CN103454362A - Online chromatography decompression sample injection device and online chromatography decompression sample injection method - Google Patents
Online chromatography decompression sample injection device and online chromatography decompression sample injection method Download PDFInfo
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- CN103454362A CN103454362A CN2013103700114A CN201310370011A CN103454362A CN 103454362 A CN103454362 A CN 103454362A CN 2013103700114 A CN2013103700114 A CN 2013103700114A CN 201310370011 A CN201310370011 A CN 201310370011A CN 103454362 A CN103454362 A CN 103454362A
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Abstract
The invention discloses an online chromatography decompression sample injection device and an online chromatography decompression sample injection method. The device at least comprises a cavity, an external screw cylinder, an internal screw rod, a movable piston body, a check valve, a visual window, an upper end cover, a lower end support, a gas detecting chromatographic instrument, a vacuum pump, a PVT fluid phase state analyzer, an oil detecting chromatographic instrument sampling bottle, an oil detecting chromatographic instrument, a densimeter, a controller, a pressure sensor, a stepping motor and an electric heater. The method comprises the following steps of vacuumizing the cavity; setting an experimental temperature; injecting a high-pressure formation fluid sample into the cavity; causing the pressure in the cavity to reach 0.5-0.1MPa; introducing an oil product into the oil detecting chromatographic instrument; introducing the oil product into the densimeter; starting the stepping motor so as to rotate the internal screw rod to drive the external screw cylinder to rotate, thus moving the movable piston body to the upper side of the cavity, introducing the gas in the cavity into the gas detecting chromatographic instrument, and stopping the stepping motor. Through device and the method disclosed by the invention, online sampling, online sample transferring and automatic sample loading of the high-pressure formation fluid are realized.
Description
Technical field
The present invention relates to a kind of on-line chromatograph decompression sampling device and method, belong to the resident fluid phase state analysis technical field in the oil-gas field development field.
Background technology
Along with domestic and international new oil gas field constantly is found, formation fluid sample phase state analysis test volume continues to increase.The test analysis project of reservoir fluid sample mainly comprises: flash distillation experiment, differential liberation, constant volume depletion, viscosity test, stratographic analysis, density measurement etc.Main test parameter mainly comprises: the parameters such as output gas oil ratio, volume factor, compressibility coefficient, well stream thing composition, dead oil density, irreducible oil density, formation oil viscosity, this wherein the acquisition of most parameters all be unable to do without and utilize chromatography analysis oil gas to form.
The gas chromatograph of main flow, general admission pressure can not be higher than 1MPa, and inlet hydraulic is normal pressure.In resident fluid phase state analysis process, for the sampling of gaseous sample, be generally after the gases at high pressure step-down in PVT fluid phase state analyser, to adopt the 100mL syringe manually to get gas, then to be injected in chromatograph; For the sampling of fluid sample, be generally by the special-purpose sampling jar of the chromatograph that is injected into 2mL after the highly pressurised liquid step-down in PVT fluid phase state analyser, then put on chromatograph and analyzed.
Yet how conventional resident fluid phase test pressure usually between 25-130MPa, realizes after the resident fluid high-pressure sampling that directly entering the chromatograph analysis is one of this area difficult problem urgently to be resolved hurrily always.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of on-line chromatograph decompression sampling device and method.On-line chromatograph decompression sampling device of the present invention and method can realize that the high pressure of high pressure formation fluid samples, turns online sample, automatic load sample online, can provide strong technical support for the Hi-pot test analysis of reservoir fluid.
For reaching above-mentioned purpose, the invention provides a kind of on-line chromatograph decompression sampling device, it at least comprises:
Cavity, outer silk cylinder, interior leading screw, moveable piston body, ball-and-seat, visual window, upper end cover, lower end holder, survey complexion spectrometer, vacuum pump, PVT fluid phase state analyser, survey oil colours spectrometer sampling jar, survey oil colours spectrometer, densitometer, controller, pressure transducer, stepper motor and electric heater;
Wherein, described outer silk cylinder, moveable piston body and ball-and-seat are positioned at the inside of described cavity, described interior leading screw partly is positioned at the inside of described cavity, described outer leading screw is cannula-like with described interior leading screw and is connected, described interior leading screw vertically runs through described cavity, the two ends of described outer leading screw contact with lower inwall with the upper inwall of described cavity, described moveable piston body be connected with described outer leading screw (being spirally connected), and the two ends of described moveable piston body contact with the both sides inwall of described cavity, described ball-and-seat is positioned on described moveable piston body, described interior leading screw drives described outer leading screw and rotates, described outer leading screw drives described moveable piston body and moves up and down, described moveable piston body is used to gas and the liquid (oil product) in formation fluid sample that the power that enters survey complexion spectrometer and survey the oil colours spectrometer is provided respectively, described ball-and-seat flows (from bottom to top for the gas unidirectional that guarantees formation fluid sample, , approach axis from formation fluid sample flows to the chromatographic direction of survey gas),
Described visual window is positioned at the bottom of the side surface of described cavity, for the amount of the crude oil of observing formation fluid sample;
Described upper end cover is positioned at the top of described cavity, and described lower end restitope is in the bottom of described cavity, and the effect of upper end cover and lower end holder is protection cavity fixing outer leading screw and interior leading screw;
Described survey complexion spectrometer is connected with the top, side of described cavity by pipeline, and be provided with the first valve in this pipeline, this survey complexion spectrometer forms (gas in formation fluid sample enters and surveys the complexion spectrometer by pipeline and the chromatographic syringe of survey gas) for the gas composition of on-line analysis formation fluid sample;
Described vacuum pump is connected with the top, side of described cavity by pipeline, and is provided with the 5th valve in this pipeline, and this vacuum pump is for being vacuumized inside cavity;
Described survey oil colours spectrometer sampling jar is connected with the bottom, side of described cavity by pipeline and threeway with described densitometer, and be provided with the 3rd valve in the pipeline near described cavity, be provided with the 6th valve in the pipeline near described survey oil colours spectrometer sampling jar, in near described densitometric pipeline, being provided with the second valve, described survey oil colours spectrometer sampling jar is arranged in described survey oil colours spectrometer, described survey oil colours spectrometer forms (crude oil in formation fluid sample enters survey oil colours spectrometer by surveying oil colours spectrometer sampling jar) for the oil component of on-line analysis formation fluid sample, described densitometer is for measuring the density of crude oil of formation fluid sample,
Described PVT fluid phase state analyser is connected with the bottom, side of described cavity by pipeline, and be provided with the 4th valve in this pipeline, this PVT fluid phase state analyser is used for the high pressure property of formation testing fluid sample and holds this formation fluid sample (cavity outlet that connects PVT fluid phase state analyser can be positioned at and connect the below of surveying oil colours spectrometer sampling jar and densitometric cavity outlet);
Described pressure transducer is connected in the top, side of described cavity, for measuring and showing the pressure in described cavity;
Described stepper motor is positioned at the bottom of described cavity and is connected with described leading screw, for controlling described interior leading screw, rotates;
Described electric heater is positioned at the bottom of described cavity, is used to described cavity that experimental temperature is provided;
Described controller is connected in described pressure transducer, described stepper motor and described electric heater, for described pressure transducer, described stepper motor and described electric heater are controlled.
In above-mentioned device, preferably, described electric heater is electric heating tube, and it is positioned at the holder of described lower end, to provide heat to cavity better.
In above-mentioned device, preferably, at described upper end cover and described lower end, ask the position contacted with described cavity to be provided with pad; The position contacted with lower inwall with the upper inwall of described cavity at the two ends of described outer leading screw, and the position that the two ends of described moveable piston body contact with the both sides inwall of described cavity is provided with O type circle.Described pad and described O type enclose the effect of seal chamber.Those skilled in the art can also increase the seal members such as pad and O type circle in said apparatus, to strengthen the sealing of cavity.
In the present invention, described survey complexion spectrometer and described survey oil colours spectrometer are the conventional gas chromatograph used in this area, to the method for the composition analysis of the gas composition in formation fluid sample and oil component, can be all the conventional vapor-phase chromatography adopted in this area.
The present invention also provides a kind of on-line chromatograph decompression sample injection method, and it is for adopting above-mentioned on-line chromatograph decompression sampling device to carry out the method for sample introduction, and the method comprises the following steps:
(1), close the first valve, the second valve, the 3rd valve, the 4th valve and the 6th valve, open the 5th valve and start vacuum pump, cavity is vacuumized;
(2) heating-up temperature of, utilizing controller to set electric heater is experimental temperature;
(3), close the first valve, the second valve, the 3rd valve, the 5th valve and the 6th valve, open the 4th valve, high pressure formation fluid sample in PVT fluid phase state analyser is injected in cavity, observe oil product (crude oil) amount visible (the oil product amount of injection can not surpass the top of visual window) of the high pressure formation fluid injected by visual window, close the 4th valve;
(4), remove vacuum pump, open the 5th valve, when the pressure in cavity reaches 0.5-1MPa, close the 5th valve;
(5), open the 3rd valve and the 6th valve, a certain amount of oil product in cavity is entered survey oil colours spectrometer sampling jar and then enters to survey the oil colours spectrometer (when connecting the position of surveying oil colours spectrometer sampling jar and densitometric cavity outlet, oil product is surveyed oil colours spectrometer sampling jar because the pressure differential inside and outside cavity enters when the position of surveying oil colours spectrometer sampling jar; In addition, can also optionally utilize controller control step motor that interior leading screw is rotated, drive outer leading screw and rotate, and then make the moveable piston body to side shifting under cavity, make the interior oil product of cavity enter survey oil colours spectrometer), close the 6th valve;
(6), open the second valve, make a certain amount of oil product enter densitometer (when the position of oil colours spectrometer sampling jar and densitometric cavity outlet is surveyed higher than connection in densitometric position, oil product is because the pressure differential inside and outside cavity enters densitometer), close the second valve and the 3rd valve;
(7), open the first valve, utilize controller control step motor that interior leading screw is rotated, driving outer leading screw rotates, and then to make the moveable piston body move and keep the pressure in cavity to cavity upside (gas one side) be 0.3-0.8MPa, gas in cavity enters surveys the complexion spectrometer, close the first valve after surveying complexion spectrometer demonstration " injecting successfully ", stop stepper motor.
In above-mentioned on-line chromatograph decompression sample injection method, preferably, the time that cavity is vacuumized is 2 hours.
In above-mentioned on-line chromatograph decompression sample injection method, preferably, described experimental temperature is room temperature to 180 ℃.
In above-mentioned on-line chromatograph decompression sample injection method, preferably, the volume that is injected into the high pressure formation fluid sample in cavity is 10-30mL.
In above-mentioned on-line chromatograph decompression sample injection method, preferably, the volume that enters the oil product of surveying oil colours spectrometer sampling jar is 0.5-1mL.
In above-mentioned on-line chromatograph decompression sample injection method, preferably, the volume that enters densitometric oil product is 3-5mL.
The invention provides a kind of on-line chromatograph decompression sampling device and method, these apparatus and method have realized that high pressure samples, turns online sample, automatic load sample online; Save the plenty of time for the Hi-pot test analysis of reservoir fluid, saved a large amount of intermediate link, avoided the interference of personal error and environment; And realized that online survey gas forms, surveys oil and forms, surveys completing continuously of oil density; Also improved the integrated level of experimental technique, for the robotization of reservoir fluid phase measuring technology control provide may, for the Hi-pot test analysis of reservoir fluid provides strong technical support, can serve better field produces.
The accompanying drawing explanation
The structural representation of the on-line chromatograph decompression sampling device that Fig. 1 is embodiment 1.
The primary clustering symbol description:
Interior leading screw 3 moveable piston body 4 ball-and-seat 5 visual windows 6 of 1 outer cylinder of cavity 2
Survey oil colours spectrometer sampling jar 12 densitometer 13 controller 14 pressure transducers 15
The 4th valve 21 the 5th valve 22 the 6th valve 23 is surveyed oil colours spectrometer 24
Embodiment
The present embodiment provides a kind of on-line chromatograph decompression sampling device, and as shown in Figure 1, it at least comprises:
Wherein, described outer silk cylinder 2, moveable piston body 4 and ball-and-seat 5 are positioned at the inside of described cavity 1, described interior leading screw 3 parts are positioned at the inside of described cavity 1, described outer leading screw 2 is cannula-like with described interior leading screw 3 and is connected, described interior leading screw 3 vertically runs through described cavity, the two ends of described outer leading screw 2 contact with lower inwall with the upper inwall of described cavity 1, the position that leading screw 2 contacts with cavity 1 outside is provided with O type circle, described moveable piston body 4 be connected with described outer leading screw 2 (being spirally connected), and the two ends of described moveable piston body 4 contact with the both sides inwall of described cavity 1, the position contacted with cavity 1 at moveable piston body 4 is provided with O type circle, described ball-and-seat 5 is positioned on described moveable piston body 4, described interior leading screw 3 drives described outer leading screw 2 and rotates, described outer leading screw 2 drives described moveable piston body 4 and moves up and down, described moveable piston body 4 is used to the gas in formation fluid sample to provide and enters the power of surveying complexion spectrometer 9, described ball-and-seat 5 flows (from bottom to top for the gas unidirectional that guarantees formation fluid sample, , approach axis from formation fluid sample flows to the direction of surveying complexion spectrometer 9),
Described visual window 6 is positioned at the bottom of the side surface of described cavity 1, for the amount of the crude oil of observing formation fluid sample;
Described upper end cover 7 is positioned at the top of described cavity 1, described lower end holder 8 is positioned at the bottom of described cavity, upper end cover 7 is protection cavity 1 fixing outer leading screw 2 and interior leading screw 3 with the effect of lower end holder 8, at upper end cover 7 and holder 8 positions that are connected with cavity 1, lower end, is provided with pad;
Described survey complexion spectrometer 9 is connected with the top, side of described cavity 1 by pipeline, and is provided with the first valve 18 in this pipeline, and this is surveyed complexion spectrometer 9 gas compositions for the on-line analysis formation fluid sample and forms;
Described vacuum pump 10 is connected with the top, side of described cavity 1 by pipeline, and is provided with the 5th valve 22 in this pipeline, and this vacuum pump 10 is for being vacuumized cavity 1 inside;
Described survey oil colours spectrometer sampling jar 12 is connected with the bottom, side of described cavity 1 by pipeline and threeway with described densitometer 13, and be provided with the 3rd valve 20 in the pipeline near described cavity 1, be provided with the 6th valve 23 in the pipeline near described survey oil colours spectrometer sampling jar 12, be provided with the second valve 19 in the pipeline near described densitometer 13, described survey oil colours spectrometer sampling jar 12 is arranged in described survey oil colours spectrometer 24, described survey oil colours spectrometer 24 oil components for the on-line analysis formation fluid sample form, described densitometer 13 is for the density of the crude oil of measuring formation fluid sample,
Described PVT fluid phase state analyser 11 is connected with the bottom, side of described cavity 1 by pipeline, and be provided with the 4th valve 21 in this pipeline, these PVT fluid phase state analyser 11 high pressure properties for the formation testing fluid sample also hold this formation fluid sample;
Described pressure transducer 15 is connected in the top, side of described cavity 1, for measuring and showing the pressure in described cavity 1;
Described stepper motor 16 is positioned at the bottom of described cavity 1 and is connected with described leading screw 3, for controlling described interior leading screw 3, rotates;
Described electric heating tube 17 is positioned at the lower end holder 8 of described cavity 1 bottom, is used to described cavity 1 that experimental temperature is provided;
Described controller 14 is connected in described pressure transducer 15, described stepper motor 16 and described electric heating tube 17, for described pressure transducer 15, described stepper motor 16 and described electric heating tube 17 are controlled.
The present embodiment provides a kind of on-line chromatograph decompression sample injection method, and its decompression of on-line chromatograph for employing embodiment 1 sampling device carries out the method for sample introduction, and the method comprises the following steps:
(1), close the first valve 18, the second valve 19, the 3rd valve 20, the 4th valve 21 and the 6th valve 23, open the 5th valve 22 and start vacuum pump 10, cavity 1 is carried out vacuumizing in 2 hours;
(2) heating-up temperature of, utilizing controller 14 to set electric heating tube 17 is 30 ℃ of experimental temperatures;
(3), close the first valve 18, the second valve 19, the 3rd valve 20, the 5th valve 22 and the 6th valve 23, open the 4th valve 21, high pressure formation fluid sample in PVT fluid phase state analyser 11 is injected in cavity 1, injection rate IR is 20mL, observe the oil product amount visible (the oil product amount of injection can not surpass the top of visual window 6) of the high pressure formation fluid injected by visual window 6, close the 4th valve 21;
(4), remove vacuum pump 10, open the 5th valve 22, when the pressure in adopts pressure sensor 15 detects cavity 1 reaches 0.6MPa, close the 5th valve 22;
(5), open the 3rd valve 20 and the 6th valve 23, make a certain amount of oil product in cavity 1 enter to survey oil colours spectrometer sampling jar 12 and then enter and survey oil colours spectrometer 24, close the 6th valve 23, the volume that enters the oil product of surveying oil colours spectrometer sampling jar 12 is 0.6mL;
(6), open the second valve 19, utilize the pressure in cavity 1 to make a certain amount of oil product enter densitometer 13, close the second valve 19 and the 3rd valve 20, the volume that enters the oil product of densitometer 13 is 3-5mL;
(7), open the first valve 18, utilize controller 14 control step motors 16 that interior leading screw 3 is rotated, driving outer leading screw 2 rotates, and then to make moveable piston body 4 move and keep the pressure in cavity 1 to cavity 1 upside (gas one side) be 0.65MPa, gas in cavity 1 enters surveys complexion spectrometer 9, close the first valve 18 after surveying 9 demonstrations " injecting successfully " of complexion spectrometer, stop stepper motor 16.
Claims (9)
1. on-line chromatograph decompression sampling device, it at least comprises:
Cavity, outer silk cylinder, interior leading screw, moveable piston body, ball-and-seat, visual window, upper end cover, lower end holder, survey complexion spectrometer, vacuum pump, PVT fluid phase state analyser, survey oil colours spectrometer sampling jar, survey oil colours spectrometer, densitometer, controller, pressure transducer, stepper motor and electric heater;
Wherein, described outer silk cylinder, moveable piston body and ball-and-seat are positioned at the inside of described cavity, described interior leading screw partly is positioned at the inside of described cavity, described outer leading screw is cannula-like with described interior leading screw and is connected, described interior leading screw vertically runs through described cavity, the two ends of described outer leading screw contact with lower inwall with the upper inwall of described cavity, described moveable piston body is connected with described outer leading screw, and the two ends of described moveable piston body contact with the both sides inwall of described cavity, described ball-and-seat is positioned on described moveable piston body, described interior leading screw drives described outer leading screw and rotates, described outer leading screw drives described moveable piston body and moves up and down,
Described visual window is positioned at the bottom of the side surface of described cavity;
Described upper end cover is positioned at the top of described cavity, and described lower end restitope is in the bottom of described cavity;
Described survey complexion spectrometer is connected with the top, side of described cavity by pipeline, and is provided with the first valve in this pipeline;
Described vacuum pump is connected with the top, side of described cavity by pipeline, and is provided with the 5th valve in this pipeline;
Described survey oil colours spectrometer sampling jar is connected with the bottom, side of described cavity by pipeline and threeway with described densitometer, and be provided with the 3rd valve in the pipeline near described cavity, be provided with the 6th valve in the pipeline near described survey oil colours spectrometer sampling jar, in near described densitometric pipeline, being provided with the second valve, described survey oil colours spectrometer sampling jar is arranged in described survey oil colours spectrometer;
Described PVT fluid phase state analyser is connected with the bottom, side of described cavity by pipeline, and is provided with the 4th valve in this pipeline;
Described pressure transducer is connected in the top, side of described cavity, for measuring and showing the pressure in described cavity;
Described stepper motor is positioned at the bottom of described cavity and is connected with described leading screw, for controlling described interior leading screw, rotates;
Described electric heater is positioned at the bottom of described cavity, is used to described cavity that experimental temperature is provided;
Described controller is connected in described pressure transducer, described stepper motor and described electric heater, for described pressure transducer, described stepper motor and described electric heater are controlled.
2. on-line chromatograph according to claim 1 decompression sampling device, wherein, described electric heater is electric heating tube, and it is positioned at the holder of described lower end.
3. on-line chromatograph decompression sampling device according to claim 1 and 2, wherein, ask the position contacted with described cavity to be provided with pad at described upper end cover and described lower end; The position contacted with lower inwall with the upper inwall of described cavity at the two ends of described outer leading screw, and the position that the two ends of described moveable piston body contact with the both sides inwall of described cavity is provided with O type circle.
4. on-line chromatograph decompression sample injection method, it is for adopting the described on-line chromatograph decompression of claim 1-3 any one sampling device to carry out the method for sample introduction, and the method comprises the following steps:
(1), close the first valve, the second valve, the 3rd valve, the 4th valve and the 6th valve, open the 5th valve and start vacuum pump, cavity is vacuumized;
(2) heating-up temperature of, utilizing controller to set electric heater is experimental temperature;
(3), close the first valve, the second valve, the 3rd valve, the 5th valve and the 6th valve, open the 4th valve, high pressure formation fluid sample in PVT fluid phase state analyser is injected in cavity, the oil product amount of observing the high pressure formation fluid injected by visual window is visible, closes the 4th valve;
(4), remove vacuum pump, open the 5th valve, when the pressure in cavity reaches 0.5-1MPa, close the 5th valve;
(5), open the 3rd valve and the 6th valve, make a certain amount of oil product in cavity enter to survey oil colours spectrometer sampling jar and then enter and survey the oil colours spectrometer, close the 6th valve;
(6), open the second valve, make a certain amount of oil product enter densitometer, close the second valve and the 3rd valve;
(7), open the first valve, utilize controller control step motor that interior leading screw is rotated, driving outer leading screw rotates, and then make the moveable piston body to side shifting on cavity and to keep the pressure in cavity be 0.3-0.8MPa, gas in cavity enters surveys the complexion spectrometer, close the first valve after surveying complexion spectrometer demonstration " injecting successfully ", stop stepper motor.
5. on-line chromatograph according to claim 4 decompression sample injection method, wherein, the time that cavity is vacuumized is 2 hours.
6. on-line chromatograph according to claim 4 decompression sample injection method, wherein, described experimental temperature is room temperature to 180 ℃.
7. on-line chromatograph according to claim 4 decompression sample injection method, wherein, the volume that is injected into the high pressure formation fluid sample in cavity is 10-30mL.
8. on-line chromatograph according to claim 4 decompression sample injection method, wherein, the volume that enters the oil product of surveying oil colours spectrometer sampling jar is 0.5-1mL.
9. on-line chromatograph according to claim 4 decompression sample injection method, wherein, the volume that enters densitometric oil product is 3-5mL.
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