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WO2007033334A2 - Essai de compositions dans un environnement corrosif - Google Patents

Essai de compositions dans un environnement corrosif Download PDF

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Publication number
WO2007033334A2
WO2007033334A2 PCT/US2006/035872 US2006035872W WO2007033334A2 WO 2007033334 A2 WO2007033334 A2 WO 2007033334A2 US 2006035872 W US2006035872 W US 2006035872W WO 2007033334 A2 WO2007033334 A2 WO 2007033334A2
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WO
WIPO (PCT)
Prior art keywords
test
test samples
fluid
samples
exposing
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Application number
PCT/US2006/035872
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English (en)
Other versions
WO2007033334A3 (fr
Inventor
H. Sam Bergh
Stephen Cypes
Damian Hajduk
Zach Hogan
Richard Tiede
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Symyx Technologies, Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Symyx Technologies, Inc filed Critical Symyx Technologies, Inc
Publication of WO2007033334A2 publication Critical patent/WO2007033334A2/fr
Publication of WO2007033334A3 publication Critical patent/WO2007033334A3/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals

Definitions

  • This invention relates to techniques for screening for the effects of exposing samples to a test environment.
  • the invention provides methods and systems implementing techniques for testing how materials respond to environmental exposures, hi general, in one aspect, the invention features methods, apparatus and systems implementing techniques for screening compositions in a test environment.
  • the techniques include positioning one or more test samples in a flow channel, exposing the test samples to a reciprocating flow of a test fluid in the flow channel under controlled wall-shear conditions, and detecting an effect of the exposing on the test samples.
  • Positioning the test samples can include positioning a plurality of different test samples in the flow channel.
  • the plurality of different test samples can differ based on then- constituent materials, coatings and/or surface treatments.
  • the test samples can include one or more metals.
  • the test samples can include one or more coatings or films.
  • the test samples can include one or more materials used in a refinery process.
  • Exposing the test samples can include exposing a surface of each of the one or more test samples to the reciprocating fluid flow. Exposing the test samples can include heating at least a portion of the flow channel.
  • Exposing the test samples can include controlling wall-shear conditions by controlling a pressure within the flow channel, such as by pumping the test fluid using a syringe pump or a diaphragm pump to provide the reciprocating fluid flow.
  • the test fluid can include a crude oil or crude oil fraction.
  • Detecting an effect can include analyzing the test samples - for example, analyzing the test samples for changes in a surface property or weight of the test samples - or analyzing the test fluid - for example, analyzing the test fluid for the presence of elements or ions or a change in pH.
  • Positioning the test samples can include positioning one or more test samples in each of a plurality of flow channels. Exposing the test samples can include exposing the test samples in each the plurality of flow channels to a reciprocating flow of one or more test fluids under controlled pressure conditions. Positioning the test samples can include positioning a different test sample in each of the plurality of flow channels. Exposing the test samples can include exposing the test samples in each of the plurality of flow channels to a reciprocating flow of a different test fluid under controlled pressure conditions.
  • the invention features methods, apparatus and systems implementing techniques for screening compositions in a test environment.
  • the techniques include providing a sample array including a substrate and a plurality of test samples mounted in or on the substrate, providing a fluid array including a plurality of wells, each of the plurality of wells containing a test fluid, immersing the test samples in the fluid array wells to expose a surface of each of the test samples to the test fluids, moving the sample array relative to the fluid array while maintaining a defined relationship between the test sample surfaces and bottom surfaces, and detecting an effect of the moving on the test samples or the test fluids.
  • the sample array can include a plurality of different test samples.
  • the test samples can include one or more metals.
  • the test samples can include one or more coatings or films.
  • the test samples can include one or more materials used in a refinery process.
  • the fluid array can include a plurality of different test fluids.
  • the test fluids can include one or more crude oils or crude oil fractions.
  • One or more side surfaces of the test samples, and the internal surfaces of the array wells, can be coated with one or more inert materials.
  • Moving the sample array relative to the fluid array can include moving the sample array relative to the fluid array while maintaining a defined gap between the test surfaces and the bottom surfaces to create a controlled wall shear stress at the test surface, and detecting can include detecting an effect of the wall shear stress on the test samples.
  • Moving the sample array relative to the fluid array can include moving the sample array relative to the fluid array while maintaining contact between the test surfaces and the bottom surfaces, and detecting can include detecting an effect of friction and/or wear on the test samples.
  • Moving the sample array can include moving the sample array in an orbital pattern about an axis perpendicular to the bottom surfaces of the fluid array. Detecting an effect can include analyzing the test surfaces and/or the test fluids for changes resulting from the moving.
  • the invention features methods, apparatus and systems implementing techniques for screening compositions in a test environment.
  • the techniques include positioning a test sample in a each of a plurality of test cells, depositing a test fluid in each of the plurality of test cells, positioning a shuttle in each of the plurality of test cells, the shuttles defining a flow region along a surface of the test samples, moving each of the shuttles in the corresponding test cells to force a flow of the corresponding test fluid through the flow region, and detecting an effect of the test fluid flow on the test samples.
  • the test samples can include one or more metals.
  • the test samples can include one or more coatings or films.
  • the test samples can include one or more materials used in a refinery process.
  • the test fluid can include a crude oil or crude oil fraction.
  • the techniques can include heating at least a portion of the test cells during the moving.
  • the shuttles can be positioned around the test samples to define the flow region as an annular space around each of the test samples.
  • the shuttles can be moved in a reciprocating motion from a first end of the test cells to a second end of the test cells, and back. Moving the shuttles can include driving the test shuttles by magnetic coupling.
  • Detecting an effect can include analyzing the test samples - for example,analyzing the test samples for changes in a surface property or weight - or analyzing the test fluid - for example, analyzing the test fluid for the presence of elements or ions or a change in pH.
  • a different test fluid and/or a different test sample can be deposited in two or more of the plurality of test cells.
  • the plurality of test cells can include a collection of test cells arranged in a reactor block.
  • the plurality of test cells can include a plurality of collections of test cells, each collection being arranged in one of a plurality of reactor blocks.
  • the test cells can be heated during the screening.
  • the invention features methods, apparatus and systems implementing techniques for screening compositions in a test environment.
  • the techniques include providing an array including a substrate and a plurality of test samples mounted in or on the substrate, each of the test samples having a test surface, exposing the test surface of each of the plurality of test samples to a test environment, and examining the test surface of each of the plurality of test samples by using a profilometry technique to detect changes resulting from exposure to the test environment.
  • the array can include a plurality of test samples each including a different material.
  • the test samples can include a plurality of test samples including the same material.
  • the test samples can include one or more metals.
  • the test samples can include one or more test samples having test surfaces formed by one or more coatings or films.
  • the array can incl ⁇ de one or more standard samples mounted in or on the substrate, and examining the test surfaces includes comparing the test surfaces to standard surfaces. Examining the test surfaces can include comparing the test surfaces to a substrate surface. Exposing the test surface of each of the plurality of test samples to a test environment can include exposing two or more of the plurality of test surfaces to different test environments.
  • Exposing the test surfaces can include exposing the test surfaces to a static or dynamic gas phase or liquid phase environment. Exposing the test surfaces can include stirring a liquid in contact with one or more of the test surfaces. Exposing the test surfaces can include transporting a gas or liquid across one or more of the test surfaces by bulk flow. Exposing the test surfaces includes transporting a gas or liquid across one or more of the test surfaces by reciprocating flow. Exposing the test surfaces can include immersing the test surfaces in the test environment and moving the test surfaces in an orbital motion relative to the test environment. [0013] Examining the test surfaces can include measuring a height difference or a roughness for each of the test samples. Examining the test surfaces can include examining the test surfaces using a optical or contact profilometry. Examining the test surfaces can include examining the test surfaces using atomic force microscopy or scanning electron microscopy.
  • the invention features a system for screening compositions in a test environment.
  • the system includes a flow channel defining a flow path for a test fluid, a sample holder for positioning a test sample in the flow path, a pumping subsystem configured to provide for a reciprocating constant pressure-driven flow past a test sample positioned in the flow path, and a temperature control subsystem configured to heat the test fluid to a desired temperature in a region of the flow channel adjacent to the sample holder.
  • the sample holder can be configured to position a plurality of test samples in the flow channel.
  • the test samples can differ based on their constituent materials, coatings and/or surface treatments.
  • the test samples can include one or more materials used in a refinery process.
  • the pumping subsystem can include a pair of syringe pumps or diaphragm pumps.
  • the test fluid can include a crude oil or crude oil fraction.
  • the system can include an analysis subsystem for detecting an effect of exposure of the test samples to the test fluid.
  • the analysis subsystem can be operable to analyze the test samples for changes resulting from the exposure.
  • the analysis subsystem can include a prof ⁇ lometer.
  • the analysis subsystem can be operable to analyze the test fluid for changes resulting from the exposure.
  • the analysis subsystem can include an inductively coupled plasma spectrometer or an atomic absorption spectrometer.
  • The can include a plurality of flow channels defining flow paths for a plurality of test fluids and a plurality of sample holders for positioning test samples in the plurality of flow paths.
  • the pumping subsystem can be configured to provide for a reciprocating constant pressure-driven flow past test samples positioned in each of the plurality of flow paths. A different test sample and/or a different test fluid can be positioned in two or more of the flow channels.
  • the pumping subsystem can include a pair of syringe pumps or diaphragm pumps in communication with each of the plurality of flow paths.
  • the invention features a system for screening compositions in a test environment.
  • the system includes a fluid array including a plurality of wells, each of the plurality of wells containing a test fluid, a sample array including a substrate and a plurality of test samples mounted in or on the substrate, each of the test samples having a test surface, the test samples being immersed in the fluid array wells to expose the test surfaces to the test fluids, the test samples and fluid array wells being positioned to define a spatial relationship between each test surface and a bottom surface of the corresponding well, a motion subsystem operable to move the sample array relative to the fluid array while maintaining the spatial relationship between the test surfaces and bottom surfaces, and a detector for detecting an effect of the moving on the test samples or the test fluids.
  • the sample array can include a plurality of different test samples.
  • the test samples can include. one or more metals.
  • the test samples can include one or more coatings or films.
  • the test samples can include one or more materials used in a refinery process.
  • the fluid array can include a plurality of different test fluids.
  • the test fluids can include one or more crude oils or crude oil fractions.
  • One or more side surfaces of the test samples, and the internal surface of the test wells, can be coated with one or more inert materials.
  • the motion subsystem can be operable to move the sample array relative to the fluid array while maintaining a defined gap between the test surfaces and the bottom surfaces to create a controlled wall shear stress at the test surface.
  • the motion subsystem can be operable to move the sample array relative to the fluid array while maintaining a contact between the test surfaces and the bottom surfaces to create friction and/or wear at the test surface.
  • the motion subsystem can be operable to move the sample array in an orbital pattern about an axis perpendicular to the bottom surfaces of the fluid array.
  • the system can include an analysis subsystem for detecting an effect of exposure of the test samples to the test fluids.
  • the analysis subsystem can be operable to analyze the test samples for changes resulting from the exposure.
  • the analysis subsystem can include a profilometer.
  • the analysis subsystem can be operable to analyze the test fluid for changes resulting from the exposure.
  • the analysis subsystem can include an inductively coupled plasma spectrometer or an atomic absorption spectrometer.
  • the invention features a system for screening compositions in a test environment.
  • the system includes a reactor block including a plurality of test cells, each of the test cells being configured to receive a test fluid and a test sample, a plurality of shuttles configured to fit in the plurality of test cells, each of the plurality of shuttles being shaped to define, when positioned in one of the plurality of test cells, a flow region along a surface of a test sample positioned in one of the plurality of test cells, each of the plurality of shuttles including a magnet, and a magnetic coupling system for driving the shuttle in a reciprocating motion along a length of the test cell.
  • Particular embodiments can include one or more of the following features.
  • the test samples can include one or more metals.
  • the test samples can include one or more coatings or films.
  • the test samples can include one or more materials used in a refinery process.
  • the test fluid can include a crude oil or crude oil fraction.
  • the system can include a temperature control subsystem configured to heat at least a portion of the test cells.
  • the shuttles define the flow region as an annular space around the corresponding test sample.
  • The includes an analysis subsystem for detecting an effect of exposure of the test samples to the test fluids.
  • the analysis subsystem can be operable to analyze the test samples for changes resulting from the exposure.
  • the analysis subsystem can include a profilometer.
  • the analysis subsystem can be operable to analyze the test fluid for changes resulting from the exposure.
  • the analysis subsystem can include an inductively coupled plasma spectrometer or an atomic absorption spectrometer.
  • Two or more of the plurality of test cells can contain different test fluids and/or different test samples.
  • the plurality of test cells can include a collection of test cells arranged in a reactor block.
  • the plurality of test cells can include a plurality of collections of test cells, where each collection is arranged in one of a plurality of reactor blocks.
  • the invention can be implemented to realize one or more of the following advantages, alone or in the various possible combinations.
  • the methods and systems of the present invention can be implemented using smaller active fluid volumes, and smaller test samples than conventional corrosion modeling techniques. Smaller fluid volumes and smaller test samples can lead to shorter residence times for test fluids at elevated test temperatures, thereby reducing the chances of fluid degradation occurring during testing.
  • the methods and systems of the present invention can be implemented to provide for parallel testing of multiple samples and/or multiple fluids in short times and a relatively small-footprint device.
  • the methods and systems of the present invention are amenable to automation, thereby facilitating development of high-throughput corrosion testing workflows.
  • the methods and systems of the present invention use pressure to control wall shear stress experienced at the surface of a sample under test, which may more accurately correlate to real-world corrosion effects than velocity control used in other techniques.
  • pressure and/or flow path shape it may be possible to accommodate a wide variety of viscosities and flow regimes, such as turbulence and cavitation.
  • multiple material samples can be incorporated in a single fluid flow path.
  • Parallel profilometry screening can be used to assess the corrosion potential of many different test samples, potentially representing many different compositions, in a very short time.
  • Profilometry screening can rapidly provide detailed information about the topography of corrosion effects in two or three dimensions, without requiring sectioning or elaborate preparation of samples for analysis. Only a small amount of each sample, and a small volume of the test fluid, may be needed to get useful corrosion data. Because the substrate and test samples can be physically very compact, and because little sample preparation is required, profilometry screening is amenable to incorporation in a high-throughput device.
  • FIG. 1 is a flow diagram illustrating a general method for performing environmental testing.
  • FIG. 2 is a schematic diagram of one embodiment of a flow channel system for screening compositions in a test environment according to one aspect of the invention.
  • FIGS. 3 A to 3 C are schematic diagrams illustrating embodiments of the system shown in FIG. 2 in more detail.
  • FIG. 4 is a schematic diagram illustrating the analysis of corrosion results using profilometry.
  • FIGS. 5A to 5C are schematic diagrams illustrating an embodiment of an array-based immersion system for screening compositions in a test environment according to one aspect of the invention.
  • FIGS. 6A and 6B are schematic diagrams illustrating an embodiment of a reciprocating shuttle-based system for screening compositions in a test environment according to one aspect of the invention.
  • FIG. 7 is a schematic diagram illustrating one embodiment of a parallel screening system incorporating a plurality of the test cells of FIG. 6 A.
  • FIGS. 8 A and 8B are schematic diagram illustrating a further embodiment of a parallel screening system incorporating a plurality of test cells of FIG. 6A.
  • FIG. 9 is a plot of observed corrosion rate of carbon steel samples in vacuum gas oil fractions of differing total acid number obtained using a multi-well reciprocating shuttle cell screening system as shown in FIG. 7.
  • the invention provides methods and apparatus for use in testing the effects of exposing a plurality of samples in parallel to a test environment.
  • the methods and apparatus may be used in studying transformations that may result from the exposure of solid materials to a test environment.
  • the test samples can include a variety of different materials, including, for example, metals, ceramics, plastics, biomaterials, gels, coatings and films, and can be provided as elemental solids, mixtures, or alloys, optionally including one or more impurities or dopants, and may be treated with one or more surface treatments, which can include treatment with other materials, such as coatings or films, or chemical or physical treatments such as polishing, etching, etc.
  • the test environment typically features one or more test fluids, which can be in liquid or gaseous form.
  • the test fluid can be a single-component fluid, or can be a mixture (including a liquid-gas mixture) of multiple components, hi some embodiments, the test fluid includes a base fluid (which may itself be a mixture of components) and one or more additives - for example, a lubricant or crude oil containing one or more anti- corrosion or anti-wear additives, hi such embodiments, the additives may include one or more additives that are specifically added to the test fluid to affect a process that is under study in the testing.
  • the test environment can also include one or more solid materials.
  • the testing involves contacting the test sample with the test environment, such as by flowing a test fluid over a surface of the test sample, or contacting a surface of the test sample with and moving the surface relative to a test solid, under controlled pressure, temperature, shear rate and/or wall shear stress conditions.
  • the test samples and/or the test environment is/are then examined to detect any effects of the exposure ⁇ in particular, transformations of the test sample and/or a test fluid, such as corrosion of the test sample surface resulting from exposure to a test fluid flow.
  • the test samples and the test environment are selected to represent a real world process.
  • the test samples can include a plurality of structural materials, such as metal alloys that are used in a refinery, and the test environment can include one or more process fluids to which the structural materials are expected to be exposed, such as crude oils or crude oil fractions to which the metal alloys will be exposed in a refinery process.
  • the testing can be implemented to examine the effects of varying environments on a given material or set of materials (e.g., some or all of the test samples can be identical, and the testing can involve exposing a plurality of identical samples to different test environments).
  • the testing can be implemented to examine the performance of different materials in a given environment (e.g., some or all of the test samples can be different, and the testing can involve exposing different test samples to the same test environment).
  • the test samples can be selected to represent equipment used in a particular refinery (e.g., metal alloys such as 1045CS 5 IOlOCS, 5Cr, 9CR, 410SS, 316SS, 317SS, 321SS, 825SS, and Al 06), and the testing can involve examining a variety of different crude oils or crude oil fractions to identify crude oils or fractions that can be advantageously processed in that refinery (or, conversely, to identify crude oils or fractions that should not be processed in the refinery).
  • metal alloys such as 1045CS 5 IOlOCS, 5Cr, 9CR, 410SS, 316SS, 317SS, 321SS, 825SS, and Al 06
  • the testing can involve examining a variety of different crude oils or crude oil fractions to identify crude oils or fractions
  • test samples can include a plurality of new materials (e.g., coatings or surface-treated materials) and the testing can be performed to identify the best performing materials under specified conditions.
  • a general method 100 for testing a plurality of test samples is illustrated in FIG. 1.
  • a plurality of test samples and one or more test fluids are loaded into a test system that includes one or more test cells (step 110).
  • the test samples can include a plurality of different materials, and/or some or all of the test samples can be identical.
  • the test samples can include one or more reference samples that will be used as standards to determine the effect upon one or more other test samples of exposure to the test environment. Each test cell can be loaded with one or more of the test samples.
  • the test samples are exposed to the test environment (step 120).
  • the exposing involves contacting the test samples with a test fluid or fluids in the test environment, such that the test fluid(s) and test samples interact.
  • the interaction typically occurs at a solid-liquid interface, and involves chemical action, whereby a test fluid contains a species that may interact with a surface of a test sample, causing a chemical transformation to the surface (although in some embodiments, the transformation may extend below the test sample surface), or flow action, whereby hydrodynamic or mechanical forces exerted on the surface of a test sample by a test fluid flow may cause removal of material from the test sample surface.
  • test samples and test fluids can interact through either or both of chemical action and/or flow action, hi some embodiments, each test sample may be exposed to identical conditions. Alternatively, some or all of the test samples may be exposed to different conditions, such as different pressures, different temperatures, different shear rates or different wall shear stress. The conditions experienced by individual test samples may be constant or may vary during the testing. [0040] In some embodiments, the test samples are exposed to one or more test fluids (or test solids) under conditions in which the test samples subjected to motion relative to the test fluids (and/or test solids) - for example, conditions under which the test samples are exposed to a flow of the test fluid(s).
  • this can involve exposure of the test samples to test fluid(s) under controlled flow conditions, such as controlled pressure, temperature, shear rate, wall shear stress, or turbulence conditions, hi particular embodiments, this may involve controlling conditions at which phase transitions can/will occur in the test fluid - for example, controlling conditions to avoid (or provide) locals drops in pressure, which can lead to vaporization and/or cavitation or to avoid (or provide) local increases in pressure, which can lead to the formation of crystals in the test fluid or the precipitation of material that is suspended in the test fluid.
  • flow conditions may be controlled to simulate conditions found or expected in a particular real-world system.
  • test samples may be exposed to simple test fluid flows that simulate systems in which the flow field at the test sample surface is well-defined (e.g., flow systems in which shear is defined at every point in the fluid flow) or undefined (e.g., turbulence arising in a high pressure pump).
  • test samples can be exposed to complex flows, such as flows that represent flows that may be encountered in fluid- filled mechanical assemblies, such as power transmission devices (e.g., gear boxes), petrochemical processing and refining equipment, or turbo machinery (e.g., jet engines).
  • the flow field experienced by the test samples in these latter embodiments may be undefined.
  • test samples and/or the test environment is/are analyzed (step 130).
  • This can involve analyzing each of the test samples (or surfaces thereof) to detect chemical or physical changes resulting from the exposure to the test environment.
  • changes can include, for example, the formation of deposits at the test sample surface (e.g., scale or varnish formation, plating), the removal of material from the test sample surface (e.g., corrosion, wear), or chemical or morphological changes to the test sample or test sample surface (e.g., annealing, migration of ions, changes in crystallinity), and can be detected using conventional techniques such as by measuring changes in resistance, weight loss, x-ray analysis, or surface analysis techniques measuring, e.g., changes in surface texture or color.
  • the analysis can involve analyzing the test fluid(s) to detect chemical or physical changes to the fluid(s).
  • changes can include, for example, the addition of material to the test fluid (e.g., the addition of test sample material or degradation products thereof to the test fluid, resulting from corrosion or flaking), the depletion of an additive to the test fluid (e.g., the disappearance of anti-wear additives), or chemical changes in the composition of the test fluid itself, and can be detected using conventional techniques such as using acoustic measurements, chromatography or elemental analysis techniques.
  • a test system 200 suitable for implementing method 100 is generally illustrated in FIG. 2.
  • a test sample 210 is supported on a sample holder 215, such that sample 210 is exposed to a flow path defined by flow channel 220 located in housing 225.
  • Flow channel 220 is in fluidic communication with fluid reservoirs 230 and 235.
  • Reservoirs 230, 235 are in communication with pumps 240 and 245, respectively, which cooperate to generate a reciprocating flow of a test fluid 250 from reservoir 230, through flow channel 220 and across the exposed surface of test sample 210 to reservoir 235, and back again.
  • Housing 225 includes and/or is coupled to temperature control hardware (not shown), and is therefore able to provide heating or cooling in temperature controlled region 255.
  • cooling can be provided in the vicinity of reservoirs 230, 235 to cool test fluid 250 after heating in region 255 (or vice versa), thereby limiting or preventing thermal degradation (e.g., cracking) of test fluid 250 that might result from long residence times at elevated test temperatures.
  • Housing 225 and/or sample holder 215 can be equipped with pressure seals (e.g., elastomeric or graphite gaskets, not shown), which make it possible to maintain elevated (or reduced) pressure within flow channel 220.
  • Test sample 210 can be provided in any desired shape or structure that provides a sufficient surface for testing. Test sample 210 can be grounded to avoid corrosion due to differences in potential between the test sample and other materials that make up sample holder 215, flow channel 220 or housing 225.
  • test sample 210 is mounted on sample holder 215, which is inserted into housing 225 such that test sample 210 is positioned within flow channel 220.
  • Test fluid 250 is loaded into the system, and temperature control region 255 is heated to a desired test temperature.
  • Pumps 240, 245 are activated, and fluid 250 is pumped back and forth between reservoirs 230 and 235 through flow channel 220 and across the surface of test sample 210.
  • After a desired number of cycles (or a desired amount of time), pumps 240 and 245 are deactivated, and sample holder 215 is removed from housing 225.
  • Test sample 210 and/or test fluid 250 is then analyzed to detect corrosion resulting from the flow of test fluid 250 across the test sample surface.
  • system 200 can be operated in combination with robotic sample handlers, automated liquid dispensers, automated analytical instruments, and control software to provide an automated, high-throughput workflow.
  • System 200 is operated under conditions of controlled pressure, temperature, shear rate and/or wall shear stress. It is known that corrosion rate has a better correlation to wall shear stress than other fluid flow properties. Accordingly, in a preferred embodiment system 200 is operated using controlled pressure driven flow rather than controlled displacement, such that the wall shear stress experienced by test sample 210 may be controlled independently of viscosity or temperature, according to the formula:
  • controlled pressure driven flow is provided by using a constant force to a pair of syringe pumps ⁇ e.g., where syringe pump 240 is actively driven and syringe pump 245 responds passively) or a pair of pressure-actuated diaphragm pumps, where the two pumps control the upstream and downstream pressure and the flow results from the pressure difference through flow channel 220.
  • a pair of syringe pumps ⁇ e.g., where syringe pump 240 is actively driven and syringe pump 245 responds passively
  • a pair of pressure-actuated diaphragm pumps where the two pumps control the upstream and downstream pressure and the flow results from the pressure difference through flow channel 220.
  • system 200 can be operated such that test sample 210 and test fluid 250 are exposed to elevated temperature or pressure.
  • temperature controlled region 255 can be heated to a temperature at which test fluid 250 or one or more components thereof undergoes a phase transition, such as a flash vaporization, in flow channel 220 (in which case, pressure changes resulting from the phase change can be controlled by applying appropriate back-pressure to pumps 240 and/or 245.
  • the temperature, pressure, and wall shear conditions can be selected to represent actual or expected conditions in a real-world process.
  • testing can be conducted under more drastic conditions with temperature, pressure, shear rate and wall shear stress elevated above actual or expected levels to provide for accelerated corrosion and/or wear of test sample 210 (thereby decreasing the amount of time required to observe the effects of corrosion and/or wear).
  • a system 300 features a heated reactor block 305, which includes a flow channel 310.
  • Reactor block 305 can be fabricated from a variety of conventional materials, including, for example, metal alloys, ceramics and the like.
  • surfaces exposed to the test environment such as surfaces that form flow channel 310 are formed from (or coated with) materials that are inert to the test environment under study.
  • a sample chamber 315 in block 305 is configured to receive test sample plate 320, positioned directly above and in contact with a channel plate 325, described in more detail in the context of FIG. 3B, below. Chamber 315 is sealed with access plug 330.
  • test sample plate 320 may be mounted on a bottom surface of access plug 330, although in typical embodiments, sample plate 325 is simply placed into chamber 315 on top of channel plate 325.
  • Inlets/outlets 335 provide fluidic communication between flow channel 310 and fluid reservoirs and pumps (not shown) as discussed above.
  • Block 305 also features fluid inlets/outlets 340, which can be used to load test fluid at the start of a test procedure, and to remove test fluid for analysis at the end of the procedure (or, optionally, while the test procedure is underway). Temperature monitoring and control is provided by means of thermocouple connection 345.
  • test sample plate 320 is positioned in reactor block 305 in communication with channel plate 325.
  • test sample plate 320 can be provided as a single, monolithic plate of a desired test material, with a smooth bottom surface (optionally, coated or surface-treated as discussed above).
  • Channel plate 325 is fabricated (by etching, micromachining or other conventional processes) to have a flow channel 350 formed in its upper surface, such that a portion of the bottom surface of test sample plate 320 forms an upper edge of flow channel 350 when test sample plate 320 and channel plate 325 are positioned in sample chamber 315 of reactor block 305. As shown in FIG.
  • channel plate 325 also features inlet/outlet ports 355, which provide for fluid communication between flow channel 350 of channel plate 325 and flow channel 310 in reactor block 305, thereby exposing a portion of the bottom surface of test sample plate 320 to a test fluid flowing in flow channel 310 (and 350).
  • system 300 can include sealing layers (e.g., elastomeric or graphite gaskets) between test sample plate 320 and channel plate 325 and/or between channel plate 325 and reactor block 305 to provide for a fluid-tight seal.
  • System 300 can be implemented to provide for high-throughput testing.
  • high-throughput testing can be achieved by providing for parallel testing of a plurality of test samples.
  • One such parallel testing embodiment featuring a single reactor block configured to support parallel (simultaneous) testing of multiple test samples, is illustrated in FIG. 3C.
  • a sample block 360 includes a substrate supporting ⁇ plurality of test samples 370 exposed at a substrate surface 365.
  • the test samples can be deposited on the surface of sample block 360 (e.g., using chemical or physical vapor deposition, or other surface deposition or coating techniques), or embedded into cavities formed in sample block 360 - for example, by press fitting, soldering, brazing, an adhesive, or the like.
  • a channel plate 375 includes a plurality of channels 380, which each extend through the thickness of and define a flow path along at least a portion of channel plate 375, such that when channel plate 375 is positioned in contact with the surface 365 of sample block 360, each channel 380 is adjacent to one or more of the test samples 370 supported by sample block 360.
  • a distribution plate 385 includes distribution channels 390, which provide for distribution of the test fluid to each channel 380 in channel plate 375. Distribution channels 390 are, in turn, in fluid communication with inlet/outlet ports 397 in base plate 395.
  • Test samples 320, 370 can be fabricated in any desired shape or structure, so long as they provide a surface for testing. Optionally, test samples 370 can be connected to a common ground to avoid corrosion due to differences in potential between test sample materials.
  • one or more sealing layers can be provided between sample block 360, channel plate 380, distribution plate 390, base plate 395 and/or reactor block 305 to provide for a fluid-tight seal.
  • a separate channel plate 375, distribution plate 385 and base plate 395 are shown in FIG. 3C, these plates can be combined in a single channel plate (e.g., plate 325, FIG. 3B), which, for example, may be fabricated from a single layer of material, or as a bonded laminate of layers 380, 390, 385, if desired.
  • sample block 360, channel plate 375, distribution plate 385 and base plate 395 are positioned in sample chamber 315 of reactor block 305, such that inlet/outlet ports 397 are in fluid communication with flow channel 310.
  • a test fluid flowing in flow channel 310 passes through an inlet port 397 in base plate 395, and split into separate flows for each of the channels 380 in channel plate 375 by means of a first distribution channel 390 in distribution plate 385.
  • the separate test fluid flows through channels 380, past test samples 370, and enters the opposite distribution channel 390 in distribution plate 385.
  • distribution channel 390 the separate flows of test fluid are combined, and the combined test fluid re-enters flow channel 310 through the outlet port 397 in base plate 395.
  • the system can be configured such that the test samples 370 associated with each channel 380 in channel plate 375 are exposed to a different test environment by providing separate heat exchangers, flow channels and/or pumps for each channel.
  • This arrangement does, however, increase the mechanical complexity of system 300 (although it should be noted that some variation in test environment conditions - specifically, pressure, shear rate and/or wall shear stress - can be provided by including channels 380 having different geometries in a single channel plate 375, such that the test samples 370 associated with one channel 380 will experience a different test environment than those associated with another channel), and it may be preferable to conduct parallel testing using a plurality of reactor blocks, each of which can be configured to house one or many test samples (e.g., the embodiments of FIG.
  • a multi-reactor block system can be provided, with each reactor block housing a multi-sample block 360 and associated plates 375, 385, 395 (or, alternatively, a single sample plate 320/channel plate 325 combination as in FIG. 3B), and with testing in each block performed under a single set of conditions (i.e., a single test fluid at a single pressure, temperature, shear rate, etc.).
  • the operating conditions for systems 200, 300 are not narrowly critical and will be determined by the particular application.
  • the systems are operated in an inert atmosphere with total liquid volumes (of test fluid) in the range from about 0.1 to about 1.0 ml, at temperatures in the range from about 15O 0 C to about 55O 0 C, pressures in the range from about 1 to about 10 bar, and wall shear stress in the range from about 0 to about 1000 Pascal to provide a measurable corrosion range from about .1 to about 10 mmpy.
  • Test samples and/or test fluids can be analyzed using a variety of different techniques, including electrical or electrochemical measurement in-situ (e.g., EIS, resistance probes, etc.), analysis of the test fluid for corrosion products (e.g., chromatography (GC, HPLC), inductively coupled plasma - mass spectrometry (ICP- MS), inductively coupled plasma - optical emission spectrometry (ICP-OES), atomic absorption spectroscopy (flame AA, graphite furnace AA, hydride-generation AA), or direct measurement of material loss (e.g., profilometry).
  • electrical or electrochemical measurement in-situ e.g., EIS, resistance probes, etc.
  • analysis of the test fluid for corrosion products e.g., chromatography (GC, HPLC), inductively coupled plasma - mass spectrometry (ICP- MS), inductively coupled plasma - optical emission spectrometry (ICP-OES), atomic absorption spectroscopy (flame
  • corrosion product analysis may be preferred.
  • Corrosion product analysis techniques can be robust, offer rapid sample analysis, low detection limits and the possibility of performing autosampling off-line.
  • Profilometry techniques can be used to measure changes in the topography (e.g., height, roughness) of the test sample surface. Suitable techniques include contact profilometry, in which a stylus (e.g., a diamond tipped stylus) is dragged across the test sample surface, and a piezoelectric sensor registers displacement of the stylus in z dimension, or optical profilometry, in which the height (again, in the z dimension) at various points across the test sample surface is measured by interferometry. Both contact and optical techniques can be used to provide measurements in two or three dimensions.
  • profilometry can include microscopy techniques such as scanning electron microscopy and atomic force microscopy. All of these techniques can be readily automated, thus supporting high-throughput workflows.
  • One embodiment of profilometry analysis will now be described in reference to FIG. 4.
  • a plurality of test samples 410 are embedded in a substrate 400 (e.g., sample block 360, FIG. 3C), and planarized to define test sample surfaces 420. The substrate is then exposed to a corrosive environment (e.g., in system 300 as discussed above.
  • the substrate topography is examined using a profilometer, and a measure of corrosion is obtained by measuring the relative height difference ⁇ between the surface 420 of each test sample and a reference surface, which can be the substrate surface 430, or the surface of a reference sample (e.g., a material, such as tantalum, that is not reactive or only weakly reactive in the test environment) embedded in substrate 400.
  • a reference surface e.g., a material, such as tantalum, that is not reactive or only weakly reactive in the test environment
  • the surface roughness of each test sample is also measured and compared to that of the reference surface.
  • the testing can include reciprocating movement of the test fluid back and forth across the test sample surface, as discussed above.
  • the testing can involve immersion of the substrate and test samples in a static or stirred volume of the test fluid, movement of the test fluid across the substrate and sample surfaces by bulk flow, or orbital movement of the substrate and sample surfaces relative to the test fluid to create shear stress at the solid-fluid interface.
  • a grid of through-holes is machined into a substrate of 316 stainless steel. Pins of various alloys are press fit into the holes, and the surface is planarized so that the height difference between the alloys and the surrounding substrate surface is less than 1 micron (as measured by surface contact profilometry).
  • the substrate is attached to a magnetically driven holder.
  • the substrate and holder are immersed in a crude oil with an unknown corrosion ability having a total acid number (TAN) between 0.7 and 6.
  • TAN total acid number
  • the apparatus is heated and magnetically driven to create thermal and shear conditions that mimic those found in crude flow in refinery piping - for example, 4 TAN at 23O 0 C for 24 hours at a series of increasing shear rates.
  • the test sample (pin) surfaces are examined using surface contact profilometry, and are observed to be recessed from the surface of the stainless steel substrate by a few hundred nanometers. The test sample surfaces are also observed to have increased surface roughness or pitting.
  • FIGS. 5A-5C An alternative test system 500 suitable for implementing method 100 is generally illustrated in FIGS. 5A-5C.
  • a multi-well plate 510 is mounted on the bottom surface of a pressure vessel 520.
  • Plate 510 includes a plurality of test wells 530 for receiving one or more test fluids 580.
  • a sample holder 540 is also positioned within pressure vessel 520.
  • a plurality of test samples 550 are mounted in sample holder 550.
  • the test samples are provided as pins or rods that protrude above a surface of sample holder 540, and are arranged in a pattern that is complementary to a pattern of the test wells in well plate 510.
  • Sample holder 540 is positioned within pressure vessel 520 by inverting sample holder 540 and lowering sample holder 540 onto plate 510 such that each of the test sample pins 550 is lowered into a corresponding test well 530.
  • a top surface 560 of each test sample 550 is exposed for testing, as will be described in more detail below. All other surfaces of test samples 550 are treated to render them inert to the test environment - for example, by coating these surfaces with an inert coating 570 (e.g., a ceramic). All exposed surfaces of sample holder 540 and test wells 530 are fabricated from or coated with such an inert material as well. [0060] In operation, pressure vessel 520 is opened, and multi-well plate 510 is positioned within. One or more test fluids 580 are dispensed into test wells 530. Depending on the particular application, the same test fluid 580 can be dispensed to some or all of the test wells 530 in plate 510.
  • test fluids 580 can be dispensed to some or all of the test wells 530.
  • Sample holder 540 is lowered onto plate 510 (as shown in FIG. 5C) such that each test sample 550 is positioned within a corresponding test well 530 with its test surface 560 immersed in the corresponding test fluid 580 at a predetermined distance 590 from the bottom surface of test well 530.
  • Pressure vessel 510 is sealed and, optionally, heated to a desired temperature.
  • a magnetic coupling subsystem (not shown) generates a rotating magnetic field within pressure vessel 510, which drives a cyclical motion of sample holder 540 relative to plate 510.
  • sample holder 540 can be moved in a linear, reciprocating motion relative to plate 510.
  • sample holder 540 can be moved in another pattern, such as a circle, an ellipse, or a more complicated pattern.
  • system 500 is configured such that a predetermined gap 590 is maintained between each test surface 560 and the bottom surface of the corresponding test well 530 throughout the motion of sample holder 540. By controlling the size of gap 590 and the speed of motion, controlled wall- shear stress conditions can be created.
  • test samples 550 and/or test fluids 580 are then analyzed to detect corrosion of the test samples.
  • Test samples 550 can be examined for visual evidence of corrosion (e.g., color change), or using profilometry techniques as discussed above.
  • Test fluids 580 can be analyzed using one or more of the corrosion product screens (e.g., ICP-MS, ICP-OES, GFAA, Flame AA, Hydride-generation AA) discussed above.
  • Sample holder 540 can be configured to hold any number of test samples 550, such as at least 8, at least 64, at least 128, at least 196 or 256 or more test samples (and plate 510 configured to include a corresponding number of test wells 530).
  • some or all of the test samples 550 can be fabricated from identical materials; alternatively, or in addition, some or all of the test samples 550 mounted on sample holder 540 can be different (either in composition, coating, surface treatment, etc.).
  • One or more of the test samples mounted in sample holder 540 can be a reference sample as discussed above.
  • Test samples 550 can be fabricated in with any desired shape or structure, so long as they provide a test surface 560 that can be positioned at the specified distance 590 from the bottom surface of test wells 530.
  • test samples 550 can be connected to a common ground to avoid corrosion due to differences in potential between test sample materials.
  • Two or more systems 500 can be operated together to provide high-throughput testing of test samples in different test environments.
  • system 500 can include robotic sample handling and liquid handling devices and automated analytical instruments to provide for an automated high- throughput workflow operating under computer control.
  • system 500 has been described in the context of corrosion testing with a precisely-defined gap maintained between test surfaces 560 and the bottom surface of test wells 530, the system is also suited for use in friction/wear testing.
  • sample holder 540 is positioned such that test surfaces 560 are in direct contact with the bottom surface of test wells 530. Movement of sample holder 540 relative to plate 510 results in friction between test surfaces 540 and test wells 540. Wear resulting from this friction can be observed using the profilometry and/or fluid analysis techniques discussed above.
  • system 500 can be operated at temperatures ranging from about 150 0 C to about 55O 0 C, at pressures ranging from about 1 to about 10 bar, and at average shear rates from about 0 to about 10,000 /s, with sample volumes in the range from about 150 to about 400 ⁇ l.
  • a temperature-controlled housing 610 includes a central cavity sized and shaped to hold a test cell 620, which includes a test chamber 630.
  • An elongated test sample 640 ⁇ e.g., a 1/16" diameter by 1" long pin) can be positioned in a notch formed in test cell 620 at the bottom of test chamber 630.
  • a shuttle 650 fits into an open end of test chamber 630, forming a flow path along at least a portion of a surface of test sample 640, as will be described in more detail below.
  • a cap 660 covers the open end of test chamber 630, forming a pressure-tight seal when a top portion of housing 610 is coupled to a bottom portion of housing 610.
  • shuttle 650 is formed as a cylindrical solid with a hollow central shaft 670 that is configured to receive a cylindrical test sample 640.
  • Shaft 670 has a larger diameter than test sample 640, such that an annular space is formed around test sample 640 when test sample 640 and shuttle 650 are positioned within test chamber 630.
  • Shuttle 650 includes a magnetic material 680 - in the illustrated embodiment, four magnetic cylinders 680 in sealed channels 690 positioned at regular intervals along the circumference of shuttle 650.
  • Housing 610, test cell 620, shuttle 650 and cap 660 can be fabricated from a variety of different materials. In some embodiments, housing 610 is fabricated from stainless steel, while test cell 620 and shuttle 650 are fabricated from ceramic materials.
  • test cell 620 can be pre-positioned in housing 610, or a test cell 620 can be positioned in a cavity in housing 610 at this time.
  • a test sample 640 is positioned in the notch at the bottom of test chamber 630, and a test fluid is dispensed into test chamber 630.
  • Shuttle 650 is then positioned within test chamber 630, such that test sample 640 extends within shaft 670 of shuttle 650.
  • Cap 660 is placed in position over the open end of test chamber 630, and housing 610 is sealed.
  • Housing 610 is heated to a desired test temperature, and a magnetic coupling subsystem (not shown) generates a magnetic field that drives shuttle 650 from one end of test chamber 630 to the other. As it moves, shuttle 650 displaces the test fluid, which is forced through the annular space and along the exposed surface of test sample 640, thereby creating a wall shear at that surface. The magnetic coupling is reversed, and the shuttle is driven in the opposite direction, back the other end of test chamber 630, again displacing test fluid as it moves. This operation is repeated for the desired duration of the testing, resulting in a reciprocating motion by shuttle 650 within test chamber 630.
  • test sample 640 stress is a function of the size of the gap between shuttle 650 and test sample 650 and, to a lesser extent, the frequency of the shuttle's motion (such that the average stress can be controlled by varying the shuttle frequency).
  • the magnetic coupling is deactivated, and housing 610 is allowed to cool and is unsealed.
  • Test sample 640 and/or the test fluid can be removed from test chamber 630 and analyzed to detect corrosion — for example, by measuring trace metals in the test fluid, by performing profilometry or elemental analysis on the surface of test sample 640, or by measuring mass change of the test sample - using the techniques discussed above.
  • a multi-cell embodiment of system 600 is illustrated in FIG. 7.
  • a system 700 features twelve test cells 710 arranged in temperature-controlled housing 720 in a ring around a central cavity.
  • Test cells 710 and housing 720 are analogous to test cells 620 and housing 610 described in the context of FIGS. 6A and 6B, above.
  • Magnetic coupling assembly 730 includes a disk that houses magnetic material arranged around the circumference of a ring that corresponds to the ring of housing 720.
  • test cells 710 are loaded as described above for test cells 620.
  • each test cell 710 may be loaded with a different combination of test sample and test fluid to provide for simultaneous testing of twelve different sample/fluid pairs.
  • test cells 710 can be loaded with the same test sample and test fluid, in order to provide replicates as a check on the validity of experimental results.
  • housing 720 is sealed and heated to a desired temperature, thus providing a uniform thermal environment for all twelve test cells 710.
  • Magnetic coupling assembly 730 is rotated below housing 720, thus creating a rotating magnetic field that drives the magnetic shuttles within each test cell 710 in a reciprocating motion as described in the context of FIGS. 6A-6B above.
  • the housing is cooled and opened, and the test samples and/or test fluids are removed for analysis as described above.
  • system 800 includes six twelve-cell modules 810 mounted on a base 820.
  • each module 810 includes a twelve-cell unit 700 as described above, positioned within a heater 830, which provides a uniform thermal environment for all of the test cells in the module.
  • An insulation shroud 840 isolates each module from the other modules in the system.
  • System 800 can be operated to provide for a wide variety of test environments in a single multi-channel experiment.
  • each module (or, in some embodiments, each test cell) can be subjected to experimental conditions for a different experiment time.
  • different shuttles e.g., shuttles providing for flow paths of different sizes around the test sample
  • different shear rates can be provided in some or all of the test cells.
  • testing can be performed under an inert atmosphere.
  • test samples can be grounded to avoid corrosion due to differences in potential.
  • multi-cell reactors e.g., 700, FIGS.
  • Typical embodiments of systems 600, 700 and/or 800 can be operated at temperatures in the range from about O 0 C to about 35O 0 C, and at pressures in the range from about 1 to about 50 bar.
  • Tests are typically performed using from about 100 to about 750 ⁇ l of test fluid (with fluids having viscosities in the range from about 1 to about 50 cSt), at wall shear stresses in the range from 0 to about 500 Pa.
  • a process for evaluating the corrosive effect of a refinery feedstock on the metallurgy of one or more refinery processes can be implemented in a system comprising a parallel 96 channel reciprocating shuttle corrosion reactor.
  • the corrosion reactor includes 96 test cells arranged in eight 12-cell metal blocks. Each block includes a two-part housing in the shape of a disc, including a lower portion with indentions for each of the test cells, and provides a uniform thermal environment for all twelve cells in the unit.
  • the test cells are set in the indentions and an upper portion of the housing is pressed against the lower portion to form a seal around each of the test-cell indentions.
  • Each test cell is fabricated from ceramic or ceramic coated stainless steel.
  • the test cell is in the shape of a hollow cylinder, with an indentation for receiving a 1" long by 1/16" diameter metal corrosion coupon along the central axis of the test cell.
  • An annular magnetic shuttle fits within the test cell cylinder and around the metal coupon, such that a defined space exists between the coupon and shuttle. Magnetic coupling is produced by a rotating quadrupole magnetic assembly located directly below the housing.
  • a robotic liquid sample preparation and loading system is used to dispense a known amount (approximately 450 mg) of a test liquid representing, e.g., one of a plurality of different crude distillate fractions, into each cell in the reactor.
  • a test liquid representing, e.g., one of a plurality of different crude distillate fractions
  • each test cell is placed into an indentation in one of the 12-cell reactor block.
  • a metal corrosion coupon and magnetic shuttle are added to each cell. Up to eight such blocks are loaded (such that up to 96 different liquid/metal pairs can be tested) and the blocks are sealed under inert atmosphere.
  • Each block is heated to a predetermined temperature and the magnets associated with each block are rotated to drive the shuttle in each cell.
  • each shuttle causes each shuttle to be alternately repelled or attracted generating a vertical reciprocating motion within each test cell.
  • the magnetic shuttle As the magnetic shuttle is driven from one end of the test cell to the other, it displaces the liquid contained in the cell, forcing the liquid through the narrow annular space between shuttle and pin and generating an alternating high velocity flow.
  • This motion creates a controlled cyclical wall shear stress at the surface of the corrosion coupon simulating shear stress experienced in pipes or other commercial fluid devices.
  • This reciprocating shuttle motion is continued at the set temperature for between 1 and 48 hours.
  • Each reactor block is then opened, and the robotic liquid sample preparation and loading system is used to transfer a sample of each test liquid (approximately 150 mg) to a glass vial and dilute the liquid by a factor of 20 (w/w) with PremiSolv ICP solvent (Conostan/ConocoPhillips Co.).
  • the diluted samples are then heated and mixed.
  • the concentration of one or more elements (e.g., iron) in the diluted test liquid is then determined by inductively coupled plasma - optical emission spectrometry (ICP-OES, IRIS Intrepid II XSP with Cetac auto-sampler, Thermo Electron Corp.).
  • a corrosion index (in mm per year) is calculated for each liquid/metal pair from the measured concentration of corrosion products, which is expected to correlate with long-term corrosion rates for the metal. Results obtained over a 12 hour period at 27O 0 C for a carbon steel test sample in vacuum gas oil at four different Total Acid Number values are shown in FIG. 9.

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Abstract

La présente invention se rapporte à des procédés, à des appareils et à des systèmes permettant de mettre en oeuvre des techniques de criblage de compositions dans un environnement d'essai. L'invention consiste à exposer des échantillons d'essai à un ou plusieurs fluides d'essai dans des conditions contrôlées, et à analyser les échantillons d'essai et/ou les fluides d'essai afin de détecter l'effet de ladite exposition.
PCT/US2006/035872 2005-09-14 2006-09-14 Essai de compositions dans un environnement corrosif WO2007033334A2 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012221673A1 (de) * 2012-11-27 2014-05-28 Humboldt-Universität Zu Berlin Probenhalter für eine Prüfvorrichtung und Verfahren zur Prüfung von Umwelteinflüssen auf eine Probe
EP2743674A1 (fr) * 2012-12-17 2014-06-18 Industrial Technology Research Institute Procédé pour diagnostiquer la corrosion de système de réservoir de stockage souterrain
GB2537837A (en) * 2015-04-27 2016-11-02 Ascott Analytical Equipment Ltd Improvements in or relating to corrosion test cabinets
CN112798519A (zh) * 2020-12-21 2021-05-14 西北工业大学 防腐涂层剩余寿命的评估方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6247542B1 (en) * 1998-03-06 2001-06-19 Baker Hughes Incorporated Non-rotating sensor assembly for measurement-while-drilling applications
US6199437B1 (en) * 1998-03-13 2001-03-13 California Institute Of Technology Apparatus for studying the effects of flow fields imposed on a material during processing

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102012221673A1 (de) * 2012-11-27 2014-05-28 Humboldt-Universität Zu Berlin Probenhalter für eine Prüfvorrichtung und Verfahren zur Prüfung von Umwelteinflüssen auf eine Probe
EP2743674A1 (fr) * 2012-12-17 2014-06-18 Industrial Technology Research Institute Procédé pour diagnostiquer la corrosion de système de réservoir de stockage souterrain
US9194856B2 (en) 2012-12-17 2015-11-24 Industrial Technology Research Institute Method for diagnosing corrosion of underground storage tank system
GB2537837A (en) * 2015-04-27 2016-11-02 Ascott Analytical Equipment Ltd Improvements in or relating to corrosion test cabinets
GB2537837B (en) * 2015-04-27 2018-04-25 Ascott Analytical Equipment Ltd Improvements in or relating to corrosion test cabinets
CN112798519A (zh) * 2020-12-21 2021-05-14 西北工业大学 防腐涂层剩余寿命的评估方法
CN112798519B (zh) * 2020-12-21 2023-07-07 西北工业大学 防腐涂层剩余寿命的评估方法

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