CN112927762B - Method for determining high-precision age of micron-sized Xie stone - Google Patents
Method for determining high-precision age of micron-sized Xie stone Download PDFInfo
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- G01N23/2255—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident ion beams, e.g. proton beams
- G01N23/2258—Measuring secondary ion emission, e.g. secondary ion mass spectrometry [SIMS]
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Abstract
The invention relates to the field of sphene age determination, and provides a method for determining micron-sized high-precision age of sphene, which is used for measuring lead and uraniumIon ratio and measurement56Fe16O+The correlation between the lead ions and the uranium ions is used for correcting the measured lead-uranium ion ratio to obtain a corrected lead-uranium ion ratio; then calculating the corrected lead-uranium isotope ratio of the titanite according to the positive correlation between the corrected lead-uranium ion ratio and the measured uranium ion ratio; and finally, obtaining the lead and uranium age of the sphene according to the corrected lead and uranium isotope ratio. The method comprises the steps of respectively manufacturing a sphene standard sample slice and an unknown rock sample slice, and splicing the sphene standard sample slice and the unknown rock sample slice into a spliced sample target. Plating a conductive material on a sample target, and finding the position of the sphene mineral by utilizing an electron microscope and an energy spectrum; cleaning sample target, plating conductive material, utilizing secondary ion mass spectrometer to test relevant ion signal of sphene, finally determining the age of sphene by using the above-mentioned method. The method can solve the problem that the micron-sized sphene is difficult to determine for years, and has great application value.
Description
Technical Field
The invention relates to the field of sphene age determination, in particular to a method for determining micron-sized high-precision age of sphene.
Background
Isotopic geology is a fundamental tool for exploring the problems of geologic body space-time evolution, continental dynamics and the like. The precise isotope chronology research has important significance in the aspects of inverting geological historical events, discussing diagenesis dynamics background and deposit cause, and particularly is an indispensable means in the research of hydrothermal deposits with less obvious sequential relation between many metamorphic rocks and multiple stages of hydrothermal activities. At present, a plurality of existing analysis means are provided, wherein the dating of a radioactive isotope system is a basic method for obtaining absolute age in geological research, and the dating of a uranium-lead (U-Pb) system is a method which is most widely applied in the current solid geoscience research due to the fact that the uranium-lead (U-Pb) system has proper characteristics. At present, the main secondary minerals used for years include zircon, monazite, rutile, sphene and the like.
Titanite (CaTiSiO)5) Is a uranium-containing accessory mineral commonly existing in various medium-acid and alkaline invaded rocks, metamorphic rocks and various hydrothermal deposit. As a tool capable of dating, the tool has very wide application value in geological research. However, many sphene minerals have the characteristics of multiple growth stages and small particle size (generally, the particle size is 5-50 microns, and most of the sphene minerals are about 10 microns) in the rock. The problem of the age of the titanite at different stages can be solved only by directly measuring the age of the titanite mineral in the rock by adopting a high-precision dating method.
International reports of accurate dating of sphene include isotope dilution thermal ionization mass spectrometry (ID-TIMS) (1: Tilton and Grunenfelder, 1968; 2: Aleinikoff et al, 2007; 3: Huyskens et al, 2016), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) (4: Willigers et al, 2002), and Secondary Ion Mass Spectrometry (SIMS) (5: Ling et al, 2015). The three dating methods have advantages and disadvantages respectively.
Isotope dilution thermal ionization mass spectrometry (ID-TIMS) is the most accurate dating method, and is required to crush a rock sample and then pick out the sphene mineral, but the particle size of the sphene in the rock is very small (mostly about 10 micrometers), so that a plurality of particles are required to be dissolved into solution at high temperature by acid, and then the uranium and lead contents in the solution are measured, and the age is calculated. However, the sphene in the rock often grows in different geological history periods, after the sphene growing in different time periods is simultaneously selected, the sphene is chemically dissolved and analyzed, the sphenes with different ages are mixed together, and the measured mixed age cannot reflect the true age of the sphene.
Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) can be performed without mineral selection, and after the rock is sliced, the sphene can be directly selected from the slice for analysis, but the analysis method can generally measure particles with diameters of more than 30 micrometers, but the age of the sphene cannot be accurately measured by the analysis method because the sphene in most rocks is too small.
The ion probe performs micro-area in-situ analysis on the sphene, and has the characteristics of small sample consumption, long-time analysis, repeatable analysis and the like. Since the titanite has a relatively low uranium lead content and a relatively high common lead content. And the sphene is analyzed in situ in a micro-area by using an ion probe instrument with high precision and high spatial resolution, so that the problem of inclusion can be effectively avoided, and a more accurate result is obtained. Therefore, many scientists have developed the research and development and application related to the year of titanite uranium lead by using ion probes. Currently, ion probing with sphene has been carried out for years at Australian National University (ANU) and australian university of science (Curtin), Korea Basic Science Institute (KBSI) and sweden natural history museum's north ion probe laboratory (NORDSIM), and the chinese academy of sciences geology and geophysical research institute ion probe laboratory (CASIMS). However, although the importance of ion probes in sphene dating has been increasingly appreciated, there are still important technical issues to be solved. The ion probe has a matrix effect which is ubiquitous in different minerals. In recent years, although the SIMS dating method and matrix effect have been reported for different kinds of dating paraminerals, no research has been reported on the matrix effect of sphene, and it has not been known clearly how much the change in the composition and structure of sphene causes the age correction of the ion probe.
The applicant found that when measuring standard samples of sphene using the previous secondary ion mass spectrometry method (SIMS), the calculated age of different sphene standards was different from the true value. For example, the lead and uranium ages of sphene in metamorphic rocks in the south african forest wave metamorphic zone (i.e., the limppoo slab) mentioned in document 6 are about 1930 million years (Ma) on average, which is 5% lower than the lead age 2010 million. This may be due to insufficient accuracy of the sphene ion probe method (reference 6: Rigby et al, 2011).
Therefore, the method for determining the age of the micron-sized titanite in situ by combining multiple instruments is designed to improve the accuracy and precision of measurement, and solves the pending problem.
Reference documents:
document 1: tilton GR, Grunnfelder MH (1968) Sphene: ultraum-lead agents, science159(3822):1458-
Document 2: aleinikoff, J.N., Winstch, R.P., Tollo, R.P., Unruh, D.M., Fanning, C.M., and Schmitz, M.D.,2007, Ags and orientations of roads of the Kilingword family, sodium-central connectivity: electronics for the technical evaluation of sodium New England: American Journal of Science, v.307, No.1, p.63-118.
Document 3: huyskens, M.H., Yin, Q.Z., Li, Q.L., Li, X.H., Liu, Y.and Tang, G.Q.2016, In Search of New Monazite and titanium standards for In Situ U-Pb geochrology, Lunar and Planet Science Conference, p.2369.
Document 4: willigers BJA, Baker JA, Krogstad EJ, Peak DW (2002) precision and acid in the site of Pb-Pb rating of aptamer, monate, and muscle by laser approximation multiple-collector ICP-MS. Geochim Cosmohim Acta 66(6): 1051. beta. 1066
Document 5: ling XX, Schmadicke E, Li QL, Gose J, Wu RH, Wang SQ, Liu Y, Tang GQ, Li XH (2015) Age determination of new by in-situ SIMS U-Pb dating synthetic titanium A case determination of the new deposition from Lunan, Henan, China, Lithos 220:289 299
Document 6: rigby MJ, Armstrong RA (2011) SHRIMP damming of titanium from metals in the Central Zone of the Lipopo Belt, South Africa.J Afr Earth Sci59(1): 149-154).
Disclosure of Invention
The technical problems solved by the invention are as follows:
when the previous age test method is designed, the influence of the change of the components of the sphene on the age test of the ion probe of the sphene is not considered, so that the previous test method causes deviation of up to 10%.
The applicant finds a reason influencing the testing age of the sphene ion probe based on a large number of experimental comparisons, improves a corresponding testing process aiming at the reason, finds a correction method through years of tests, and greatly improves the accuracy of the sphene age. The method can reduce the error from more than 10% to within 1.5%, and is the latest international test design and correction method in the field at present.
The invention adopts the following technical scheme:
method for determining high-precision age of micron-sized Xie stone, and method for measuring lead-uranium ion ratio by using sphene
And measuring iron signal intensity56Fe16O+The correlation between the lead and the uranium ions for the measurement of the lead-uranium ion ratio
Correcting to obtain corrected lead-uranium ion ratio
Correcting the lead-uranium ion ratio according to the correction
With measurement of uranium ion ratio
The positive correlation between the titanite and the mother liquor is calculated to obtain the corrected lead-uranium isotope ratio of the titanite
Finally, correcting the lead-uranium isotope ratio according to the correction
Obtaining the lead and uranium age t of sphenesample。
Further, the method specifically comprises the following steps:
s1, measuring the sphene sample to be measured by adopting a secondary ion mass spectrometer, and directly obtaining the measured lead-uranium ion ratio of the sphene sample to be measured
And the iron signal intensity in the secondary ions of the sphene sample to be measured56Fe16O+Ratio to primary ion beam intensity PB
Correcting lead-uranium ion ratio of sample to be detected
The calculation formula is as follows:
s2, based on the standard sample, correcting the lead-uranium isotope ratio of the sample to be detected to obtain the corrected lead-uranium isotope ratio of the sample to be detected
Wherein,
the lead-uranium isotope ratio of the standard sample is obtained;
correcting the lead-uranium ion ratio of a sample to be detected;
measuring the uranium ion ratio of a sample to be measured; A. b is a regression coefficient obtained by regression of standard sample measurement data;
s3, determining lead and uranium age t of sample to be detectedsample：
Wherein: lambda [ alpha ]238Is the decay constant, λ238＝1.55125×10-10。
Further, in step S2, the standard sample was titanite BLR-1 or titanite YQ 82.
Further, in step S2, the regression coefficient A, B is determined by:
measuring the known age of sphene standard sample BLR-1 to obtain 10 groups of data, and measuring the data
And
correcting according to the following formula;
obtained
And
fitting according to the following functional relation;
values for the regression coefficients A, B were obtained by fitting.
And further, preparing a sphene sample to be detected and a standard sample, and splicing the sphene sample to be detected and the standard sample to form a spliced sample target, so that the test detection of the sphene sample to be detected and the standard sample can be conveniently carried out under the same instrument condition.
Further, the specific preparation process of the spliced sample target comprises the following steps:
s0.1 preparation of standard sample sheet:
embedding a sphene standard sample with the particle size of 100-10 and 150 microns into a circular resin sheet with the diameter of about 2 millimeters and the thickness of 1-2 millimeters by adopting an electrostatic targeting technology, so that the sphene standard sample is exposed on one side surface of the resin sheet;
s0.2, preparing a sphene sample slice to be tested:
drilling a sample to be tested to obtain a circular slice to be tested with the diameter of about 25 mm and the thickness of 2 mm, and drilling a hole with the diameter of 5mm at the center of the slice to be tested;
s0.3, manufacturing a spliced sample target:
adhering a double-sided adhesive to one glass sheet, adhering the plane with the sphene sample on the sheet to be detected, which is obtained in the step S0.2, to the double-sided adhesive in a downward mode, placing the resin sheet obtained in the step S0.1 in the middle of the 5-millimeter hole of the sheet to be detected, and adhering the front plane to the double-sided adhesive in a downward mode, wherein the exposed side of the sphene is the front plane; filling resin in the annular gap between the resin sheet and the sheet to be detected, and forming a spliced sample target after the resin is solidified; the spliced sample target simultaneously has a sphene sample to be detected and a standard sample.
Further, in step S0.1, the sphene standard sample on the standard sample sheet is 1, or 2, or several sphene varieties of known ages.
Further, the titanite varieties of known age include the titanite standard YQ82 and the titanite standard BLR-1.
Further, the specific process of measuring the sphene sample to be measured and the standard sample is as follows:
Further, in step 1, a Hitachi bench electron microscope (TM) 4000 equipped with an Oxford spectrometer is used to distinguish different mineral phases by scanning the gray level of the sample image, and the sample containing Ca, Ti and Si elements is set as Xie stones.
The invention has the beneficial effects that: according to the method, on the basis of a large number of experimental comparisons, the reason influencing the test age of the sphene ion probe (namely, the iron content influences the yield of lead and uranium in a sample) is found, a corresponding test flow is improved and designed for the reason, and a correction method is found through years of experiments, so that the accuracy of the sphene age is greatly improved, the error can be reduced to be within 1.5% from more than 10%, and the method is the current international latest test design and correction method in the field; the method has great application value and wide application prospect.
Drawings
FIG. 1 is a schematic view showing a sheet of a standard sample in the examples.
FIG. 2 is a schematic view of a sphene sample slice to be tested in the examples.
FIG. 3 is a schematic view of a spliced sample target according to an embodiment.
FIG. 4 is a schematic view showing the spliced sample target after the sphene position is calibrated in the examples.
Fig. 5 shows uranium lead calibration curves for two sphene standards BLR and sphene YQ 82.
FIG. 6 is a schematic diagram illustrating the titanite age error determined by the method of the present invention and the conventional method; wherein, the abscissa represents the ratio of the iron content of different unknown samples to the iron content of the standard substance, the ordinate represents the error (%) between the corrected age and the real age, the red open icon represents the age error corrected by the traditional method, and the blue solid icon represents the age error corrected by the method of the invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects.
Sample and standard are used herein to distinguish between the test sample and the standard, marked below the right of the ratio; measure and calibrate are used to distinguish between the direct measurement and the corrected value, marked on the top right.
The symbols, formulas and representations referred to in this application have the following meanings in table 1:
TABLE 1
The embodiment of the invention provides a method for determining high-precision age of micron-sized sphene, which is used for measuring lead-uranium ion ratio by using the sphene
And measurement of56Fe16O+The correlation between the lead and the uranium ions for the measurement of the lead-uranium ion ratio
Correcting to obtain corrected lead-uranium ion ratio
Correcting the lead-uranium ion ratio according to the correction
With measurement of uranium ion ratio
The positive correlation between the titanite and the mother solution is calculated to obtain the corrected lead-uranium isotope ratio of the titanite sample
Finally, correcting the lead-uranium isotope ratio according to the correction
Obtaining the lead and uranium age t of sphenesample。
The overall technical scheme of the invention is explained in detail by the specific examples below.
Firstly, manufacturing a spliced sample target containing a sphene sample to be detected and a standard sample
The content of the unknown sphene mineral in the nature is changed, and the sphene standard sample with different components is required to be used as a calibration substance. Therefore, the invention respectively selects the titanite standard sample YQ82 (SiO) with different components2≈30.3％，TiO2≈36.7％，CaO≈28.6％，Al2O31.6%, FeO 1.0%) and sphene standard BLR-1(SiO2≈29.8％，TiO2≈31.9％，CaO≈27.1％，Al2O33.0%, FeO 2.3%) as standard substance for calibrating the instrument. During the calibration of the instrument, it is also necessary to use known instruments204A Pb content glass standard (e.g., the glass standard designated NIST 610) is used to calibrate the instrument (since the Pb content of sphene samples is often very low, if the instrument is calibrated using Pb from sphene, a deviation may result, and therefore a higher Pb content glass standard is required to calibrate the instrument, as is well known in the art).
According to the requirements of national measurement technical specifications, in order to check the repeatability of the test result, the repeated measurement times are all selected to be 10 times in a short time under the same instrument and the same test condition. Generally, one particle of the sphene standard substance can be tested 0-2 times, and therefore, the number of the particles of the two sphene standards is selected to be 7-10 in order to ensure the testing amount.
1.1 preparation of Standard sample sheet
Specifically, 7-10 sphene standard samples YQ82 with the particle size of 100-150 microns, 7-10 sphene standard samples BLR-1 with the particle size of 100-150 microns and 1-3 glass standard samples NIST610 with the particle size of 100-300 microns are inlaid into a circular resin sheet with the diameter of about 2 millimeters and the thickness of 1-2 millimeters by adopting an electrostatic targeting technology, so that the sphene standard samples and the glass standard samples are exposed on one side surface of the sheet.
The electrostatic target making process comprises the following steps: applying static electricity to a first insulating material plate with a smooth, transparent and firm surface by using an electrostatic generator; drawing a 2 mm diameter circle on a second sheet of insulating material; placing mineral samples sphene standard YQ82, sphene standard BLR-1, and glass standard NIST610 in an area of the electrostatically charged first sheet of insulating material corresponding to the circle; mixing epoxy resin with a coagulant in an environment of eliminating static electricity; vertically placing a polyethylene hollow column with a smooth surface on the region, corresponding to the circle, on the first insulating material plate with static electricity; and slowly injecting the mixture of the epoxy resin and the coagulant after vacuum pumping along the inner surface of the polyethylene hollow column, and standing to solidify the mixture, thereby obtaining the solidified sphene standard sample slice which can be taken out of the polyethylene hollow column. As shown in fig. 1.
1.2 preparing sphene sample slice to be measured
Specifically, in the first step, a boviet mine basalt slice sample is taken, the slice sample contains unknown boviet, and the slice sample is drilled by a TBH 28124 type desktop drill floor of PROXXON company and a hollow drill bit with the inner diameter of 26 mm. A circular sheet sample having a diameter of about 25 mm and a thickness of 2 mm was obtained. In the second step, the table drill floor was used, a solid drill bit with a diameter of 5mm was provided, and a hole with a diameter of 5mm was drilled in the center of the circular sheet, as shown in fig. 2.
1.3 splicing the standard sample slice and the sphene sample slice to be measured to obtain a spliced sample target
The method comprises the steps of firstly, adhering 10cm by 5cm double-sided adhesive on a glass sheet with the size of 10cm by 10cm, secondly, adhering the circular sheet with the diameter of about 25 mm to the double-sided adhesive with the front side facing downwards, and thirdly, putting the resin sheet with the diameter of 2 mm in the middle of the 5mm hole of the circular sheet, and adhering the resin sheet to the double-sided adhesive with the front side facing downwards. And fourthly, filling resin into the annular gaps between the resin sheet and the circular thin sheet, and splicing the solidified sample and the standard sample together to form a circular sheet with the diameter of 25 mm, wherein the circular sheet comprises the unknown sample of the sphene, the sphene standard samples YQ82 and BLR-1 and the glass standard sample NIST 610. A split sample target is shown in fig. 3.
Secondly, finding titanite by using electron microscope and energy spectrum instrument
2.1 plating of conductive Material
Specifically, a gold plating instrument of Q150TE model of Quorum company is adopted to plate a continuous gold film on the surface of the exposed side of the wafer sample, and in order to ensure that the sample to be detected can be conductive and cannot influence the observation of the sample, the thickness of the gold plating film layer needs to be controlled to be 10nm-20nm, for example, 10nm or 15nm and the like.
2.2 finding the position of sphene in the sample by electron microscopy and energy spectroscopy
The method comprises the following steps of (1) specifically, placing a sample into a Hitachi desk type electron microscope (TM 4000) equipped with an Oxford spectrometer, vacuumizing, and adjusting the working distance to 10 mm; secondly, by utilizing the characteristic function of an Oxford spectrometer (the function can automatically search a target sample in an analysis area according to the size, the appearance, the chemical composition and the like of the sample), under the conditions that the accelerating voltage is 15kV, the magnification is 200 times, and the input counting rate and the output counting rate both exceed 10000cps, different mineral phases are distinguished by scanning the gray level of a sample image, and thirdly, the threshold value of a specific detection sample is set, in the embodiment, the mineral sample to be detected is sphene, in the embodiment, the threshold value is set to be more than 10000, and the granularity of the detection particles is set to be more than 5 um; fourthly, after information collection is carried out on the samples, the samples containing Ca, Ti and Si elements are set as Xie stones; and fifthly, performing multi-field scanning on the inner circle with the outer diameter of 10mm and the inner diameter of 5mm at the center of the sample, in the embodiment, dividing the sample into 8 sub-areas, and then automatically operating. After the test, a plurality of regions containing Ca, Ti and Si elements were detected. And sixthly, confirming the found mineral to be the sphene mineral again by utilizing the elemental analysis function of the energy spectrometer again. Seventhly, using the back scattering image function of the Hitachi desktop electron microscope (TM) 4000, the position of YQ82 on the target is marked as (X1, Y1), the position of BLR-1 is marked as (X2, Y2), the position of NIST610 is marked as (X3, Y3), and the positions of the other sphene samples found are marked as (Xn, Yn), as shown in FIG. 4.
Third, testing titanite by secondary ion mass spectrometer method SIMS
3.1 cleaning samples
Specifically, the method comprises the steps of firstly polishing the surface of a sample by using 0.25um polishing paste, secondly cleaning the surface of the sample by using clear water, thirdly placing the sample in a beaker containing alcohol, ultrasonically cleaning the sample for three minutes by using an ultrasonic instrument, and fourthly drying the sample in a drying oven for one hour.
3.2 plating conductive material again.
Specifically, a gold plating instrument of Q150TE model by the company Quorum is used to plate a continuous gold film on the exposed surface of the cleaned wafer sample, and in order to ensure good conductivity of the sample, the plating thickness is 20nm to 50nm, for example, 20nm or 45 nm.
3.3 finding particles to be tested in a Secondary ion Mass spectrometer
Specifically, the sample target is placed into a sample cavity of a secondary ion mass spectrometer in the first step, the position of YQ82 on the target is firstly found and marked as (X1 ', Y1'), the position of BLR is marked as (X2 ', Y2'), the position of NIST610 is marked as (X3 ', Y3'), and the position of (Xn ', Yn') is calculated and obtained by utilizing a seven-parameter Boolean model in the second step. Thirdly, scanning the ion image nearby Xn ', Yn' (in the area with the diameter of 50 microns)40Ca48Ti2 16O4 +Signal, find40Ca48Ti2 16O4 +And setting the position as a test position in the area with the highest signal.
3.4: testing the signal of sphene by secondary ion mass spectrometer
Specifically, in the first step, an oxygen plasma ion source is adopted and focused to the sphene sample on the sample target in a gauss mode so as to generate secondary ions of the sphene sample; making secondary ion of sphene sample56Fe16O+，49Ti16O4 +，40Ca48Ti2 16O4 +，204Pb+，206Pb+，207Pb+，208Pb+，238U+，232Th16O+And are and238U16O+the ion signal detection system is reached through an electric field and a magnetic field in sequence; the test results are shown in table 2 below.
TABLE 2
Fourthly, determining the lead and uranium age t of sphene to be measured by adopting the methodsample
The method of the present invention will be described with reference to specific examples, wherein a sphene standard substance BLR-1 of a known age (1047Ma) is selected and described, the sphene standard substance BLR-1 is an age standard substance of sphene developed by isotope dilution thermal ionization mass spectrometry (ID-TIMS) in reference 2, and herein, a sphene sample YQ82 of a known age from shanxi in reference 3 is determined (corrected) using BLR-1 as a standard substance (to observe the accuracy of the method of the present invention).
Using a formula
Calculating lead and uranium age tsampleWhen the ratio of lead to uranium isotopes is adopted208Pb/238U, however, we have found that it is the ratio of lead to uranium ions that can be measured by the instrument206Pb+/238U+And this isRatio of lead to uranium ions206Pb+/238U+To true lead-uranium isotope ratio206Pb/238U is not the same, since when the primary ion O is2 -When bombarding the surface of the sample, the secondary ions Pb sputtered from the sample+And U+The yield difference results and therefore, when the secondary ion mass spectrometer is used for year-keeping measurement of sphene uranium lead, the yield of uranium and lead needs to be corrected so as to obtain the accurate lead-uranium age of the sphene sample.
In order to solve this problem, the applicant has found that the yield of uranium and lead in sphene is also affected by the iron content of the sphene sample. And the ratio of lead to uranium ions of sphene samples with iron influence eliminated
Ratio to uranium ion
There is a good positive correlation between the ions, as shown in fig. 5, showing the ratio of lead to uranium ions of sphene at different ages
Ratio to uranium ion
Positive correlation of (i.e. of sphene of different ages)
And
schematic of the positive correlation of) showing measurements of two different ages of sphene (e.g., sphene BLR and sphene YQ 82). Two straight lines can be respectively fitted according to the ratio measurement result of two sphenes with different ages, as shown in fig. 5, and the intercept difference of the two straight lines represents the age difference of the two sphenes with different ages (as the age of the sphene BLR is known, the age of the sphene BLR can be determined according to the ageCalculating the age of sphene YQ82 by intercept difference).
The specific determination process is as follows:
the first step is as follows: correcting the fractionation influence on uranium and lead caused by different iron contents in samples
The ion probe is adopted to test the related signal of sphene, and the lead-uranium ion ratio can be directly obtained
And the intensity of the iron signal in the secondary ion of the sphene sample56Fe16O+Ratio to primary ion beam intensity (PB) (i.e. ratio of primary ion beam intensity to primary ion beam intensity
). According to the experimental summary of years, the lead-uranium ion ratio obtained by correction
The relationship to the above two can be expressed by the following function, as in equation (1):
the second step is that: correcting for fractional distillation effects of uranium lead in a sample based on a standard
2.1, the Applicant has found that the lead-to-uranium ion ratio of titanite obtained after correction
Ratio to uranium ion
The positive correlation existing between them can be expressed by the formula (2): wherein A and B are constants:
transforming equation (2) can result in the following equation (3):
2.2, according to tests of the applicant, when
The ratio of the lead-uranium isotope to the ratio of the lead-uranium ion of the sphene sample, i.e.
Ratio of lead-to-uranium isotope ratio to lead-to-uranium ion ratio of sphene standard substance, i.e. ratio of lead-to-uranium isotope ratio to lead-to-uranium ion ratio
The measurement is carried out under the same instrument condition, and the same change relation is realized. The relationship between the aforementioned sphene sample YQ82 and a known-age sphene standard BLR-1 may be expressed by the following equation (4), where sample represents the sphene sample, standard represents the known standard, and calibrmation represents the ratio after preliminary calibration.
Combining equation (3) and equation (4) may translate into equation (5) below.
2.3 establishing a calibration curve for the current measurement based on the measurement standard
Measuring sphene standard substance BLR-1 with known age to obtain 10 groups of data, and obtaining measurement array
And
corrected according to the formula (1) to obtain
Then will be
And
according to formula (2)
Fitting to obtain the values of A and B.
2.4 Using the calibration curves, the ratio of Pb to U isotopes of sphene sample YQ82 was calculated
Of sphene standard substance BLR-1
Substituting the recommended value (e.g. 0.176379, which is calculated from the known age 1047Ma) and the values of a and B into equation (6), and based on the ratio of lead to uranium ions of sphene obtained after the first step of correction of the single point of the current measurement
And uranium ion ratio
Then obtaining the corrected lead-uranium ratio value of the sphene sample (such as YQ82)
Thirdly, calculating the age based on the corrected isotope ratio of uranium and lead in the sample
According to the formula
The lead-uranium age t of a sphene sample of unknown age can be calculated using the following equation (7), where λ238Is the decay constant (1.55125X 10)-10)。
According to the derivation of the above formula, the specific process for correcting the lead-uranium ratio in the present application can be simplified to include the following steps:
(1) the measured lead-uranium ion ratio
Converted into corrected lead-uranium ion ratio
(2) Array of standard substances to be measured
And
fitting according to the power function relationship to obtain values of A and B;
(3) the lead-uranium ion ratio of the tested sample is measured
And uranium ion ratio
Substituting into the relation function of the standard sample and the sample to obtain the corrected lead-uranium ratio value
(4) By using
And decay constant lambda238Calculating the lead-uranium age t of the measured samplesample
Since the previous age test method was designed without considering that the change of the composition of sphene may affect the age test of the ion probe of sphene, the previous method may cause a deviation of up to 20%. According to the method, on the basis of a large number of experimental comparisons, the reason influencing the test age of the sphene ion probe is found, the corresponding test process is improved and designed according to the reason, a correction method is found through years of experiments, the accuracy of the sphene age is greatly improved, the error can be reduced to be within 1.5% from more than 10%, as shown in fig. 6, the abscissa represents the ratio of the iron content of different unknown samples to the iron content of a standard substance, the ordinate represents the difference (%) between the corrected age and the true age, the red hollow icon represents the difference of the age obtained after the previous method is corrected, the difference of the age and the true age can reach more than 10%, and the blue solid icon represents the age difference corrected by the method and is reduced to be within 1.5%. This is the current international latest test design and calibration method in this field.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.
Claims (9)
1. The method for determining high-precision age of micron-sized sphene is characterized in that the method utilizes the measured lead-uranium ion ratio of the sphene
And measuring iron signal intensity56Fe16O+The correlation between the lead-uranium ion ratio and the measured lead-uranium ion ratio
Correcting to obtain corrected lead-uranium ion ratio
Correcting the lead-uranium ion ratio according to the correction
With measurement of uranium ion ratio
The positive correlation between the titanite and the mother liquor is calculated to obtain the corrected lead-uranium isotope ratio of the titanite
Finally, correcting the lead-uranium isotope ratio according to the correction
Obtaining the lead and uranium age t of sphenesample；
The method specifically comprises the following steps:
s1, measuring the sphene sample to be measured by adopting a secondary ion mass spectrometer, and directly obtaining the measured lead-uranium ion ratio of the sphene sample to be measured
And the iron signal intensity in the secondary ions of the sphene sample to be measured56Fe16O+Ratio to primary ion beam intensity PB56Fe16O+(ii)/PB; correcting lead-uranium ion ratio of sample to be detected
The calculation formula is as follows:
s2, based on the standard sample, correcting the lead-uranium isotope ratio of the sample to be detected to obtain the corrected lead-uranium isotope ratio of the sample to be detected
Wherein,
the lead-uranium isotope ratio of the standard sample is obtained;
correcting the lead-uranium ion ratio of a sample to be detected;
measuring the uranium ion ratio of a sample to be measured; A. b is a regression coefficient obtained by regression of standard sample measurement data;
s3, determining lead and uranium age t of sample to be detectedsample：
Wherein: lambda [ alpha ]238Is the decay constant, λ238＝1.55125×10-10。
2. The method of determining the high-precision age of micron-sized Xie stone of claim 1, wherein the standard sample is a sphene standard sample of a known age, and the standard sample is sphene BLR-1 or sphene YQ82 in step S2.
3. The method for determining the high-precision age of Xie micron-sized stones according to claim 1, wherein in step S2, the regression coefficients A, B are determined by:
measuring the known age of sphene standard sample BLR-1 to obtain 10 groups of data, and measuring the data
And
correcting according to the following formula;
obtained
And
fitting according to the following functional relation;
values for the regression coefficients A, B were obtained by fitting.
4. The method of claim 1, wherein the method for determining the high-precision age of micron-sized Xie stone comprises the steps of preparing a sphene sample to be tested and a standard sample, and combining the sphene sample to be tested and the standard sample to form a combined sample target, so as to facilitate simultaneous testing and detection of the sphene sample to be tested and the standard sample under the same instrument condition.
5. The method for determining the high-precision age of Xie micrometer-sized stone according to claim 4, wherein the specific preparation process of the spliced sample target comprises:
s0.1 preparation of standard sample sheet:
embedding a sphene standard sample with the particle size of 100-10 and 150 microns into a circular resin sheet with the diameter of about 2 millimeters and the thickness of 1-2 millimeters by adopting an electrostatic targeting technology, so that the sphene standard sample is exposed on one side surface of the resin sheet;
s0.2, preparing a sphene sample slice to be tested:
drilling a sample to be tested to obtain a circular slice to be tested with the diameter of about 25 mm and the thickness of 2 mm, and drilling a hole with the diameter of 5mm at the center of the slice to be tested;
s0.3, manufacturing a spliced sample target:
adhering a double-sided adhesive to one glass sheet, adhering the sphene sample-containing surface of the sheet to be tested obtained in the step S0.2 to the double-sided adhesive in a downward mode, placing the resin sheet obtained in the step S0.1 in the middle of the 5-millimeter hole of the sheet to be tested, and adhering the exposed surface of the sphene to the double-sided adhesive in a downward mode; filling resin in the annular gap between the resin sheet and the sheet to be detected, and forming a spliced sample target after the resin is solidified; the spliced sample target simultaneously has a sphene sample to be detected and a standard sample.
6. The method of determining the high accuracy age of Xie micron level stones according to claim 5, wherein in step S0.1, the titanite specimen of said master specimen sheet is 1, or 2, or several titanite species of known age.
7. The method of determining the high accuracy age of micron-sized Xie stone of claim 6, wherein the titanite species of known age includes titanite standard YQ82 and titanite standard BLR-1.
8. The method for determining the high-precision age of micron-sized Xie stone according to claim 5, wherein the specific process for measuring the titanite sample to be measured and the standard sample is as follows:
step 1, plating a conductive material on the spliced sample target, and finding the position of the sphene mineral in the spliced sample target by using an electron microscope and an energy spectrum instrument:
step 2, testing the sphene found in the step 1 by using a secondary ion mass spectrometer, and detecting to obtain a sphene sample to be tested and secondary ions of the sphene in the standard sample56Fe16O+，49Ti16O4 +，40Ca48Ti2 16O4 +，204Pb+，206Pb+，207Pb+，208Pb+，238U+，232Th16O+And are and238U16O+the signal strength of (c).
9. The method for determining the high-precision age of Xie micron-sized stones according to claim 8, wherein in step 1, the Hitachi bench electron microscope (TM) 4000 equipped with an Oxford spectrometer is used to distinguish different mineral phases by scanning the gray scale of the sample image, and the sample containing Ca, Ti and Si elements is set as Xie stones.
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