CN113624830A - In-situ micro-area calcite U-Pb dating method - Google Patents
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Abstract
The invention discloses an in-situ micro-area calcite U-Pb dating method, which comprises the following steps: a calcite sample is cut to prepare an epoxy resin sample target; placing a sample into a laser ablation sample chamber, and adjusting the position of the sample in the optical axis direction; carrying out line scanning and denudation on the sample target to obtain43Ca,88Sr,139La,238U plasma signal intensity data; performing two-dimensional element imaging to obtain a two-dimensional element content distribution map; determining a high U analysis target area through a two-dimensional element content distribution map, carrying out point denudation on the high U target area, and measuring206Pb,207Pb,238U-ion signal intensity data; after obtaining the element signal data, calculating to obtain207Pb/206Pb and238U/206pb fractionation coefficient, correcting unknown sample ratio, constructing Tera-Wasserback diagram, and calculating age data and initial Pb isotope of calcite sample (b: (b))207Pb/206Pb). The invention has the advantages that: the technology has short test period, high spatial resolution and high success rate.
Description
Technical Field
The invention relates to the technical field of geological exploration, in particular to an in-situ micro-area calcite U-Pb dating method.
Background
Calcite (chemical formula CaCO)3) As a common mineral, it is widely present in various geological environments. During the crystallization of calcite, a certain amount of uranium (U) ((U))<10μg g-1) And a small amount of lead (Pb), which makes it potentially viable for U-Pb dating. The U-Pb dating technology for calcite has great application potential, particularly in the aspects of ancient environment, deposition process, diagenesis, structural deformation, mineral deposit cause, carbohydrate migration and the like. The previous age definition of these geological processes was mainly based on indirect minerals such as biotite Ar-Ar dating. But dating based on indirect minerals often has disputes, such as indirect minerals not representing the age of the geological process. Calcite is the direct mineral for these geological processes, and therefore calcite U-Pb dating technology can provide important chronologic data for these geological processes.
Traditionally, Isotope Dilution-Thermal Ionization Mass Spectrometry (ID-TIMS) is mainly adopted for carrying out U-Pb fixed-year development of calcite. The technology acquires data through four steps of sample drilling, acid dissolution digestion, separation and purification, computer test and the like. ID-TIMS can provide high-precision data quality, but the technical operation flow is complex and takes long time (>2 weeks), the amount of data acquired is limited. Meanwhile, as an integral analysis technology, the spatial resolution of the ID-TIMS is low, which causes great limitation when analyzing samples with varying zones. Laser ablation inductively coupled plasma mass spectrometry (Laser A)blation-Inductively Coupled Plasma-Mass Spectrometry, LA-ICP-MS for short) is widely used in U-Pb geology. LA-ICP-MS has the advantages of relative cheapness, simple maintenance and fast analysis speed (single-point analysis)<3mins), etc. However, the U content of calcite is generally low (<10μg g-1) This requires to obtain a sufficiently high signal intensity by increasing the sampling amount (laser ablation beam spot), but increasing the laser beam spot significantly reduces the spatial resolution, which is detrimental to calcite with complex compositional variations. Meanwhile, the U and Pb contents of calcite are extremely nonuniform on a micrometer scale, so that how to accurately determine the sampling position is a difficulty of the technology.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an in-situ micro-area calcite U-Pb dating method.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
an in-situ micro-area calcite U-Pb dating method comprises the following steps:
1) for a calcite sample or a rock sample containing calcite, firstly cutting to prepare an epoxy resin sample target, wherein the diameter of the sample target is 1 inch, and the thickness of the sample target is about 5mm so as to adapt to the size of a laser ablation sample chamber;
2) placing a sample into a laser ablation sample chamber, and adjusting the position of the sample in the optical axis direction to ensure that the laser beam is well focused;
3) carrying out line scanning ablation on calcite in a sample target by using a laser beam, loading the ablated aerosol into a four-stage rod ICP-MS plasma source for ionization by using helium as a carrier gas, and measuring43Ca,88Sr,139La,238U plasma signal intensity data;
4) performing two-dimensional element imaging by adopting Iolite 4 software to obtain a two-dimensional element content distribution diagram;
5) determining a high U analysis target area through a two-dimensional element content distribution diagram, performing point ablation on the high U target area by using laser beams, loading the ablated aerosol into a double-focusing fan-shaped magnetic field ICP-MS plasma source for ionization by using carrier gas, and measuring206Pb,207Pb,238U plasma signal intensity data;
6) during the measurement, two repeated tests of the calibration standard substance NIST SRM 614 (for testing the NIST SRM) were carried out after every ten unknown samples were tested207Pb/206Pb calibration), three calibration standards WC-1 (for use in238U/206Pb correction) and two quality monitoring standard substances Duff Brown Tank, ensuring that the measurement conditions of the standard substances and unknown samples are the same;
7) after obtaining elemental signal data, according to standard substances207Pb/206Pb、238U/206Measured value of Pb and its standard value to obtain corresponding fractional coefficient, for unknown sample207Pb/206Pb、238U/206Correcting the Pb ratio;
8) after correction as described above207Pb/206Pb、238U/206Constructing a Tera-Wasserback diagram of the Pb ratio, and calculating the age data and the initial Pb isotope (Pb) of the calcite sample207Pb/206Pb).
Compared with the prior art, the invention has the advantages that:
the existing LA-ICP-MS U-Pb fixed-year measurement mode is fused, a high-sensitivity interface cone is adopted, nitrogen is assisted to carry out sensitization sensitivity on an instrument, and meanwhile, a two-step measurement process is adopted, namely (1) two-dimensional element imaging is carried out; (2) and selecting a target area with high U content for U-Pb dating. The defects of long test period, small sample analysis quantity, low spatial resolution, low success rate and the like in the prior art are overcome.
Drawings
FIG. 1 is a two-dimensional elemental content distribution plot for an example of the present invention;
FIG. 2 shows age data and initial Pb isotope(s) of calcite samples according to examples of the invention207Pb/206Pb) composition diagram;
FIG. 3 is a graph showing the results of the elemental fractionation effects of NIST SRM 614, ARM-3 and WC-1 in accordance with an embodiment of the present invention;
FIG. 4 is a graph showing the effect of the different cone sets and the auxiliary nitrogen on the sensitization of the instrument according to the embodiment of the present invention;
FIG. 5 is a graph of the result of JT analysis according to an embodiment of the present invention, where FIG. 5a is set of S + H cone + Ar plasma, FIG. 5b is set of Jet + H cone + Ar plasma, and FIG. 5c is set of Jet + X cone + Ar-N2 plasma.
FIG. 6 is a graph comparing the results of the two-step process (a) and the one-step process (b) according to the example of the present invention
FIG. 7 is a graph of the results of Duff Brown Tank analysis in accordance with the present invention, wherein a b c d represents the results of 4 independent tests at different times, and the U content of the 4 tests is shown accordingly. a b c with an 85 micron laser beam spot and d with a 50 micron laser beam spot.
FIG. 8 is a graph of JT analysis results for inventive examples, where a is JT calcite results and b is JT calcite wall rock results, and U contents for 2 tests are also listed. The laser beam spot is 110 microns.
FIG. 9 shows the results of ASH-15 of the present invention, wherein a b represents the results of 2 independent tests at different times, and the U content of 2 tests is shown correspondingly. The laser beam spot is 110 microns.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings by way of examples.
An in-situ micro-area uranium-lead aging method for calcite, which comprises the following steps:
1) at four calcite age standards: WC-1(254 +/-6.4 Ma), Duff Brown Tank (64.04 +/-0.67 Ma), JT (13.797 +/-0.031 Ma) and ASH-15(2.965 +/-0.011 Ma) by the method of the invention. The U content of four calcite standard samples is widely distributed (0.5-20 mu g g)-1) The universality of the method for various calcites is fully demonstrated. These known ages serve as validation criteria in the present method for verifying the accuracy and precision of the method.
2) Firstly, the calcite sample is cast into a sample target (the diameter is 1 inch, the thickness is about 5mm) by using epoxy resin, the calcite section is exposed after slight grinding, and the calcite target is prepared for later use after polishing, cleaning and drying.
3) The calcite sample target was placed in the laser ablation instrument chamber and the chamber was purged with helium to fill it with helium.
4) The NIST SRM612 glass standard substance is adopted to optimize the condition of the four-stage rod ICP-MS instrument, so that206Pb and238the U signal is optimized while ensuring the oxide yield (ThO)+/Th+) Less than 1.0%, secondary ion yield (Ca)2+/Ca+) Less than 2.0%, Th+/U+The signal ratio is between 0.95 and 1.05.
5) In the on-line scanning mode, the laser beam spot is adjusted to be circular, the diameter is 50 mu m, and the laser energy density is 2.0J/cm2The surface scanning was carried out at a ablation frequency of 15Hz and a line scanning speed of 40 μm/s. The area of the area scan is typically 5.0mm by 5.0 mm.
6) The acquisition procedure was 10 seconds blank before instrumental analysis, several seconds (depending on the length of the line) of laser ablated line scan data, and 10 seconds blank after instrumental analysis. After each line scan of 10 unknown samples, 1 NIST SRM612 glass standard (used for instrument drift correction and elemental content calculation) was tested in duplicate to ensure that the standard and unknown samples were measured under the same conditions.
7) In this embodiment, when two-dimensional elemental imaging is performed, the ions to be measured and the characterized mass numbers are respectively24Mg,29Si,43Ca,55Mn,57Fe,69Ga,85Rb,88Sr,90Zr,137Ba,139La,140Ce,141Pr,146Nd,147Sm,153Eu,158Gd,159Tb,163Dy,165Ho,166Er,169Tm,173Yb,175Lu,206Pb,207Pb,208Pb,232Th,238U, the measurement integration time is 6 ms.
8) And performing offline processing on the data by adopting Iolite software (version 4.0), and performing instrument blank deduction and deduction on signals and instrument drift correction to calculate the signal intensity of different elements. The instrument response coefficient was calculated from the signal intensities and their contents of each element of NIST SRM612, as shown in equation (1) below,
wherein k is the instrument response coefficient, el is an element, I is the signal intensity, and C is the element content.
And (3) calculating an unknown sample content formula (2) according to the instrument response coefficient, and imaging a two-dimensional content distribution diagram.
9) Determining a high U target area through a two-dimensional element content distribution diagram, and performing point ablation on the high U target area by using laser beams (the diameter of a laser ablation beam spot is 50-110 mu m, and the laser energy density is 2.0J/cm)2The ablation frequency is 10Hz), the aerosol generated by ablation is carried into a double-focusing fan-shaped magnetic field ICP-MS plasma source by using carrier gas for ionization, and the ionization is measured206Pb,207Pb,238U plasma signal data;
10) the acquisition procedure is blank for 5 seconds before instrument analysis, laser ablation line scanning data for 30 seconds, and blank for 10 seconds after instrument analysis. Repeat 2 NIST SRM 614 (for each 10 unknown samples) tests207Pb/206Pb corrected), 3 WC-1 (for238U/206Pb calibration), 2 Duff Brow Tank (for data quality monitoring), ensuring that the standard and unknown samples are measured under the same conditions.
11) In the invention, when the U-Pb dating experiment is carried out, ions to be measured and the characterized mass numbers are respectively202Hg,204Pb,206Pb,207Pb,208Pb,232Th,235U,238U, measurement integration times are 2 ms, 15 ms, 25 ms, 2 ms, 10 ms, respectively.
12) Data were processed offline using Iolite software (version 3.7), firstThe signal is subtracted from the instrument blank and corrected for instrument drift. Is calculated to obtain207Pb/206Pb、238U/206The Pb ratio. Elemental fractionation curves were modeled according to NIST SRM 614 and used to correct for elemental fractionation of unknown samples. Then respectively calculating according to NIST SRM 614 and WC-1 to obtain207Pb/206Pb、238U/206The Pb instrument fractionation coefficient is shown in the following formulas (3) and (4),
where k is the instrument fractionation coefficient and 7/6 is207Pb/206Abbreviation for Pb ratio.
Wherein 8/6 is238U/206Abbreviation for Pb ratio
Correcting unknown samples according to fractional distillation coefficient207Pb/206Pb、238U/206The ratio of Pb, as shown by the following formula,
then according to the corrected207Pb/206Pb、238U/206Constructing a Tera-Wasserback graph by using Pb ratio data, and calculating the age data and the initial Pb isotope (Pb) of the calcite sample207Pb/206Pb) composition as shown in fig. 2.
The element fractionation effect of LA-ICP-MS is one of the main reasons for influencing the accuracy and precision of data results, therefore, the invention takes NIST SRM 614, ARM-3 and WC-1 as examples, and the element fractionation effect is researched. The results are shown in figure 3, where it can be seen that the effects of three different matrix elemental fractionation are similar, and therefore the fractionation model of NIST STM 614 can be used directly for the elemental fractionation correction of calcite.
The low U content of calcite requires high instrument sensitivity, so that the invention researches the sensitization effect of nitrogen gas added to the instrument in different cone groups. Under six modes (S + H cone group + Ar plasma, S + H cone group + Ar-N)2Plasma, Jet + H cone group + Ar-N2Plasma, Jet + X cone group + Ar-N2Plasma) to adjust instrument parameters such that206Pb and238the U signal is optimized while ensuring the oxide yield (ThO)+/Th+) Less than 1.0%, secondary ion yield (Ca)2+/Ca+) Less than 2.0%, Th+/U+The signal ratio is between 0.95 and 1.05. The results are shown in FIG. 4. The Jet + X cone group + Ar-N can be seen from the figure2The signal intensity is optimal under the condition of a plasma instrument, and the sensitivity of the instrument is improved by 3-5 times.
In order to further verify the influence of different instrument sensitivity modes on the experimental results, the JT calcite is taken as a research object, U-Pb dating experiments are respectively carried out in three modes, and the experimental results are shown in the following figure 5. As can be seen, the results for JT are best in the Jet + X cone group + nitrogen addition mode. And it is shown that only this pattern gives accurate age data. In conclusion, our experiments show that in Jet + X cone group + Ar-N2The instrument performance is best in the plasma mode, and calcite U-Pb age is accurately measured. With optimized instrument sensitivity, JT can be dating only 110 microns, which is significantly better than the 150-200 microns reported previously.
To further verify the perennial advantages of the two-step method proposed by the present invention, namely (1) performing two-dimensional elemental imaging; (2) the region with high U content was selected for U-Pb dating, and we compared the results of the two-step process with the one-step process, as shown in FIG. 6. As can be seen from the figure, the annual success rate of the two-step process is clearly superior to that of the one-step process.
To further verify the reliability of the process, we analyzed 3 calcite samples, as shown in figures 7, 8, 9. As can be seen from the figure, the age results for the 3 calcite standard are consistent with the recommended values within the error range. The analysis precision is 2% -3%.
In combination with the data, the invention provides an in-situ micro-area calcite U-Pb dating method, which can provide more favorable technical support for the chronogeological application of calcite.
The data in the above examples were all done on LA-ICP-MS of a Photo Machine analysis G2 excimer laser in series with a pyroelectric Element XR ICP-MS. The examples are given solely for the purpose of illustration and are not intended to be limiting. One skilled in the art can achieve the same results on a similar LA-ICP-MS instrument according to the present method.
It will be appreciated by those of ordinary skill in the art that the examples described herein are intended to assist the reader in understanding the manner in which the invention is practiced, and it is to be understood that the scope of the invention is not limited to such specifically recited statements and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (1)
1. An in-situ micro-area calcite U-Pb dating method is characterized by comprising the following steps:
1) for a calcite sample or a rock sample containing calcite, firstly cutting to prepare an epoxy resin sample target, wherein the diameter of the sample target is 1 inch, and the thickness of the sample target is 5mm so as to adapt to the size of a laser ablation sample chamber;
2) placing a sample into a laser ablation sample chamber, and adjusting the position of the sample in the optical axis direction to ensure that the laser beam is well focused;
3) carrying out line scanning ablation on calcite in a sample target by using a laser beam, loading the ablated aerosol into a four-stage rod ICP-MS plasma source for ionization by using helium as a carrier gas, and measuring the content of the aerosol43Ca,88Sr,139La,238Ion signal intensity data for U;
4) and (3) performing two-dimensional element imaging by adopting Iolite 4 software, performing offline processing on data, performing instrument blank deduction and deduction on signals, performing instrument drift correction, and calculating the signal intensity of different elements. Calculating an instrument response coefficient according to the signal intensity and the content of each element of the NIST SRM612, calculating the content of an unknown sample according to the instrument response coefficient, and imaging a two-dimensional content distribution map.
5) Determining a high U analysis target area through a two-dimensional element content distribution diagram, performing point ablation on the high U target area by using a laser beam, loading the ablated aerosol into a double-focusing fan-shaped magnetic field ICP-MS plasma source for ionization by using a carrier gas, and measuring the content of the aerosol206Pb,207Pb,238Ion signal intensity data for U;
6) during the measurement, after every ten unknown samples were tested, two repeated tests of the calibration standard substance NIST SRM 614 were carried out for207Pb/206Pb calibration, three calibration standards WC-1, for238U/206Pb corrects and two quality control standard substance Duff Brown Tank, guarantee the standard substance is the same with unknown sample measurement condition;
7) after obtaining elemental signal data, according to standard substances207Pb/206Pb、238U/206Measured value of Pb and its standard value to obtain corresponding fractional coefficient, for unknown sample207Pb/206Pb、238U/206Correcting the Pb ratio;
8) after correction as described above207Pb/206Pb、238U/206Constructing a Tera-Wasserback diagram of the Pb ratio, and calculating the age data and the initial Pb isotope (Pb) of the calcite sample207Pb/206Pb).
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| CN115561052A (en) * | 2022-10-12 | 2023-01-03 | 中国地质大学（武汉） | Preparation method and application of submicron calcite sample target |
| CN115561052B (en) * | 2022-10-12 | 2023-12-12 | 中国地质大学（武汉） | Preparation method and application of submicron calcite sample target |
| CN115825212A (en) * | 2023-01-09 | 2023-03-21 | 中国科学院地质与地球物理研究所 | In-situ micro-area xenotime Lu-Hf dating method |
| CN116203117A (en) * | 2023-01-30 | 2023-06-02 | 中国科学院地质与地球物理研究所 | In-situ microcell garnet Lu-Hf annual determining method |
| CN116203117B (en) * | 2023-01-30 | 2023-09-12 | 中国科学院地质与地球物理研究所 | In-situ microcell garnet Lu-Hf annual determining method |
| CN117420167A (en) * | 2023-12-14 | 2024-01-19 | 北京大学 | Method for measuring years of deep land shale natural crack calcite filling |
| CN117420167B (en) * | 2023-12-14 | 2024-03-05 | 北京大学 | Method for measuring years of deep land shale natural crack calcite filling |
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