CN116609421A - Annual survey method based on monazite fission track - Google Patents
Annual survey method based on monazite fission track Download PDFInfo
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 5
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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
- G01N27/626—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 using heat to ionise a gas
- G01N27/628—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 using heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
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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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- 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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Abstract
The application discloses a yearn testing method based on monazite fission tracks, which comprises the following steps: etching the plurality of monazite samples; placing the etched plurality of monazite samples under a fission track analyzer for observation, counting track density of each monazite sample, and marking corresponding test position coordinates; performing laser ablation on the monazite sample and the selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the marked test position coordinates, and calculating the monazite sample according to the laser ablation data 238 U content; based on the track density of each individual sample 238 The U content, the analysis determines the fission track age of a plurality of individual monolithic samples. The application breaks through the technical barriers that the monazite cannot be used for measuring the quantity of radioactive parent bodies by an external detector method because of too high Gd content and strongly absorbs neutrons, realizes the measurement of the fission track age of monazite minerals, and makes up forThe prior art is blank.
Description
Technical Field
The application relates to the technical field of yearning, in particular to a yearning method based on monazite fission tracks.
Background
In the field of earth science, the principle of dating by utilizing the characteristic of radioactive decay of heavy elements is widely applied to various dating methods, including a U-Th-Pb dating method, a fission track dating method and the like. The basic principle of the radioactive decay system annual measurement method is similar, the radioactive decay equation is relied on, and the time duration after the system is kept closed is deduced by testing or calculating the relative abundance of the radioactive parent and the daughter, so that relevant important geological time nodes such as mineral crystallization, rock formation, deterioration peak period, rock lifting cooling time and the like are obtained.
For fission track processes, minerals are contained 238 When a U spontaneously fissions, high-energy fragments moving in opposite directions are formed, the high-energy fissile fragments interact with surrounding electrons, and high temperatures are locally generated, so that damage traces, namely fission tracks, are formed (Gledow et al, 2002). For the dating of fission tracks, the prior art is obtained 238 The number of U atoms (parent) and the number of spontaneous fission tracks (reflecting the fissile 238 Number of U-children), the age can be obtained. Wherein the number of fissile tracks can be measured by counting under a microscope after chemical etching has been enlarged.
For the established years of apatite fission tracks and zircon fission tracks, the parent body is 238 The U content is obtained by an external detector method. The external detector method is to use the existing method 238 U and 235 the ratio of the U content is a constant and only needs to be measured 235 The U content can be known 238 U content. 235 The U content can be induced by placing a sample into the reactor 235 U fission, the induced fission track can be generated by the induced fission, and the number of the induced fission tracks is counted to obtain 235 U content, thereby obtaining 238 U content.
Monazite fission tracks have great potential as an important indicator of geological low temperature events because of their greater sensitivity to temperature relative to other minerals, and have received attention in recent years. However, for monazite, the neutron absorption cross section of Gd is far higher than that of Gd because of the rich element Gd 235 U, lead to in the reactor 235 The induced fission of U is greatly limited and is not available 235 The accurate content of U is not obtained 238 The exact content of U. This is the caseLimitations have led to the inability of conventional external probe methods to be applied to the annual methods of monazite fission tracks. Thus, the annual approach to monazite fission tracks has been less studied in the prior art.
Disclosure of Invention
Aiming at the problems, the embodiment of the application provides a yearn measuring method based on monazite fission tracks, which aims to overcome the defects of the prior art.
In a first aspect, an embodiment of the present application provides a monazite fission track based yearning method, the method including:
etching a plurality of monazite samples to expand the fission track of each of the monazite samples to a degree that is observable by a fission track analyzer;
placing the etched plurality of monazite samples under a fission track analyzer for observation, counting track density of each monazite sample, and marking test position coordinates of each monazite sample;
performing laser ablation on each monazite sample and a selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the test position coordinates of each monazite sample, and calculating the monazite samples according to laser ablation data 238 U content;
based on the track density of each of the monazite samples, the track density of each of the monazite samples 238 And (3) determining the fission track age of the plurality of monazite samples through analysis.
Optionally, the method further comprises:
determining the relative content of U, th and Pb isotopes in each monazite sample according to the laser ablation data;
based on the relative amounts of U, th and Pb isotopes in each of the monazite samples, analysis can determine the U-Th-Pb age of the plurality of monazite samples.
Optionally, in the above method, the selected standard sample includes an age standard sample and a U content standard sample;
the age standard samples are 44069 standard samples and RW-1 standard samples;
the U content standard sample is an NIST610 standard sample.
Optionally, in the above method, the etching the plurality of monazite samples includes:
placing the plurality of monazite samples into a closed container filled with 12 mol/L concentrated hydrochloric acid;
200 h-650 h are etched at room temperature to expand the fission track of each of the monazite samples.
Alternatively, in the above method, in summer or autumn, the room temperature condition is maintained at 23 ℃ or higher and 27 ℃ or lower, and the etching time is 200 h or higher and 450 h or lower.
Alternatively, in the above method, the room temperature condition is kept at 25 ℃ in summer or autumn, and the etching period is 250 h.
Alternatively, in the above method, the room temperature condition is maintained at 18 ℃ or higher and 23 ℃ or lower in spring or winter, and the etching time period is 450 ℃ or higher h and 650 ℃ or lower h.
Alternatively, in the above method, the room temperature condition is maintained at 20 ℃ in spring or winter, and the etching period is 560 h.
Optionally, in the above method, etching the plurality of monazite samples is performed under heating using a monazite etching device;
the monazite etching device includes: glass reagent bottle, rubber stopper, water bath, thermometer and conduit;
the glass reagent bottle is inserted into the water of the water bath kettle;
the bottle mouth of the glass reagent bottle is plugged by the rubber plug;
the thermometer is inserted into the middle part of the glass reagent bottle through a first through hole of the rubber plug;
the guide pipe is inserted into the glass reagent bottle through the second through hole of the rubber plug so as to balance the pressure inside and outside the glass reagent bottle.
Optionally, in the above method, etching the plurality of monazite samples is performed according to the following method:
loading 12 mol/L concentrated hydrochloric acid into the glass reagent bottle, and placing the plurality of monazite samples into the glass reagent bottle;
the rubber plug is plugged into the bottle mouth of the glass reagent bottle, the thermometer is inserted into the middle part of the glass reagent bottle through the first through hole, and the guide pipe is inserted above the liquid level of concentrated hydrochloric acid in the glass reagent bottle through the second through hole;
and placing the glass reagent bottle in the water bath kettle preheated to 90 ℃ for 45 min to obtain an etched monazite sample.
The above at least one technical scheme adopted by the embodiment of the application can achieve the following beneficial effects:
the application provides a yearn testing method based on monazite fission tracks, which comprises the following steps: etching a plurality of monazite samples to expand the fission track of each of the monazite samples to a degree that is observable by a fission track analyzer; placing the etched plurality of monazite samples under a fission track analyzer for observation, counting track density of each monazite sample, and marking test position coordinates of each monazite sample; performing laser ablation on each monazite sample and a selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the test position coordinates of each monazite sample, and calculating the monazite samples according to laser ablation data 238 U content; based on the track density of each of the monazite samples, the track density of each of the monazite samples 238 And (3) determining the fission track age of the plurality of monazite samples through analysis. The application obtains the U element content of the same position area of the monazite fission track test by the laser ablation inductively coupled plasma mass spectrometer technology, calculates and obtains the fission track 238 Number of U-radioactive precursors, number of fission tracks to be etched and 238 the method breaks through the technical barriers that the monazite cannot be used for measuring the number of the radioactive precursors by using an external detector method, successfully realizes the measurement of the fission track age of the monazite mineral, and fills up the blank of the prior art; to obtainThe important geological time nodes such as the related mineral crystallization, rock formation, deterioration peak period, rock lifting and cooling time and the like have important and accurate reference significance, and are particularly used for representing low-temperature geological events.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 shows a flow diagram of a monazite fission track based yearly method according to one embodiment of the application;
FIG. 2 shows a schematic structural view of a monazite etching apparatus according to one embodiment of the present application;
FIG. 3 illustrates a flow diagram of a method of ambient etching of monazite fission tracks according to one embodiment of the application;
FIG. 4 illustrates an etch effect resulting from a room temperature etching process of monazite fission tracks according to one embodiment of the application;
fig. 5 shows a flow diagram of a monazite fission track based joint yearn method according to another embodiment of the application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below with reference to specific embodiments of the present application and corresponding drawings. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The following describes in detail the technical solutions provided by the embodiments of the present application with reference to the accompanying drawings.
In research methods in the field of earth science today, yearly technology is a vital one. The fissile track yearn method is a widely used yearn method and is generally characterized by the age of low-temperature thermal events during geological historic periods.
The fission track year principle is as follows: according to 238 The fission equation for the U isotope only requires the acquisition of the radioactive daughter (fission track or number of fissile atoms) and the parent (existing 238 Number of U atoms) to calculate the age of the associated rock/mineral.
Wherein, for monazite, the relative abundance of its daughter, namely the number of fission tracks, can be obtained by counting under a fission track analyzer (the principle of which is the same as that of a microscope) after chemical etching expansion.
The parent is obtained by the traditional fission track method 238 The method for the content of the U) is as follows: placing the sample in a reactor by induction 235 U fission is obtained 235 U content, reuse 238 U and 235 the ratio of U is a constant (137.88) to obtain 238 U content. Apatite and zircon are common minerals of traditional fission track years. However, since monazite is not available with conventional external probe methods 238 The U content, therefore, has been less studied for its fission track to date. The specific reason why monazite cannot obtain U content by the conventional method is as follows: the monazite is rich in rare earth elements such as Gd, the neutron reaction section of Gd is very large and far exceeds that of the monazite 235 U, if the monazite is placed in a reactor, causes a great deal of neutron self-absorption and severe nuclear heating during neutron irradiation, even if the direct melting of the minerals themselves severely limits the induction 235 The amount of U fission, unable to obtain 235 And the accurate content of U. Therefore, the characteristics lead to the fact that the monazite mineral cannot be measured by adopting a traditional external detection method, and the application of the monazite fission track annual measurement method is seriously hindered.
In this regard, the application proposes a monazite fission track based yearn testing method, which adopts a laser ablation inductively coupled plasma mass spectrometer in-situ micro-area analysis technology to overcome the technical barrier of the monazite fission track yearn testing method, and fig. 1 shows a flow diagram of the monazite fission track based yearn testing method according to one embodiment of the application, as can be seen from fig. 1, the application at least comprises steps S110-S140:
step S110: etching the plurality of monazite samples to expand the fission track of each of the monazite samples to a degree that is observable by a fission track analyzer.
The minerals being contained in minerals 238 When the U spontaneously fissions into high-energy fragments moving in opposite directions, the high-energy fissile fragments interact with surrounding electrons, locally generating high temperatures, and forming damage tracks, i.e., fission tracks (Gleadow et al, 2002). The fission track is typically an elongated damaged region with a width of less than 10 nm and a length of tens of microns (Li et al 2012). Because the fission track diameter is very thin, only a few nanometers, far below the resolution of the fission track analyzer (250-nm), it is necessary to expand its chemical etching. This process is called etching, i.e. a process in which a chemical reagent such as an acid or alkali can react with minerals and a fission track is more easily reacted in a damaged area, and the fission track is enlarged to a diameter of about 1 μm. The amplified traces are etched and can be observed and counted under a fission trace analyzer.
The chemical etching condition of the monazite fission track commonly used in the traditional technology is that in concentrated hydrochloric acid (12 mol/L), the temperature is 90 ℃ and the time lasts for 45 min; alternatively, in hydrochloric acid (6 mol/L), the temperature is 90℃for 30 min-60 min.
In some embodiments, the monazite sample may be etched in a conventional manner, such as by placing the monazite sample in a container containing concentrated hydrochloric acid and etching at 90 ℃ for 45 minutes.
For etching devices, the conventional etching method is to put concentrated hydrochloric acid in an open beaker, put a sample in the beaker, put the beaker on a heating plate, put a beaker filled with water on the heating plate at the same time, determine the temperature of hydrochloric acid by measuring the temperature of water, the method cannot directly determine the temperature of hydrochloric acid, and meanwhile, the concentrated hydrochloric acid has strong volatility, so that the concentration of hydrochloric acid is reduced in the etching process.
To this end, in some embodiments of the present application, a monazite etching apparatus is provided, which is adapted to perform high temperature etching on a monazite, and fig. 2 shows a schematic structural view of the monazite etching apparatus according to one embodiment of the present application, and as can be seen from fig. 2, a monazite etching apparatus 200 includes: a glass reagent bottle 1, a rubber plug 2, a water bath 3, a thermometer 4 and a conduit 5; wherein, the glass reagent bottle 1 is inserted into the water of the water bath kettle 3; the bottle mouth of the glass reagent bottle 1 is plugged by the rubber plug 2; the thermometer 4 is inserted into the middle or bottom of the glass reagent bottle 1 (below the liquid level of the reagent in the glass reagent bottle) through the first through hole of the rubber stopper 2 so as to test the temperature of the reagent therein; the conduit 5 is inserted into the glass reagent bottle 1 through the second through hole of the rubber stopper 2, specifically above the liquid surface of the reagent, so as to balance the pressure inside and outside the glass reagent bottle 1.
Taking the above etching conditions as an example, in concentrated hydrochloric acid (12 mol/L) at 90 ℃ for 45 min, the monazite etching device 200 is mainly suitable for high-temperature etching of monazite, and the specific steps mainly include:
loading 12 mol/L concentrated hydrochloric acid into the glass reagent bottle, and placing a plurality of monazite into the glass reagent bottle; plugging a rubber plug into a bottle mouth of the glass reagent bottle, inserting the thermometer into the middle part or the bottom of the glass reagent bottle through the first through hole, and inserting the guide pipe into the glass reagent bottle above the liquid level of concentrated hydrochloric acid through the second through hole; and placing the glass reagent bottle in the water bath kettle preheated to 90 ℃ for 45 min to obtain an etched monazite sample.
The monazite etching device can furthest reduce the volatilization of concentrated hydrochloric acid, has smaller and more accurate etching temperature fluctuation, and can lead the whole process to be more stable by heating in water bath, thus the etching track density is more reliable.
In addition, different minerals require different etching solutions for etching due to the different chemical composition and properties of the minerals. Monazite [ (Ce, la, nd, th) PO 4 ]Is a light rare earth phosphate mineral, is an important occurrence mineral of Rare Earth Elements (REE),the mineral minerals are mainly in the form of accessory minerals such as aluminized granite, pegmatite, argillite, sandstone, carbonate and hydrothermally, and are common clastic minerals in sedimentary rocks (Williams et al, 2007). The fission track generally has a temperature sensitive property, which is called annealing. Track annealing, i.e. the length reduction even completely disappears, can affect the accuracy of the result of inverting the thermal history with track length and the age of the fissile track. Whereas monazite fission tracks are more sensitive to low temperatures than other minerals, such low temperature chronology indicators are now urgently needed in the dating process. Therefore, the monazite fission track method has extremely important application prospect. In addition, monazite fission tracks are sensitive to low-temperature annealing temperatures, and thermal annealing is possibly caused by heating in the etching process, so that development of a normal-temperature etching method without heating is necessary.
For this reason, the application develops a normal temperature etching method of monazite without heating, fig. 3 shows a flow chart of a normal temperature etching method of monazite fission tracks according to an embodiment of the application, and as can be seen from fig. 3, the normal temperature etching method of monazite fission tracks of the application includes steps S310 to S320:
step S310: a plurality of monazite samples were placed in a closed container containing 12 mol/L concentrated hydrochloric acid.
Step S320: 200 h-650 h are etched at room temperature to expand the fission track of each of the monazite samples.
Through a great number of continuous tests, the applicant of the application successfully etches the monazite at normal temperature, and the specific etching process is that a monazite sample is put into a container filled with 12 mol/L concentrated hydrochloric acid, and the container is preferably a closed container so that the concentrated hydrochloric acid is not volatilized.
Then etching 200 h-650 h under room temperature (without additional heating or cooling treatment), and expanding the diameter of the fission track of the monazite from about 10 nm to about 1 mu m, and after etching, washing with ultrapure water, and observing by using a fission track analyzer.
As the room temperature also changes throughout the four seasons, through continuous tests, taking the northern season temperature as an example, if the current season is summer or autumn, namely, the room temperature is higher, the room temperature is kept to be more than or equal to 23 ℃ and less than or equal to 27 ℃, the etching time length is more than or equal to 200 h and less than 450 h, under the conditions, the room temperature is increased, the etching time length can be properly shortened, the room temperature is reduced, and the etching time length can be properly prolonged; in some embodiments, the etching duration is 250 h to achieve the best etching effect if the current season is summer or autumn, and the room temperature condition is 25 ℃.
In other embodiments, still taking the northern season temperature as an example, if the current season is spring or winter, the room temperature condition is maintained at 18 ℃ or higher and 23 ℃ or lower, and the etching time period is 450 ℃ or higher h and 650 h or lower. Under the above conditions, the room temperature is raised, the etching duration can be properly shortened, the room temperature is lowered, and the etching duration can be properly prolonged; in some embodiments, if the current season is spring or winter, the room temperature condition is maintained at 20 ℃ and the etching period is 560 h.
The etching conditions described above are based on the fact that the etching time is continuously tested, eventually found suitable conditions, by expanding the track from around 10 nm to around 1 μm in diameter.
Referring to fig. 4, fig. 4 shows an etching effect diagram obtained by a normal temperature etching method for monazite fission tracks according to an embodiment of the present application, and as can be seen from fig. 4, the normal temperature etching method for monazite fission tracks provided by the embodiment of the present application is used for etching monazite, so that expansion of monazite fission tracks can be successfully achieved.
It should be noted that other possible normal temperature etching conditions are also implemented in the present application, including 98% concentrated sulfuric acid, 50% concentrated sulfuric acid, 25% concentrated sulfuric acid, 85% H 3 PO 4 、70%HClO 4 In the middle, at room temperature, no effective expansion of the monazite fission track was observed by etching 100 h-800 h.
As can be seen from fig. 3 and 4, the embodiment of the application provides a method for etching monazite fission tracks without heating, which omits a heating process, does not need a heating device, and is simpler to operate; and the problem of monazite fission track annealing possibly caused by a heating and etching process is solved, and the accuracy of fission track year measurement can be improved.
Step S120: and placing the etched plurality of monazite samples under a fission track analyzer for observation, counting the track density of each monazite sample, and marking the test position coordinates of each monazite sample.
After etching a plurality of monazite samples, the original fission tracks of the monazite are enlarged to about 1 mu m, and the monazite is placed under a fission track analyzer for observation, wherein the fission track analyzer is an instrument for specially researching the fission tracks, namely an optical microscope, can count the fission tracks under a lens, for example, the number of the fission tracks in a circular area with the diameter of 30 mu m is counted, then the track density in the monazite sample, namely the density of a daughter, can be obtained by dividing the area of the circular area, and the measurement of the number of the fission track radiosomes can be realized by adopting the fission track analyzer.
In order to make the follow-up to 238 And U is measured and the track density measured in the step is the same area, and the positions of the test areas of the individual samples are marked under a fission track analyzer to obtain the test position coordinates of the individual samples.
Specifically, a marker is set below the fission track analyzer as an origin, and the coordinates of a test area of the statistical density of each solitary stone mineral particle are recorded by taking the origin as a reference and are recorded as test position coordinates, so that the purpose of the method is to ensure that the same position can be found again in a laser ablation inductively coupled plasma mass spectrometer (LA-ICP-MS).
Step S130: performing laser ablation on each monazite sample and a selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the test position coordinates of each monazite sample, and calculating the positions of each monazite sample according to laser ablation data 238 U content.
And placing the monazite sample with the calculated track density on a sample table of a laser ablation inductively coupled plasma mass spectrometer, and simultaneously placing a preselected standard sample (standard sample for short) for laser ablation.
The laser ablation is characterized in that a mineral to be detected is ablated into an aerosol state which can be measured by a mass spectrometer by taking laser ablation as a sampling system, generated aerosol particles are sent to the mass spectrometer by taking inert gases such as helium and argon as carrier gases, most elements (such as U, th, pb and the like) in the aerosol particles are ionized into positive ions with +1 valence at an ion source position of the mass spectrometer, charged ions with different mass-to-charge ratios (mass number/charge number of isotopes) at a mass analyzer position of the mass spectrometer are respectively transmitted to a detector position of the mass spectrometer for detection, and finally the relative ion signal size of each isotope is calculated by a computer system to obtain the relative abundance of each radioactive element.
During specific operation, according to the test position coordinates of the monazite sample marked under the fission track analyzer, finding out the area with the track density already counted, selecting points at the same position as laser ablation points, and selecting points needing laser ablation on the standard sample; then, laser ablation conditions are set, and different laser ablation conditions can be set according to the characteristics of the monazite sample. In some embodiments of the application, the conditions for laser ablation are set for some samples, based on the characteristics of the monazite sample: 3J/cm 2 The monazite and standard samples were laser ablated under this condition at an energy density of 5 Hz, ablation frequency, and laser beam spot size of 30 um. Different conditions may be set for different samples, and the present application is not limited to this, and may be set as needed.
The data obtained by laser ablation is recorded as laser ablation data, the laser ablation data is processed, and the basic principle of data processing is as follows: the signal intensity (CPS) and the element (isotope) content are in positive correlation, and the correction coefficient can be obtained by using the standard sample so as to be applied to the sample, based on the principle, the signal intensity ratio and the correction coefficient in the standard sample are calculated 238 The U content can obtain each individual house counted under a fission track analyzerTest area of stone sample 238 U content.
For selected standard samples, including age standard samples and U content standard samples; in some embodiments of the application, the age standard includes, but is not limited to, 44069 standard and RW-1 standard; the U content standard sample is an NIST610 standard sample. In some embodiments, 44069 standard is often used as the primary standard and RW-1 standard is used as the monitoring standard. The RW-1 standard sample and the monazite sample are measured simultaneously, so that a basis can be provided for the accuracy of the experiment.
A common mineral for laser ablation inductively coupled plasma mass spectrometry by-product in situ micro-zone U-Th-Pb dating is zircon, as this mineral has a very high U-Pb system blocking temperature (> 900 ℃) which can represent the age of rock formation. Monazite also has a relatively high U-Th-Pb system blocking temperature (about 800 ℃ to 900 ℃) almost comparable to zircon, which often can be mutually verified, even for some formations where zircon does not develop, monazite may be the sole choice.
However, in practical application, due to the lack of monazite standard reference substances (standard samples), monazite fission track age standard samples are not existed, and the monazite mineral annual measurement technology is limited to a great extent. In this in situ micro-area annual technique, matrix-matched standards are necessary to correct for experimental data error sources such as instrument signal drift, mass discrimination and depth fractionation correction for lasers and mass spectrometers.
In an actual testing process, at least two standard substances matched with a matrix are generally required, one is used as a first standard substance for correcting and testing to obtain the isotope ratio initially, and the other is used as a second standard substance, is used as an unknown sample, and is used for monitoring the reliability of a test result.
The single particle size of RW-1 is much larger than 44069. 44069 standard samples and RW-1 standard samples can be used as age standard samples of the solitary stone in the annual survey process, and are particularly used in the U-Th-Pb annual survey process.
The U content standard is NIST610 standard, because the monazite has higher U content, and if NIST series is used, NIST610 with higher U content should be selected.
It should be noted that the U content standard sample can be used for measuring fissile track and U-Th-Pb; whereas age standards are typically used only for U-Th-Pb year tests.
It should be noted that, for 238 The calculation formula of the U content is built in a computer system of the laser ablation inductively coupled plasma mass spectrometer, manual calculation is not needed, and the calculation formula can refer to the prior art.
Step S140: based on the track density of each of the monazite samples, the track density of each of the monazite samples 238 And (3) determining the fission track age of the plurality of monazite samples through analysis.
Obtaining each of the monazite samples 238 The U content can be determined according to the track density of each monazite sample and the content of each monazite sample 238 The U content and the age of the fission track of the batch of monazite samples are determined by analysis means. Specifically, for a monazite sample, the track density of the monazite sample is determined based on the track density of the monazite sample and the track density of the monazite sample 238 The U content, as well as some other necessary known parameters, can be analyzed to obtain the age of the monazite sample's fission track.
Specifically, in some embodiments, the analysis process is understood to be the calculation of the fission track age of each individual monolithic sample by the parameters described above, followed by data analysis.
As can be seen from the method shown in fig. 1, the present application provides a monazite fission track based yearning method comprising: etching a plurality of monazite samples to expand the fission track of each of the monazite samples to a degree that is observable by a fission track analyzer; placing the etched plurality of monazite samples under a fission track analyzer for observation, counting track density of each monazite sample, and marking test position coordinates of each monazite sample; performing laser ablation on each monazite sample and a selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the test position coordinates of each monazite sample, and calculating the monazite sample according to laser ablation dataIn the monazite sample 238 U content; based on the track density of each of the monazite samples, the track density of each of the monazite samples 238 And (3) determining the fission track age of the plurality of monazite samples through analysis. The application obtains the U element content of the same position area of the monazite fission track test by the laser ablation inductively coupled plasma mass spectrometer technology, calculates and obtains the fission track 238 Number of U-radioactive precursors, number of fission tracks to be etched and 238 the method breaks through the technical barriers that the monazite cannot be used for measuring the number of the radioactive precursors by using an external detector method, successfully realizes the measurement of the fission track age of the monazite mineral, and makes up the blank of the prior art; the method has important and accurate reference significance for obtaining important geological time nodes such as related mineral crystallization, rock formation, deterioration peak period, rock lifting and cooling time and the like, and is particularly used for representing low-temperature geological events.
The U element has 235 U and 238 two isotopes of U are used for preparing the fluorescent dye, 238 u and 235 after a series of alpha decay, the U isotopes are respectively and finally stabilized into 206 Pb、 207 Two radioactive daughter isotopes of Pb; simultaneously releasing a certain amount of He nuclei; at the same time 238 U also undergoes spontaneous fission, producing another radioactive sub-body product-a fission track (for the aforementioned fission track year); in addition, in the case of the optical fiber, 232 th also decays, eventually stabilizing after a series of radioactive decays 208 Since the Pb isotopes, both of which are radioactive isotopes of Pb element, are co-produced in the same mineral carrier, U-Pb and Th-Pb are generally combined into one annual method, which is described as the U-Th-Pb annual method.
The U-Th-Pb annual testing method and the fission track annual testing method are common geological chronology testing technology, and the two methods have the same radioactive parent body 238 In the laser ablation process of the U, laser ablation inductively coupled plasma mass spectrometer on the monazite sample, U, th and Pb can be obtainedThe relative content of the potential elements; therefore, in some embodiments of the application, the U-Th-Pb annual measurement method of the monazite sample can be realized through a laser ablation inductively coupled plasma mass spectrometer, the age result of the U-Th-Pb is obtained, and different annual measurement results correspond to different geological evolution processes and can be combined together for use. Wherein the relative contents of U, th and Pb isotopes refer to 238 U pair 206 The relative Pb content, 235 U pair 207 The relative Pb content, 232 Th pair 208 The relative Pb content can obtain three ages from the three contents, the obtained three ages are integrated together for analysis, and a year measurement result, namely the U-Th-Pb age, can be obtained, and the specific calculation process can refer to the prior art.
Specifically, the method further comprises the following steps: and determining the relative content of U, th and Pb isotopes in each monazite sample according to the laser ablation data, and analyzing to determine the U-Th-Pb ages of the plurality of monazite samples.
The relative contents of U, th and Pb isotopes can be obtained simultaneously in the testing process of the laser ablation inductively coupled plasma mass spectrometer, and the U-Th-Pb age of the monazite mineral can be calculated through the existing correction method and the data processing software iolite or glitter. In combination with the embodiment shown in fig. 1, a test method for simultaneously measuring the years of U-Th-Pb and fission tracks in the same position area of the same monazite mineral is realized.
The calculation formula of the U-Th-Pb year measurement method can refer to the prior art.
Fig. 5 shows a flow diagram of a monazite fission track based joint yearn method according to another embodiment of the application, and as can be seen from fig. 5, the embodiment includes:
a plurality of monazite samples are etched.
And placing the etched plurality of monazite samples under a fission track analyzer for observation, respectively counting the track density of each monazite sample, and marking the coordinates of the test area.
And placing the marked solitary stone samples and the selected standard samples (comprising the age standard sample and the U content standard sample) under a laser ablation inductively coupled plasma mass spectrometer for laser ablation to obtain laser ablation data.
Obtaining individual monazite samples according to laser ablation data 238 U content and according to track density and sum of individual monazite samples 238 The U content, the age of the fission track of the batch of monazite samples was determined by analysis.
The relative contents of U, th and Pb isotopes in each monazite sample were obtained from the laser ablation data, and the U-Th-Pb age of the batch of monazite samples was determined by analysis.
As can be seen from fig. 5, in this embodiment, the single mineral monazite is taken as a research object, on the one hand, by using a normal temperature etching method and combining with an existing fission track analyzer in a laboratory, the accurate measurement of the number of radioactive subunits in the fission track is realized, and the process can accurately mark the measurement position of the fission track of each test particle, and the accuracy can reach the micrometer level; then obtaining the content of U element in the same position area of the fission track test by using a laser ablation inductively coupled plasma mass spectrometer technology, and calculating to obtain the fission track 238 The number of the U radioactive precursors, and the number of the U radioactive precursors are combined to calculate the fission track age of the monazite mineral through a decay equation; on the other hand, the relative contents of U, th and Pb isotopes are obtained simultaneously in the testing process of the laser ablation inductively coupled plasma mass spectrometer, and the U-Th-Pb age of the monazite mineral is calculated through the existing correction method and the data processing software iolite or glitter. The method can be used for simultaneously measuring the U-Th-Pb age and the fission track age of the same location area of the same monazite mineral, and not only can the fission track age representing the low-temperature geological event be obtained, but also the age representing the mineral formation or deterioration high-temperature geological event can be obtained, so that the high-efficiency single mineral multi-legal year is realized.
Ambient etching of monazite samples
Example 1
A plurality of monazite samples were placed in a closed container containing 12 mol/L concentrated hydrochloric acid, and placed in a laboratory, and etched 250 h under room temperature conditions (maintaining room temperature at about 25 ℃) in summer.
The original fission track of the monazite can be enlarged to about 1 mu m by observation under a fission track analyzer.
Example 2
A plurality of monazite samples were placed in a closed container containing 12 mol/L concentrated hydrochloric acid, and placed in a laboratory, and etched 560 and h under room temperature conditions in winter (maintaining room temperature conditions at about 20 ℃).
The original fission track of the monazite can be enlarged to about 1 mu m by observation under a fission track analyzer.
Example 3
A plurality of monazite samples were placed in a closed container containing 12 mol/L concentrated hydrochloric acid, and placed in a laboratory, and etched 210 h under room temperature conditions (maintaining room temperature at about 27 ℃) in summer.
The original fission track of the monazite can be enlarged to about 1 mu m by observation under a fission track analyzer.
Example 4
Samples of the monazite were placed in a closed container containing 12 mol/L concentrated hydrochloric acid and placed in a laboratory and etched 650 h at room temperature in winter (maintaining room temperature at about 18 ℃).
The original fission track of the monazite can be enlarged to about 1 mu m by observation under a fission track analyzer.
Comparative example 1
The application also implements other possible normal temperature etching conditions, including 98% concentrated sulfuric acid, 50% concentrated sulfuric acid, 25% concentrated sulfuric acid, 85% H 3 PO 4 、70%HClO 4 In the middle, at room temperature, no effective expansion of the monazite fission track was observed by etching 100 h-800 h.
Combined determination of monazite fission track age and U-Th-Pb age
Example 5
The etched monolithic samples of example 1 were observed under fission tracks, track densities of the individual monolithic samples were counted, and the test areas were labeled with coordinates. Wherein the monazite sample is from motor gas.
And placing the marked individual stone samples and the selected standard samples under a LA-ICP-MS instrument for laser ablation to obtain laser ablation data, wherein the age standard sample is a 44069 standard sample+RW-1 standard sample, the U content standard sample is a NIST610 standard sample, the 44069 standard sample is used as a main standard sample, and the RW-1 standard sample is used as a monitoring standard sample. The RW-1 standard sample and the monazite sample are measured simultaneously, so that a basis can be provided for the accuracy of the experiment.
Obtaining individual monazite samples according to laser ablation data 238 U content and according to track density and sum of individual monazite samples 238 And (3) analyzing and calculating the fission track age of the batch of monazite samples to obtain the track fission age of 5.1Ma.
And obtaining the relative content of U, th and Pb isotopes in each monazite sample according to the laser ablation data, and analyzing and determining the age of U-Th-Pb of the monazite samples, wherein the age of the obtained U-Th-Pb is 513 Ma.
Example 6
The etched monolithic samples of example 2 were observed under fission tracks, track densities of the individual monolithic samples were counted, and the test areas were labeled with coordinates.
And placing the marked individual stone samples and the selected standard samples under a LA-ICP-MS instrument for laser ablation to obtain laser ablation data, wherein the age standard sample is a 44069 standard sample+RW-1 standard sample, the U content standard sample is a NIST610 standard sample, the 44069 standard sample is used as a main standard sample, and the RW-1 standard sample is used as a monitoring standard sample. The RW-1 standard sample and the monazite sample are measured simultaneously, so that a basis can be provided for the accuracy of the experiment.
Obtaining individual monazite samples according to laser ablation data 238 U content and according to track density and sum of individual monazite samples 238 The U content, the age of the fission track of the batch of monazite samples was determined by analysis.
The relative amounts of U, th and Pb isotopes in each monazite sample were obtained from the laser ablation data and further analyzed to determine the U-Th-Pb age of the batch of monazite samples.
Example 7
The etched monolithic samples of example 3 were observed under fission tracks, track densities of the individual monolithic samples were counted, and the test areas were labeled with coordinates.
And placing the marked individual stone samples and the selected standard samples under a LA-ICP-MS instrument for laser ablation to obtain laser ablation data, wherein the age standard sample is a 44069 standard sample+RW-1 standard sample, the U content standard sample is a NIST610 standard sample, the 44069 standard sample is used as a main standard sample, and the RW-1 standard sample is used as a monitoring standard sample. The RW-1 standard sample and the monazite sample are measured simultaneously, so that a basis can be provided for the accuracy of the experiment.
Obtaining individual monazite samples according to laser ablation data 238 U content and according to track density and sum of individual monazite samples 238 The U content was analyzed to determine the age of the fission track for this batch of monazite samples.
The relative amounts of U, th and Pb isotopes in each monazite sample were obtained from the laser ablation data and further analyzed to determine the U-Th-Pb age of the batch of monazite samples.
Example 8
The etched monolithic samples of example 4 were observed under fission tracks, track densities of the individual monolithic samples were counted, and the test areas were labeled with coordinates.
And placing the marked individual stone samples and the selected standard samples under a LA-ICP-MS instrument for laser ablation to obtain laser ablation data, wherein the age standard sample is a RW-1 standard sample+ 44069 standard sample, the U content standard sample is a NIST610 standard sample, the RW-1 standard sample is used as a main standard sample, and the 44069 standard sample is used as a monitoring standard sample. The 44069 standard sample and the monazite sample are measured simultaneously, so that a basis can be provided for the accuracy of the experiment.
Obtaining individual monazite samples according to laser ablation data 238 U content and according to track density and sum of individual monazite samples 238 The U content, the age of the fission track of the batch of monazite samples was determined by analysis.
The relative amounts of U, th and Pb isotopes in each monazite sample were obtained from the laser ablation data and further analyzed to determine the U-Th-Pb age of the batch of monazite samples.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
Claims (10)
1. A monazite fission track based yearn method, the method comprising:
etching a plurality of monazite samples to expand the fission track of each of the monazite samples to a degree that is observable by a fission track analyzer;
placing the etched plurality of monazite samples under a fission track analyzer for observation, counting track density of each monazite sample, and marking test position coordinates of each monazite sample;
performing laser ablation on each monazite sample and a selected standard sample by using a laser ablation inductively coupled plasma mass spectrometer according to the test position coordinates of each monazite sample, and calculating the positions of each monazite sample according to laser ablation data 238 U content;
based on the track density of each of the monazite samples, the track density of each of the monazite samples 238 And (3) determining the fission track age of the plurality of monazite samples through analysis.
2. The method according to claim 1, wherein the method further comprises: determining the relative content of U, th and Pb isotopes in each monazite sample according to the laser ablation data;
and analyzing and determining the U-Th-Pb ages of the plurality of monazite samples according to the relative content of U, th and Pb isotopes in each monazite sample.
3. The method of claim 2, wherein the selected standard samples comprise age standards and U-content standards;
the age standard samples are 44069 standard samples and RW-1 standard samples;
the U content standard sample is an NIST610 standard sample.
4. The method of claim 1, wherein the etching the plurality of monazite samples comprises:
placing the plurality of monazite samples into a closed container filled with 12 mol/L concentrated hydrochloric acid;
200 h-650 h are etched at room temperature to expand the fission track of each of the monazite samples.
5. The method of claim 4, wherein the room temperature condition is maintained at 23 ℃ or higher and 27 ℃ or lower in summer or autumn, and the etching time is 200 h or higher and 450 h or lower.
6. The method of claim 5, wherein the room temperature condition is maintained at 25 ℃ and the etching time period is 250 h.
7. The method of claim 4, wherein the room temperature condition is maintained at 18 ℃ or higher and 23 ℃ or lower in spring or winter, and the etching time is 450 ℃ or higher and 650 h or lower.
8. The method of claim 7, wherein the room temperature condition is maintained at 20 ℃ and the etching duration is 560 h.
9. The method of claim 1, wherein etching the plurality of monazite samples is performed with a monazite etching device under heating;
wherein, the monazite etching device includes: glass reagent bottle, rubber stopper, water bath, thermometer and conduit;
the glass reagent bottle is inserted into the water of the water bath kettle;
the bottle mouth of the glass reagent bottle is plugged by the rubber plug;
the thermometer is inserted into the middle part of the glass reagent bottle through a first through hole of the rubber plug;
the guide pipe is inserted into the glass reagent bottle through the second through hole of the rubber plug so as to balance the pressure inside and outside the glass reagent bottle.
10. The method of claim 9, wherein etching the plurality of monazite samples is performed according to the following method:
loading 12 mol/L concentrated hydrochloric acid into the glass reagent bottle, and placing the plurality of monazite samples into the glass reagent bottle;
the rubber plug is plugged into the bottle mouth of the glass reagent bottle, the thermometer is inserted into the middle part of the glass reagent bottle through the first through hole, and the guide pipe is inserted above the liquid level of concentrated hydrochloric acid in the glass reagent bottle through the second through hole;
and placing the glass reagent bottle in the water bath kettle preheated to 90 ℃ for 45 min to obtain an etched monazite sample.
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| CN117330734A (en) * | 2023-11-22 | 2024-01-02 | 中国地质科学院地质力学研究所 | Standard sample analysis method based on zircon fission track legal year |
| CN117330734B (en) * | 2023-11-22 | 2024-05-28 | 中国地质科学院地质力学研究所 | Standard sample analysis method based on zircon fission track legal year |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117330734A (en) * | 2023-11-22 | 2024-01-02 | 中国地质科学院地质力学研究所 | Standard sample analysis method based on zircon fission track legal year |
| CN117330734B (en) * | 2023-11-22 | 2024-05-28 | 中国地质科学院地质力学研究所 | Standard sample analysis method based on zircon fission track legal year |
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