CN103411879A - High temperature and high pressure dynamic electrochemical test and pH in situ monitoring experimental device - Google Patents
High temperature and high pressure dynamic electrochemical test and pH in situ monitoring experimental device Download PDFInfo
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- CN103411879A CN103411879A CN2013103039615A CN201310303961A CN103411879A CN 103411879 A CN103411879 A CN 103411879A CN 2013103039615 A CN2013103039615 A CN 2013103039615A CN 201310303961 A CN201310303961 A CN 201310303961A CN 103411879 A CN103411879 A CN 103411879A
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Abstract
The invention relates to a high temperature and high pressure dynamic electrochemical test and pH in situ monitoring experimental device. The device includes a high temperature and high pressure reaction kettle, a rotation system, a heating insulation system, an external air supply system, a three-electrode system, a first pH composite electrode system, a second pH composite electrode system, a signal transduction pathway, a control box, an external electrochemical workstation, an external pH instrument and a computer. The device utilizes the high temperature resistance, cold resistance, wear resistance, corrosion resistance, anti-magnetoelectric insulation, oil-free self-lubricating, high rotation speed, high strength and other characteristics of a ceramic bearing, can be used in a severe corrosion environment, and also improves the rotation speed and concentricity precision of a rotary working electrode. A collector ring is employed to realize connection of a moving lead and a static lead. The electrochemical signal of a working electrode under a high temperature and high pressure dynamic state can be tested. A high temperature and high pressure pH composite electrode system is employed to realize in situ continuous monitoring and record the pH change of a solution in the vicinity of the rotary working electrode and a bulk solution. The device can be used for high temperature and high pressure dynamic corrosion behavior and mechanism study.
Description
Technical field
The invention belongs to the corrosion electrochemistry field, the corrosion electrochemical action, the pH that relate to metal material under a kind of dynamic high temperature high pressure corrosion environment affect the experimental provision of rule and mechanism research use.Be applicable to the high temperature pressure corrosion medium in the work of dynamic operation condition condition, be particularly useful for High Temperature High Pressure CO under dynamic condition
2Corrosion electrochemical in-situ signal testing, and the metal material electrochemical reaction is near the pH impact research of solution it.
Background technology
The corrosion of High Temperature High Pressure multiphase medium is a kind of common phenomenon that causes material failure because of the galvanic corrosion effect.For example oil and gas industry exploitation and the corrosion that integrates various pipelines and container in defeated process just with the corrosion of High Temperature High Pressure multiphase medium as main failure forms, relate to corrosive medium and mainly contain CO
2In sour gas and water.Carrying out the corrosion simulated experiment of dynamic high temperature high pressure is corrosion stability and the corrosion mechanism of material under the research flow media, and the important means of estimating and study corrosion inhibiter.Therefore, the device of the dynamic high-temperature and pressure electro-chemical corrosion experiment that can simulate under physical condition must be arranged, and can realize the pH monitoring record of this n-body simulation n solution and near the solution of metal material surface.But under high-temperature and high-pressure conditions, the structures such as dynamic duty electrode, contrast electrode and pH electrode and pressure bearing and seal are had to very high requirement, be not easy to realize the output of electrochemical signals and the monitoring of pH.Usually, after in the dynamic high temperature autoclave, carrying out simulated experiment, then in static synthesis under normal pressure container, carry out electro-chemical test and pH and detect, can not draw the electrochemical behavior in corrosion process under actual conditions and on the impact of material surface pH value of solution.Therefore, the shortage owing to measuring dynamic high-temperature and pressure electro-chemical signal and monitoring pH device, affected the further investigation to the behavior of High Temperature High Pressure Dynamic Corrosion and mechanism.
Summary of the invention
The object of the present invention is to provide a kind of dynamic high-temperature and pressure electro-chemical measurement experimental device, and can realize the continuous monitoring record of this n-body simulation n solution and near the pH value of solution of material surface.Solved in the past and can not measure and monitor the problem that pH changes to corrosion process electrochemical signals under actual conditions, can measure easily the pH value of electrochemical signals and continuous monitoring record two place's solution of sample under dynamic condition.
Technical scheme of the present invention is: a kind of High Temperature High Pressure dynamic electric test chemical and pH in-situ monitoring device, this device comprise high-temperature high-pressure reaction kettle, rotary system, heat tracing system, external air supply system (not showing on figure), three-electrode system, a pH combination electrode system, the 2nd pH combination electrode system, working electrode signal transduction pathway, external control box (not showing on figure), external electro-chemical test instrument (not showing on figure), external pH instrument (not showing on figure) and computing machine (not showing on figure);
Described high-temperature high-pressure reaction kettle consists of high pressure kettle cover, autoclave body, draft tube, escape pipe, pressure transducer, tensimeter and safety valve;
Described rotary system is comprised of magnetic driving equipment, the first ceramic bearing, the second ceramic bearing, metal axle sleeve and turning axle;
Described heat tracing system is for heating to described high-temperature high-pressure reaction kettle, and this system consists of heating and heat-insulating device and temperature sensor;
Described external air supply system is for providing corrosive gas;
Described three-electrode system is comprised of rotary work electrode, the first contrast electrode and auxiliary electrode;
A described pH combination electrode system consists of the 2nd pH electrode and the 3rd contrast electrode;
Described the 2nd pH combination electrode system consists of a pH electrode and the second contrast electrode;
Described working electrode signal transduction pathway consists of conduction stage clip, rotary wire, flange seat, collector ring, flexible circuit conductor and working electrode wire;
Described external electro-chemical test instrument is for gathering and transmit the Electrochemistry Information of rotary work electrode 24, the first contrast electrode 21 and auxiliary electrode 32; Described external pH instrument is used for gathering a described pH combination electrode system (specimen surface) and the 2nd pH combination electrode system (away from the solution of specimen surface) measures the pH value;
Computing machine (on figure show) for the data to described external electrochemical test (demonstration figure on) and external pH instrument to collect (demonstration on figure) record, analyzing and processing and output;
Wherein, described autoclave covers and is provided with the first contrast electrode hole, the second contrast electrode hole, a pH electrode hole, temperature sensor hole, auxiliary electrode hole, the 2nd pH electrode hole, rotary work electrode hole, the 3rd contrast electrode hole, and the two sides of described high pressure kettle cover arrange respectively described draft tube and escape pipe; Described rotary work electrode hole is positioned at the home position of described high pressure kettle cover, described pressure transducer, tensimeter and safety valve are by pipeline and described escape pipe UNICOM, described high pressure kettle cover is connected by fastening bolt with autoclave body, described heating and heat-insulating device is set, described external air supply system and described draft tube UNICOM on the sidewall of described autoclave body;
Described turning axle is arranged on described rotary work electrode hole, the lower end of described turning axle is inserted in described autoclave body affixed by back tightening nut and described teflon fixture, described rotary work electrode is embedded on described teflon fixture, described metal axle sleeve is installed on the upper end of described turning axle by ceramic bearing, described working electrode wire is arranged on and covers by nut and stage clip, described upper cover is arranged on the top of described metal axle sleeve, by gland, fixes institute
Stating magnetic driving equipment installs on described metal axle sleeve, described rotary wire is arranged in described turning axle by insulation crust, described rotary work electrode is connected with described rotary wire one end by the conduction stage clip be arranged in described teflon fixture, described flange seat is by the second fastening bolt, the first insulation spacer and insulated bolt cover are arranged on the top of described turning axle, described electricity ring is arranged on described flange seat, the rotor of described collector ring bottom is connected with the other end of described rotary wire, the stator on described collector ring top is connected with the lower end of the described working electrode wire that is fixed on described metal axle sleeve top by described flexible circuit conductor,
Described temperature sensor is inserted in described autoclave body by described temperature sensor hole, and described the first contrast electrode is installed on the first contrast electrode hole, described auxiliary electrode is installed on the auxiliary electrode hole, described the 2nd pH electrode is installed on the 2nd pH electrode hole, described the 3rd contrast electrode is installed on the 3rd contrast electrode hole, a described pH electrode is installed on a pH electrode hole, described the second contrast electrode is installed on the second contrast electrode hole;
Described external control box is connected with pressure transducer with described magnetic driving equipment, heating and heat-insulating device and temperature sensor by wire, a described pH electrode, the 2nd pH electrode, the second contrast electrode and the 3rd contrast electrode are by wire and described external pH Instrument connection, described working electrode wire, the first contrast electrode and auxiliary electrode are connected with described external electrochemical test by wire, and described external electrochemical test is connected with described computer data by wire with external pH instrument.
Further, this device also comprises the circulating cooling system for cooling rotary system, and this system comprises circulating cooling water pump and cooling water pipe, and described cooling water pipe arranges on described metal axle sleeve, and the water inlet end of described cooling water pipe is connected with described circulating cooling water pump.
Further, described the first contrast electrode, the second contrast electrode and the 3rd contrast electrode are high
Temperature high pressure contrast electrode.
Apparatus of the present invention are used maximum temperature 200 C, top pressure is High Temperature High Pressure Ag/AgCl contrast electrode and the Pt metal auxiliary electrode 32 of 20Mpa, High Temperature High Pressure pH electrode can be according to experimental temperature and pressure selection glass-based pH electrode (temperature 1-80 C, top pressure are 13Mpa) and ZrO
2Base pH electrode (temperature 70-200 C, top pressure are 13Mpa).Use annular test piece when eliminating the sample rotation due to and contrast electrode and auxiliary electrode between solution resistance changes between the electrode that causes of change of distance impact.
The invention has the advantages that: this device adopts the high temperature resistant of ceramic bearing, cold-resistant, wear-resisting, corrosion-resistant, diamagnetic electrical isolation, oil-free self lubrication, high rotating speed, the characteristics such as high strength, can be applied to severe corrosion environment, rotating speed and the concentricity precision of rotary work electrode have also been improved, adopt collector ring to realize the connection of two ends sound wire, can test job electrode High Temperature High Pressure electrochemical signals under dynamically, the pH variation of adopting High Temperature High Pressure pH combination electrode system to realize the original position continuous monitoring and record near the solution of rotary work electrode and bulk solution, can be for the behavior of High Temperature High Pressure Dynamic Corrosion and mechanism research.
The accompanying drawing explanation
Fig. 1 is autoclave superstructure schematic diagram of the present invention.
Fig. 2 is the whole still structural representation along A-A section in Fig. 1 of the present invention.
Fig. 3 is the whole still structural representation along B-B section in Fig. 1 of the present invention.
Fig. 4 is the whole still structural representation along C-C section in Fig. 1 of the present invention.
Fig. 5 is the sectional structure schematic diagram in A district in Fig. 2 of the present invention.
Fig. 6 is the sectional structure schematic diagram in B district in Fig. 2 of the present invention.
In figure:
1. bolt hole, 2. the first contrast electrode hole, 3. the second contrast electrode hole, 4. a pH electrode hole, 5. temperature sensor hole, 6. auxiliary electrode hole, 7. the 2nd pH electrode hole, 8. rotary work electrode hole, 9. the 3rd contrast electrode hole, 10. cooling water pipe, 11. magnetic driving equipment, 12 third high temperature high pressure contrast electrodes, 13. temperature sensor, 14. the first fastening bolt, 15. escape pipe, 16. autoclave heating and heat-insulating device, 17. autoclave body, 18. back tightening nut, 19. ceramic bearing, 20. axle sleeve, 21. the first High Temperature High Pressure contrast electrode, 22. high pressure kettle cover, 23. draft tube, 24. annular test piece, 25. turning axle, 26. the second High Temperature High Pressure contrast electrode, 27. pressure transducer, 28. tensimeter, 29. safety valve, 30. the 2nd pH electrode, a 31. pH electrode, 32. auxiliary electrode, 33. the first nut, 34. insulating mat, 35, gland, 36. the second nut, 37. floating, draw collector ring, 38. flange seat, 39. the first insulation spacer, 40. the second insulation spacer, 41. insulation crust, 42. working electrode wire, 43. stage clip, 44. upper cover, 45. flexible circuit conductor, 46. the second fastening bolt, 47. the 3rd insulation spacer, 48. insulated bolt cover, 49. rotary wire, 50. teflon specimen holder, 51. conduction stage clip.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is described further.
As shown in Figures 1 to 6, the present invention's a kind of High Temperature High Pressure dynamic electric test chemical and pH in-situ monitoring device, this device comprise high-temperature high-pressure reaction kettle, heat tracing system, three-electrode system, a pH combination electrode system, the 2nd pH combination electrode system, working electrode signal transduction pathway, rotary system, external control box, external air supply system, external electro-chemical test instrument, external pH instrument and computing machine;
High-temperature high-pressure reaction kettle by high pressure kettle cover 22, autoclave body 17, draft tube 23, give vent to anger
Three-electrode system is comprised of rotary work electrode 24, the first contrast electrode 21 and auxiliary electrode 32;
Described rotary system is comprised of magnetic driving equipment 11, ceramic bearing 19, metal axle sleeve 20 and turning axle 25;
Described working electrode signal transduction pathway consists of conduction stage clip 51, rotary wire 49, flange seat 38, collector ring 37, flexible circuit conductor 45 and working electrode wire 42;
The one pH combination electrode system the 2nd pH electrode 30 and the 3rd contrast electrode 12 form;
The 2nd pH combination electrode system the one pH electrode 31 and the second contrast electrode 26 form;
External air supply system (showing on figure) is be used to providing corrosive gas;
The heat tracing system is for heating to described high-temperature high-pressure reaction kettle, and this system consists of heating and heat-insulating device 16 and temperature sensor 13;
External electro-chemical test instrument is for gathering and transmit the Electrochemistry Information of rotary work electrode 24, the first contrast electrode 21 and auxiliary electrode 32; Described external pH instrument is used for gathering a described pH combination electrode system (specimen surface) and the 2nd pH combination electrode system (away from the solution of specimen surface) measures the pH value;
Computing machine (on figure show) for the data to described external electrochemical test (demonstration figure on) and external pH instrument to collect (demonstration on figure) record, analyzing and processing and output;
Wherein, described high pressure kettle cover 22 is provided with the first contrast electrode hole 2, the second contrast electrode hole 3, a pH electrode hole 4, temperature sensor hole 5, auxiliary electrode hole 6, the 2nd pH electrode hole 7, rotary work electrode hole 8, the 3rd contrast electrode hole 9, described high pressure kettle cover 22
Two sides described draft tube 23 and escape pipe 15 are set respectively; Described rotary work electrode hole 8 is positioned at the home position of described high pressure kettle cover 22, described pressure transducer 27, tensimeter 28 and safety valve 29 are by pipeline and described escape pipe 15 UNICOMs, described high pressure kettle cover 22 is connected by fastening bolt 14 with autoclave body 17, described heating and heat-insulating device 16 is set, described external air supply system and described draft tube 23 UNICOMs on the sidewall of described autoclave body 17;
Described turning axle 25 is arranged on described rotary work electrode hole 8, insert in described autoclave body 17 lower end of described turning axle 25, and affixed by back tightening nut 18 and described teflon fixture 50, described rotary work electrode 24 is embedded on described teflon fixture 50, described metal axle sleeve 20 is installed on the upper end of described turning axle 25 by ceramic bearing 19, described working electrode wire 42 is arranged on upper cover 4 by nut 33 and stage clip 43, described upper cover 44 is arranged on the top of described metal axle sleeve 20, fixing by gland 35, described magnetic driving equipment 11 is installed on described metal axle sleeve 20, described rotary wire 49 is arranged in described turning axle 25 by insulation crust 41, described rotary work electrode 24 is connected with described rotary wire 49 1 ends by the conduction stage clip 51 be arranged in described teflon fixture 50, described flange seat 38 is by the second fastening bolt 46, the first insulation spacer 39 and insulated bolt cover 48 are arranged on the top of described turning axle 25, described floating draws collector ring 37 to be arranged on described flange seat 38, the rotor of described collector ring 37 bottoms is connected with the other end of described rotary wire 49, the stator on described collector ring 37 tops is connected with the lower end of the described working electrode wire 42 that is fixed on described metal axle sleeve 25 tops by described flexible circuit conductor 45,
Described temperature sensor 13 is inserted in described autoclave body 17 by described temperature sensor hole 5, and described the first contrast electrode 21 is installed on the first contrast electrode hole 2, described auxiliary electrode 32 is installed on auxiliary electrode hole 6, described the 2nd pH electrode 30 is installed the 2nd pH electrode
On hole 7, on described the 3rd contrast electrode 12 installation the 3rd contrast electrode holes 9, on described pH electrode 31 installation the one pH electrode holes 4, on described second contrast electrode 26 installation the second contrast electrode holes 3;
Described external control box is connected with pressure transducer 27 with temperature sensor 13 by the described magnetic driving equipment 11 of wire, heating and heat-insulating device 16, a described pH electrode 31, the 2nd pH electrode 30, the second contrast electrode 26 and the 3rd contrast electrode 12 are by wire and described external pH Instrument connection, described working electrode wire 42, the first contrast electrode 21 and auxiliary electrode 32 are connected with described external electrochemical test by wire, and described external electrochemical test is connected with described computing machine by wire with external pH instrument.
Principle of work of the present invention.Open high pressure kettle cover 22, rotary work electrode 24 is embedded on teflon fixture 50, utilize back tightening nut 18 that teflon fixture 51 is fixed on turning axle 25, rotary work electrode 24 is connected with rotary wire 49 by power spring 51, forms the rotary work electrode of three-electrode system.The first High Temperature High Pressure contrast electrode 21, the second High Temperature High Pressure contrast electrode 26, third high temperature high pressure contrast electrode 9, a pH electrode 31 and the 2nd pH electrode 30 on high pressure kettle cover 22, installed, make probe end and the rotary work electrode 24 of above-mentioned electrode be in the same level line, form a galvanochemistry three-electrode system and two pH composite electrode systems.Simulation medium solution to pouring certain volume in autoclave body 17 into, by the complete submergence of rotary work electrode 24, cover high pressure kettle cover 22, tightens fastening bolt 14.By extraneous air supply system, pass into gas N from draft tube 23
2Deoxygenation is more than 8 hours, after pass into the experimental gas of certain pressure (as CO
2Gas).By external control box, start heating and heat-insulating device 16, in the heating high-pressure still, solution is to setting experimental temperature insulation.Start magnetic driving equipment 11, magnetic driving equipment 11 drives turning axle 25 and presses the setting speed rotation, with
The time open the circulating cooling pump switch, make chilled water along along cooling water pipe 10, circulating, keep turning axle 25 temperature to be in steady state (SS).Pressure and temperature on control box in the demonstration autoclave and the rotating speed of turning axle 25.
The electric signal that rotary work electrode 24 produces sends electrochemical workstation to by rotary wire 49, collector ring 37 and static working electrode wire 42, the first High Temperature High Pressure contrast electrode 21 sends electrochemical workstation with the signal that auxiliary electrode 32 gathers to by wire and is connected, carry out electro-chemical test, as electrokinetic potential polarization curve or ac impedance spectroscopy etc.The 2nd pH electrode 30 passes through T-shaped adapter and pH Instrument connection with the wire that third high temperature high pressure contrast electrode 12 is drawn, near the pH of solution monitoring rotary work electrode 24.The wire that the first High Temperature High Pressure pH electrode 31 and the second High Temperature High Pressure contrast electrode 26 are drawn is by T-shaped adapter and pH Instrument connection, and monitoring is away from the bulk solution pH value of sample.Electrochemical workstation and the external computing machine of pH instrument carry out the functions such as data output, record, processing and analysis.
With preferred embodiment openly as above they are not to limit the present invention although the present invention is own, and the content that protection scope of the present invention should be defined with the application's claim protection domain is as the criterion.Anyly have the knack of the art person, without departing from the spirit and scope of the present invention, various variations and the retouching done, all should belong to protection scope of the present invention.
Claims (1)
1. a High Temperature High Pressure dynamic electric test chemical and pH in-situ monitoring device, it is characterized in that: this device comprises high-temperature high-pressure reaction kettle, rotary system, heat tracing system, external air supply system, three-electrode system, a pH combination electrode system, the 2nd pH combination electrode system, working electrode signal transduction pathway, external control box, external electro-chemical test instrument, external pH instrument and computing machine;
Described high-temperature high-pressure reaction kettle consists of high pressure kettle cover (22), autoclave body (17), draft tube (23), escape pipe (15), pressure transducer (27), tensimeter (28) and safety valve (29);
Described rotary system is comprised of magnetic driving equipment (11), ceramic bearing (19), metal axle sleeve (20) and turning axle (25);
Described heat tracing system is for to described high-temperature high-pressure reaction kettle, heating, and this system consists of heating and heat-insulating device (16) and temperature sensor (13);
Described external air supply system is for providing corrosive gas;
Described three-electrode system is comprised of rotary work electrode (24), the first contrast electrode (21) and auxiliary electrode (32);
A described pH combination electrode system consists of the 2nd pH electrode (30) and the 3rd contrast electrode (12);
Described the 2nd pH combination electrode system consists of a pH electrode (31) and the second contrast electrode (26);
Described working electrode signal transduction pathway consists of conduction stage clip (51), rotary wire (49), flange seat (38), collector ring (37), flexible circuit conductor (45) and working electrode wire (42);
Described external electro-chemical test instrument is for gathering and transmit the Electrochemistry Information of rotary work electrode (24), the first contrast electrode (21) and auxiliary electrode (32); Described external pH instrument is for gathering the pH value in solution away from specimen surface of near the pH value in solution of a described pH combination electrode systematic survey specimen surface and the 2nd pH combination electrode system acquisition;
Described computing machine for the data of described external electrochemical test and external pH instrument to collect are recorded, analyzing and processing and output;
Wherein, described high pressure kettle cover (22) is provided with the first contrast electrode hole (2), the second contrast electrode hole (3), a pH electrode hole (4), temperature sensor hole (5), auxiliary electrode hole (6), the 2nd pH electrode hole (7), rotary work electrode hole (8), the 3rd contrast electrode hole (9), and the two sides of described high pressure kettle cover (22) arrange respectively described draft tube (23) and escape pipe (15); Described rotary work electrode hole (8) is positioned at the home position of described high pressure kettle cover (22), described pressure transducer (27), tensimeter (28) and safety valve (29) are by pipeline and described escape pipe (15) UNICOM, described high pressure kettle cover (22) is connected by fastening bolt (14) with autoclave body (17), described heating and heat-insulating device (16) is set, described external air supply system and described draft tube (23) UNICOM on the sidewall of described autoclave body (17);
Described turning axle (25) is arranged on described rotary work electrode hole (8), the lower end of described turning axle (25) is inserted in described autoclave body (17) affixed by back tightening nut (18) and described teflon fixture (50), described rotary work electrode (24) is embedded on described teflon fixture (50), described metal axle sleeve (20) is installed on the upper end of described turning axle (25) by ceramic bearing (19), described working electrode wire (42) is arranged on upper cover (44) by nut (33) and stage clip (43), described upper cover (44) is arranged on the top of described metal axle sleeve (20), fixing by gland (35), described magnetic driving equipment (11) is installed on described metal axle sleeve (20), described rotary wire (49) is arranged in described turning axle (25) by insulation crust (41), described rotary work electrode (24) is connected with described rotary wire (49) one ends by the conduction stage clip (51) be arranged in described teflon fixture (50), described flange seat (38) is by the second fastening bolt (46), the first insulation spacer (39) and insulated bolt cover (48) are arranged on the top of described turning axle (25), described collector ring (37) is arranged on described flange seat (38), the rotor of described collector ring (37) bottom is connected with the other end of described rotary wire (49), the stator on described collector ring (37) top is connected with the lower end of the described working electrode wire (42) that is fixed on described metal axle sleeve (20) top by described flexible circuit conductor (45),
Described temperature sensor (13) is inserted in described autoclave body (17) by described temperature sensor hole (5), described the first contrast electrode (21) is installed on the first contrast electrode hole (2), described auxiliary electrode (32) is installed on auxiliary electrode hole (6), described the 2nd pH electrode (30) is installed on the 2nd pH electrode hole (7), described the 3rd contrast electrode (12) is installed on the 3rd contrast electrode hole (9), a described pH electrode (31) is installed on a pH electrode hole (4), described the second contrast electrode (26) is installed on the second contrast electrode hole (3),
Described external control box is by wire and described magnetic driving equipment (11), heating and heat-insulating device (16), temperature sensor (13) is connected with pressure transducer (27), a described pH electrode (31), the 2nd pH electrode (30), the second contrast electrode (26) and the 3rd contrast electrode (12) are by wire and described external pH Instrument connection, described working electrode wire (42), the first contrast electrode (21) is connected with described external electrochemical test by wire with auxiliary electrode (32), described external electrochemical test is connected with described computing machine by wire with external pH instrument.
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