopy (ftir) analysis - Google Patents

Characterization of crude oil and its fractions by fourier transform infrared spectroscopy (ftir) analysis Download PDF

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US20160195507A1
US20160195507A1 US14/987,802 US201614987802A US2016195507A1 US 20160195507 A1 US20160195507 A1 US 20160195507A1 US 201614987802 A US201614987802 A US 201614987802A US 2016195507 A1 US2016195507 A1 US 2016195507A1
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crude oil
fourier transform
transform infrared
infrared spectroscopy
indicative
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Omer Refa Koseoglu
Adnan Al-Hajji
Amer A. Al-Tuwailib
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Saudi Arabian Oil Co
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Saudi Arabian Oil Co
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Priority to US14/987,802 priority Critical patent/US20160195507A1/en
Publication of US20160195507A1 publication Critical patent/US20160195507A1/en
Assigned to SAUDI ARABIAN OIL COMPANY reassignment SAUDI ARABIAN OIL COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AL-TUWAILIB, AMER A., AL-HAJJI, ADNAN, KOSEOGLU, OMER REFA
Priority to US16/869,466 priority patent/US10942160B2/en
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    • 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—Raw oil, drilling fluid or polyphasic mixtures
    • 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
    • G01N21/59—Transmissivity
    • 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
    • G01N33/2835—Specific substances contained in the oils or fuels
    • G01N33/2841—Gas in oils, e.g. hydrogen in insulating oils
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106—General arrangement of respective parts
    • G01N2021/0118—Apparatus with remote processing
    • G01N2021/0137—Apparatus with remote processing with PC or the like
    • 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
    • G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

Definitions

  • This invention relates to a method and process for the evaluation of samples of crude oil and its fractions by Fourier transform infrared spectroscopy (FTIR) analysis.
  • FTIR Fourier transform infrared spectroscopy
  • Crude oil originates from the decomposition and transformation of aquatic, mainly marine, living organisms and/or land plants that became buried under successive layers of mud and silt some 15-500 million years ago. They are essentially very complex mixtures of many thousands of different hydrocarbons. Depending on the source, the oil predominantly contains various proportions of straight and branched-chain paraffins, cycloparaffins, and naphthenic, aromatic, and polynuclear aromatic hydrocarbons. These hydrocarbons can be gaseous, liquid, or solid under normal conditions of temperature and pressure, depending on the number and arrangement of carbon atoms in the molecules.
  • Crude oils vary widely in their physical and chemical properties from one geographical region to another and from field to field. Crude oils are usually classified into three groups according to the nature of the hydrocarbons they contain: paraffinic, naphthenic, asphaltic, and their mixtures. The differences are due to the different proportions of the various molecular types and sizes.
  • One crude oil can contain mostly paraffins, another mostly naphthenes. Whether paraffinic or naphthenic, one can contain a large quantity of lighter hydrocarbons and be mobile or contain dissolved gases; another can consist mainly of heavier hydrocarbons and be highly viscous, with little or no dissolved gas.
  • Crude oils can also include heteroatoms containing sulfur, nitrogen, nickel, vanadium and other elements in quantities that impact the refinery processing of the crude oil fractions. Light crude oils or condensates can contain sulfur in concentrations as low as 0.01 W %; in contrast, heavy crude oils can contain as much as 5-6 W %. Similarly, the nitrogen content of crude oils can range from 0.001-1.0 W
  • a naphthenic crude oil will be more suitable for the production of asphaltic bitumen, a paraffinic crude oil for wax.
  • a naphthenic crude oil, and even more so an aromatic one, will yield lubricating oils with viscosities that are sensitive to temperature.
  • modern refining methods there is greater flexibility in the use of various crude oils to produce many desired type of products.
  • a crude oil assay is a traditional method of determining the nature of crude oils for benchmarking purposes. Crude oils are subjected to true boiling point (TBP) distillations and fractionations to provide different boiling point fractions. The crude oil distillations are carried out using the American Standard Testing Association (ASTM) Method D 2892. The common fractions and their nominal boiling points are given in Table 1.
  • crude oil is first fractionated in the atmospheric distillation column to separate sour gas and light hydrocarbons, including methane, ethane, propane, butanes and hydrogen sulfide, naphtha (36-180° C.), kerosene (180-240° C.), gas oil (240-370° C.) and atmospheric residue (>370° C.).
  • the atmospheric residue from the atmospheric distillation column is either used as fuel oil or sent to a vacuum distillation unit, depending on the configuration of the refinery.
  • the principal products obtained from vacuum distillation are vacuum gas oil, comprising hydrocarbons boiling in the range 370-520° C., and vacuum residue, comprising hydrocarbons boiling above 520° C.
  • Crude assay data is conventionally obtained from individual analysis of these cuts to help refiners to understand the general composition of the crude oil fractions and properties so that the fractions can be processed most efficiently and effectively in an appropriate refining unit.
  • Indicative properties are used to determine the engine/fuel performance or usability or flow characteristic or composition. A summary of the indicative properties and their determination methods with description is given below.
  • the cetane number of diesel fuel oil determines the cetane number of diesel fuel oil; as determined in a standard single cylinder test engine; which measures ignition delay compared to primary reference fuels. The higher the cetane number; the easier the high-speed; direct-injection engine will start; and the less white smoking and diesel knock after start-up are.
  • the cetane number of a diesel fuel oil is determined by comparing its combustion characteristics in a test engine with those for blends of reference fuels of known cetane number under standard operating conditions. This is accomplished using the bracketing hand wheel procedure which varies the compression ratio (hand wheel reading) for the sample and each of the two bracketing reference fuels to obtain a specific ignition delay, thus permitting interpolation of cetane number in terms of hand wheel reading.
  • the cloud point determined by the ASTM D2500 method, is the temperature at which a cloud of wax crystals appears when a lubricant or distillate fuel is cooled under standard conditions. Cloud point indicates the tendency of the material to plug filters or small orifices under cold weather conditions.
  • the specimen is cooled at a specified rate and examined periodically. The temperature at which cloud is first observed at the bottom of the test jar is recorded as the cloud point.
  • This test method covers only petroleum products and biodiesel fuels that are transparent in 40 mm thick layers, and with a cloud point below 49° C.
  • the pour point of petroleum products is an indicator of the ability of oil or distillate fuel to flow at cold operating temperatures. It is the lowest temperature at which the fluid will flow when cooled under prescribed conditions. After preliminary heating, the sample is cooled at a specified rate and examined at intervals of 3° C. for flow characteristics. The lowest temperature at which movement of the specimen is observed is recorded as the pour point.
  • the aniline point determined by the ASTM D611 method, is the lowest temperature at which equal volumes of aniline and hydrocarbon fuel or lubricant base stock are completely miscible.
  • a measure of the aromatic content of a hydrocarbon blend is used to predict the solvency of a base stock or the cetane number of a distillate fuel.
  • Specified volumes of aniline and sample, or aniline and sample plus n-heptane, are placed in a tube and mixed mechanically. The mixture is heated at a controlled rate until the two phases become miscible. The mixture is then cooled at a controlled rate and the temperature at which two separate phases are again formed is recorded as the aniline point or mixed aniline point.
  • the octane number is a measure of a fuel's ability to prevent detonation in a spark ignition engine. Measured in a standard single-cylinder; variable-compression-ratio engine by comparison with primary reference fuels. Under mild conditions, the engine measures research octane number (RON), while under severe conditions, the engine measures motor octane number (MON). Where the law requires posting of octane numbers on dispensing pumps, the antiknock index (AKI) is used. This is the arithmetic average of RON and MON, (R+M)/2. It approximates the road octane number, which is a measure of how an average car responds to the fuel.
  • FTIR Fourier transform infrared spectroscopy
  • FTIR Fourier transform infrared spectroscopy
  • the peaks correspond to the frequencies of vibrations of the bonds of the atoms making up the material as the sample molecules selectively absorb radiation of specific wavelengths.
  • the FTIR spectrum represents the molecular vibrational spectrum of the sample, providing a fingerprint of the composition of the material under testing.
  • the FTIR spectrum is characteristic of the structure of the molecule and can be used for identification (qualitative analysis).
  • FTIR is also a good monitoring tool for chemical reactions where functional information about a specific chemical can be obtained.
  • FTIR can also be used for quantitative analysis.
  • the commonly used region for infrared absorption fluorescence spectroscopy is approximately 4000-400 cm ⁇ 1 because most organic compounds absorb IR radiation within this region.
  • This invention discloses a system and method in which FTIR analysis is employed to disclose physical and indicative properties (i.e., cetane number, pour point, cloud point, and aniline point) of gas oil fraction of crude oils, as well as the octane number of the naphtha fraction and the aromaticity of whole crude oils.
  • the invention provides insight into the gas oil properties without fractionation/distillation (crude oil assays) and will help producers, refiners, and marketers to benchmark the oil quality and, as a result, valuate the oils without going thru costly and time consuming crude oil assays. Whereas a conventional crude oil assay method could take up to two months, this invention provides results within one hour.
  • Indicative properties in a crude oil sample e.g., cetane number, pour point, cloud point and aniline point
  • gas oil fraction e.g., cetane number, pour point, cloud point and aniline point
  • octane number of a naptha fraction e.g., octane number of a naptha fraction
  • WCO aromaticity for the whole crude oil
  • the indicative properties provide information about the gas oil and naphtha properties without fractionation/distillation (crude oil assays) and help producers, refiners, and marketers to benchmark the oil quality and, as a result, valuate the oils without performing the customary extensive and time-consuming crude oil assays.
  • FIG. 1 is a graphic plot of typical FTIR data for typical crude oil samples with different API gravities
  • FIG. 2 is a block diagram of a method in which an embodiment of the invention is implemented
  • FIG. 3 is a schematic block diagram of modules of an embodiment of the invention.
  • FIG. 4 is a block diagram of a computer system in which an embodiment of the invention is implemented.
  • a system and a method are provided for determining one or more indicative properties of a hydrocarbon sample.
  • Indicative properties e.g., cetane number, pour point, cloud point, and aniline point
  • the indicative properties provide information about the gas oil and naphtha properties without fractionation/distillation (crude oil assays) and help producers, refiners, and marketers to benchmark the oil quality and, as a result, valuate the oils without performing the customary extensive and time-consuming crude oil assays.
  • the systems and methods are applicable for naturally occurring hydrocarbons derived from crude oils, bitumens, heavy oils, shale oils and from refinery process units including hydrotreating, hydroprocessing, fluid catalytic cracking, coking, and visbreaking or coal liquefaction.
  • FTIR analysis is obtained by a suitable known or to-be-developed process.
  • Fourier transform infrared spectroscopy uses an FTIR spectrophotometer to simultaneously collect spectral data of a solid, liquid, or gas over a wide spectral range.
  • a Fourier transform is employed to convert the raw data into the actual spectrum.
  • the method confers a significant advantage over a dispersive spectrophotometer that measures intensity over a narrow range of wavelengths at a time.
  • a Varian 660-IR (FTIR) spectrophotometer equipped with a Specac's Golden Gate ATR accessory with a diamond crystal was used for the analysis of the crude oil.
  • the background FTIR run was taken against a clean accessory.
  • three drops of crude oil were placed on the diamond crystal and the crystal was covered with a plastic cap to minimize sample evaporation.
  • the instrument was then scanned over the wavelength range from 4000-700 CM ⁇ 1 .
  • FIG. 1 Typical Fourier transform infrared spectroscopy data for crude oils with different API gravities are shown in FIG. 1 .
  • the FTIR index is calculated as follows.
  • the maximum transmittances (maxtrans) are determined for each of a number of crude oils under investigation.
  • FTIRI desired crude maxtrans desired crude ⁇ maxtrans lowest value (1)
  • FIG. 2 shows a process flowchart of steps in a method according to one embodiment herein, in which crude oil samples are prepared and analyzed by FTIR according to the method 200 described below.
  • step 210 a sample of three drops of crude oil is placed via a pipette on the diamond crystal and the crystal was covered with a plastic cap to minimize sample evaporation. No sample dilution or special sample preparation is required. The instrument was then scanned over the wavelength range from 4000-700 CM ⁇ 1 .
  • step 215 the FTIR data is arranged so that maximum transmittances are determined.
  • step 220 an FTIR index (FTIRI) is calculated according to equation (1).
  • the indicative properties (e.g., the cetane number, pour point, cloud point and aniline point) of the gas oil fraction e.g. boiling in the range of 150-400° C. and in certain embodiments in the range of 180-370° C., the octane number of the naphtha fraction, and the aromaticity for the whole crude oil (WCO), can be assigned as a function of the density and the FTIRI of crude oil.
  • Equation (3) is a detailed example of this relationship, showing the cetane number, pour point, cloud point and aniline point that can be predicted for the gas oil (GO) fraction of the crude oil, as well as the aromaticity that can be predicted for the whole crude oil (WCO), as well as the octane number that can be predicted for the naphtha fraction.
  • steps 235 , 240 , 245 , and 250 respectively, the properties of a cetane number, pour point, cloud point and aniline point for the gas oil (GO) fraction of the crude oil are calculated, in step 253 the aromaticity for the whole crude oil (WCO) is calculated, and in step 255 the property of an octane number for the naphtha fraction of the crude oil is calculated. While FIG. 2 shows the steps performed sequentially, they can be performed in parallel or in any order. In certain embodiments, only one or more steps 235 , 240 , 245 , 250 , 253 , 255 are carried out. In these steps, the one or more indicative properties are determined as follows:
  • DEN density of the crude oil sample
  • K, X1-X7 are constants for the properties to be predicted that are developed using linear regression analysis of hydrocarbon data from FTIR.
  • FIG. 3 illustrates a schematic block diagram of modules in accordance with an embodiment of the present invention, system 300 .
  • Density and raw data receiving module 310 receives the density of a sample of crude oil and Fourier transform infrared fluorescence spectroscopy data derived from the crude oil.
  • FTIR index calculation module 315 calculates the Fourier transform infrared spectroscopy index from the FTIR data.
  • Cetane number calculation module 335 derives the cetane number for the gas oil fraction of the crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • Pour point calculation module 340 derives the pour point for the gas oil fraction of the crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • Cloud point calculation module 345 derives the cloud point for the gas oil fraction of the crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • Aniline point calculation module 350 derives the aniline point for the gas oil fraction of the crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • Aromaticity calculation module 352 derives the aromaticity for the whole crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • Octane number calculation module 355 derives the octane number for the naphtha fraction of the crude oil as a function of the Fourier transform infrared spectroscopy index and density of the sample.
  • FIG. 4 shows an exemplary block diagram of a computer system 400 in which one embodiment of the present invention can be implemented.
  • Computer system 400 includes a processor 420 , such as a central processing unit, an input/output interface 430 and support circuitry 440 .
  • a display 410 and an input device 450 such as a keyboard, mouse or pointer are also provided.
  • the display 410 , input device 450 , processor 420 , and support circuitry 440 are shown connected to a bus 490 which also connects to a memory 460 .
  • Memory 460 includes program storage memory 470 and data storage memory 480 .
  • computer system 400 is depicted with direct human interface components display 410 and input device 450 , programming of modules and exportation of data can alternatively be accomplished over the input/output interface 430 , for instance, where the computer system 400 is connected to a network and the programming and display operations occur on another associated computer, or via a detachable input device as is known with respect to interfacing programmable logic controllers.
  • Program storage memory 470 and data storage memory 480 can each comprise volatile (RAM) and non-volatile (ROM) memory units and can also comprise hard disk and backup storage capacity, and both program storage memory 470 and data storage memory 480 can be embodied in a single memory device or separated in plural memory devices.
  • Program storage memory 470 stores software program modules and associated data, and in particular stores a density and raw data receiving module 310 , Fourier transform infrared spectroscopy index calculation module 315 , cetane number calculation module 335 , pour point calculation module 340 , cloud point calculation module 345 , aniline point calculation module 350 , aromaticity calculation module 352 , and octane number calculation module 355 .
  • Data storage memory 480 stores results and other data generated by the one or more modules of the present invention.
  • the computer system 400 can be any computer such as a personal computer, minicomputer, workstation, mainframe, a dedicated controller such as a programmable logic controller, or a combination thereof. While the computer system 400 is shown, for illustration purposes, as a single computer unit, the system can comprise a group of computers which can be scaled depending on the processing load and database size.
  • Computer system 400 preferably supports an operating system, for example stored in program storage memory 470 and executed by the processor 420 from volatile memory.
  • the operating system contains instructions for interfacing computer system 400 to the Internet and/or to private networks.
  • K and X1-X7 was determined using linear regression for the indicative properties cetane number, pour point, cloud point, aniline point, octane number, and aromaticity. These constants were determined based on known actual distillation data for plural crude oil samples and their corresponding indicative properties. These constants are given in Table 3.
  • FTIRI is calculated by comparing the maximum transmittances for a number of crude oils under investigation.
  • the maximum transmittance maxtrans AM 108.797.
  • indicative properties including cetane number, pour point, cloud point, aniline point, and aromaticity can be assigned to the crude oil samples without fractionation/distillation (crude oil assays).
  • the present invention can be implemented as a computer program product for use with a computerized computing system.
  • programs defining the functions of the present invention can be written in any appropriate programming language and delivered to a computer in any form, including but not limited to: (a) information permanently stored on non-writeable storage media (e.g., read-only memory devices such as ROMs or CD-ROM disks); (b) information alterably stored on writeable storage media (e.g., floppy disks and hard drives); and/or (c) information conveyed to a computer through communication media, such as a local area network, a telephone network, or a public network such as the Internet.
  • non-writeable storage media e.g., read-only memory devices such as ROMs or CD-ROM disks
  • writeable storage media e.g., floppy disks and hard drives
  • information conveyed to a computer through communication media such as a local area network, a telephone network, or a public network such as the Internet.
  • the system embodiments can incorporate a variety of computer readable media that comprise a computer usable medium having computer readable code means embodied therein.
  • One skilled in the art will recognize that the software associated with the various processes described can be embodied in a wide variety of computer accessible media from which the software is loaded and activated.
  • the present invention contemplates and includes this type of computer readable media within the scope of the invention.
  • the scope of the present claims is limited to computer readable media, wherein the media is both tangible and non-transitory.

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US10942160B2 (en) 2021-03-09
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