CN112147208B - In mineral particles 4 He quantitative device and method and uranium-thorium/helium dating method - Google Patents
In mineral particles 4 He quantitative device and method and uranium-thorium/helium dating method Download PDFInfo
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- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 106
- 239000011707 mineral Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims description 49
- 229910052734 helium Inorganic materials 0.000 title claims description 18
- 239000001307 helium Substances 0.000 title claims description 17
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 title claims description 14
- GFRMDONOCHESDE-UHFFFAOYSA-N [Th].[U] Chemical compound [Th].[U] GFRMDONOCHESDE-UHFFFAOYSA-N 0.000 title claims description 13
- 238000010790 dilution Methods 0.000 claims abstract description 51
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- 238000012545 processing Methods 0.000 claims abstract description 29
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- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000007865 diluting Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 46
- 229910052845 zircon Inorganic materials 0.000 claims description 38
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 38
- 229910052586 apatite Inorganic materials 0.000 claims description 28
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
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- 238000011002 quantification Methods 0.000 claims description 19
- 108010083687 Ion Pumps Proteins 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- DNXNYEBMOSARMM-UHFFFAOYSA-N alumane;zirconium Chemical compound [AlH3].[Zr] DNXNYEBMOSARMM-UHFFFAOYSA-N 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- 239000003085 diluting agent Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052770 Uranium Inorganic materials 0.000 claims description 8
- 239000012086 standard solution Substances 0.000 claims description 8
- 229910000628 Ferrovanadium Inorganic materials 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- ZGTNJINJRMRGNV-UHFFFAOYSA-N [V].[Fe].[Zr] Chemical compound [V].[Fe].[Zr] ZGTNJINJRMRGNV-UHFFFAOYSA-N 0.000 claims description 7
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000009489 vacuum treatment Methods 0.000 claims description 6
- 238000009616 inductively coupled plasma Methods 0.000 claims description 5
- 238000004445 quantitative analysis Methods 0.000 claims description 5
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims description 3
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- 239000007924 injection Substances 0.000 abstract description 3
- 239000003208 petroleum Substances 0.000 abstract description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 11
- BILXWNHAXOTCQI-UHFFFAOYSA-N [Pb].[U] Chemical compound [Pb].[U] BILXWNHAXOTCQI-UHFFFAOYSA-N 0.000 description 9
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- 229910052758 niobium Inorganic materials 0.000 description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 5
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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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Physics & Mathematics (AREA)
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- Electrochemistry (AREA)
- Engineering & Computer Science (AREA)
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- Molecular Biology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of petroleum exploration, and relates to a mineral particle 4 He quantitative device. The quantitative device comprises: the device comprises a laser heating system, a purification and enrichment system, a standard sample mixing system, a detection and analysis system, an automatic control and data processing system and a vacuum processing system; the laser heating system, the purification and enrichment system and the detection and analysis system are sequentially connected in series; the laser heating system is used for heating the mineral particles to enable the mineral particles to release gas, and extracting the gas, wherein the gas contains 4 He; the purification and enrichment system is used for purifying and enriching gas 4 He; the standard sample mixing system comprises 4 He standard metering tube, and apparatus 4 He standard quantitative tube connected 4 He standard tank, 3 He dilution metering tube and 3 he dilution metering tube communicates with 3 A He dilution tank; 4 he standard metering tube 4 He standard tank, and 3 he dilution metering tube 3 He diluting tanks are connected in parallel; the detection analysis system is used for detecting 4 He (He) 3 He content. The isotope dilution method is utilized, and the mineral particles can be accurately detected by one sample injection 4 He content.
Description
Technical Field
The invention belongs to the technical field of petroleum exploration, and particularly relates to a mineral particle 4 He quantification apparatus and method and uranium-thorium/helium dating method.
Background
The (U-Th)/He is based on the disintegration of U, th radioactive elements in mineral particles such as apatite and zircon 4 He and at certain temperature point makes mineral particles enter a He closed system due to certain geological event and then starts a geological clock for a definite year, is a new technology of low-temperature thermal chronology research which is rapidly developed in recent years, mineral (U-Th)/He age refers to the time from the (U-Th)/He system to the present of rock cooling to the corresponding mineral, records the structure evolution history after the mineral is subjected to the closed temperature, is widely applied in the aspects of geologic body definite year, differential ablation, thermal evolution, topography and relief evolution, sediment source analysis and the like, and particularly has wide application prospect in the researches of structure lifting ablation time and ablation thickness recovery in a sediment basin, the age of thermal history dynamic evolution, petroleum generation after structure formation, the oil and gas reservoir adjustment transformation time caused by structure lifting, the constraint of the age of formation and the like. The invention provides a method and a device for determining the (U-Th)/He of mineral particles, which are used for determining the years of the selection of the mineral particles of apatite or zircon, releasing helium gas, decomposing the acid of the mineral particles, measuring the content of the U/Th, calculating the age and correcting the (U-Th)/He of the mineral particles, and providing a low temperature for determining the years of the geologic body, differential ablation, thermal evolution, topographic and geomorphic evolution, sediment source analysis and the likeThermal chronology information.
Patent document CN106908510a discloses a method for determining the uranium-lead age of zircon samples. The method comprises the following steps: (1) Embedding a zircon sample and a zircon standard substance into an epoxy resin to form a sample target; (2) Respectively carrying out laser ablation on zircon in the sample target by utilizing laser beams so as to obtain solid sol; (3) Loading the solid solution glue into a plasma ion source of a multi-receiving inductively coupled plasma mass spectrometer by using carrier gas for ionization, so as to obtain primary ions; (4) Passing the primary ions through the bifocal primary ions and calculating the raw uranium-lead ratio of the primary ions of the zircon sample and the zircon standard substance; (6) Correcting the raw uranium-lead ratio of the zircon sample using a known nominal uranium-lead ratio of the zircon standard substance and the measured raw uranium-lead ratio, thereby obtaining a corrected uranium-lead ratio of the zircon sample; (7) And calculating the uranium-lead age of the zircon sample by using the corrected uranium-lead ratio. The method has the following defects: the given uranium-lead age is crystallization age, and can only provide thermal chronology information under geological high-temperature conditions, but cannot give low-temperature thermal evolution history information.
Patent document CN108020862a discloses a method for determining the active time limit of brittle faults by apatite fission track yearly measurement. The specific disclosure is as follows: step one, analyzing a regional structure, namely acquiring stratum time division of a research area, rock invasion period, a geoconstruction unit, earth dynamic background and fault activity data, particularly the period and the property of fault activity, and determining a fault to be specifically researched through the regional structure analysis; step two, collecting field samples, namely collecting samples at specific faults to be researched, wherein the samples comprise an upper disc sample, a lower disc sample and a fault zone sample; analyzing experimental data, namely analyzing data obtained by testing an apatite sample, and grasping cooling age and track distribution characteristic information of the sample in detail; judging the activity time of the fault, and preliminarily determining the possible activity time of the fault through judging the property of the fault, and the cooling age and track distribution characteristic information of the samples in the upper and lower plates of the fault and the step three; step five, simulating a cooling history, namely inverting all T-T evolution tracks of the samples by performing temperature time simulation on the track age and the track length of the samples, and verifying whether the fault activity time in the step four is correct; and step six, comprehensively utilizing regional geological data, and verifying the fault activity time again. The method has the following defects: the length, density and the like of particle tracks generated in the nuclear decay process of apatite and zircon are adopted for measuring the fissile track, and the accuracy of the fixed year is relatively low.
Disclosure of Invention
The invention aims to provide a method for preparing a sample in mineral particles with low sealing temperature and high detection accuracy 4 He quantification apparatus and method and uranium-thorium/helium dating method.
In order to achieve the above object, the present invention provides a mineral particle 4 He quantitative device. The quantitative device comprises: the device comprises a laser heating system, a purification and enrichment system, a standard sample mixing system, a detection and analysis system, an automatic control and data processing system and a vacuum processing system;
the laser heating system, the purification and enrichment system and the detection and analysis system are sequentially connected in series;
the laser heating system is used for heating mineral particles to enable the mineral particles to release gas, and extracting the gas, wherein the gas contains 4 He；
The purification and enrichment system is used for purifying and enriching the gas 4 He；
The standard sample mixing system comprises 4 He standard metering tube and the method 4 He standard quantitative tube connected 4 He standard tank, 3 He dilution quantitative tube and the same 3 He dilution metering tube communicates with 3 A He dilution tank; the said 4 He standard metering tube and the same 4 He standard tank, and the 3 He dilution metering tube and the same 3 He diluting tanks are connected in parallel;
the detection analysis system is used for detecting 4 He (He) 3 Content of He;
the vacuum treatment system is used for carrying out vacuum treatment on the quantitative device;
the automatic control and data processing system is used for controlling the laser heating system, the purification and enrichment system, the standard sample mixing system, the detection and analysis system and the vacuum processing system and calculating the mineral particles 4 He content.
Specifically, the standard sample mixing system further comprises 4 He calibration metering tube, and apparatus therefor 4 He calibration metering tube communicates 4 He calibration tank, an 4 He calibration metering tube and the same 4 He calibration tank, and the 4 He standard metering tube and the same 4 He standard tanks are connected in parallel.
More specifically, the standard sample mixing system further comprises: is arranged at the said 4 A first pneumatic valve arranged on the gas outlet end pipeline of the He standard metering tube and arranged on 4 He standard metering tube and the device 4 A second pneumatic valve arranged on the communicating pipe of the He standard tank and arranged on the 3 A third pneumatic valve arranged on the air outlet end pipeline of the He dilution quantitative pipe and arranged on the air outlet end pipeline 3 He dilution metering tube and the device 3 And a fourth pneumatic valve on the communicating pipe line of the He diluting tank.
More specifically, the 4 He standard metering tube, the 3 He dilution quantitative tube and the same 4 A He calibration metering tube is in communication with the purification enrichment system.
More specifically, the 4 He standard metering tube, the 3 He dilution quantitative tube and the same 4 He calibrates the volume of the metering tube the same.
More specifically, the standard sample mixing system further comprises: is arranged at the said 4 Fifth pneumatic valve on air outlet end pipeline of He calibration quantitative pipe and arranged on the same 4 He calibrates the metering tube and the 4 He calibrates the sixth pneumatic valve on the tank connection line.
Specifically, the laser heating system includes: a diode laser heater, a lens focusing system, a sample cell, and a sample tray;
the laser emitted by the diode laser heater heats mineral particles in the sample tray through the lens focusing system;
the sample tray is positioned on the sample cell;
the sample cell drives the sample tray to rotate so that laser emitted by the diode laser heater is aligned with the mineral particles in the sample tray for heating.
Specifically, the purification and enrichment system comprises: an activated carbon cold trap, a zirconium aluminum aspirator and a zirconium ferrovanadium aspirator which are sequentially connected in series; the zirconium ferrovanadium aspirator is arranged close to the detection and analysis system.
More specifically, the activated carbon cold trap is in line communication with the sample tray.
More specifically, a first electromagnetic valve is arranged on a pipeline of the laser heating system communicated with the activated carbon cold trap;
a seventh pneumatic valve is arranged on a communicating pipe between the air outlet end of the zirconium aluminum aspirator and the standard sample mixing system;
an eighth pneumatic valve is arranged on a pipeline close to the air inlet end of the zirconium ferrovanadium aspirator.
In particular, the detection analysis system comprises a quadrupole mass spectrometer.
Specifically, the vacuum processing system includes: a mechanical pump, a molecular pump, an ion pump, a mechanical pump pressure meter monitor, a molecular pump pressure meter monitor, an ion pump pressure meter monitor, a second solenoid valve, a third solenoid valve, a fourth solenoid valve, and a ninth pneumatic valve;
the mechanical pump is connected with the molecular pump in series;
the mechanical pump pressure gauge monitor, the molecular pump pressure gauge monitor, and the ion pump pressure gauge monitor vacuum pressures of the mechanical pump, the molecular pump, and the ion pump, respectively;
the second electromagnetic valve controls the mechanical pump to vacuumize the quantitative device;
the third electromagnetic valve is arranged on a connecting pipeline between the mechanical pump and the molecular pump;
the ninth pneumatic valve is arranged on a pipeline which is communicated with the purification and enrichment system through the molecular pump;
and the fourth electromagnetic valve controls the ion pump to vacuumize the quantitative device.
More specifically, the ninth pneumatic valve is arranged on a main pipeline of the molecular pump, wherein the main pipeline is communicated with the air outlet end of the zirconium aluminum getter and the air inlet end of the zirconium vanadium iron getter.
The invention also provides a mineral particle 4 He quantification method. The quantitative method is carried out in the quantitative device, and comprises the following steps:
s1, selecting and measuring mineral particles;
s2, vacuumizing the quantifying device through the vacuum treatment system;
s3, heating the mineral particles by the laser heating system so as to enable the mineral particles to release gas;
s4, purifying and enriching the gas by using the purifying and enriching system 4 He; the said 3 He diluting tank toward the 3 He dilution metering tube release 3 He up to the point 3 The pressure of the He dilution quantitative tube is a first preset pressure; the said 4 He standard tank is directed to 4 He standard dosing tube release 4 He up to the point 4 The pressure of the He standard metering tube is a second preset pressure; from the said 3 In He dilution metering tubes 3 He. From the said 4 In He standard metering tubes 4 He. In the gas 4 He forms a mixed gas, and enters the detection analysis system for detection;
s5, calculating the mineral particles according to the detection result of the step S4 4 He content.
Specifically, the mineral particles are apatite or zircon.
In detail, step S1 is to observe the crystal form, the degree of breakage, the degree of development of inclusion, cracks, and inclusion of impurities of the mineral particles by using a stereo microscope, and to select 3 to 5 mineral particles having no inclusion or inclusion having a diameter of less than 10 μm, no cracks, and no impurities, and having a height and width of 60 μm or more.
More specifically, the quantification method further comprises: by using the said 4 He calibration metering tube and the same 4 He calibration tank pair 4 He standard tanks were calibrated.
More specifically, step S4 includes the steps of:
opening the first electromagnetic valve, and sequentially absorbing non-gases in the gas by the activated carbon cold trap and the zirconium aluminum getter 4 He composition;
opening the fourth pneumatic valve and the second pneumatic valve respectively, the 3 He diluting tank toward the 3 He dilution metering tube release 3 He, described 4 He standard tank is directed to 4 He standard dosing tube release 4 He up to the point 3 The pressure of the He dilution quantitative tube is a first preset pressure, the 4 The pressure of the He standard metering tube is a second preset pressure, the fourth pneumatic valve and the second pneumatic valve are closed, the third pneumatic valve and the first pneumatic valve are opened, and the He standard metering tube is from the following components 3 In He dilution metering tubes 3 He. From the said 4 In He standard metering tubes 4 He. In the gas 4 He forms a mixed gas;
opening the eighth pneumatic valve, and absorbing non-matters in the mixed gas by the zirconium ferrovanadium aspirator 4 He component, and then enters the detection analysis system for detection.
Specifically, the quantification method further includes: an automated control and data processing system controls the laser heating system, the purification enrichment system, the standard sample mixing system, the detection analysis system, and the vacuum processing system, and calculates the mineral particles 4 He content.
The invention also provides a uranium-thorium/helium annual method in the mineral particles. The uranium-thorium/helium dating method comprises the quantitative method, and the uranium-thorium/helium dating method comprises the following steps:
s6, continuing to the mineral particlesAcid digestion is carried out continuously, and the mineral particles are measured 238 U/ 235 Ratio of U 232 Th/ 230 Ratio of Th;
s7, according to the mineral particles 4 He、 238 U/ 235 Ratio of U 232 Th/ 230 The ratio of Th, combined with the uranium/thorium-helium decay equation, calculates the apparent age of the mineral particles.
Specifically, the step S6 includes the steps of:
formulation with known 238 U/ 235 U and 232 Th/ 230 a standard solution of Th ratio;
preparing acid liquor, and diluting the acid liquor to a constant volume to prepare a blank control;
preparing a blank control containing a metal capsule;
dissolving the mineral particles wrapped by the metal capsules by using acid liquor, and adding the known mineral particles 238 U/ 235 U and 232 Th/ 230 the isotope diluent with the Th ratio is prepared into a sample to be measured by constant volume;
measuring at least one blank, at least 1 metal capsule blank, at least 1 standard solution and the sample to be measured using an inductively coupled plasma mass spectrometer 238 U/ 235 Ratio of U 232 Th/ 230 Ratio of Th.
Specifically, the mineral particles are apatite or zircon;
in the case where the mineral particles are apatite, the acid solution is a nitric acid solution;
in the case where the mineral particles are zircon, the acid solution includes a mixed solution of hydrofluoric acid and nitric acid, and a hydrochloric acid solution; firstly, dissolving zircon by using a mixed solution of hydrofluoric acid and nitric acid under the heating condition, and adding a hydrochloric acid solution for dissolving after the mixed solution is evaporated, so that the zircon is completely dissolved.
In the mineral particles provided by the invention 4 He quantitative device, using isotope dilution method, can accurately detect mineral particles by one sample injection 4 The content of He is small, the required sample amount is small, only single particles are needed, and the sample preparation period is short.
In the mineral particles provided by the invention 4 He dosing device has a calibration function.
In the mineral particles provided by the invention 4 He dosing device is capable of removing a substantial portion of the impurity gases, such as H, generated by mineral particles during heating 2 、CO、CO 2 、H 2 O, SO 2 The detection result is more accurate.
The invention provides a mineral particle 4 He quantitative method, utilizing isotope dilution method, can accurately detect mineral particles through one sample injection 4 The content of He is small, the required sample amount is small, only single particles are needed, and the sample preparation period is short.
The sealing temperature of the apatite and zircon (U-Th)/He dating system is lower than that of minerals of any other known dating method (the sealing temperature of the apatite and the zircon He is 75-90 ℃ and 170-190 ℃), and the maximum advantage is sensitivity to low-temperature conditions, so that the low-temperature evolution research range of rock is widened; the required sample amount is small, only single particles are needed, and the sample preparation period is short; the isotope content can be measured with high precision by using a quadrupole mass spectrometer, and the measuring precision is higher; the age given has a low-temperature thermal chronology meaning for the last phase of the cooling effect.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 shows a mineral particle according to the invention 4 Schematic diagram of He dosing device.
FIG. 2 shows another mineral particle according to the invention 4 Schematic diagram of He dosing device.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein.
Example 1
Example 1 provides a mineral particle 4 He quantitative device. As shown in fig. 1, the quantitative device includes: a laser heating system 10, a purification enrichment system 20, a standard sample mixing system 30, a detection analysis system 40, and a vacuum processing system 60; the laser heating system 10, the purification and enrichment system 20 and the detection and analysis system 40 are sequentially connected in series; the laser heating system 10 is used to heat the mineral particles so that the mineral particles release gas and extract the gas, the gas containing 4 He; the purification and enrichment system 20 is used to purify enriched gas 4 He; the standard mixing system 30 includes 4 He standard metering tube 302, and 4 the He standard metering tube 302 is connected with 4 He standard tank 301, 3 He dilution metering tube 304, and 3 he dilution quantitative tube 304 is connected with 3 He dilution tank 303, 4 He calibration metering tube 306, and 4 he calibration metering tube 306 is in communication with 4 He calibrates the tank 305; 4 he standard metering tube 302 4 A He standard tank 301, 3 he dilution metering tube 304 3 He dilution tank 303 4 He calibration tank 305 4 The He calibration quantitative pipes 306 are connected in parallel; the detection analysis system 40 is used for detection 4 He (He) 3 Content of He; the vacuum processing system 60 is used for vacuum processing the dosing device.
Example 2
Example 2 provides a mineral particle 4 He quantitative device. As shown in fig. 2, the quantitative device includes: a laser heating system 10, a purification enrichment system 20, a standard sample mixing system 30, a detection analysis system 40, and a vacuum processing system 60; the laser heating system 10, the purification and enrichment system 20 and the detection and analysis system 40 are sequentially connected in seriesThe method comprises the steps of carrying out a first treatment on the surface of the The laser heating system 10 is used to heat the mineral particles so that the mineral particles release gas and extract the gas, the gas containing 4 He; the purification and enrichment system 20 is used to purify enriched gas 4 He; the automated control and data processing system 50 is used to control the laser heating system 10, the purification and enrichment system 20, the standard sample mixing system 30, the detection and analysis system 40, and the vacuum processing system 60, and calculate the mineral particles 4 Content of He; the detection analysis system 40 is used for detection 4 He (He) 3 Content of He; the vacuum processing system 60 is used for vacuum processing the dosing device.
The laser heating system 10 includes: a diode laser heater 101, a lens focusing system 102, a sample cell 103, and a sample plate 104; wherein the laser emitted by the diode laser heater 101 heats the mineral particles in the sample tray 104 via the lens focusing system 102; sample pan 104 is positioned on sample cell 103; the sample cell 103 drives the sample plate 104 to rotate so that the laser light emitted from the diode laser heater 101 is directed to the mineral particles in the sample plate 104 for heating.
The purification and enrichment system 20 includes: an activated carbon cold trap 201, a zirconium aluminum getter 202 and a zirconium vanadium iron getter 203 which are sequentially connected in series; the zirconium ferrovanadium aspirator 203 is arranged near the detection and analysis system 40; a first electromagnetic valve C1 is arranged on a pipeline of the laser heating system 10 communicated with the activated carbon cold trap 201; a seventh pneumatic valve F7 is arranged on a communicating pipe between the air outlet end of the zirconium aluminum aspirator 202 and the standard sample mixing system 30; an eighth pneumatic valve F8 is provided in the line near the intake end of the zirconium vanadium iron aspirator 203.
The standard mixing system 30 includes 4 He standard metering tube 302, and 4 the He standard metering tube 302 is connected with 4 He standard tank 301, 3 He dilution metering tube 304, and 3 he dilution quantitative tube 304 is connected with 3 He dilution tank 303, 4 He calibration metering tube 306, and 4 he calibration metering tube 306 is in communication with 4 He calibrates the tank 305; 4 he standard metering tube 302 4 A He standard tank 301, 3 he dilution metering tube 304 3 He dilution tank 303 4 He calibration tank 305 4 The He calibration quantitative pipes 306 are connected in parallel; is arranged at 4 First pneumatic valve F1 on the gas outlet end line of He standard metering tube 302, disposed on 4 He standard metering tube 302 4 A second pneumatic valve F2 arranged on the communicating pipe line of the He standard tank 301 3 A third pneumatic valve F3 on the outlet end line of the He dilution quantitative pipe 304 and arranged on 3 He dilution quantitative tube 304 3 A fourth pneumatic valve F4 on the He dilution tank 303 communicating line; is arranged at 4 Fifth pneumatic valve F5 on the outlet end line of He calibration quantitative tube 306 and disposed on 4 He calibrates the metering tube 306 4 He calibrates the sixth pneumatic valve F6 on the tank 305 communication line.
The detection analysis system 40 comprises a quadrupole mass spectrometer.
The detection analysis system 40 is used for detection 4 He (He) 3 Content of He; the vacuum processing system 60 is used for vacuum processing the dosing device.
The vacuum processing system 60 includes: a mechanical pump 601, a molecular pump 602, an ion pump 603, a mechanical pump pressure gauge monitor 604, a molecular pump pressure gauge monitor 605, an ion pump pressure gauge monitor 606, a second solenoid valve C2, a third solenoid valve C3, a fourth solenoid valve C4, and a ninth pneumatic valve F9;
the mechanical pump 601 is connected in series with the molecular pump 602;
mechanical pump pressure gauge monitor 604, molecular pump pressure gauge monitor 605, and ion pump pressure gauge monitor 606 monitor the vacuum pressures of mechanical pump 601, molecular pump 602, and ion pump 603, respectively;
the second electromagnetic valve C2 controls the mechanical pump 601 to vacuumize the quantitative device;
the third solenoid valve C3 is provided on a connection line between the mechanical pump 601 and the molecular pump 602;
the ninth pneumatic valve F9 is arranged on a main pipeline of the molecular pump 602, which is communicated with the air outlet end of the zirconium aluminum getter 202 and the air inlet end of the zirconium vanadium iron getter 203;
the fourth solenoid valve C4 controls the ion pump 603 to evacuate the dosing device.
Example 3
Implementation of the embodimentsExample 3 provides a mineral particle 4 He quantification method. The quantitative method is carried out in the quantitative device, and comprises the following steps:
s1, selecting and measuring mineral particles.
S2, vacuumizing the quantifying device through a vacuum treatment system 60.
S3, the laser heating system 10 heats the mineral particles so that the mineral particles release gas.
S4, purifying and enriching the enriched gas by using the purifying and enriching system 20 4 He； 3 He dilution tank 303 is oriented 3 He dilution metering tube 304 release 3 He up to 3 The pressure of He dilutes metering tube 304 to a first preset pressure; 4 he standard tank 301 orientation 4 He standard metering tube 302 release 4 He up to 4 The pressure of the He standard metering tube 302 is a second preset pressure; from 3 In He dilution quantitative tube 304 3 He. From 4 In He standard metering tube 302 4 He. In the gas 4 He forms a mixture that enters the detection analysis system 40 for detection.
S5, calculating mineral particles according to the detection result of the step S4 4 He content.
Example 4
Example 4 provides a mineral particle 4 He quantification method. The quantifying method comprises the following steps:
s1, turning on a power supply, reflected light and transmitted light of a stereoscopic microscope with binoculars, adjusting the height of a lens column, and adjusting the brightness and the magnification of lamplight; the apatite or zircon particles are placed on a glass slide dipped with alcohol and placed on a stereo microscope stage; observing crystal forms, crushing degrees, inclusion development, cracks and impurity-containing conditions of the apatite or zircon particles in a view field under a 200-time mirror, selecting 3-5 self-formed apatite or zircon crystals which are relatively good in crystal forms, free of rounding, free of crushing, free of inclusion or inclusion as much as possible less than 10 mu m, free of cracks and free of impurities, and have heights and widths of more than 60 mu m, selecting proper particles, carrying out detailed description, and measuring and photographing the shapes, the length, the width, the height and the like of the selected mineral particles so as to carry out final age correction; and then loading the apatite, the zircon particles, 1-2 standard samples of the apatite and 1-2 standard samples of the zircon with the platinum capsule and the niobium capsule respectively, flattening the two ends of the platinum capsule and the niobium capsule by forceps to ensure that the particles cannot fall off from the capsules, and putting the loaded particles into a sample bottle with a coded sample number. 1-2 apatite standard samples and 1-2 zircon standard samples are used for verifying whether the detection result is reliable.
S2, sequentially opening the mechanical pump 601 and the second electromagnetic valve C2 to vacuumize, closing the second electromagnetic valve C2 after vacuuming for 4-5 min, opening the molecular pump 602, and opening the third electromagnetic valve C3, the first electromagnetic valve C1 and the ninth pneumatic valve F9 to vacuumize continuously; when the vacuum degree of the molecular pump 602 reaches 1E-7mbar, the ion pump 603, the fourth electromagnetic valve C4, the eighth pneumatic valve F8 and the four-stage rod mass spectrometer are opened, the vacuum degree of the device to be metered reaches 1E-8mbar, and the seventh pneumatic valve F7, the fourth electromagnetic valve C4, the eighth pneumatic valve F8 and the ion pump 603 are sequentially closed.
S3, starting a 970nm diode laser 101, a lens focusing system 102 and a sample cell 103, positioning a sample disc 104 according to the number, and setting coordinates to ensure that each sample can be found by the diode laser 101; under the irradiation of a diode laser 101 with the working current of 8-12A, heating apatite at the constant temperature of 900-1000 ℃ for 3-5 min; zircon is heated at a constant temperature of 1200 ℃ for 10min to 12min under the irradiation of a diode laser 101 with an operating current of 14A to 16A, in order to ensure that the zircon is in the particles 4 He release was complete, each sample had to be tested at least twice repeatedly, and the last test was considered to be less than 1% of the total 4 He is completely released.
S4, starting the zirconium aluminum aspirator 202, setting the voltage of the zirconium aluminum aspirator 202 to be 35V and the temperature to be 350 ℃, and removing part H after the gas is frozen and enriched by the active carbon cold trap 201 2 O、CO 2 、SO 2 Wait gas and then remove H through the zirconium aluminum getter 202 2 、CO、SO 2 An inert gas. The fourth pneumatic valve F4 and the second pneumatic valve F2 are opened respectively, 3 he dilution tank 303 is oriented 3 He dilution rationTube 304 release 3 He， 4 He standard tank 301 orientation 4 He standard metering tube 302 release 4 He up to 3 The He dilutes the pressure of the metering tube 304 to a first preset pressure, 4 the He gauge tube 302 has a second preset pressure, closes the fourth pneumatic valve F4 and the second pneumatic valve F2, and opens the third pneumatic valve F3, the first pneumatic valve F1, and the seventh pneumatic valve F7, from 3 In He dilution quantitative tube 304 3 He. From 4 In He standard metering tube 302 4 He. In a gas 4 He forms a mixture. Opening the eighth pneumatic valve F8, and absorbing non-matters in the mixed gas by the zirconium vanadium iron aspirator 203 4 He component, and then enters the quadrupole mass spectrometer for detection.
S5, calculating the content of the apatite and the zircon by the automatic control and data processing system 50 4 He content.
Example 5
Example 5 provides a uranium-thorium/helium annual process in mineral particles. The uranium-thorium/helium dating method further comprises the following steps: the following steps are continued for the apatite and zircon finish of example 4:
s6, cleaning a vessel, and preparing a standard solution and a blank solution: all vessels were treated with HNO 3 Cleaning the solution, heating on an electric furnace for 30min, repeatedly flushing with ultrapure water, and drying for later use; using diluent U with concentration of 25ng/mL 235 U/ 238 U= 0.007252 ± 0.000036) and Th at a concentration of 25ng/mL 230 Th/ 232 Th=0) was prepared as 25 μl of the mixed solution in a teflon flask, and 25 μl of the isotope diluent was added (wherein, 235 U＝15ng/mL， 230 Th＝5ng/mL， 235 U/ 238 U＝838±7， 230 Th/ 232 th=10.45±0.05), and ultrasonic-treating in an ultrasonic cleaner for 15min to prepare a standard solution with diluent.
25 mu L of 7mol/L HNO is added into a polytetrafluoroethylene sample dissolving bottle 3 Placing the mixture into an ultrasonic cleaner for ultrasonic oscillation for 15min, and then adding ultrapure water to dilute the mixture to 350 mu L to prepare a blank control.
Platinum capsules and niobium capsules were added to 2 blank controls, respectively, to prepare 1 platinum capsule-containing blank control and 1 niobium capsule-containing blank control.
Content determination of apatite particles U, th: will be released completely 4 The He mineral particles together with the Pt-loaded capsules were placed in a Teflon sample flask and 25. Mu.L of 7mol/L HNO was added 3 Solution and 25. Mu.L 235 U isotope diluent and 25. Mu.L 230 Placing a Th isotope diluent into a sample dissolving bottle added with the diluent into an ultrasonic cleaner, performing ultrasonic vibration for 15min, slowly heating to accelerate dissolution of apatite particles, standing at room temperature for more than 4h to ensure complete dissolution of apatite, and then adding ultrapure water to dilute to 350 mu L to prepare a sample to be detected; analyzing and measuring 1 blank control, 1 blank control containing platinum capsule, 1 standard solution and sample to be measured in each sample analysis process, and measuring U, th content on an inductively coupled plasma mass spectrometer (ICP-MS) to finally obtain apatite digestion solution 238 U/ 235 U、 232 Th/ 230 Th.
Zircon particle U, th content determination: will be released completely 4 The He mineral particles are put into a polytetrafluoroethylene sample dissolving bottle together with a niobium-loaded capsule, 300 mu L of HF solution and 50 mu L of HNO are added 3 Solution, 25. Mu.L 235 U isotope diluent and 25 mu L 230 Dissolving Th isotope diluent at 200deg.C for 72 hr, evaporating to dryness, adding 300 μL HCl solution, dissolving in oven at 200deg.C for 24 hr to ensure insoluble fluoride salt formed during dissolving process, cooling, evaporating to dryness, adding 200 μL HNO 3 And 25. Mu.L HF, then heating at low temperature on a hot plate for about 30min, evaporating to about 50. Mu.L, and diluting with ultra-pure water to 350. Mu.L; at least 1 blank control, 1 blank control containing Nb capsule, 1 standard solution and sample to be tested are analyzed and measured in each sample analysis process, and the U, th content is measured on an inductively coupled plasma mass spectrometer (ICP-MS) to finally obtain the mineral particle digestion solution 238 U/ 235 U、 232 Th/ 230 Th.
S7, respectively according to the apatite and zircon 4 He、 238 U/ 235 Ratio of U 232 Th/ 230 The ratio of Th, combined with the uranium/thorium-helium decay equation, calculates the apparent ages of the apatite and zircon, respectively.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (17)
1. In mineral particles 4 He dosing device, characterized in that it comprises: a laser heating system (10), a purification and enrichment system (20), a standard sample mixing system (30), a detection and analysis system (40), an automatic control and data processing system (50) and a vacuum processing system (60);
the laser heating system (10), the purification and enrichment system (20) and the detection and analysis system (40) are sequentially connected in series;
the laser heating system (10) is used for heating mineral particles to release gas from the mineral particles and extracting gas, the gas containing 4 He；
The purification and enrichment system (20) is used for purifying and enriching the gas 4 He；
The standard mixing system (30) comprises 4 He standard metering tube (302), and the device 4 He standard metering tube (302) is connected with 4 He standard tank (301), 3 He dilution quantitative tube (304), and the same 3 He dilution metering tube (304) is communicated with 3 A He dilution tank (303); the said 4 He standard metering tube (302) and said 4 He standard tank (301), and the 3 He dilution quantitative tube (304) and the method 3 He dilution tanks (303) are connected in parallel;
the detection analysis system (40) is used for detecting 4 He (He) 3 Content of He;
the vacuum processing system (60) is used for performing vacuum processing on the quantitative device;
the automatic control and data processing system (50) is used for controlling the laser heating system (10), the purification and enrichment system (20), the standard sample mixing system (30), the detection and analysis system (40) and the vacuum processing system (60) and calculating the mineral particles 4 He content.
2. In the mineral particles of claim 1 4 He dosing device, characterized in that the standard sample mixing system (30) further comprises 4 He calibration volume tube (306), and the same 4 He calibration metering tube (306) is connected with 4 He calibration tank (305), said 4 He calibration metering tube (306) and said 4 A He calibration tank (305), and the 4 He standard metering tube (302) and said 4 He standard tanks (301) are connected in parallel.
3. In the mineral particles according to claim 2 4 He dosing device, characterized in that the standard sample mixing system (30) further comprises: is arranged at the said 4 A first pneumatic valve (F1) arranged on the air outlet end pipeline of the He standard metering tube (302) 4 He standard metering tube (302) and the method 4 A second pneumatic valve (F2) arranged on the communicating pipe line of the He standard tank (301) 3 A third pneumatic valve (F3) arranged on the outlet end pipeline of the He dilution quantitative pipe (304) 3 He dilution quantitative tube (304) and the method 3 And a fourth pneumatic valve (F4) on the communicating pipe line of the He diluting tank (303).
4. In the mineral particles according to claim 2 4 He dosing device, characterized in that the standard sample mixing system (30) further comprises: is arranged at the said 4 A fifth pneumatic valve (F5) on the outlet end line of the He calibration quantitative pipe (306), and a valve provided on the outlet end line 4 He calibrates the quantitative tube (306) and the 4 And a sixth pneumatic valve (F6) on the communicating pipe line of the He calibration tank (305).
5. According to claim 1-4In any one of the mineral particles 4 He dosing device, characterized in that the laser heating system (10) comprises: a diode laser heater (101), a lens focusing system (102), a sample cell (103), and a sample plate (104);
wherein the laser emitted by the diode laser heater (101) heats mineral particles in the sample tray (104) via the lens focusing system (102);
the sample tray (104) is positioned on the sample cell (103);
the sample cell (103) drives the sample tray (104) to rotate so that laser emitted by the diode laser heater (101) is aligned with the mineral particles in the sample tray (104) for heating.
6. Mineral particles according to any one of claims 1 to 4 4 He quantification device, characterized in that the purification and enrichment system (20) comprises: an activated carbon cold trap (201), a zirconium aluminum getter (202) and a zirconium vanadium iron getter (203) which are sequentially connected in series; the zirconium ferrovanadium getter (203) is arranged close to the detection and analysis system (40).
7. In the mineral particles according to claim 6 4 He quantitative device, characterized by that, the said laser heating system (10) is provided with the first electromagnetic valve (C1) on the pipeline that the said activated carbon cold trap (201) communicates;
a seventh pneumatic valve (F7) is arranged on a communicating pipe between the air outlet end of the zirconium aluminum aspirator (202) and the standard sample mixing system (30);
an eighth pneumatic valve (F8) is arranged on the pipeline close to the air inlet end of the zirconium vanadium iron aspirator (203).
8. In the mineral particles according to claim 6 4 He quantification apparatus, characterized in that the detection analysis system (40) comprises a quadrupole mass spectrometer.
9. Mineral particles according to any one of claims 1 to 4 4 He rationDevice, characterized in that the vacuum treatment system (60) comprises: a mechanical pump (601), a molecular pump (602), an ion pump (603), a mechanical pump pressure gauge monitor (604), a molecular pump pressure gauge monitor (605), an ion pump pressure gauge monitor (606), a second solenoid valve (C2), a third solenoid valve (C3), a fourth solenoid valve (C4), and a ninth pneumatic valve (F9);
the mechanical pump (601) is connected in series with the molecular pump (602);
the mechanical pump pressure gauge monitor (604), the molecular pump pressure gauge monitor (605), and the ion pump pressure gauge monitor (606) monitor vacuum pressures of the mechanical pump (601), the molecular pump (602), and the ion pump (603), respectively;
the second electromagnetic valve (C2) controls the mechanical pump (601) to vacuumize the quantitative device;
the third electromagnetic valve (C3) is arranged on a connecting pipeline between the mechanical pump (601) and the molecular pump (602);
the ninth pneumatic valve (F9) is disposed on a line through which the molecular pump (602) communicates with the purification enrichment system (20);
the fourth electromagnetic valve (C4) controls the ion pump (603) to vacuumize the quantitative device.
10. In mineral particles 4 A He quantification method characterized in that the quantification method is performed in the quantification apparatus according to any one of claims 1 to 9, the quantification method comprising the steps of:
s1, selecting and measuring mineral particles;
s2, vacuumizing the quantifying device through the vacuum treatment system (60);
s3, heating the mineral particles by the laser heating system (10) so as to enable the mineral particles to release gas;
s4, purifying and enriching the gas by the purifying and enriching system (20) 4 He; the said 3 A He dilution tank (303) toward the 3 He dilution metering tube (304) release 3 He up to the point 3 The pressure of the He dilution quantitative tube (304) is a first preset valuePressure; the said 4 He standard tank (301) toward the 4 He standard metering tube (302) release 4 He up to the point 4 The pressure of the He standard metering tube (302) is a second preset pressure; from the said 3 In He dilution quantitative tube (304) 3 He. From the said 4 In He standard metering tubes (302) 4 He. In the gas 4 He forms a mixed gas, and enters the detection analysis system (40) for detection;
s5, calculating the mineral particles according to the detection result of the step S4 4 He content.
11. In the mineral particles of claim 10 4 He quantification method, characterized in that the mineral particles are apatite or zircon.
12. In the mineral particles of claim 10 4 A He quantification method, characterized in that the quantification method further comprises: by using the said 4 He calibration metering tube (306) and said 4 He alignment tank (305) pair 4 He standard tank (301) is calibrated.
13. In the mineral particles of claim 10 4 The He quantification method is characterized in that step S4 includes the steps of:
opening a first electromagnetic valve (C1), and sequentially absorbing non-gases in the gas by an activated carbon cold trap (201) and a zirconium aluminum getter (202) 4 He composition;
opening a fourth pneumatic valve (F4) and a second pneumatic valve (F2) respectively, said valves 3 A He dilution tank (303) toward the 3 He dilution metering tube (304) release 3 He, described 4 He standard tank (301) toward the 4 He standard metering tube (302) release 4 He up to the point 3 The He dilutes the pressure of the metering tube (304) to a first preset pressure, the 4 The pressure of the He standard metering tube (302) is a second preset pressure, the fourth pneumatic valve (F4) and the second pneumatic valve (F2) are closed, and the third pneumatic valve (F3) and the first pneumatic valve (F1) are opened from theThe said 3 In He dilution quantitative tube (304) 3 He. From the said 4 In He standard metering tubes (302) 4 He. In the gas 4 He forms a mixed gas;
opening an eighth pneumatic valve (F8), and absorbing non-matters in the mixed gas by a zirconium ferrovanadium aspirator (203) 4 He composition, and then enters the detection analysis system (40) for detection.
14. In the mineral particles of claim 13 4 A He quantification method, characterized in that the quantification method further comprises: an automatic control and data processing system (50) controls the laser heating system (10), the purification and enrichment system (20), the standard sample mixing system (30), the detection and analysis system (40), and the vacuum processing system (60), and calculates the mineral particles 4 He content.
15. A uranium-thorium/helium dating method in mineral particles, characterized in that it comprises the quantitative method of any one of claims 12 to 14, said uranium-thorium/helium dating method further comprising:
s6, continuously carrying out acid digestion on the mineral particles, and measuring the mineral particles 238 U/ 235 Ratio of U 232 Th/ 230 Ratio of Th;
s7, according to the mineral particles 4 He、 238 U/ 235 Ratio of U 232 Th/ 230 The ratio of Th, combined with the uranium/thorium-helium decay equation, calculates the apparent age of the mineral particles.
16. Uranium-thorium/helium dating method according to claim 15, wherein step S6 includes the steps of:
formulation with known 238 U/ 235 U and 232 Th/ 230 a standard solution of Th ratio;
preparing acid liquor, and diluting the acid liquor to a constant volume to prepare a blank control;
preparing a blank control containing a metal capsule;
dissolving the mineral particles wrapped by the metal capsules by using acid liquor, and adding known materials 238 U/ 235 U and 232 Th/ 230 the isotope diluent with the Th ratio is prepared into a sample to be measured by constant volume;
measuring at least one blank, at least 1 metal capsule blank, at least 1 standard solution and the sample to be measured using an inductively coupled plasma mass spectrometer 238 U/ 235 Ratio of U 232 Th/ 230 Ratio of Th.
17. The uranium-thorium/helium dating method of claim 16,
the mineral particles are apatite or zircon;
in the case where the mineral particles are apatite, the acid solution is a nitric acid solution;
in the case where the mineral particles are zircon, the acid solution includes a mixed solution of hydrofluoric acid and nitric acid, and a hydrochloric acid solution; firstly, dissolving zircon by using a mixed solution of hydrofluoric acid and nitric acid under the heating condition, and adding a hydrochloric acid solution for dissolving after the mixed solution is evaporated, so that the zircon is completely dissolved.
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