CN109540735A - A kind of shale gas-bearing property comprehensive analysis device and its method - Google Patents
A kind of shale gas-bearing property comprehensive analysis device and its method Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
- G01N7/16—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
-
- 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
-
- 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
- G01N30/66—Thermal conductivity detectors
-
- 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
Abstract
The present invention relates to a kind of shale gas-bearing property comprehensive analysis devices, including air content test cell, hydrocarbon gas component analysis unit, inorganic gas component analysis unit and operation control unit；The invention also discloses the shale gas-bearing property comprehensive analysis methods based on the device.Technical solution of the present invention realizes while shale gas drill site carries out air content parsing test to shale core, resolution gas gas composition and its technical solution of variation in on-line analysis and monitoring resolving, it can effectively improve the reliability and timeliness of test data, the implementation of shale gas exploration and development engineering is preferably served, provides more scientific, more reliable gas-bearing property data for shale gas resource exploration and evaluation.
Description
Technical field
The present invention relates to oil-gas exploration and development technical fields, and in particular to a kind of shale gas-bearing property comprehensive analysis device and its
Method is a set of while carrying out air content parsing test to shale core, is parsed in on-line analysis and monitoring resolving
Gas gas composition and its technical solution of variation.
Background technique
Shale gas-bearing property is the key parameter of shale gas resource assessment, and the quality of test data is directly related to shale
The reliability standard of gas resource assessment result.The test of shale gas-bearing property includes both sides content: first is that the gassiness of measurement shale
Amount, second is that measuring the content of each gas component in shale gas.This two parts test at present be different time and place respectively into
Capable, i.e., parsing test is carried out to shale Gas content in drill site first, collect resolution gas gas, then in fixed laboratory
The interior gas component to collected resolution gas is analyzed.This test mode has the following deficiencies: first is that different time, no
Chemical component with the resolution gas gaseous sample of resolution phase collection forms not fully, and gas composition analysis result cannot
Accurately reflect the true chemical composition of shale gas；Second is that saving improper and resting period in sample transportational process too long will cause gas
Bulk diffusion and change of component, lead to test error；Third is that gas-composition data cannot be provided to Field Force in time, it is unfavorable for existing
Field engineering decision.
The patent application having application No. is 201410406372.4 being worth mentioning in terms of shale gas-bearing property comprehensive analysis
It discloses a kind of unconventional reservoir rock nano adsorption gas extraction element and extracts and hydrocarbon analysis method comprising the steps of:
1) it is nanoscale by the closed partial size that is crushed to of rock core, obtains nanometric sample；2) using rock nano adsorption gas extraction element and
Operating method obtains rock nano adsorption gas sample product；3) packed column gas chromatography detection method is utilized, rock nano adsorption is obtained
Gas hydrocarbon analysis data；4) hydrocarbon component carbon isotope detection method is utilized, it is same to obtain rock nano adsorption gas hydrocarbon component carbon
Position element analysis result；5) quantitative calculating is carried out using external standard method, obtains rock nano adsorption gas hydrocarbon component and the analysis of total hydrocarbon amount
As a result；6) it calculates and obtains rock nano adsorption gas assay parameter.The unconventional reservoir rock nano adsorption gas extraction element
And extracting obtained with hydrocarbon analysis method is the bound, information of gas that will not parse naturally in reservoir rock,
It needs to carry out on rock nanoscale crushing in technical solution and needs rock carrying out acidolysis, be not suitable in shale gas in content
The analysis of the prevailing gas part that can be parsed naturally is also not easy to analyze in shale gas drilling field conduct.
It in view of the foregoing, can be right the present invention provides a kind of shale gas-bearing property comprehensive analysis device and its method
While shale core carries out air content parsing test, the gas group of resolution gas in on-line analysis and monitoring shale gas resolving
At and its variation.
Summary of the invention
The purpose of the present invention is to provide a kind of shale gas-bearing property comprehensive analysis device and the shale gassiness based on the device
Property comprehensive analysis method, realize shale gas drill site to shale core carry out air content parsing test while, online
Analysis with monitoring resolving in resolution gas gas composition and its variation, can effectively improve test data reliability and in time
Property, the implementation of shale gas exploration and development engineering is preferably served, is provided for shale gas resource exploration with evaluation more scientific, more reliable
Gas-bearing property data.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of shale gas-bearing property comprehensive analysis device, including
Air content test cell, hydrocarbon gas component analysis unit, inorganic gas component analysis unit, operation control unit；
The air content test cell includes constant temperature parsing chamber, parsing tank, the first flow stabilizing valve, pneumatic filter, more than first
Port valve, Gas flow-limiting valve, the first detector, carrier gas one；The parsing tank is placed in the constant temperature parsing chamber；Described first is steady
Stream valve one end is connect with the parsing tank, the other end connects the carrier gas one；One end of the pneumatic filter connects the solution
Analyse tank, the other end connects first multiple-way valve；First multiple-way valve passes through the Gas flow-limiting valve and first detection
Device connection；
The hydrocarbon gas component analysis unit includes the first load sample ring, the first splitter, the second detector, the first multi-pass
Valve, the second multiple-way valve, the second flow stabilizing valve, carrier gas two；Described first load sample ring one end connect with first multiple-way valve, the other end
Connect second multiple-way valve；Second multiple-way valve also connects with first multiple-way valve, the second flow stabilizing valve, the first splitter
It connects；The other end of first splitter connects second detector；The other end of second flow stabilizing valve connects the load
Gas two；
The inorganic gas component analysis unit includes the second load sample ring, third flow stabilizing valve, the 4th flow stabilizing valve, the first multi-pass
Valve, third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve, third detector, carrier gas three, carrier gas four, the outlet of carrier gas four and the
Two, the third and fourth splitter；The third multiple-way valve and first multiple-way valve, the 4th multiple-way valve, the second load sample ring, third
Flow stabilizing valve connection；The other end of the second load sample ring is connect with first multiple-way valve；The other end of the third flow stabilizing valve
Connect the carrier gas three；The positioned inside of 4th multiple-way valve has second splitter, and is also separately connected outward described
Third splitter, the 4th flow stabilizing valve, carrier gas four export；The other end of 4th flow stabilizing valve connects the carrier gas four；Described
The other end of three splitters connects the 5th multiple-way valve；4th splitter described in the 5th multiple-way valve positioned inside, also to
The outer connection third detector；
The operation control unit includes computer, intelligent switch, digital communication component, controlled part；The number is logical
Interrogate component and connect the computer, one end of the intelligent switch connect the digital communication component, other end connection it is described by
Control component.
Further, further include splitter temperature-controlled cabinet, first splitter, the second splitter, third splitter,
4th splitter is all set in the splitter temperature-controlled cabinet.
Further, first multiple-way valve, the second multiple-way valve, third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve are equal
It is respectively arranged with independent heating and temperature control cavity.
Further, constant temperature parsing chamber, heating and temperature control cavity, splitter temperature-controlled cabinet, the first detector, the
Two detectors, third detector, the first flow stabilizing valve, the second flow stabilizing valve, third flow stabilizing valve, the 4th flow stabilizing valve, the first multiple-way valve,
Two multiple-way valves, third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve are connected to the operation control unit.
Further, first detector, the second detector are flame ionization ditector (FID), the third
Detector is thermal conductivity detector (TCD) (TCD).
Further, gas path on-off switch and the Standard Gases with gas path on-off switch are provided on the pneumatic filter
Body access port.
Further, the carrier gas one, carrier gas two, carrier gas three, carrier gas are fourth is that same source gas；
Or the carrier gas one, carrier gas two, carrier gas three, carrier gas are fourth is that different source gas；
Or the carrier gas one, carrier gas two, carrier gas three, carrier gas are fourth is that variety classes gas.
The invention also discloses the analysis methods for using shale gas-bearing property comprehensive analysis device as described above, including shale
Measurement of air content part and gas component analysis method part.The specific steps of the shale measurement of air content are such as
Under:
1) it sets analysis condition: the constant temperature being set by the operation control unit and parses chamber temperature and described first surely
The gas flow parameter of valve and the operating temperature and working gas flow of first detector are flowed, the constant temperature parsing is started
Chamber and first detector；
2) it loads core sample: core sample to be measured being put into the parsing tank and is sealed, and the parsing tank is put into
The constant temperature parsing is intracavitary；Material time point is recorded, the material time point includes the time point for sealing the parsing tank, rock core
Brills of sample locating rock stratum originally exceed time point, the core barrel for being loaded with core sample mention bore time point and its arrival well head when
Between point；
3) it carries out parsing test: " the first flow stabilizing valve-parsing tank-pneumatic filter " gas circuit is made by operation control unit
Connection allows shale gas in rock core to parse and be discharged in time under the carrying of the carrier gas one the parsing tank naturally, into described
First detector, the operation control unit are persistently acquired the detection signal of first detector, handle and record；
Record the time point of " the first flow stabilizing valve-parsing tank-pneumatic filter " gas circuit connection；
4) it weighs core quality: weighing to the core sample for completing parsing test, weigh and record its quality m0；
5) measurement bound gas product: a certain amount of core sample after step 3) parsing test is taken, weighs and records
Its quality m1, its bound gas volume is measured with step 1) and the identical method and condition of step 3) after closed crushing；
6) test result is calculated.
Specific step is as follows for the gas composition analysis method:
1) acquire sample: under the carrying of the carrier gas one, the gas parsed in the parsing tank successively passes through described
Pneumatic filter, the first multiple-way valve, the first load sample ring, the second multiple-way valve, the first multiple-way valve, third multiple-way valve, the second load sample ring,
During first multiple-way valve, Gas flow-limiting valve enter first detector progress gas content test, regulation described first
Multiple-way valve, the second multiple-way valve, third multiple-way valve, in uninterrupted first detector for the resolution gas from the parsing tank
Switching gas circuit in the case where the detection of body acquires gas composition analysis sample, the carrier gas two is made to carry the first load sample ring
In parsing gaseous sample enter the hydrocarbon gas component analysis unit, carry the carrier gas 3 in the second load sample ring
Parsing gaseous sample enter the inorganic gas component analysis unit, carry out parsing gas composition analysis；Record gas component
Analyze the time point of sample acquisition gas circuit switching；
2) component is analyzed:
A, it analyzes hydrocarbon gas component: adjusting first multiple-way valve, the second multiple-way valve, make described in the process of carrier gas two
Second multiple-way valve, the first multiple-way valve carry the gaseous sample in the first load sample ring by described in second multiple-way valve entrance
First splitter carries out component separation, is detected with second detector, carries out quantitative analysis to hydrocarbon gas component；
B, it analyzes inorganic gas component: adjusting first multiple-way valve, third multiple-way valve, the 4th multiple-way valve, the 5th multi-pass
Valve makes the carrier gas three carry the gaseous sample warp in the second load sample ring by the third multiple-way valve, the first multiple-way valve
Second splitter, third splitter, the 4th are sequentially entered by the third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve
Splitter carries out component separation, is detected with the third detector, carries out quantitative analysis to inorganic gas component；
3) calculated result:
A, the chromatographic peak area correction coefficient of second detector, third detector is demarcated respectively；
B, based on second detector to methane, ethane, propane, iso-butane, normal butane, isopentane, positive penta in sample
The detection signal data of alkane, the chromatographic peak area of difference each gas component of integral calculation, further according to it respectively for described second
The chromatographic peak area correction coefficient of detector calculates separately ethane in sample, propane, iso-butane, normal butane, isopentane, pentane
The volume fraction by methane on the basis of volume fraction；
C, methane, nitrogen, oxygen, carbon monoxide, carbon dioxide in the sample based on third detector detection record
Signal strength data, the chromatographic peak area of each gas component is calculated separately, further according to it respectively for the third detector
Chromatographic peak area correction coefficient calculate nitrogen, oxygen, carbon monoxide, carbon dioxide in sample and with the volume fraction of methane be
The volume fraction of benchmark；
D, ethane, propane, the iso-butane, positive fourth detected based on second detector and the third detector
Alkane, isopentane, pentane, nitrogen, oxygen, methane, carbon monoxide, carbon dioxide the volume fraction by methane on the basis of body
Fraction calculates methane, ethane, propane, iso-butane, normal butane, isopentane, pentane, oxygen, nitrogen, one with normalization method
The relative volume fraction of carbonoxide, carbon dioxide gas component.
Further, the step 6) concrete operations of the shale measurement of air content are as follows:
A, hydro carbons is calculated according to the detection signal data of first detector and parses gas volume Vdes；
B, the detection letter of the first detector according to the parsing test of the step 3) of the shale measurement of air content
Number calculates the accumulative hydro carbons parsing gas volume that different parsing time point T parse gas according to parsing time sequencing
Vdes(ac), and draw relation curve T-V of parsing time and accumulative hydro carbons parsing gas volumedes(ac)Curve；When according to parsing
Between with accumulative hydro carbons resolution gas volume relationship curve, calculate core sample enter it is described parsing tank before loss gas volume
Vlos；
C, according to following equation 1) calculate core sample in hydro carbons free gas content Gfree:
D, the first detector according to the test of step 5) the bound gas volume of the shale measurement of air content
Detection signal data calculate hydro carbons bound gas volume Vres, according to following formula 2) and calculate hydro carbons constraint gas in core sample
The content G of bodyres:
E, according to following formula 3) calculate core sample in hydrocarbon gas overall content G:
G=Gfree+Gres 3)
Agreement: formula 1), formula 2) and formula 3) in, gas volume Vdes、Vdes(ac)、Vlos、VresUnit be milliliter (mL), rock
Heart sample quality m0And m1Unit be gram (g), gas content G, Gfree、GresUnit be every gram of milliliter (mL/g) or cubic meter
(m per ton3/t)。
Further, the first load sample ring, the gaseous sample in the second load sample ring acquire simultaneously.
Further, step a, the step b in the step 2) of the gas composition analysis method can be carried out simultaneously, can also
With separated progress.
Further, gas composition analysis operation repeats at a certain time interval.
Further, the time point of described " the first flow stabilizing valve-parsing tank-pneumatic filter " the gas circuit connection and gas group
The time point of analysis sample acquisition is accurate to the second, according to " when-point-second " format record.
Further, it in test process, except core sample tinning sealing, load, unloading, closed crushing, weighs by artificial
Outside completing, remaining whole instrumentation is controlled by computer to be implemented.
It is possible to further carry out comprehensive analysis to shale air content test data and gas composition analysis data, according to
Shale gas geological prospecting, shale gas exploitation engineering, the research of shale gas geological theory etc. need to carry out depth excavation.
The invention has the following advantages:
1) shale gas-bearing property comprehensive analysis device of the present invention and method can on-line analyses while measuring shale air content
The different hydro carbons of resolution phase and the composition of non-hydrocarbon gases component, shale content measurement effect are full in shale gas resolving
It is required as defined in sufficient rower " shale measurement of air content " (SY/T 6940-2013), it is full that shale gas constituent content measures effect
It requires, is suitable for as defined in sufficient current standard methods " the composition analysis gas chromatography of natural gas " (GB/T 13610-2014)
Shale content measurement and shale gas gas composition analysis；
2) relative to traditional shale gas-bearing property analysis method, avoid saved in sample transportational process it is improper and storage when
Between it is too long will cause test error caused by gas loss and change of component, can effectively improve test data reliability and
Timeliness ensures the timeliness of data, provides timely data support to field engineering decision, preferably serves shale gas and survey
It visits Development Engineering to implement, provides more scientific, more reliable shale gas-bearing property data for shale gas resource exploration and evaluation.
Detailed description of the invention
Fig. 1 is gas circuit Mode A schematic diagram of the invention；
Fig. 2 is gas circuit Mode B schematic diagram of the invention；
Fig. 3 is gas circuit mode C schematic diagram of the invention.
In figure: the first flow stabilizing valve of 1-, the second flow stabilizing valve of 2-, 3- third flow stabilizing valve, the 4th flow stabilizing valve of 4-, 5- Gas flow-limiting
Valve, 6- constant temperature parsing chamber, 7- parsing tank, 8- pneumatic filter (band standard gas entrance), 9- the first load sample ring, 10- the second load sample ring,
The first multiple-way valve of 11-, the second multiple-way valve of 12-, 13- third multiple-way valve, the 4th multiple-way valve of 14-, the 5th multiple-way valve of 15-, 16- first
Splitter, the second splitter of 17-, 18- third splitter, the 4th splitter of 19-, the first detector of 20-, the second detector of 21-,
22- third detector, 23- operation control unit, a1, a2, a3, a4, a5, a6, b1, b2, b3, b4, b5, b6, c1, c2, c3,
C4, d1, d2, d3, d4, e1, e2, e3, e4- multiple-way valve connection point.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
As shown in FIG. 1 to 3, shale gas-bearing property comprehensive analysis device of the present invention, it includes air content test cell, hydro carbons
Gas composition analysis unit, inorganic gas component analysis unit and operation control unit.The air content test cell, hydrocarbon
Class gas composition analysis unit, inorganic gas component analysis unit are connected to the operation control unit.The division of each unit
And non-physical, but it is functional.
The air content test cell includes the first flow stabilizing valve 1, and constant temperature parses chamber 6, parses tank 7, pneumatic filter 8, and the
One multiple-way valve 11, Gas flow-limiting valve 5 and the first detector 20.Wherein, the first flow stabilizing valve 1 is used for carrier gas 1, and working range is not small
In 5~50mL/min；It is cylinder, 30~140mm of intracavity diameter, 50~250mm of height, thermostatic control model that constant temperature, which parses chamber 6,
35 DEG C~220 DEG C are enclosed, temperature-controlled precision ± 2 DEG C；Parsing tank 7 has upper and lower two gas circuit ports, cylindrical, and intracavity diameter 25~
135mm, 45~220mm of height；First multiple-way valve 11 is six-way valve；First detector 20 is flame ionization ditector
(FID)；Pneumatic filter 8 is that material fills type filter；Gas flow-limiting valve 5 is air-resistance type structure, and structure is to ensure test
It is design premises that the hydrogen flame of the first detector is not blown out by excessive air-flow in the process.First flow stabilizing valve 1 connection parsing tank 7,
Parsing tank 7 be placed in constant temperature parsing chamber 6 in, parsing tank 7 another port connect pneumatic filter 8, pneumatic filter 8 it is another
Port connects the first multiple-way valve 11, and a port of the first multiple-way valve 11 is connect by Gas flow-limiting valve 5 with the first detector 20.
The hydrocarbon gas component analysis unit includes the second flow stabilizing valve 2, the first multiple-way valve 11, the second multiple-way valve 12, the
One load sample ring 9, the first splitter 16 and the second detector 21.Wherein, the second flow stabilizing valve 2 is used for carrier gas 2, working range covering
10~100mL/min；The load sample volume of first load sample ring 9 is 0.1~3mL；First splitter 16 is quartz capillary column (PONA
Column), internal diameter 0.20mm, 35~60m of length；Second detector 21 is flame ionization ditector (FID)；Second multiple-way valve 12
For four-way valve.Second flow stabilizing valve 2 connects the second multiple-way valve 12, and a port of the second multiple-way valve 12 and the first multiple-way valve 11 connect
Connect, the both ends of the first load sample ring 9 are connect with the first multiple-way valve 11 and the second multiple-way valve 12 respectively, the second multiple-way valve 12 another
Port is connect with the gas access end of the first splitter 16, and the gas outlet end of the first splitter 16 and the second detector 21 connect
It connects.
The inorganic gas component analysis unit includes third flow stabilizing valve 3, the 4th flow stabilizing valve 4, the first multiple-way valve 11, third
Multiple-way valve 13, the 4th multiple-way valve 14, the 5th multiple-way valve 15, the second load sample ring 10, the second splitter 17, third splitter 18,
Four splitters 19 and third detector 22.Wherein, third flow stabilizing valve 3 is used for carrier gas 3, and working range covers 10~80mL/
min；4th flow stabilizing valve 4 is used for carrier gas 4, and working range covers 5~50mL/min；4th multiple-way valve 14 is six-way valve, third
Multiple-way valve 13, the 5th multiple-way valve 15 are four-way valve；The volume of second load sample ring 10 is 0.25~5mL；Second splitter 17,
Three splitters 18, the 4th splitter 19 are packed column, and filler distinguishes DC200, PraQ and 13X, and column length is respectively 2.5~
3.5m, internal diameter are 3.0mm；Third detector 22 is thermal conductivity detector (TCD) (TCD).Third flow stabilizing valve 3 connects third multiple-way valve 13,
4th flow stabilizing valve 4 connect the 4th multiple-way valve 14, the other three port of third multiple-way valve 13 respectively with the first multiple-way valve the 11, the 4th
Multiple-way valve 14, the connection of the second load sample ring 10, the other end of the second load sample ring 10 are connect with a port of the first multiple-way valve 11, the
Two splitters 17 are connected to inside the 4th multiple-way valve 14, the other three port of the 4th multiple-way valve 14 respectively with third splitter
18, the 4th flow stabilizing valve 4, the outlet of carrier gas 4 connection, the gas outlet end of third splitter 18 are connect with the 5th multiple-way valve 15, and the 4th
Splitter 19 is placed in inside the 5th multiple-way valve 15, another port of the 5th multiple-way valve 15 connects third detector 22.
The operation control unit 23 includes computer, intelligent switch, digital communication component, operation control software.It is described
Digital communication component connects the computer, and one end of the intelligent switch connects the digital communication component, other end connection
Accordingly by control unit, the operation control software is installed on the computer.
Further, the first pressure maintaining valve 1, the second pressure maintaining valve 2, third pressure maintaining valve 3, the 4th pressure maintaining valve 4 are mass flow
Controller.
Further, gas path on-off switch, and the Standard Gases with gas path on-off switch are mounted on pneumatic filter 8
Body access port.
Further, carrier gas 1, carrier gas 2, carrier gas 3, carrier gas 4 blowing mouth be mounted on pressure reducing valve.
Further, carrier gas 1, carrier gas 2, carrier gas 3, carrier gas 4 can be same source gas, be also possible to different source gas or not of the same race
Class gas.Wherein, the carrier gas 1, carrier gas 3, carrier gas 4 can be hydrogen or helium, and the carrier gas 2 can be hydrogen, helium or nitrogen
Gas.
Further, fire extinguishing monitoring is provided with and function of lighting a fire again automatically for the first detector 20 and the second detector 21
Energy.
Embodiment 1
Analyze operating process
Shale gas assay and gas composition analysis based on shale gas-bearing property comprehensive analysis device of the present invention remove rock core
Sample load, unloading, crushing and weighing operation are outer by manually completing, remaining instrument manipulation work whole process is controlled by the operation
Unit processed is implemented according to the program of setting and parameter under the control of the computer.Specifically include the following steps and content:
1. instrument prepares
(1) connection instrument power source, the computer of start-up operation control unit 23 run operation control software.Conditioning instrumentation
Gas circuit is at " gas circuit Mode A " (see Fig. 1).Open the pressure reducing valve of carrier gas 1, carrier gas 2, carrier gas 3, carrier gas 4.
(2) temperature of setting constant temperature parsing chamber 6, sets the first flow stabilizing valve 1, the second flow stabilizing valve 2, third flow stabilizing valve the 3, the 4th
The gas flow parameter of flow stabilizing valve 4.Start constant temperature parsing chamber 6 temperature control and the first flow stabilizing valve 1, the second flow stabilizing valve 2,
The gas flow control program of third flow stabilizing valve 3, the 4th flow stabilizing valve 4, makes relevant parameter be in setting value.Constant temperature parses chamber 6
The formation temperature setting of temperature layer position according to locating for core sample original to be measured.The gas stream of first flow stabilizing valve 1, the 4th flow stabilizing valve 4
Amount is generally arranged in 5~50mL/min, and the gas flow of the second flow stabilizing valve 2 is generally arranged in 10~100mL/min, third current stabilization
The gas flow of valve 3 is generally arranged in 10~80mL/min, and the gas flow limit value of Gas flow-limiting valve 5 is generally at 0.2 mpa
150~300mL/min.
(3) the work gas source of the first detector 20, the second detector 21, third detector 22 is opened；The first detection of setting
The operating temperature of device 20, the second detector 21, third detector 22；Regulate and control the hydrogen of the first detector 20 and the second detector 21
The reference gas flow velocity of flow velocity and air velocity and third detector 22.Start the first detector 20, the second detector 21,
Three detectors 22, are at steady-working state.The operating temperature of first detector 20 and the second detector 21 is generally 150
~250 DEG C, hydrogen flow rate general control is in 20~50mL/min, and air velocity is generally in 250~350mL/min.Third detection
For the operating temperature of device 22 generally at 80~150 DEG C, reference gas is carrier gas 3, setting value of the flow velocity with third flow stabilizing valve 3.
2. core sample loads
(1) the fresh well rock core out of 25~5000g is chosen, mud is quickly washed off, is put into rapidly in parsing tank 7, and seal solution
Analyse tank 7.
(2) parsing tank 7 is put into constant temperature parsing chamber 6.The time point of record capping parsing tank 7 and the core sample
The brill of rock stratum locating for product exceedes the time for mentioning brill time point and reaching well head of core barrel locating for time point and core sample time
Point.Each time point is by " year-month-day-when-point (YY-MM-DD-hh-mm) " format record.
3. content measurement
3.1 parsing Determination of octafluoropropane content
Parsing gas refer to can be made by natural resolving in shale its discharge gas part, including free gas,
Adsorbed gas, solution gas.Nature parsing test is carried out to this portion gas, is performed the following operations:
(1) start related gas circuit regulatory process, in the case where instrument gas circuit is in " gas circuit Mode A ", allow the first current stabilization
Valve 1 and pneumatic filter 8 realize gas circuit connection by parsing tank 7, make to parse the resolution gas in tank 7 under the carrying of carrier gas 1 into
Enter the detection of the first detector 20.Start the detection signal acquisition of the first detector 20, by " year-month-day-when-point (YY-MM-DD-
Hh-mm) " format record starts the time point of acquisition.In subsequent operation, no matter gas circuit is switched to " gas circuit Mode B " (Fig. 2),
Still " gas circuit mode C " (Fig. 3), is constantly acquired and saves to the detection signal of the first detector 20, is sequentially recorded each
The intensity of secondary acquisition signal, until parsing test terminates.
(2) condition or time or manual intervention that setting parsing test terminates terminate parsing test.
(3) test to be resolved terminates, and weighs core sample quality, is recorded as m0。
3.2 bound gas assays
Bound gas refers to the gas part that it cannot be made to discharge with the method for parsing naturally in shale, also known as residual gas.
Manual intervention release test, test process are carried out to this portion gas are as follows:
(1) core sample (20~500g) after taking a certain amount of parsing to test, weighs its quality, is recorded as m1。
(2) the weighed core sample of institute dedicated parsing potting dress matched with instrument, after closed crushing, with measurement
The identical method of parsing gas content, condition and operating process are tested.
Illustrate: dedicated parsing tank matched with instrument refers to, outer dimension and instrument matched with instrument of the present invention
General analytical tank used is consistent, has and carries out closed crushing function, sample to core sample in tank by ancillary equipment
After crushing can directly examination with computer parsing tank.
4. gas composition analysis
Gas composition analysis includes to the resolution gas gas group parsed when gas carries out nature parsing test in core sample
It analyzes and release gas composition analysis when manual intervention release is tested is carried out to bound gas in core sample.
During carrying out parsing test to parsing Gas content or carrying out release test to constraint Gas content, uninterrupted
In the case that core sample air content is tested, the first multiple-way valve 11, the second multiple-way valve 12, third multiple-way valve more than the 13, the 4th are adjusted
Port valve 14, the 5th multiple-way valve 15 switch gas circuit sequentially between " gas circuit Mode A ", " gas circuit Mode B ", " gas circuit mode C ",
Chromatography cyclically is carried out to gas component.
It needs to be arranged the time point that each single gas component analysis operation starts according to test, or waits durations setting twice
Time interval between gas composition analysis operation.
4.1 hydrocarbon gas component analyses
In the case where instrument gas circuit is in " gas circuit Mode A ", instrument gas circuit is switched to " gas circuit Mode B ", is opened simultaneously
The detection signal acquisition and data of dynamic second detector 21 save, and are sequentially recorded signal collected intensity.At this point, carrier gas 2 is taken
Enter the first splitter 16 with the gaseous sample in the first load sample ring 9 and carry out component separation, realizes methane, ethane, propane, isobutyl
The separation of alkane, normal butane, isopentane, pentane, and then sequence enters the second detector 21 and is detected, and obtains methane, ethane, third
The detection data of the hydrocarbon components such as alkane, iso-butane, normal butane, isopentane, pentane.In subsequent operation, even if gas circuit switches
To " gas circuit mode C " or " gas circuit Mode A ", the second detector 21 persistently carries out detection signal acquisition, until when time gaseous sample
Whole hydrocarbon gas component appearances finish.
When secondary gaseous sample hydrocarbon gas component analysis terminates, stop the detection signal acquisition and data of the second detector 21
Record, is saved by operation control unit 23 in computer storage medium by recorded with independent data files.Data text
Should be switched to comprising gas circuit in part " gas circuit Mode B " time point information, the time is accurate to the second.
4.2 inorganic gas component analyses
In the case where instrument gas circuit is in " gas circuit Mode A ", instrument gas circuit is switched to " gas circuit Mode B ", is opened simultaneously
The detection signal acquisition and data record of dynamic third detector 22, measurement nitrogen, oxygen, carbon monoxide, carbon dioxide etc. are inorganic
The hydrocarbon gas component such as gas component and methane, ethane.At this point, carrier gas 3 is by carrying the second load sample after third flow stabilizing valve 3
Gaseous sample in ring 10 sequentially enters the second splitter 17, third splitter 18, the 4th splitter 19 and implements component separation.
Wherein, the second splitter 17 functions as preposition splitter to heavy hydrocarbon component, the moisture etc. in gaseous sample
It is isolated, in order to avoid its separating effect for influencing under test gas component, Interference Detection signal；Third splitter 18 is first to gas sample
Gas component in product carries out initial gross separation, and allows four kinds of methane, nitrogen, oxygen, carbon monoxide gas components incomplete
Continue to separate into the waiting of the 4th splitter 19 in advance by third splitter 18 as a mixture in the case where separation.
After methane, nitrogen, oxygen, carbon monoxide fully enter the 4th splitter 19 not to be kept completely separate state, immediately
The first multiple-way valve 11, the second multiple-way valve 12, third multiple-way valve 13, the 4th multiple-way valve 14 and the 5th multiple-way valve 15 are adjusted, by gas circuit
It is switched to " gas circuit mode C ", it is caused to poison to prevent carbon dioxide from entering the 4th splitter 19.At this point, methane, nitrogen,
Oxygen, carbon monoxide temporal persistence are in the 4th splitter 19, and the gases such as carbon dioxide and ethane are then in third splitter 18
In continue to complete separation, and third detector 22 is directly entered by the 5th multiple-way valve 15 and is detected.Meanwhile carrier gas 4 passes through the
Four flow stabilizing valves 4 and the 4th multiple-way valve 14 carry out blowback cleaning to the second splitter 17, blow out heavy hydrocarbon component therein, moisture etc.,
It prepares for gas composition analysis next time；Shale gas resolution unit enters resolution gas sample online acquisition gas circuit mode, under
Gas composition analysis carries out sample acquisition and prepares.
22 appearances sequentially are detected in third detector to gases such as carbon dioxide, ethane to finish, and immediately switch back into gas circuit
To " gas circuit Mode A ", allow nitrogen, oxygen, methane, carbon monoxide mixtures under the carrying of carrier gas 3 in the 4th splitter 19
Separation is completed, and sequentially enters third detector 22 and is detected.
When nitrogen, oxygen, methane, carbon monoxide appearance finish, stop the detection signal acquisition and number of third detector 22
According to record, saved by operation control unit 23 in computer storage medium by recorded with independent data files.Data
The time point information of " gas circuit Mode B " should be switched in file comprising gas circuit, the time is accurate to the second.
Embodiment 2
Analysis result calculation processing
1. detector is demarcated
The calibration test of 1.1 detectors
Close the 1 incoming road on-off switch of carrier gas on pneumatic filter 8.From installing in the calibrating gas on pneumatic filter 8
Access port access containing methane, ethane, propane, iso-butane, normal butane, isopentane, pentane, nitrogen, oxygen, carbon monoxide,
Carbon dioxide etc. contains the calibrating gas of all target detection gas components.It allows calibrating gas constant speed inflow gas filter 8, presses
Calibrating gas is tested according to normal sample test instrument condition and operation sequence, to the first detector 20 under the flow velocity
Detection signal strength and the relationship of hydrocarbon gas total volume demarcated, to the second detector 21,22 each group of third detector
The relationship of the relative peak area of color separation spectral peak normal volume corresponding thereto is demarcated respectively.
Note: it is required that calibration test is carried out with 5 or more calibrating gas, same gas component in each calibrating gas used
Concentration is different and should cover reasonable concentration range.
1.2 detectors demarcate test data processing
Agreement: the volume fraction of methane in calibrating gas is denoted as CMe, the volume fraction of other hydrocarbon gas components is denoted as
Ci(i=ethane, propane, iso-butane, normal butane, isopentane, pentane)；The volume fraction of inorganic gas component is denoted as Cj(j
=nitrogen, oxygen, carbon monoxide, carbon dioxide).
1.2.1 20 unit volume signal strength of the first detector calculates method
The signal strength that first detector 20 obtains calibrating gas n test is denoted as I by agreementn, week signal acquisition time
Phase is denoted as p, and calibrating gas is denoted as F by the volume flow rate of the first detector 20n, the first detector 20 is for calibrating gas n's
Population unit's volume signals intensity of hydrocarbon gas is denoted as Rn, then RnIt is calculated with following formula:
Formula 1) in, i=ethane, propane, iso-butane, normal butane, isopentane, pentane.
1.2.2 21 chromatographic peak area correction coefficient calculating method of the second detector
The methane chromatographic peak area that the test of second detector 21 obtains is denoted as A by agreementMe, other hydrocarbon gas component i's
Chromatographic peak area is denoted as Ai。
If the hydrocarbon gas component i of the second detector 21 is k relative to the chromatographic peak area correction coefficient of methanei, expire
Foot:
ki·Ai∶AMe=Ci∶CMe
Have
Formula 2) in, i=ethane, propane, iso-butane, normal butane, isopentane, pentane.
1.2.3 22 chromatographic peak area correction coefficient calculating method of third detector
The methane chromatographic peak area that the test of third detector 22 obtains is denoted as A' by agreementMe, the chromatography of inorganic gas component j
Peak area is denoted as A'j。
If the inorganic gas component j of third detector 22 is k' relative to the chromatographic peak area correction coefficient of methanej, expire
Foot:
k'j·A'j∶A'Me=Cj∶CMe
Have
Formula 3) in, j=nitrogen, oxygen, carbon monoxide, carbon dioxide.
1.2.4 detector parameters calibration result calculates
Data obtained are tested according to calibration is carried out to detector with calibrating gas, according to formula 1), formula 2) and formula 3), by
One calculates the detection of its total appropriate hydrocarbon gas and each gas component for the first detector 20, the second detector 21, third detector 22
Device parameter Rn、kiAnd k'jValue.
Note: R should be calculated for the calibrating gas all testedn、kiAnd k'jAverage value, average value is used for following
The core sample Measurement results calculate.
2. air content test result calculations
2.1 hydrocarbon gas volumes calculate
2.1.1 Computing Principle
Agreement will take down in short-hand in core sample parsing test by the gas volume flow of the first detector 20 as F, be examined first
It surveys the instantaneous detection signal strength obtained on device 20 and is denoted as I, the instantaneous volume fraction of each hydrocarbon component is remembered respectively in gas at this time
For CMe(Me=methane) and Ci(i=ethane, propane, iso-butane, normal butane, isopentane, pentane), then according to formula 1), first
The hydrocarbon gas component total volume E that detector 20 detects within a signal acquisition periods p time can be calculated with following formula:
Then, the Z during core sample parsing testtTo Zt+1In period, hydro carbons that the first detector 20 detects
The total volume V of gas componentdes(t)Are as follows:
I.e.
Formula 4) in, T is the testing time, and I is the instantaneous detection signal strength of the first detector of T time 20.
According to formula 4), can be according to following formula 5) calculate the hydrocarbon gas total volume V that the first detector 20 detectsdes:
In formula 5,0 is the test time started, and Z is the test end time.
2.1.2 calculation method
In actually calculating, it can operate in accordance with the following steps:
Step 1: by the parsing testing time of core sample by etc. durations be segmented, according to formula 4), calculate test process one by one
In each period (Zt~Zt+1) the hydrocarbon gas volume (V that detects of the first detector 20des(t)), draw hydrocarbon gas body
Product (Vdes(t)) with the graph of relation (V of testing time (T)des(t)- T figure).
Step 2: to Vdes(t)In-T figure because carry out gas composition analysis make caused by gas circuit switching data catastrophe point by
One does data smoothing processing.
Step 3: according to formula 5), in 0~Z time range of the time Z tested from the time 0 for starting test to end,
To the hydrocarbon gas volume (V of All Time segmentationdes(t)) sum up, obtain the total volume (V of hydrocarbon gasdes)。
2.2 hydrocarbon loss air volumes calculate
According to carrying out data smoothing treated hydrocarbon gas volume (Vdes(t)) with the graph of relation of testing time (T)
(Vdes(t)- T figure) data, the accumulative hydrocarbon gas volume of different testing time points (T) is calculated according to certain time interval
(Vdes(ac)), draw accumulative hydrocarbon gas volume (Vdes(ac)) with the graph of relation (V of testing time (T)des(ac)- T figure), it presses
Air volume restoration methods (USBM method or other standard methods) is lost according to as defined in shale gas parsing testing standard method, according to
Vdes(ac)- T diagram data calculates core sample and enters the hydrocarbon gas loss volume (V before the parsing tanklos)。
The free gas content of 2.3 shale calculates
The hydrocarbon gas obtained product (V is calculated according to test data is parsed by core sampledes), and on this basis
By restoring to calculate the hydrocarbon loss gas volume (V obtainedlos), according to following equation 6) calculate shale representated by core sample
Unit mass rock hydro carbons parse volume concentration of gas phase Gfree:
Formula 6) in, m0For carry out parsing test core sample quality.
The hydro carbons bound gas content of 2.4 shale calculates
According to formula 5), according to following formula 7), referring to the calculation method of 2.1.2, based on the first inspection in rock core constraint gas test
It surveys the detection signal strength of device 20 and its calculates hydro carbons bound gas volume V with the data of testing time variationres:
Wherein, 0 is starts the testing time, and Z' is to terminate the testing time.
Note:, should be to because carrying out detecting signal strength mutation caused by gas circuit switching is made in gas composition analysis before calculating
Point (if there is) does data smoothing processing one by one.
According to following equation 8) calculate core sample hydro carbons bound gas content Gres:
Formula 8) in, m1For the quality of the core sample for carrying out bound gas release test.
The hydrocarbon gas overall content of 2.5 shale calculates
According to following equation 9) calculate the overall content G of hydrocarbon gas in shale representated by core sample:
G=Gfree+Gres 9)
Agreement: formula 4)~formula 9) in, air volume Vdes、Vlos、Vres、Vdes(t)、Vdes(ac)Unit be milliliter (mL), rock core
Sample quality m0And m1Unit be gram (g), gas content Gfree、Gres, G unit can for every gram of milliliter (mL/g) or cube
Rice (m per ton3/t)。
3. gas composition Analysis result calculation
3.1 single sample Analysis result calculations
Step 1: integral chromatographic peak area
For single sample analyze, to the methane of the second detector 21, ethane, propane, iso-butane, normal butane, isopentane,
The chromatographic peak of pentane carries out area integral respectively, obtains the chromatographic peak area (A of each componentMe, Ai；Me=methane, i=ethane,
Propane, iso-butane, normal butane, isopentane, pentane)；To the carbon dioxide of third detector 22, nitrogen, oxygen, methane, one
The chromatographic peak of carbonoxide carries out area integral respectively, obtains the chromatographic peak area (A' of each componentMe, A'j；Me=methane, j=bis-
Carbonoxide, nitrogen, oxygen, carbon monoxide).
Step 2: calculating volume fraction
The relative volume fraction of each component is calculated with normalization method.Circular and based on the following:
(1) according to formula 2), the volume fraction of hydrocarbon gas component i is
Wherein, i=ethane, propane, iso-butane, normal butane, isopentane, pentane；
(2) according to formula 3), the volume fraction of inorganic gas component j is
Wherein, j=carbon dioxide, nitrogen, oxygen, carbon monoxide.
(3) arranging will be when the normalization volume fraction of methane in time analysis sample is denoted as UMe, other hydrocarbon gas component i's
Normalization volume fraction is denoted as Ui(i=ethane, propane, iso-butane, normal butane, isopentane, pentane), inorganic gas component j
Normalization volume fraction be denoted as Uj(j=carbon dioxide, nitrogen, oxygen, carbon monoxide).
Then, be based on formula 10) and formula 11), when it is secondary analyze sample in methane normalization volume fraction can calculate it is as follows:
I.e.
When other hydrocarbon such as ethane, propane, iso-butane, normal butane, isopentane, pentane in secondary analysis sample
When the normalizing of the inorganic gas component such as nitrogen, oxygen, carbon monoxide, carbon dioxide in secondary analysis sample
Special suggestion: there are air in parsing tank before being tested due to parsing, and the gas composition data of early stage can be dry by air
Disturb, therefore, in actual operation, when the normalization volume fraction of hydrocarbon gas preferably only being reached maximum value from single gas group
Analysis data are considered as the truthful data of sample.
4. gas-bearing property test data comprehensive analysis processing
Various synthesis are carried out to test data according to geological prospecting, drilling engineering, theoretical research etc. requirements of one's work
Analysis, processing, Cheng Tu, can get, but be not limited to following shale gas geological analysis data.
(1) shale gas production parsing Potentials data
Hydrocarbon gas volume (the V obtained based on the test of shale gas resolution gasdes(t)) with parsing time (T) relation curve
Scheme (Vdes(t)- T figure) data and resolution gas gas component relative volume fraction analysis data series, calculate resolution gas solution
During analysis in rock core relevant gaseous components parsing amount delta data, and draw related graph.Data are for shale gas production
In gas gross or gas type, or single gas component parsing release potential and trend analysis use.
(2) data are analyzed in shale gas resource assessment
Hydrocarbon gas content data G, G in the shale gas that test obtains is parsed based on shalefree、Gres, to each gas group
On the basis of dividing relative volume fraction data to carry out comprehensive analysis processing, each gas component contains in calculating free gas and constraint gas
Amount, for the oil in place evaluation of shale gas resource, Economic Evaluation, the evaluation of exploitation engineering technical feasibility etc. provide it is accurate,
Fine shale Gas content, composition, distribution and its occurrence status data.
(3) shale gas geological condition analysis data
Based on comprehensive point of the serial shale gas-bearing property obtained with instrument and method of the invention for individual well or geologic province
Data are analysed, in conjunction with related geology, geochemistry, geophysical data, by aggregation of data analysis, data correlation and are illustrated table
Up to processing, fine, comprehensive, system, solid, intuitive shale gas-bearing property item are provided for the analysis of region Geological Condition of Shale Gas Accumulation
Part description.
Embodiment 3
Calibrating gas analysis
(1) gas composition: methane 85.88%, ethane 3.04%, propane 0.77%, iso-butane 0.29%, normal butane
0.22%, isopentane 0.10%, pentane 0.10%, nitrogen 3.01%, oxygen 0.57%, carbon monoxide 4.98%, titanium dioxide
Carbon 0.96%, other 0.08%.
(2) test condition
Carrier gas and its flow velocity: carrier gas 1, hydrogen, flow 20mL/min；Carrier gas 2, hydrogen, flow 63mL/min；Carrier gas 3, hydrogen
Gas, flow 22mL/min；Carrier gas 4, hydrogen, flow 30mL/min.
5 cut-off current of Gas flow-limiting valve: 200mL/min under 0.2MPa.
Load sample ring body product: 9 volume 0.5mL of the first load sample ring；Second load sample ring, 10 volume 2.5mL.
Parsing constant temperature parsing 6 temperature of chamber: 100 DEG C,
Separate column temperature: 50 DEG C of post case temperature of separation.
Multiple-way valve temperature: 11 temperature 60 C of the first multiple-way valve, 12 temperature 60 C of the second multiple-way valve, 13 temperature of third multiple-way valve
60 DEG C, 14 temperature 60 C of the 4th multiple-way valve, 15 temperature 60 C of the 5th multiple-way valve.
Sensors work condition: 150 DEG C, air velocity 300mL/min of 20 operating temperature of the first detector, hydrogen flow rate
35mL/min；150 DEG C, air velocity 280mL/min, hydrogen flow rate 25mL/min of second detector, 21 operating temperature；Third inspection
Survey 100 DEG C of 21 operating temperature of device, reference gas H2, flow velocity 22mL/min.
Single gas component analysis duration: analytical cycle 14min, intermittent time 3min.
(3) test result
Total hydrocarbon length of testing speech: 273min.
Hydrocarbon gas volume: 1682.72mL.
The quasi- volume of gas of mark: 1860.39mL.
Gas component normalizes volume fraction measurement result:
Embodiment 4
FIG. 1 to FIG. 3 is structure, working principle and gas circuit the conversion signal of shale gas-bearing property comprehensive analysis device of the present invention
Figure.
The gas circuit of Fig. 1 is in gas circuit Mode A.Under the mode, device makes to parse air-flow while carrying out content measurement
Through the first load sample ring 9 and the second load sample ring 10, prepare for the sampling of gas composition analysis next time；Gas composition analysis unit after
It is continuous to carry out last gas composition analysis process, or in gas composition analysis next time to be performed such as idle running.
The gas circuit of Fig. 2 is in gas circuit Mode B.Gaseous sample under the mode, in the first load sample ring 9 and the second load sample ring 10
Enter hydrocarbon gas component analysis unit under the carrying of carrier gas 2 and carrier gas 3 respectively and inorganic gas component analysis unit carries out
Gas composition analysis；So simultaneously, air content test cell persistently carries out air content test process without interruption.
The gas circuit of Fig. 3 is in gas circuit mode C.Under the mode, last gas composition analysis enters mid-term stage, device
Gas circuit is adjusted to prepare resolution gas component analysis next time.First load sample ring 9 and the second load sample ring 10 return to resolution gas
In sample online acquisition gas circuit, prepare for the sampling of gas composition analysis next time；The second splitter as preposition splitter
17 are cleaned by carrier gas blowback, to ensure the effect of inorganic gas component analysis next time；4th splitter 19 carries methane, oxygen
Gas, nitrogen, carbon monoxide component are separated with gas circuit, wait the separation and detection that this four components are completed when returning to gas circuit Mode A；
So simultaneously, air content test cell persistently carries out air content test process without interruption.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (10)
1. a kind of shale gas-bearing property comprehensive analysis device, which is characterized in that including air content test cell, hydrocarbon gas component point
Analyse unit, inorganic gas component analysis unit, operation control unit；
The air content test cell include constant temperature parsing chamber, parsing tank, the first flow stabilizing valve, pneumatic filter, the first multiple-way valve,
Gas flow-limiting valve, the first detector, carrier gas one；The parsing tank is placed in the constant temperature parsing chamber；First flow stabilizing valve
One end is connect with parsing tank, the other end connects carrier gas；One end connection parsing tank, the other end of pneumatic filter connect the first multi-pass
Valve；First multiple-way valve is connect by Gas flow-limiting valve with the first detector；
The hydrocarbon gas component analysis unit include the first load sample ring, the first splitter, the second detector, the first multiple-way valve,
Second multiple-way valve, the second flow stabilizing valve, carrier gas two；Described first load sample ring one end connect with the first multiple-way valve, other end connection the
Two multiple-way valves；Second multiple-way valve is also connect with the first multiple-way valve, the second flow stabilizing valve, the first splitter；First splitter it is another
The second detector of end connection；The other end of second flow stabilizing valve connects the carrier gas two；
The inorganic gas component analysis unit include the second load sample ring, third flow stabilizing valve, the 4th flow stabilizing valve, the first multiple-way valve,
Third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve, third detector, carrier gas three, carrier gas four, the outlet of carrier gas four and second,
Third and fourth splitter；The third multiple-way valve and first multiple-way valve, the 4th multiple-way valve, the second load sample ring, third are steady
Flow valve connection；The other end of the second load sample ring is connect with the first multiple-way valve；The other end of the third flow stabilizing valve connects institute
State carrier gas three；The positioned inside of 4th multiple-way valve has the second splitter, and is also separately connected third splitter, the 4th outward
Flow stabilizing valve, carrier gas four export；The other end of 4th flow stabilizing valve connects carrier gas four；The other end of third splitter connects the 5th multi-pass
Valve；4th splitter described in 5th multiple-way valve positioned inside also connects third detector outward；
The operation control unit includes computer, intelligent switch, digital communication component, controlled part；The digital communication portion
Part connects computer, and one end of intelligent switch connects digital communication component, the other end connects controlled part.
2. shale gas-bearing property comprehensive analysis device as described in claim 1, which is characterized in that further include separation column temperature control
Case, first splitter, the second splitter, third splitter, the 4th splitter are all set in splitter temperature-controlled cabinet.
3. shale gas-bearing property comprehensive analysis device as described in claim 1, which is characterized in that the first multiple-way valve, the second multi-pass
Valve, third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve are respectively arranged with independent heating and temperature control cavity.
4. shale gas-bearing property comprehensive analysis device as described in claim 1, which is characterized in that the constant temperature parsing chamber, heating
With temperature control cavity, splitter temperature-controlled cabinet, the first detector, the second detector, third detector, the first flow stabilizing valve, second
Flow stabilizing valve, third flow stabilizing valve, the 4th flow stabilizing valve, the first multiple-way valve, the second multiple-way valve, third multiple-way valve, the 4th multiple-way valve, the 5th
Multiple-way valve is connected to operation control unit.
5. shale gas-bearing property comprehensive analysis device as described in claim 1, which is characterized in that first detector, second
Detector is flame ionization ditector (FID), and the third detector is thermal conductivity detector (TCD) (TCD)；The gas filtration
Gas path on-off switch and the calibrating gas access port with gas path on-off switch are provided on device.
6. shale gas-bearing property comprehensive analysis device as described in claim 1, which is characterized in that the carrier gas one, carries carrier gas two
Gas three, carrier gas are fourth is that same source gas；
Or the carrier gas one, carrier gas two, carrier gas three, carrier gas are fourth is that different source gas；
Or the carrier gas one, carrier gas two, carrier gas three, carrier gas are fourth is that variety classes gas.
7. a kind of analysis method using shale gas-bearing property comprehensive analysis device as described in claim 1, including shale gassiness
Quantity measuring method part and gas component analysis method part, which is characterized in that the shale measurement of air content it is specific
Steps are as follows:
1) it sets analysis condition: the gas flow ginseng that constant temperature parses chamber temperature and the first flow stabilizing valve is set by operation control unit
Several and the first detector operating temperature and working gas flow, starting constant temperature parsing chamber and the first detector；
2) it loads core sample: core sample to be measured being put into parsing tank and is sealed, and parsing tank is put into the constant temperature and is parsed
It is intracavitary；Record material time point, the material time point includes that seal parsing time point of tank, core sample originally locating
The brill of rock stratum exceedes the time point for mentioning brill time point and its reaching well head at time point, the core barrel for being loaded with core sample；
3) it carries out parsing test: joining " the first flow stabilizing valve-parsing tank-pneumatic filter " gas circuit by operation control unit
It is logical, it allows in rock core shale gas parse and be discharged in time naturally under the carrying of the carrier gas one and parses tank, into the first detector,
The operation control unit is persistently acquired the detection signal of first detector, handles and record；" first is steady for record
The time point of stream valve-parsing tank-pneumatic filter " gas circuit connection；
4) it weighs core quality: weighing to the core sample for completing parsing test, weigh and record its quality m0；
5) measurement bound gas product: a certain amount of core sample after step 3) parsing test is taken, weighs and records its quality
m1, its bound gas volume is measured with step 1) and the identical method and condition of step 3) after closed crushing；
6) test result is calculated；
Specific step is as follows for the gas composition analysis method:
1) it acquires sample: under the carrying of carrier gas one, parsing the gas parsed in tank and successively pass through pneumatic filter, more than first
Port valve, the first load sample ring, the second multiple-way valve, the first multiple-way valve, third multiple-way valve, the second load sample ring, the first multiple-way valve, gas limit
During stream valve enters the progress gas content test of the first detector, regulate and control the first multiple-way valve, the second multiple-way valve, third multi-pass
Valve, switching gas circuit in the case where detection of uninterrupted first detector for the parsing gas for carrying out self-analytic data tank, acquires gas
Component analysis sample, the parsing gaseous sample for carrying the carrier gas 2 in first load sample ring enter hydrocarbon gas component analysis list
Member makes carrier gas three carry the parsing gaseous sample in the second load sample ring and enters inorganic gas component analysis unit, carries out resolution gas
Body component analysis；Record the time point of gas composition analysis sample acquisition gas circuit switching；
2) component is analyzed:
A, it analyzes hydrocarbon gas component: adjusting the first multiple-way valve, the second multiple-way valve, carrier gas two is made to pass through the second multiple-way valve, first
Multiple-way valve, which carries the gaseous sample in the first load sample ring and enters the first splitter by the second multiple-way valve, carries out component separation, with the
Two detectors are detected, and carry out quantitative analysis to hydrocarbon gas component；
B, it analyzes inorganic gas component: adjusting the first multiple-way valve, third multiple-way valve, the 4th multiple-way valve, the 5th multiple-way valve, make carrier gas
Three carry the gaseous sample in the second load sample ring via third multiple-way valve, the 4th multi-pass by third multiple-way valve, the first multiple-way valve
Valve, the 5th multiple-way valve sequentially enter the second splitter, third splitter, the 4th splitter and carry out component separation, are detected with third
Device is detected, and carries out quantitative analysis to inorganic gas component；
3) calculated result:
A, the chromatographic peak area correction coefficient of the second detector, third detector is demarcated respectively；
B, the detection based on the second detector to methane, ethane, propane, iso-butane, normal butane, isopentane, pentane in sample
Signal data, the chromatographic peak area of difference each gas component of integral calculation, further according to it respectively for the chromatography of the second detector
Peak area correction coefficient calculates separately the body with methane of ethane in sample, propane, iso-butane, normal butane, isopentane, pentane
Volume fraction on the basis of fraction；
C, methane, nitrogen, oxygen, carbon monoxide, the signal of carbon dioxide are strong in the sample based on third detector detection record
Degree evidence calculates separately the chromatographic peak area of each gas component, further according to it respectively for the chromatographic peak area of third detector
Correction coefficient calculates the volume point in sample on the basis of the volume fraction by methane of nitrogen, oxygen, carbon monoxide, carbon dioxide
Number；
D, ethane, propane, iso-butane, normal butane, the isopentane, positive penta detected based on the second detector and third detector
Alkane, nitrogen, oxygen, carbon monoxide, carbon dioxide the volume fraction by methane on the basis of volume fraction, with normalization method meter
Calculate methane, ethane, propane, iso-butane, normal butane, isopentane, pentane, oxygen, nitrogen, carbon monoxide, carbon dioxide gas
The relative volume fraction of component.
8. analysis method as claimed in claim 7, which is characterized in that the tool of the step 6) of the shale measurement of air content
Gymnastics is made as follows:
A, hydro carbons is calculated according to the detection signal data of first detector and parses gas volume Vdes；
B, the detection signal number of the first detector according to the parsing test of the step 3) of the shale measurement of air content
According to, according to parsing time sequencing calculate different parsing time point T parse gas accumulative hydro carbons parsing gas volume Vdes(ac),
And draw relation curve T-V of parsing time and accumulative hydro carbons parsing gas volumedes(ac)Curve；According to the parsing time and tire out
It counts hydro carbons and parses gas volume relationship curve, calculate core sample and enter the loss gas volume V parsed before tanklos；
C, according to following equation 1) calculate core sample in hydro carbons free gas content Gfree:
D, the detection of the first detector according to the product test of the step 5) bound gas of the shale measurement of air content
Signal data calculates bound gas volume Vres, according to following formula 2) calculate core sample in hydro carbons bound gas content
Gres:
E, according to following formula 3) calculate core sample in hydrocarbon gas overall content G:
G=Gfree+Gres 3)
Agreement: formula 1), formula 2) and formula 3) in, gas volume Vdes、Vdes(ac)、Vlos、VresUnit be milliliter (mL), core sample
Quality m0And m1Unit be gram (g), gas content G, Gfree、GresUnit be every gram of milliliter (mL/g) or cubic meter it is per ton
(m3/t)。
9. analysis method as claimed in claim 7, which is characterized in that the gaseous sample in the first load sample ring, the second load sample ring
It acquires simultaneously.
10. analysis method as claimed in claim 7, which is characterized in that in the step 2) of the gas composition analysis method
Step a, step b can be carried out simultaneously, can also be separated and be carried out.
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