CN112147208A - In mineral particles4He quantitative device and method and uranium-thorium/helium dating method - Google Patents
In mineral particles4He quantitative device and method and uranium-thorium/helium dating method Download PDFInfo
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- 239000011707 mineral Substances 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims description 45
- 239000001307 helium Substances 0.000 title claims description 14
- 229910052734 helium Inorganic materials 0.000 title claims description 14
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 title claims description 11
- GFRMDONOCHESDE-UHFFFAOYSA-N [Th].[U] Chemical compound [Th].[U] GFRMDONOCHESDE-UHFFFAOYSA-N 0.000 title claims description 10
- 239000002245 particle Substances 0.000 claims abstract description 101
- 238000001514 detection method Methods 0.000 claims abstract description 46
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- 238000004458 analytical method Methods 0.000 claims abstract description 37
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- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims description 47
- 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 29
- 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 29
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- 238000004445 quantitative analysis Methods 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
- 229910052770 Uranium Inorganic materials 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 8
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- 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
- 229910000628 Ferrovanadium Inorganic materials 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- ZGTNJINJRMRGNV-UHFFFAOYSA-N [V].[Fe].[Zr] Chemical compound [V].[Fe].[Zr] ZGTNJINJRMRGNV-UHFFFAOYSA-N 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 5
- 238000009616 inductively coupled plasma Methods 0.000 claims description 5
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 claims description 5
- 238000011002 quantification Methods 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims description 4
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- 238000009472 formulation Methods 0.000 claims description 2
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- 229910052720 vanadium Inorganic materials 0.000 claims 1
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- 238000003113 dilution method Methods 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 8
- 230000000694 effects Effects 0.000 description 8
- 238000001816 cooling Methods 0.000 description 6
- 239000010955 niobium Substances 0.000 description 6
- 229910052776 Thorium Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 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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- RYYVLZVUVIJVGH-UHFFFAOYSA-N trimethylxanthine Natural products CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 1
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- 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
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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
- G01N1/34—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
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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
- G01N1/44—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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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the technical field of oil exploration, and relates to mineral particles4And (4) a He quantitative device. The dosing device comprises: the system 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 communicated in series; the laser heating system is used for heating the mineral particles to cause the mineral particles to release a gas and to extract the gas, the gas containing4He; the purification and enrichment system is used for purifying the enriched gasIn vivo4He; the standard sample mixing system comprises4He standard quantitative tube, and4communicated with He standard quantitative tube4A He standard tank,3He dilution quantitative tube, and3communicated with He dilution quantitative pipe3A He dilution tank;4he standard quantitative tube and4he standard can, with3He dilution quantitative tube and3the He dilution tanks are connected in parallel; detection analysis system for detecting4He and3he content. By using isotope dilution method, the mineral particles can be accurately detected by one-time sample introduction4He content.
Description
Technical Field
The invention belongs to the technical field of oil exploration, and particularly relates to a mineral particle medium4He quantification apparatus and method and uranium-thorium/helium dating method.
Background
The (U-Th)/He dating year is based on U, Th radioactive element disintegration generation in mineral particles such as apatite and zircon4He, mineral particles enter a He closed system at a certain temperature point due to a certain geological event so as to start a geological clock for dating, and the technology is a new technology for low-temperature thermal chronology research which is rapidly developed in recent years, wherein the age of the mineral (U-Th)/He refers to the time from the cooling of a rock to the closing of a corresponding mineral from the (U-Th)/He system to the present, the history of structural evolution of the mineral after the mineral is subjected to the closing temperature is recorded, and the history of structural evolution, the dating, the differential degradation, the thermal evolution, the topographic and topographic evolution, the sediment source analysis and the like of the geologic body are carried outThe method is widely applied, and particularly has wide application prospect in the research on the aspects of the formation lifting and denudation time and denudation thickness recovery in the sedimentary basin, the dynamic evolution of the thermal history, the petroleum generation era after the formation of the formation, the adjustment and modification time of the oil and gas reservoir caused by the lifting of the formation, the constraint of the storage age and the like. The invention provides a (U-Th)/He dating method and a device for mineral particles, which are used for dating (U-Th)/He dating method and analysis device for apatite or zircon mineral particle selection, helium release, mineral particle acid chemical digestion, U/Th content determination, age calculation and correction, and provide low-temperature thermal chronology information for geologic body dating, differential degradation, thermal evolution, topographic and topographic evolution, sediment source analysis and the like.
Patent document CN106908510A discloses a method for determining the uranium lead age of a zircon sample. The method comprises the following steps: (1) respectively embedding a zircon sample and a zircon standard substance into epoxy resin to prepare 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 sol into a plasma ion source of a multi-receiving inductively coupled plasma mass spectrometer by using carrier gas for ionization, thereby obtaining primary ions; (4) subjecting the primary ions to double focusing of the primary ions and calculating the original uranium-lead ratio of the primary ions of the zircon sample and the zircon standard; (6) correcting the original uranium-lead ratio of the zircon sample using the known nominal uranium-lead ratio and the measured original uranium-lead ratio of the zircon standard, 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 disadvantages: the given uranium-lead age is the crystallization age, and only the thermal chronology information of the geologic body under the high-temperature condition can be provided, but the low-temperature thermal evolution historical information cannot be provided.
Patent document CN108020862A discloses a method for determining the brittle fracture activity time limit by using apatite fission track dating. Specifically disclosed is: the method comprises the steps of firstly, analyzing the regional structure, acquiring stratum epoch division, magma invasion period, earth structure units, earth dynamics background and fault activity data of a research region, particularly the period and the property of fault activity, and determining a specific fault to be researched; collecting field samples, namely collecting samples at a specific fault 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 the cooling age and track distribution characteristic information of the sample in detail; step four, fault activity time judgment, namely preliminarily determining the possible activity time of the fault through judgment of fault properties, cooling ages and track distribution characteristic information of samples in the upper and lower disks of the fault and the step three; step five, cooling history simulation, namely performing temperature time simulation on the sample track age and the track length, inverting all sample T-T evolution tracks and verifying whether fault activity time in the step four is correct or not; and step six, comprehensively utilizing regional geological data, and verifying fault activity time again. The method has the following disadvantages: the fission track dating is obtained by adopting the length, the density and the like of particle tracks generated in the process of nuclear decay of apatite and zircon, and the dating precision is relatively low.
Disclosure of Invention
The invention aims to provide a method for detecting mineral particles with simple sample preparation, low sealing temperature and high detection accuracy4He quantification apparatus and method and uranium-thorium/helium dating method.
In order to achieve the above object, the present invention provides a mineral particle4And (4) a He quantitative device. The dosing device comprises: the system 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 communicated in series;
the laser heating system is used for heating mineral particles to make the mineral particles release gas and extract gas, and the gas contains4He；
The purification and enrichment system is used for purifying and enriching theIn a gas4He；
The standard sample mixing system comprises4He standard quantitative tube and the same4Communicated with He standard quantitative tube4A He standard tank,3He dilution quantitative tube and method for producing the same3Communicated with He dilution quantitative pipe3A He dilution tank; the above-mentioned4He standard quantitative tube and said4He standard can, and3he dilution quantitative tube and said3The He dilution tanks are connected in parallel;
the detection analysis system is used for detecting4He and3the 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 particles4He content.
Specifically, the standard sample mixing system further comprises4He calibration quantitative tube, and method for preparing the same4Communicated by He calibrating quantitative tube4He calibration tank, said4He calibration quantitative tube and said4He calibration tank, and said4He standard quantitative tube and said4He standard tanks are connected in parallel.
More specifically, the standard mixing system further comprises: is arranged at the4The first pneumatic valve on the air outlet end pipeline of the He standard quantitative pipe is arranged on the He standard quantitative pipe4He standard quantitative tube and the same4A second pneumatic valve arranged on the He standard tank communication pipeline3A third pneumatic valve arranged on the air outlet end pipeline of the He dilution quantitative pipe3He dilution quantitative tube and the same3The He dilution tank communicates with a fourth pneumatic valve on the line.
More particularly, the4He standard quantitative tube and method3He dilution quantitative tube, and the same4And the He calibration quantitative pipe is communicated with the purification enrichment system.
More particularly, the4He standard quantitative tube and method3He dilution quantitative tube, and the same4He calibrated burette volumes were the same.
More specifically, the standard mixing system further comprises: is arranged at the4A fifth pneumatic valve on the outlet end pipeline of the He calibration quantitative pipe and a valve arranged on the outlet end pipeline4He calibration quantitative tube and the same4The He calibration tank communicates with a sixth pneumatic valve on the line.
Specifically, the laser heating system includes: the device comprises a diode laser heater, a lens focusing system, a sample cell and a sample disc;
wherein the laser emitted by the diode laser heater heats the mineral particles in the sample disc through the lens focusing system;
the sample tray is positioned on the sample cell;
the sample cell drives the sample disc to rotate, so that laser emitted by the diode laser heater is aligned with the mineral particles in the sample disc to heat.
Specifically, the purification and enrichment system comprises: the activated carbon cold trap, the zirconium-aluminum aspirator and the zirconium-vanadium-iron aspirator are sequentially communicated in series; the zirconium ferrovanadium aspirator is arranged close to the detection and analysis system.
More specifically, the activated carbon cold trap is in communication with the sample tray via a pipeline.
More specifically, a first electromagnetic valve is arranged on a pipeline of the laser heating system communicated with the active carbon cold trap;
a seventh pneumatic valve is arranged on a communicating pipe line between the air outlet end of the zirconium-aluminum aspirator and the standard sample mixing system;
and an eighth pneumatic valve is arranged on the pipeline of the gas inlet end close to the zirconium ferrovanadium aspirator.
Specifically, the detection analysis system comprises a quadrupole mass spectrometer.
Specifically, the vacuum processing system includes: the system comprises a mechanical pump, a molecular pump, an ion pump, a mechanical pump pressure gauge monitor, a molecular pump pressure gauge monitor, an ion pump pressure gauge monitor, a second electromagnetic valve, a third electromagnetic valve, a fourth electromagnetic 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 respectively monitor the vacuum pressures of the mechanical pump, the molecular pump and the ion pump;
the second solenoid 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 of the molecular pump communicated with the purification enrichment system;
and the fourth electromagnetic valve controls the ion pump to vacuumize the quantitative device.
More specifically, the ninth pneumatic valve is arranged on a header line of the molecular pump communicated with the air outlet end of the zirconium aluminum aspirator and the air inlet end of the zirconium vanadium iron aspirator.
The invention also provides a mineral particle4He quantitative method. The quantitative method is carried out in the quantitative device, and the quantitative method comprises the following steps:
s1, selecting and measuring mineral particles;
s2, vacuumizing the quantitative device through the vacuum treatment system;
s3, heating the mineral particles by the laser heating system so that the mineral particles release gas;
s4, the purification and enrichment system purifies and enriches the gas4He; the above-mentioned3He diluting tank to3He dilution quantitative tube release3He up to said3The pressure of the He diluting quantitative pipe is a first preset pressure; the above-mentioned4He standard can to4He Standard quantitative tube Release4He up to said4The pressure of the He standard quantitative pipe is a second preset pressure; from the above3In He-diluting quantitative tube3He. From the above4In He standard quantitative tube4He. In said gas4Forming mixed gas by the He, and detecting the mixed gas in the detection analysis system;
s5, calculating the mineral particles according to the detection result of the step S44He content.
In particular, the mineral particles are apatite or zircon.
Specifically, step S1 is to observe the crystal form, the crushing degree, the inclusion development degree, the cracks and the impurity-containing condition of the mineral particles by using a stereo microscope, and 3-5 mineral particles which are free of inclusions or have inclusion diameters of less than 10 μm, no cracks and no impurities and have heights and widths of more than or equal to 60 μm are selected.
More specifically, the quantification method further comprises: by using the said4He calibration quantitative tube and said4He calibration tank pair4He standard can was 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 getter4A He component;
opening the fourth and second pneumatic valves, respectively, the3He diluting tank to3He dilution quantitative tube release3He, said4He standard can to4He Standard quantitative tube Release4He up to said3The pressure of the He diluting quantitative pipe is a first preset pressure, and4the pressure of the He standard quantitative pipe 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 quantitative pipe comes from3In He-diluting quantitative tube3He. From the above4In He standard quantitative tube4He. And in said gas4He forms mixed gas;
opening the eighth pneumatic valve, and absorbing non-gases in the mixed gas by the zirconium ferrovanadium aspirator4And the He component enters the detection analysis system for detection.
Specifically, the quantitative method further comprises: an automatic control and data processing system controls the laser heating system, the purification and enrichment system, the standard mixing system, the detection and analysis system, and the vacuum processing system, and calculates the concentration of the mineral particles4He content.
The invention also provides a method for determining the year of uranium-thorium/helium in mineral particles. The uranium-thorium/helium dating method comprises the quantitative method, and comprises the following steps:
s6, continuously carrying out acid chemical digestion on the mineral particles, and measuring the contents of the mineral particles238U/235The ratio of U and232Th/230the ratio of Th;
s7, according to the mineral particles4He、238U/235The ratio of U and232Th/230the 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:
the formulation has the known238U/235U and232Th/230a standard solution of the Th ratio;
preparing an acid solution, and diluting the acid solution to a constant volume to prepare a blank control;
preparing a blank control containing the metal capsule;
dissolving the mineral particles coated by the metal capsules by using acid liquor, and adding the known mineral particles238U/235U and232Th/230preparing a sample to be detected by using an isotope diluent with a Th ratio in a constant volume manner;
measuring at least one blank, at least 1 metal capsule blank, at least 1 standard solution and the sample to be measured by using an inductively coupled plasma mass spectrometer238U/235The ratio of U and232Th/230the ratio of Th.
In particular, the mineral particles are apatite or zircon;
in the case that 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, under the condition of heating, the zircon is dissolved by using a mixed solution of hydrofluoric acid and nitric acid, and after the mixed solution is evaporated, a hydrochloric acid solution is added for dissolving so as to completely dissolve the zircon.
In the mineral particles provided by the invention4He quantitative device, by using isotope dilution method, can accurately detect mineral particles by one-time sample injection4The content of He is not only the content, but also the required sample amount is small, the sample is only single particles, and the sample preparation period is short.
In the mineral particles provided by the invention4The He dosing device has a calibration function.
In the mineral particles provided by the invention4He dosing device is capable of removing a substantial portion of impurity gases, such as H, from mineral particles during heating2、CO、CO2、H2O, and SO2And the detection result is more accurate.
The invention provides a mineral particle4He quantitative method, which can accurately detect mineral particles by one-time sample injection by using isotope dilution method4The content of He is not only the content, but also the required sample amount is small, the sample is only single particles, 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 any other known dating method minerals (the sealing temperature of the apatite He is 75-90 ℃, and the sealing temperature of the zircon He is 170-190 ℃), and the apatite and zircon He sealing system has the greatest advantage of sensitivity to low-temperature conditions, so that the low-temperature thermal evolution research range of rocks is expanded; 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 utilizing a quadrupole mass spectrometer, and the measuring precision is higher; the age given has a low temperature thermal chronology meaning for the final stage of the cooling effect.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
FIG. 1 shows a mineral particle provided by the present invention4Schematic of He dosing apparatus.
FIG. 2 shows another mineral particle provided by the present invention4Schematic of He dosing apparatus.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Example 1
Example 1 provides a mineral granule4And (4) a He quantitative device. As shown in fig. 1, the dosing device comprises: a laser heating system 10, a purification and enrichment system 20, a standard sample mixing system 30, a detection and 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 communicated in series; the laser heating system 10 is used to heat mineral particles to cause the mineral particles to release a gas and extract the gas, the gas containing4He; purification enrichment System 20 for purifying enriched gas4He; the standard mixing system 30 comprises4He standard quantitative tube 302, and4communicated with He standard quantitative pipe 3024He standard can 301,3He dilution quantitative tube 304, and3connected by He dilution quantitative tube 3043He diluting tank 303,4He calibrating burette 306, and4he calibrating burette 3064 He calibration tank 305;4he standard quantitative tubes 302 and4the standard can 301 of He is used for,3he dilution quantitative tubes 304 and3he dilution tank 303, and4he calibration tanks 305 and4he calibration dosing tubes 306 are connected in parallel; the detection analysis system 40 is used for detection4He and3the content of He; the vacuum processing system 60 is used to vacuum process the dosing device.
Example 2
Example 2 provides a mineral granule4And (4) a He quantitative device. As shown in fig. 2, the dosing device comprises: a laser heating system 10, a purification and enrichment system 20, a standard sample mixing system 30, a detection and 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 communicated in series; the laser heating system 10 is used to heat mineral particles to cause the mineral particles to release a gas and extract the gas, the gas containing4He; purification enrichment System 20 for purifying enriched gas4He; 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 in4The content of He; the detection analysis system 40 is used for detection4He and3the content of He; the vacuum processing system 60 is used to vacuum process 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 tray 104; wherein, the laser emitted by the diode laser heater 101 heats the mineral particles in the sample disc 104 through the lens focusing system 102; sample pan 104 is positioned over sample cell 103; the sample cell 103 drives the sample plate 104 to rotate so that the laser emitted by the diode laser heater 101 is directed at the mineral particles in the sample plate 104 for heating.
The purification enrichment system 20 includes: the activated carbon cold trap 201, the zirconium-aluminum aspirator 202 and the zirconium-vanadium-iron aspirator 203 are sequentially communicated in series; the zirconium ferrovanadium getter 203 is arranged close to 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 active carbon cold trap 201; a seventh pneumatic valve F7 is arranged on a communicating pipeline 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 on the intake end line near the zircaloy aspirator 203.
The standard mixing system 30 comprises4He standard quantitative tube 302, and4communicated with He standard quantitative pipe 3024He standard can 301,3He dilution quantitative tube 304, and3connected by He dilution quantitative tube 3043He diluting tank 303,4He calibrating burette 306, and4he calibrating burette 3064 He calibration tank 305;4he standard quantitative tubes 302 and4the standard can 301 of He is used for,3he dilution quantitative tubes 304 and3he dilution tank 303, and4he calibration tanks 305 and4he calibration dosing tubes 306 are connected in parallel; is arranged at4A first pneumatic valve F1 arranged on the outlet end pipeline of the He standard quantitative pipe 3024He standard quantitative tubes 302 and4a second air-operated valve F2 arranged on the communication line of the He standard tank 3013A third pneumatic valve F3 arranged on the outlet end line of the He diluting quantitative pipe 3043He dilution quantitative tubes 304 and3he dilution tank 303 is connected to a fourth pneumatic valve F4 on the line; is arranged at4A fifth pneumatic valve F5 on the outlet end line of the He calibration dosing tube 306, and a valve disposed on the outlet end line of the He calibration dosing tube4He calibrating burette 306 and4he calibration tank 305 communicates with a sixth pneumatic valve F6 on the line.
The detection analysis system 40 comprises a quadrupole mass spectrometer.
The detection analysis system 40 is used for detection4He and3the content of He; the vacuum processing system 60 is used to vacuum process 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;
the mechanical pump pressure gauge monitor 604, the molecular pump pressure gauge monitor 605, and the ion pump pressure gauge monitor 606 monitor the 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;
a third electromagnetic valve C3 is provided on the connection line between the mechanical pump 601 and the molecular pump 602;
the ninth pneumatic valve F9 is arranged on a main pipeline which is communicated with the air outlet end of the zirconium aluminum aspirator 202 and the air inlet end of the zirconium vanadium iron aspirator 203 by the molecular pump 602;
the fourth solenoid valve C4 controls the ion pump 603 to evacuate the dosing device.
Example 3
Example 3 provides a mineral granule4He quantitative 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 quantitative 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 in the enriched gas by the purification and enrichment system 204He；3He diluting tank 303 to3 He dilution burette 304 release3He to3The pressure of the He dilution dosing tube 304 is a first preset pressure;4he standard can 301 to4He Standard burette 302 Release4He to4The pressure of He standard burette 302 is a second preset pressure; from3In He-diluting quantitative tube 3043He. From4In He standard quantitative tube 3024He. In said gas4He forms a gas mixture that enters the detection and analysis system 40 for detection.
S5, calculating the mineral particles according to the detection result of the step S44He content.
Example 4
Example 4 provides a mineral granule4He quantitative method. The quantitative method comprises the following steps:
s1, opening a power supply, reflected light and transmitted light of a stereo microscope with binoculars, adjusting the height of a lens column, and adjusting the brightness and the magnification of lamplight; placing apatite or zircon particles on a glass slide dipped with alcohol and placing the glass slide on a stereo microscope objective table; observing the crystal form, the crushing degree, the inclusion development, the cracks and the impurity-containing conditions of apatite or zircon particles in an observation area under a 200-fold lens, selecting 3-5 self-shaped apatite or zircon crystals which have relatively good crystal form, no rounding, no crushing, no inclusion as much as possible or no inclusion less than 10 mu m, no cracks and no impurities, and have the height and the width greater than 60 mu m, selecting proper particles, then describing in detail, and measuring and photographing the shapes, the lengths, the widths, the heights and other dimensions of the selected mineral particles so as to correct the final age; then, a platinum bag and a niobium bag are respectively used for loading apatite, zircon particles, 1-2 apatite standard samples and 1-2 zircon standard samples, forceps are used for flattening two ends of the platinum bag and the niobium bag to prevent the particles from falling off from the bags, and the loaded particles are placed into a sample bottle with a sample number. And the 1-2 apatite standard samples and the 1-2 zircon standard samples are used for verifying whether the detection result is reliable or not.
S2, sequentially opening the mechanical pump 601 and the second electromagnetic valve C2 for vacuumizing, closing the second electromagnetic valve C2 after vacuumizing for 4-5 min, starting the molecular pump 602, and opening the third electromagnetic valve C3, the first electromagnetic valve C1 and the ninth pneumatic valve F9 for continuously vacuumizing; and when the vacuum degree of the molecular pump 602 reaches 1E-7mbar, starting the ion pump 603, the fourth electromagnetic valve C4, the eighth pneumatic valve F8 and the quadrupole mass spectrometer 306, continuously vacuumizing, and sequentially closing the seventh pneumatic valve F7, the fourth electromagnetic valve C4, the eighth pneumatic valve F8 and the ion pump 603 when the vacuum degree of the device to be measured reaches 1E-8 mbar.
S3, starting the 970nm diode laser 101, the lens focusing system 102 and the sample pool 103, positioning the sample disc 104 according to the number, setting the coordinates and ensuring that the diode laser 101 can find each sample; 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; under the irradiation of a diode laser 101 with the working current of 14A-16A, zircon is heated at the constant temperature of 1200 DEG C10 min-12 min, in order to ensure the concentration in the granules4He release is complete, each sample must be tested at least twice, and the last test results are considered to be less than 1% of the total4He is released completely.
S4, opening 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 of H after the gas is frozen and enriched by the activated carbon cold trap 2012O、CO2、SO2The gas is made equal, and then H is removed by a Zr-Al getter 2022、CO、SO2And the like. The fourth and second pneumatic valves F4 and F2 are opened respectively,3he diluting tank 303 to3 He dilution burette 304 release3He，4He standard can 301 to4He Standard burette 302 Release4He to3The pressure of He diluting dosing tube 304 is a first preset pressure,4the pressure of He standard fixed-amount pipe 302 is the second preset pressure, the fourth pneumatic valve F4 and the second pneumatic valve F2 are closed, and the third pneumatic valve F3, the first pneumatic valve F1 and the seventh pneumatic valve F7 are opened, from the point of view of3In He-diluting quantitative tube 3043He. From4In He standard quantitative tube 3024He. And in gas4He forms a mixed gas. The eighth air-operated valve F8 is opened, and the ferrozirconium getter 203 absorbs the non-components in the mixture4He component, and then enters the quadrupole mass spectrometer for detection.
S5, the automatic control and data processing system 50 calculates apatite and zircon4He content.
Example 5
Example 5 provides a dating method of uranium-thorium/helium in mineral particles. The uranium-thorium/helium dating method further comprises the following steps: the following steps were continued for the apatite and zircon completed in example 4:
s6, ware cleaning and preparation of a standard solution and a blank solution: all utensils were HNO3Cleaning the solution, heating on an electric furnace for 30min, repeatedly washing with ultrapure water, and drying for later use; using diluent U (at a concentration of 25 ng/mL)235U/238U0.007252 ± 0.000036) and Th (25 ng/mL)230Th/232Th ═ 0) was prepared into 25 μ L of a mixed solution in a teflon sample-dissolving bottle, and 25 μ L of an isotope diluent (among them,235U＝15ng/mL，230Th＝5ng/mL，235U/238U＝838±7，230Th/232th ═ 10.45 ± 0.05), and the mixture was put into an ultrasonic cleaner and sonicated for 15min to prepare a standard solution to which a diluent was added.
Adding 25 mu L of 7mol/L HNO into a polytetrafluoroethylene sample dissolving bottle3Placing the mixture into an ultrasonic cleaner, ultrasonically oscillating for 15min, then adding ultrapure water to dilute the mixture to 350 mu L, and preparing a blank control.
Platinum capsules and niobium capsules were added to 2 blanks, respectively, to prepare 1 blank containing a platinum capsule and 1 blank containing a niobium capsule.
Determination of content of apatite particles U, Th: will be released completely4Putting He mineral particles and Pt-loaded capsules into a polytetrafluoroethylene sample dissolving bottle, and adding 25 mu L of 7mol/L HNO3Solution and 25. mu.L235U isotope diluent and 25. mu.L230A Th isotope diluent, namely placing a sample dissolving bottle added with the diluent into an ultrasonic cleaner for ultrasonic oscillation for 15min, then slowly heating to accelerate dissolution of apatite particles, standing for more than 4h at room temperature to ensure complete dissolution of apatite, and then adding ultrapure water for dilution 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 a sample to be measured in each batch of sample analysis process, wherein U, Th content is measured on an inductively coupled plasma mass spectrometer (ICP-MS), and finally obtaining the apatite digestion solution238U/235U、232Th/230The value of Th.
Determination of content of zircon particles U, Th: will be released completely4Putting He mineral particles and a niobium capsule into a polytetrafluoroethylene sample dissolving bottle, adding 300 mu L HF solution and 50 mu L HNO3Solution, 25. mu.L235U isotope diluent, and 25. mu.L230Slowly heating Th isotope diluent to 200 deg.C for dissolving for 72 hr, evaporating to dry, adding 300 μ L HCl solution, and dissolving in oven at 200 deg.C for 24 hrDuring the dissolving process, the indissolvable fluoride salt formed in the dissolving process is ensured to be dissolved, the solution is evaporated to dryness again after cooling, and 200 mu L of HNO is added3Heating at low temperature for about 30min on an electric heating plate after 25 μ L HF, evaporating to about 50 μ L, and adding ultrapure water to dilute to 350 μ L; at least 1 blank control, 1 blank control containing Nb capsules, 1 standard solution and a sample to be detected are analyzed and determined in each sample analysis process, the determination of U, Th content is carried out on an inductively coupled plasma mass spectrometer (ICP-MS), and the mineral particle digestion solution is finally obtained238U/235U、232Th/230The value of Th.
S7, according to apatite and zircon respectively4He、238U/235The ratio of U and232Th/230the ratio of Th, combined with the uranium/thorium-helium decay equation, calculates the apparent age of the apatite and zircon, respectively.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not 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 described embodiments.
Claims (10)
1. In a mineral granule4He dosing apparatus, characterized in that the dosing apparatus comprises: the system 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 communicated in series;
the laser heating system (10) is used for heating mineral particles so that the mineral particles release a gas and extract a gas, the gas containing4He；
The purification and enrichment system (20) is used for purifying and enriching the gas4He；
The standard sample mixing system (30) packComprises4He standard quantitative tube (302) and the same4He standard quantitative pipe (302) connected4A He standard tank (301),3He dilution quantitative tube (304), and method for producing the same3He dilution quantitative tube (304) connected3A He dilution tank (303); the above-mentioned4He standard quantitative tube (302) and said4He standard can (301) and the same3He dilution quantitative tube (304) and the3The He dilution tanks (303) are connected in parallel;
the detection analysis system (40) is used for detecting4He and3the content of He;
the vacuum treatment system (60) is used for carrying out vacuum treatment 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 particles4He content.
2. In the mineral particles of claim 14He metering device, characterized in that the standard sample mixing system (30) further comprises4He calibration dosing tube (306), and methods of making same4He calibrated dosing tube (306) communicating4He calibration tank (305), said4He calibrating dosing tube (306) and said4He calibration tank (305) with said4He standard quantitative tube (302) and said4The He standard tanks (301) are connected in parallel;
preferably, the standard mixing system (30) further comprises: is arranged at the4A first pneumatic valve (F1) arranged on the outlet end pipeline of the He standard quantitative pipe (302)4He standard quantitative tube (302) and the same4A second air-operated valve (F2) arranged on the communication line of the He standard tank (301)3A third pneumatic valve (F3) arranged on the outlet end pipeline of the He dilution quantitative pipe (304)3He dilution quantitative tube (304) and the3A fourth pneumatic valve (F4) on the line communicating with the He dilution tank (303);
preferablyThe standards mixing system (30) further comprises: is arranged at the4A fifth pneumatic valve (F5) on the outlet end line of the He calibration dosing tube (306), and a valve disposed on the outlet end line of the He calibration dosing tube4He calibrating dosing tube (306) and said4He calibration tank (305) communicates with a sixth pneumatic valve (F6) on the line.
3. In the mineral particles according to claim 1 or 24He dosing apparatus, characterized in that said laser heating system (10) comprises: a diode laser heater (101), a lens focusing system (102), a sample cell (103), and a sample tray (104);
wherein the laser light emitted by the diode laser heater (101) heats the mineral particles in the sample plate (104) via the lens focusing system (102);
the sample tray (104) is located on the sample cell (103);
the sample pool (103) drives the sample plate (104) to rotate, so that the laser emitted by the diode laser heater (101) is aligned with the mineral particles in the sample plate (104) to heat.
4. In the mineral particles according to claim 1 or 24He dosing apparatus, characterized in that said purification enrichment system (20) comprises: the activated carbon cold trap (201), the zirconium-aluminum getter (202) and the zirconium-vanadium-iron getter (203) are sequentially communicated in series; the ferrozirconium vanadium aspirator (203) is arranged close to the detection and analysis system (40);
preferably, a first electromagnetic valve (C1) is arranged on a pipeline of the laser heating system (10) communicated with the active carbon cold trap (201);
a seventh pneumatic valve (F7) is arranged on a communicating pipeline 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 a pipeline close to the air inlet end of the ferrozirconium aspirator (203);
preferably, the detection analysis system (40) comprises a quadrupole mass spectrometer.
5. In the mineral particles according to claim 1 or 24He dosing apparatus, characterized in that said 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 the vacuum pressure 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 dosing device;
the third electromagnetic valve (C3) is arranged on a connecting line between the mechanical pump (601) and the molecular pump (602);
said ninth pneumatic valve (F9) being arranged on the line of communication of said molecular pump (602) with said purification enrichment system (20);
the fourth electromagnetic valve (C4) controls the ion pump (603) to vacuumize the dosing device.
6. In a mineral granule4A method for quantifying He, the method being carried out in the quantification apparatus according to any one of claims 1 to 5, the method comprising the steps of:
s1, selecting and measuring mineral particles;
s2, vacuumizing the quantitative device through the vacuum treatment system (60);
s3, heating the mineral particles by the laser heating system (10) so that the mineral particles release gas;
s4, the purification and enrichment system (20) purifies and enriches the gas4He; the above-mentioned3He dilution tank (303) to said3He dilution dosing tube (304) release3He up to said3The pressure of the He diluting quantitative pipe (304) is a first preset pressure; the above-mentioned4He standard can (301) to4He Standard burette (302) release4He up to said4The pressure of the He standard quantitative pipe (302) is a second preset pressure; from the above3In He-diluting quantitative tube (304)3He. From the above4In He standard quantitative tube (302)4He. In said gas4He forms mixed gas, and the mixed gas enters the detection analysis system (40) for detection;
s5, calculating the mineral particles according to the detection result of the step S44The content of He;
preferably, the mineral particles are apatite or zircon.
7. In the mineral particles of claim 64A He quantifying method, characterized in that the quantifying method further comprises: by using the said4He calibrating dosing tube (306) and said4He calibration pot (305) pair4He standard can (301) is used for calibration.
8. In the mineral particles of claim 64The He quantifying method, wherein step S4 includes the steps of:
opening the first electromagnetic valve (C1), and enabling the activated carbon cold trap (201) and the zirconium-aluminum getter (202) to sequentially absorb non-ions in the gas4A He component;
opening the fourth and second pneumatic valves (F4, F2), respectively3He dilution tank (303) to said3He dilution dosing tube (304) release3He, said4He standard can (301) to4He Standard burette (302) release4He up to said3The pressure of the He diluting quantitative pipe (304) is a first preset pressure4The pressure of the He standard quantitative pipe (302) is a second preset pressure, the fourth pneumatic valve (F4) and the second pneumatic valve (F2) are closed, the third pneumatic valve (F3) and the first pneumatic valve (F1) are opened, and the pressure comes from3In He-diluting quantitative tube (304)3He. From the above4In He standard quantitative tube (302)4He. And in said gas4He forms mixed gas;
opening the eighth pneumatic valve (F8), the zirconium ferrovanadium aspirator (203) absorbing non-gases in the mixture4He component, and then enters the detection analysis system (40) for detection;
preferably, the quantification method further comprises: an automated control and data processing system (50) controls the laser heating system (10), the purification and enrichment system (20), the standard mixing system (30), the detection and analysis system (40), and the vacuum processing system (60) and calculates the concentration of mineral particles in the mineral particles4He content.
9. A uranium-thorium/helium dating method in mineral particles, characterized in that it comprises the quantitative method of claim 7 or 8, and in that it further comprises:
s6, continuously carrying out acid chemical digestion on the mineral particles, and measuring the contents of the mineral particles238U/235The ratio of U and232Th/230the ratio of Th;
s7, according to the mineral particles4He、238U/235The ratio of U and232Th/230the ratio of Th, combined with the uranium/thorium-helium decay equation, calculates the apparent age of the mineral particles.
10. A uranium-thorium/helium dating method according to claim 9, the step S6 comprising the steps of:
the formulation has the known238U/235U and232Th/230a standard solution of the Th ratio;
preparing an acid solution, and diluting the acid solution to a constant volume to prepare a blank control;
preparing a blank control containing the metal capsule;
dissolving the mineral particles wrapped by the metal capsules by using acid liquor, and adding the dissolved mineral particlesTo know238U/235U and232Th/230preparing a sample to be detected by using an isotope diluent with a Th ratio in a constant volume manner;
measuring at least one blank, at least 1 metal capsule blank, at least 1 standard solution and the sample to be measured by using an inductively coupled plasma mass spectrometer238U/235The ratio of U and232Th/230the ratio of Th;
preferably, the mineral particles are apatite or zircon;
in the case that 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, under the condition of heating, the zircon is dissolved by using a mixed solution of hydrofluoric acid and nitric acid, and after the mixed solution is evaporated, a hydrochloric acid solution is added for dissolving so as to completely dissolve the zircon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101929968A (en) * | 2009-10-30 | 2010-12-29 | 中国计量科学研究院 | Device for measuring thermal diffusivity |
| US20140264012A1 (en) * | 2013-03-15 | 2014-09-18 | Gary Michael McMurtry | Portable Field 3He/4He Stable Isotope Detector for Use in Survey Work and Autonomous Monitoring |
| CN107991378A (en) * | 2017-11-17 | 2018-05-04 | 中国科学院青海盐湖研究所 | The separation method of boron and the assay method of boron istope in gypsoide and/or anhydrite mineral |
| CN108459070A (en) * | 2018-02-11 | 2018-08-28 | 中国科学院地质与地球物理研究所 | A kind of diluent free measures apatite (U-Th)/He and determines year method |
| CN109142499A (en) * | 2017-06-16 | 2019-01-04 | 中国石油化工股份有限公司 | In-situ micro area Isotope Dating device and method |
| CN109632939A (en) * | 2018-12-04 | 2019-04-16 | 中国科学院地质与地球物理研究所 | A kind of method and its system using ion probe measurement inert gas |
-
2019
- 2019-06-28 CN CN201910578248.9A patent/CN112147208B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101929968A (en) * | 2009-10-30 | 2010-12-29 | 中国计量科学研究院 | Device for measuring thermal diffusivity |
| US20140264012A1 (en) * | 2013-03-15 | 2014-09-18 | Gary Michael McMurtry | Portable Field 3He/4He Stable Isotope Detector for Use in Survey Work and Autonomous Monitoring |
| CN109142499A (en) * | 2017-06-16 | 2019-01-04 | 中国石油化工股份有限公司 | In-situ micro area Isotope Dating device and method |
| CN107991378A (en) * | 2017-11-17 | 2018-05-04 | 中国科学院青海盐湖研究所 | The separation method of boron and the assay method of boron istope in gypsoide and/or anhydrite mineral |
| CN108459070A (en) * | 2018-02-11 | 2018-08-28 | 中国科学院地质与地球物理研究所 | A kind of diluent free measures apatite (U-Th)/He and determines year method |
| CN109632939A (en) * | 2018-12-04 | 2019-04-16 | 中国科学院地质与地球物理研究所 | A kind of method and its system using ion probe measurement inert gas |
Non-Patent Citations (1)
| Title |
|---|
| 王英;郑德文;武颖;李又娟;王一舟;: "磷灰石单颗粒(U-Th)/He测年实验流程的建立及验证", 地震地质, no. 06 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117110412A (en) * | 2023-08-23 | 2023-11-24 | 中国科学院地质与地球物理研究所 | Method for calibrating discrimination effect of neon isotope ratio mass |
| CN117110412B (en) * | 2023-08-23 | 2024-03-01 | 中国科学院地质与地球物理研究所 | Method for calibrating discrimination effect of neon isotope ratio mass |
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