CN105651912A - Rock pyrologger and pyrolytic analysis method - Google Patents
Rock pyrologger and pyrolytic analysis method Download PDFInfo
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- CN105651912A CN105651912A CN201511017849.0A CN201511017849A CN105651912A CN 105651912 A CN105651912 A CN 105651912A CN 201511017849 A CN201511017849 A CN 201511017849A CN 105651912 A CN105651912 A CN 105651912A
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- 239000011435 rock Substances 0.000 title claims abstract description 37
- 238000004458 analytical method Methods 0.000 title claims abstract description 36
- 238000000197 pyrolysis Methods 0.000 claims abstract description 77
- 238000001514 detection method Methods 0.000 claims abstract description 30
- 238000004868 gas analysis Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 85
- 229930195733 hydrocarbon Natural products 0.000 claims description 49
- 150000002430 hydrocarbons Chemical class 0.000 claims description 49
- 230000000087 stabilizing effect Effects 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 230000003647 oxidation Effects 0.000 claims description 18
- 238000007254 oxidation reaction Methods 0.000 claims description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 17
- 239000004215 Carbon black (E152) Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 7
- 238000005336 cracking Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 230000004083 survival effect Effects 0.000 claims description 6
- 238000004227 thermal cracking Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 2
- 238000011160 research Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical fields of rock pyrolysis and component analysis and in particular relates to a rock pyrologger and a pyrolytic analysis method. The rock pyrologger is characterized by comprising a pyrolytic detecting system, a gas analysis system connected with the pyrolytic detecting system and a sample residual analysis system connected with the pyrolytic detecting system. According to the rock pyrologger and the pyrolytic analysis method disclosed by the invention, various indicators of S0, S1, S2, S3, S4 and Tmax can be tested at one time by using one sample, and S0, S1 and S2 components can be subdivided; the highest splitting temperature can reach the national standard of 800DEG C; in addition, the rock pyrologger has the advantages of high precision, high stability, high detection precision and high analysis speed; the rock pyrologger can be widely applied to scientific research institutions and oil fields for detection analysis, can adapt to field severe conditions and the like; the blank of domestic instrument of the kind is filled in, and the urgent demand of the domestic scientific research institutions on the instrument is met.
Description
Technical field
The invention belongs to rock pyrolysis and component analysis technical field, especially relate to a kind of rock pyrolysis analysis instrument and pyrolysis analysis method.
Background technology
In petroleum exploration in China process, stratum is timely, accurate, quantitative evaluates the target and requirement that oil gas characteristic is well logging work. In recent years, progress and development along with exploration, the complexity on stratum is also gradually by while cognition, for strengthening especially by the comprehensive of site mud logging data, the data on explored stratum can be analyzed time so with regard to exigence well logging, the oil exploration industry of current China has been carried out decades, and a lot of oil fields all come into or be faced with the stage entering Middle-later Development Stage of Oilfield, and therefore high ripe or post-mature hydrocarbon source rock the investigation and prospecting of each block is paid close attention to by everybody gradually. But rock pyrolysis analysis instrument domestic at present can only record hydrocarbon source rock S0Content, S1Content, S2Content, the highest cracking temperature Tmax value or obtain reservoir rock S0��S11��S21��S22��S23Five indexs, it is impossible to record 300 DEG C of-400 DEG C of carbon dioxide and 300 DEG C of-500 DEG C of carbon monoxides content (the two and be S3Content), hot-vibration sifter (S cannot be carried out simultaneously0+S1) and hydrocarbon thermal cracking (S2) segmentation of component, and the final temperature of pyrolysis is 600 DEG C, it is impossible to meet the requirement of existing national standards " GB/T18602-2012 rock pyrolysis analysis " the highest cracking temperature 800 DEG C, is not suitable for high ripe or post-mature hydrocarbon source rock detection and analyzes.
Summary of the invention
It is an object of the invention to provide a kind of rock pyrolysis analysis instrument and pyrolysis analysis method, once can test out S with one piece of sample0��S1��S2��S3��S4, Tmax indices, and S can be carried out0��S1��S2Component is segmented, and the highest cracking temperature can reach the national standard of 800 DEG C, and its precision is high, degree of stability is high, adapt to field extreme environment.
It is an object of the invention to be realized by following technical proposals:
The rock pyrolysis analysis instrument of the present invention, it is characterised in that include pyrolysis detection system, detect, with this pyrolysis, the gas analysis system that system is connected, detect, with described pyrolysis, the sample survival analysis system that system is connected,
Described pyrolysis detection system includes pyrolysis oven, the gas pipeline I being connected with this pyrolysis oven, and this gas pipeline I fid detector I being connected,
Described gas analysis system includes and the described gas pipeline I gas pipeline II being connected, the gas distribution pipeline I that is respectively connected with this gas pipeline II, gas distribution pipeline II, gas distribution pipeline III and gas shunt conduit IV,
It is successively set on flow stabilizing valve I, the vacuum pump I on described gas distribution pipeline I and carbon monoxide Infrared Detectors,
It is successively set on flow stabilizing valve II, the vacuum pump II on described gas distribution pipeline II and carbon dioxide Infrared Detectors,
It is successively set on the flow stabilizing valve III on described gas distribution pipeline III, vacuum pump III, multiple-way valve I, pressure maintaining valve I, capillary chromatograph I, flow stabilizing valve V and fid detector II, described multiple-way valve I is also associated with quantity tube I, described pressure maintaining valve I is also associated with Pressure gauge I
It is successively set on the flow stabilizing valve IV on described gas distribution pipeline IV, vacuum pump IV, multiple-way valve II, pressure maintaining valve II, capillary chromatograph II, flow stabilizing valve VI and fid detector III, described multiple-way valve II is also associated with quantity tube II, the pressure Table II being also associated with on described pressure maintaining valve II
Described pressure maintaining valve I is arranged on the front end of described capillary chromatograph I,
Described pressure maintaining valve II is arranged on the front end of described capillary chromatograph II,
Described sample survival analysis system includes the oxidation furnace being connected with described pyrolysis oven, is arranged on the oxygen delivery pipeline of this oxidation furnace bottom, the trapping well being connected with described oxidation furnace top, the infrared detector being connected with this trapping well.
The internal heater strip of described pyrolysis oven is the armouring heater strip of heatproof 1000 DEG C.
A kind of pyrolysis analysis method utilizing rock pyrolysis analysis instrument, it is characterised in that its pyrolytic process is as follows:
(1) sample pyrolysis detection
A () pyrolysis oven is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by A in sample (hydrocarbon source rock) evaporate, crack, enter in fid detector I along gas pipeline I, thus detecting the S contained by A in sample (hydrocarbon source rock)0��S1��S2Content and the highest cracking temperature Tmax value;
B () pyrolysis oven is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by B in sample (reservoir rock) evaporate, crack, enter in fid detector I along gas pipeline I, thus detecting the hydro carbons S contained by B in sample (reservoir rock)0��S11��S21��S22��S23Content;
(2) pyrolysis gas detection
A internal sample is being heated in the process of 800 DEG C by () pyrolysis oven, vacuum pump I action, and through flow stabilizing valve I, vacuum pump I, the gas containing hydro carbons information is sent into carbon monoxide Infrared Detectors and then the CO content of 300 DEG C-500 DEG C in detection sample;
B internal sample is being heated in the process of 800 DEG C by () pyrolysis oven, vacuum pump II action simultaneously, and through flow stabilizing valve II, vacuum pump II, the gas containing hydro carbons information is sent into carbon dioxide Infrared Detectors and then the CO of 300 DEG C-400 DEG C in detection sample2Content;
C internal sample is being heated in the process of 300 DEG C by () pyrolysis oven, vacuum pump III action, by the gas containing hydro carbons information through flow stabilizing valve III, vacuum pump III sends into multiple-way valve I, and adsorb in quantity tube I, after specimen temperature is heated to 300 DEG C, multiple-way valve I action, by the air seal that collects in quantity tube I, after sample has heated, multiple-way valve I action again, the gas containing hydro carbons information preserved in quantity tube I is sent in capillary chromatograph I, carrier gas (nitrogen) is through the pressure maintaining valve I of capillary chromatograph I front end, Pressure gauge I enters capillary chromatograph I, carry the gas containing hydro carbons from quantity tube I entrance capillary chromatograph I to flow out from capillary chromatograph I rear end, it is carried along into fid detector II from flow stabilizing valve V through make-up gas (nitrogen), and then the hot-vibration sifter (S contained by detection sample0+S1) component;
D internal sample is being heated to the process of 600 DEG C from 300 DEG C by () pyrolysis oven, vacuum pump IV action, by the gas containing hydro carbons information through flow stabilizing valve IV, vacuum pump IV sends into multiple-way valve II, and adsorb in quantity tube II, after specimen temperature is heated to 600 DEG C, multiple-way valve II action, by the air seal that collects in quantity tube II, after sample has heated, multiple-way valve II action again, the gas containing hydro carbons information preserved in quantity tube II is sent in capillary chromatograph II, carrier gas (nitrogen) is through the pressure maintaining valve II of capillary chromatograph II front end, pressure Table II enters capillary chromatograph II, carry the gas containing hydro carbons from quantity tube II entrance capillary chromatograph II to flow out from capillary chromatograph II rear end, it is carried along into fid detector III from flow stabilizing valve capillary chromatograph II through make-up gas (nitrogen), thus detecting the hydrocarbon thermal cracking (S contained by sample2) component;
(3) residual sample detection
After pyrolysis oven has heated, remaining sample is removed from pyrolysis oven, send in oxidation furnace, oxidized stove heats, and sample is heated to 600 DEG C, and sends into oxygen from the oxygen delivery pipeline of oxidation furnace bottom, making hydro carbons remaining in sample oxidized, the gas after oxidation is (containing CO2) enter in trapping well, low temperature (55 DEG C-65 DEG C) absorption in trapping well, after oxidizing process terminates, trap derrick design to 260 DEG C, make the CO of absorption2Gas enters in infrared detector, thus detecting residual carbon (S in sample4Value) content.
Advantages of the present invention:
The rock pyrolysis analysis instrument of the present invention and pyrolysis analysis method once can test out S with one piece of sample0��S1��S2��S3��S4, Tmax indices, and S can be carried out0��S1��S2Component is segmented, the highest cracking temperature can reach the national standard of 800 DEG C, and its precision is high, degree of stability is high, can be widely applied to Ge great scientific research institutions and each elephant carries out detection and analyzes, there is accuracy of detection height, analyze speed soon, can adapt to the advantages such as field mal-condition, fill up the blank of this quasi-instrument domestic, solve the Domestic Scientific Research institutes eager demand to this quasi-instrument.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Fig. 2 is (S0+S1) the collection of illustrative plates schematic diagram of component.
Fig. 3 is (S2) the collection of illustrative plates schematic diagram of component.
Detailed description of the invention
The specific embodiment of the present invention is further illustrated below in conjunction with accompanying drawing.
As it is shown in figure 1, the rock pyrolysis analysis instrument of the present invention, it is characterised in that include pyrolysis detection system, detect, with this pyrolysis, the gas analysis system that system is connected, detect, with described pyrolysis, the sample survival analysis system that system is connected,
Described pyrolysis detection system includes pyrolysis oven 1, the gas pipeline I2 being connected with this pyrolysis oven, and this gas pipeline I2 fid detector I3 being connected,
Described gas analysis system includes and the described gas pipeline I2 gas pipeline II10 being connected, the gas distribution pipeline I that is respectively connected with this gas pipeline II10, gas distribution pipeline II, gas distribution pipeline III and gas shunt conduit IV,
It is successively set on flow stabilizing valve I4, the vacuum pump I5 on described gas distribution pipeline I and carbon monoxide Infrared Detectors 6,
It is successively set on flow stabilizing valve II7, the vacuum pump II8 on described gas distribution pipeline II and carbon dioxide Infrared Detectors 9,
It is successively set on the flow stabilizing valve III12 on described gas distribution pipeline III, vacuum pump III13, multiple-way valve I11, pressure maintaining valve I16, capillary chromatograph I17, flow stabilizing valve V19 and fid detector II18, described multiple-way valve I11 is also associated with quantity tube I14, described pressure maintaining valve I16 is also associated with Pressure gauge I15
It is successively set on the flow stabilizing valve IV21 on described gas distribution pipeline IV, vacuum pump IV22, multiple-way valve II20, pressure maintaining valve II25, capillary chromatograph II26, flow stabilizing valve VI28 and fid detector III27, described multiple-way valve II20 is also associated with quantity tube II23, the Pressure gauge II24 being also associated with on described pressure maintaining valve II25
Described pressure maintaining valve I16 is arranged on the front end of described capillary chromatograph I17,
Described pressure maintaining valve II25 is arranged on the front end of described capillary chromatograph II26,
Described sample survival analysis system includes the oxidation furnace 29 being connected with described pyrolysis oven, is arranged on the oxygen delivery pipeline of this oxidation furnace 29 bottom, the trapping well 30 being connected with described oxidation furnace 29 top, the infrared detector 31 being connected with this trapping well 30.
The internal heater strip of described pyrolysis oven 1 is the armouring heater strip of heatproof 1000 DEG C.
A kind of pyrolysis analysis method utilizing rock pyrolysis analysis instrument, it is characterised in that its pyrolytic process is as follows:
Embodiment:
(1) sample pyrolysis detection
A () pyrolysis oven 1 is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by A in sample (hydrocarbon source rock) evaporate, crack, enter in fid detector I3 along gas pipeline I2, thus detecting the S contained by A in sample (hydrocarbon source rock)0��S1��S2Content and the highest cracking temperature Tmax value, as shown in table 1;
Table 1
Sample basic parameter
B () pyrolysis oven 1 is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by B in sample (reservoir rock) evaporate, crack, enter in fid detector I3 along gas pipeline I2, thus detecting the hydro carbons S contained by B in sample (reservoir rock)0��S11��S21��S22��S23Content, as shown in table 2;
Table 2
(2) pyrolysis gas detection
A internal sample is being heated in the process of 800 DEG C by () pyrolysis oven 1, vacuum pump I5 action, gas containing hydro carbons information is sent into carbon monoxide Infrared Detectors 6 and then the CO content of 300 DEG C-500 DEG C in detection sample through flow stabilizing valve I4, vacuum pump I5, as shown in table 3;
B internal sample is being heated in the process of 800 DEG C by () pyrolysis oven 1, vacuum pump II8 action simultaneously, gas containing hydro carbons information is sent into carbon dioxide Infrared Detectors 9 and then the CO of 300 DEG C-400 DEG C in detection sample through flow stabilizing valve II7, vacuum pump II82Content, as shown in table 3;
Table 3
C internal sample is being heated in the process of 300 DEG C by () pyrolysis oven 1, vacuum pump III13 action, by the gas containing hydro carbons information through flow stabilizing valve III12, vacuum pump III12 sends into multiple-way valve I11, and adsorb in quantity tube I14, after specimen temperature is heated to 300 DEG C, multiple-way valve I11 action, by the air seal that collects in quantity tube I14, after sample has heated, multiple-way valve I11 action again, the gas containing hydro carbons information preserved in quantity tube I14 is sent in capillary chromatograph I17, carrier gas (nitrogen) is through the pressure maintaining valve I16 of capillary chromatograph I17 front end, Pressure gauge I15 enters capillary chromatograph I17, carry the gas containing hydro carbons from quantity tube I14 entrance capillary chromatograph I17 to flow out from capillary chromatograph I17 rear end, it is carried along into fid detector II18 from flow stabilizing valve V19 through make-up gas (nitrogen), and then the hot-vibration sifter (S contained by detection sample0+S1) component, as shown in Fig. 2 and Biao 4, table 4 is to (S0+S1) component made a concrete analysis of;
Table 4
D internal sample is being heated to the process of 600 DEG C from 300 DEG C by () pyrolysis oven 1, vacuum pump IV22 action, by the gas containing hydro carbons information through flow stabilizing valve IV21, vacuum pump IV22 sends into multiple-way valve II20, and adsorb in quantity tube II23, after specimen temperature is heated to 600 DEG C, multiple-way valve II20 action, by the air seal that collects in quantity tube II23, after sample has heated, multiple-way valve II20 action again, the gas containing hydro carbons information preserved in quantity tube II23 is sent in capillary chromatograph II26, carrier gas (nitrogen) is through the pressure maintaining valve II25 of capillary chromatograph II26 front end, Pressure gauge II24 enters capillary chromatograph II26, carry the gas containing hydro carbons from quantity tube II23 entrance capillary chromatograph II26 to flow out from capillary chromatograph II26 rear end, it is carried along into fid detector III27 from flow stabilizing valve VI28 through make-up gas (nitrogen), and then the hydrocarbon thermal cracking (S contained by detection sample2) component, as shown in fig. 3 and table 5, table 5 is to (S2) component made a concrete analysis of;
Table 5
(3) residual sample detection
After pyrolysis oven 1 has heated, remaining sample is removed from pyrolysis oven 1, send in oxidation furnace 29, oxidized stove 29 heats, sample is heated to 600 DEG C, and send into oxygen from the oxygen delivery pipeline of oxidation furnace 29 bottom, and make hydro carbons remaining in sample oxidized, the gas after oxidation is (containing CO2) enter in trapping well 30, low temperature (55 DEG C-65 DEG C) absorption in trapping well 30, after oxidizing process terminates, trapping well 30 is heated to 260 DEG C, makes the CO of absorption2Gas enters in infrared detector 31, thus detecting residual carbon (S in sample4Value) content, the S of the test of the method1��S2��S4And Tmax is all in same data base, specifically as shown in table 1.
Claims (3)
1. a rock pyrolysis analysis instrument, it is characterised in that include pyrolysis detection system, detect, with this pyrolysis, the gas analysis system that system is connected, detect, with described pyrolysis, the sample survival analysis system that system is connected,
Described pyrolysis detection system includes pyrolysis oven, the gas pipeline I being connected with this pyrolysis oven, and this gas pipeline I fid detector I being connected,
Described gas analysis system includes and the described gas pipeline I gas pipeline II being connected, the gas distribution pipeline I that is respectively connected with this gas pipeline II, gas distribution pipeline II, gas distribution pipeline III and gas shunt conduit IV,
It is successively set on flow stabilizing valve I, the vacuum pump I on described gas distribution pipeline I and carbon monoxide Infrared Detectors,
It is successively set on flow stabilizing valve II, the vacuum pump II on described gas distribution pipeline II and carbon dioxide Infrared Detectors,
It is successively set on the flow stabilizing valve III on described gas distribution pipeline III, vacuum pump III, multiple-way valve I, pressure maintaining valve I, capillary chromatograph I, flow stabilizing valve V and fid detector II, described multiple-way valve I is also associated with quantity tube I, described pressure maintaining valve I is also associated with Pressure gauge I
It is successively set on the flow stabilizing valve IV on described gas distribution pipeline IV, vacuum pump IV, multiple-way valve II, pressure maintaining valve II, capillary chromatograph II, flow stabilizing valve VI and fid detector III, described multiple-way valve II is also associated with quantity tube II, the pressure Table II being also associated with on described pressure maintaining valve II
Described pressure maintaining valve I is arranged on the front end of described capillary chromatograph I,
Described pressure maintaining valve II is arranged on the front end of described capillary chromatograph II,
Described sample survival analysis system includes the oxidation furnace being connected with described pyrolysis oven, is arranged on the oxygen delivery pipeline of this oxidation furnace bottom, the trapping well being connected with described oxidation furnace top, the infrared detector being connected with this trapping well.
2. rock pyrolysis analysis instrument according to claim 1, it is characterised in that the internal heater strip of described pyrolysis oven is the armouring heater strip of heatproof 1000 DEG C.
3. the pyrolysis analysis method utilizing rock pyrolysis analysis instrument, it is characterised in that its pyrolytic process is as follows:
(1) sample pyrolysis detection
A () pyrolysis oven is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by A in sample (hydrocarbon source rock) evaporate, crack, enter in fid detector I along gas pipeline I, thus detecting the S contained by A in sample (hydrocarbon source rock)0��S1��S2Content and the highest cracking temperature Tmax value;
B () pyrolysis oven is heated to 800 DEG C by entering its internal sample from room temperature, make the hydro carbons contained by B in sample (reservoir rock) evaporate, crack, enter in fid detector I along gas pipeline I, thus detecting the hydro carbons S contained by B in sample (reservoir rock)0��S11��S21��S22��S23Content;
(2) pyrolysis gas detection
A internal sample is being heated in the process of 800 DEG C by () pyrolysis oven, vacuum pump I action, and through flow stabilizing valve I, vacuum pump I, the gas containing hydro carbons information is sent into carbon monoxide Infrared Detectors and then the CO content of 300 DEG C-500 DEG C in detection sample;
B internal sample is being heated in the process of 800 DEG C by () pyrolysis oven, vacuum pump II action simultaneously, and through flow stabilizing valve II, vacuum pump II, the gas containing hydro carbons information is sent into carbon dioxide Infrared Detectors and then the CO of 300 DEG C-400 DEG C in detection sample2Content;
C internal sample is being heated in the process of 300 DEG C by () pyrolysis oven, vacuum pump III action, by the gas containing hydro carbons information through flow stabilizing valve III, vacuum pump III sends into multiple-way valve I, and adsorb in quantity tube I, after specimen temperature is heated to 300 DEG C, multiple-way valve I action, by the air seal that collects in quantity tube I, after sample has heated, multiple-way valve I action again, the gas containing hydro carbons information preserved in quantity tube I is sent in capillary chromatograph I, carrier gas (nitrogen) is through the pressure maintaining valve I of capillary chromatograph I front end, Pressure gauge I enters capillary chromatograph I, carry the gas containing hydro carbons from quantity tube I entrance capillary chromatograph I to flow out from capillary chromatograph I rear end, it is carried along into fid detector II from flow stabilizing valve V through make-up gas (nitrogen), and then the hot-vibration sifter (S contained by detection sample0+S1) component;
D internal sample is being heated to the process of 600 DEG C from 300 DEG C by () pyrolysis oven, vacuum pump IV action, by the gas containing hydro carbons information through flow stabilizing valve IV, vacuum pump IV sends into multiple-way valve II, and adsorb in quantity tube II, after specimen temperature is heated to 600 DEG C, multiple-way valve II action, by the air seal that collects in quantity tube II, after sample has heated, multiple-way valve II action again, the gas containing hydro carbons information preserved in quantity tube II is sent in capillary chromatograph II, carrier gas (nitrogen) is through the pressure maintaining valve II of capillary chromatograph II front end, pressure Table II enters capillary chromatograph II, carry the gas containing hydro carbons from quantity tube II entrance capillary chromatograph II to flow out from capillary chromatograph II rear end, it is carried along into fid detector III from flow stabilizing valve capillary chromatograph II through make-up gas (nitrogen), thus detecting the hydrocarbon thermal cracking (S contained by sample2) component;
(3) residual sample detection
After pyrolysis oven has heated, remaining sample is removed from pyrolysis oven, send in oxidation furnace, oxidized stove heats, and sample is heated to 600 DEG C, and sends into oxygen from the oxygen delivery pipeline of oxidation furnace bottom, making hydro carbons remaining in sample oxidized, the gas after oxidation is (containing CO2) enter in trapping well, low temperature (55 DEG C-65 DEG C) absorption in trapping well, after oxidizing process terminates, trap derrick design to 260 DEG C, make the CO of absorption2Gas enters in infrared detector, thus detecting residual carbon (S in sample4Value) content.
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CN110849765A (en) * | 2019-11-19 | 2020-02-28 | 中国石油化工股份有限公司 | Oil sample pollution-free carbonization instrument and application thereof |
CN111610266A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Synchronous experimental analysis method for oil content and fine components of shale |
CN111610267A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Shale oil content and fine component synchronous experimental analysis device |
CN111610265A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Synchronous analysis method for oil content and molecular composition of shale fraction |
CN111678940A (en) * | 2020-06-18 | 2020-09-18 | 中国科学院地质与地球物理研究所 | Compact rock pyrolysis analysis evaluation appearance |
RU223334U1 (en) * | 2023-07-27 | 2024-02-14 | Общество с ограниченной ответственностью "ФИАНУМ ЛАБ" | Device for pyrolytic analysis of rock samples |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3711120A1 (en) * | 1987-04-02 | 1988-10-27 | Wolfgang Guenther Fischer | Fully automatic sample dispenser |
CN1050612A (en) * | 1989-09-28 | 1991-04-10 | 石油勘探开发科学研究院实验中心 | The quantitative analysis method of oil and gas constituents of oil reservoir rock |
CN1158993A (en) * | 1995-10-05 | 1997-09-10 | 法国石油研究所 | Method and device for determining petroleum characteristics of geologic sediments |
CN1376918A (en) * | 2001-03-22 | 2002-10-30 | 海城市石油化工仪器厂 | Gas chromatography for rock pyrolysis |
CN1947008A (en) * | 2004-04-28 | 2007-04-11 | 法国石油研究所 | Method and device for determining oil characteristics of geological sediments |
CN101149363A (en) * | 2007-10-29 | 2008-03-26 | 中国科学院广州地球化学研究所 | Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device |
CN201060200Y (en) * | 2007-06-06 | 2008-05-14 | 海城市石油化工仪器厂 | Oil gas evaluating workstation |
CN101689102A (en) * | 2007-02-16 | 2010-03-31 | 沙特阿拉伯石油公司 | Method for determining volume of organic matter in reservoir rock |
CN102165313A (en) * | 2008-10-29 | 2011-08-24 | Ifp新能源公司 | Method and device for rapidly characterising and quantifying sulphur in sedimentary rocks and petroleum products |
CN205388593U (en) * | 2015-12-30 | 2016-07-20 | 海城市石油化工仪器厂 | Rock pyrolysis analysis appearance |
-
2015
- 2015-12-30 CN CN201511017849.0A patent/CN105651912A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3711120A1 (en) * | 1987-04-02 | 1988-10-27 | Wolfgang Guenther Fischer | Fully automatic sample dispenser |
CN1050612A (en) * | 1989-09-28 | 1991-04-10 | 石油勘探开发科学研究院实验中心 | The quantitative analysis method of oil and gas constituents of oil reservoir rock |
CN1158993A (en) * | 1995-10-05 | 1997-09-10 | 法国石油研究所 | Method and device for determining petroleum characteristics of geologic sediments |
CN1376918A (en) * | 2001-03-22 | 2002-10-30 | 海城市石油化工仪器厂 | Gas chromatography for rock pyrolysis |
CN1947008A (en) * | 2004-04-28 | 2007-04-11 | 法国石油研究所 | Method and device for determining oil characteristics of geological sediments |
CN101689102A (en) * | 2007-02-16 | 2010-03-31 | 沙特阿拉伯石油公司 | Method for determining volume of organic matter in reservoir rock |
CN201060200Y (en) * | 2007-06-06 | 2008-05-14 | 海城市石油化工仪器厂 | Oil gas evaluating workstation |
CN101149363A (en) * | 2007-10-29 | 2008-03-26 | 中国科学院广州地球化学研究所 | Rock sample hydrocarbon generation kinetics high pressure thermal simulation experimental method and device |
CN102165313A (en) * | 2008-10-29 | 2011-08-24 | Ifp新能源公司 | Method and device for rapidly characterising and quantifying sulphur in sedimentary rocks and petroleum products |
CN205388593U (en) * | 2015-12-30 | 2016-07-20 | 海城市石油化工仪器厂 | Rock pyrolysis analysis appearance |
Non-Patent Citations (7)
Title |
---|
ADRIANO MAZZINI ET AL: "Fluid origin, gas fluxes and plumbing system in the sediment-hosted Salton Sea Geothermal System (California, USA)", 《JOURNAL OF VOLCANOLOGY AND GEOTHERMAL RESEARCH》 * |
N. HARTOG ET AL: "Depositional and paleohydrogeological controls on the distribution of organic matter and other reactive reductants in aquifer sediments", 《CHEMICAL GEOLOGY》 * |
中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《中华人民共和国国家标准 GB/T 18602-2012》", 31 December 2012 * |
全杰: "岩石热解仪及其温度程序控制技术", 《石油仪器》 * |
王春丽 主编: "《环境仪器分析》", 30 April 2014 * |
罗万江 等: "油页岩微波热解气态产物析出特性", 《化工进展》 * |
韩方 等: "热解气相色谱分析技术在石油地质中的应用", 《录井技术》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107219245A (en) * | 2017-05-26 | 2017-09-29 | 国家地质实验测试中心 | A kind of hydrocarbon source rock organic carbon pyrolysis analysis apparatus and method |
CN107219245B (en) * | 2017-05-26 | 2023-11-24 | 国家地质实验测试中心 | Organic carbon pyrolysis analysis device for hydrocarbon source rock |
CN110849765A (en) * | 2019-11-19 | 2020-02-28 | 中国石油化工股份有限公司 | Oil sample pollution-free carbonization instrument and application thereof |
CN111610266A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Synchronous experimental analysis method for oil content and fine components of shale |
CN111610267A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Shale oil content and fine component synchronous experimental analysis device |
CN111610265A (en) * | 2020-05-30 | 2020-09-01 | 中国石油天然气股份有限公司 | Synchronous analysis method for oil content and molecular composition of shale fraction |
CN111678940A (en) * | 2020-06-18 | 2020-09-18 | 中国科学院地质与地球物理研究所 | Compact rock pyrolysis analysis evaluation appearance |
CN111678940B (en) * | 2020-06-18 | 2021-06-01 | 中国科学院地质与地球物理研究所 | Compact rock pyrolysis analysis evaluation appearance |
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