CN112649492A - Method for rapidly determining years of zircon U-Pb of LA-ICP-MS - Google Patents
Method for rapidly determining years of zircon U-Pb of LA-ICP-MS Download PDFInfo
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Abstract
The invention belongs to the field of analysis and detection, and particularly relates to a zircon U-Pb quick dating method for LA-ICP-MS (inductively coupled plasma-Mass Spectrometry). The method improves the traditional U-Pb dating test efficiency of LA-ICP-MS zircon to 240 points per hour from 20 points per hour, reduces the analysis time to 5 to 9 seconds from 60 to 80 seconds, and improves the analysis efficiency by one order of magnitude. The quality of the denudation substance in unit time is improved, so that the signals of the elements Pb and U to be detected are improved, and the capability of LA-ICP-MS for analyzing low-content substances is improved due to high-frequency denudation; the number of laser pulses is only 100-180 times, which significantly reduces the amount of zircon consumed and the depth of the denudation pits. The test cost of relevant basic geoscience research, regional geological survey and regional mineral resource exploration in the geological industry is greatly saved.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a zircon U-Pb quick dating method for LA-ICP-MS.
Background
Isotopic geology has become a fundamental tool for exploring problems in geologic bodies, air evolution, continental dynamics, and the like. The most common isotope dating method is the paramineral U-Pb dating method. Zircon is a by-product mineral widely found in nature and is commonly found in various rocks including sedimentary, magmatic, and metamorphic rocks. The age of the zircon U-Pb is combined with the formation temperature, trace elements, Hf-O isotopes and the like, and important geological parameters are provided for determining the space-time evolution of geological action. Statistically, more than 1 million academic papers published with age data for zircon U-Pb have been published. At present, the requirement of the earth science field of China on the U-Pb annual quantity of zircon is high, and 10-20 data points are needed to be analyzed and tested for the zircon pulp formed in a simple rock body. However, more data points are needed to provide more valuable information for the source tracing research using the clastic zircon, and experts in the industry are required to develop a clastic zircon research of a sample, which provides at least 100-300 data points. The enormous data volume requirements present a significant challenge to the efficiency of analytical testing techniques.
Two main techniques for carrying out U-Pb dating in situ in zircon micro-area are secondary ion probe technique (SIMS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The current SIMS technology can measure U-Pb age of zircon in a three-dimensional sampling space scale with the diameter of 5-20 microns and the depth of 1-2 microns. The external accuracy of SIMS zircon U-Pb fixed-year analysis can reach 1%, the analysis speed is low (one-point analysis is about 10-15 minutes), and in most cases, the SIMS analysis method is only considered to be adopted when important scientific research is carried out. And the age of U-Pb of the zircon is measured by LA-ICP-MS in a three-dimensional sampling space scale with the diameter of 30-40 micrometers and the depth of 20-30 micrometers. The technology has the characteristics of low cost, high analysis speed (about 2 minutes for one-point analysis) and external accuracy of U-Pb dating year reaching 2-3%. Therefore, LA-ICP-MS becomes an analysis testing technology which is more selective for a large number of basic geologists.
At present, when LA-ICP-MS zircon U-Pb dating is carried out by colleges and universities, scientific research units or third-party detection institutions in the market all over the country, the conventional analysis and test scheme is that laser beam spots are 20-40 microns, single-point analysis time is about 2 minutes, and price is 70-100 yuan. Plus the time of analysis of the standard sample (about 8-10 standards per hour), the actual sample testing efficiency per hour is typically 20-22 points per hour at a price of 1400-2200 dollars per hour. A rock for which clastic zircon research is to be conducted requires an average analysis of 200 zircon points, which may take about 10 hours and about 14000-. Therefore, if the annual analysis and test efficiency of zircon U-Pb can be further improved, the method has a great promoting effect on relevant research in the field of earth science and has the effect of saving research expenses.
The rapid zircon dating technology has been studied internationally and reported in related papers. The highest analytical efficiency reported in the current paper is 1200 dots per hour. This result was obtained from 2020 research results of Arizona project group (Sundell et al 2020, Rapid U-Pb geocerology by Laser alignment Multi-Collector ICP-MS) which utilized Laser Ablation in combination with large multiple-receiver plasma magnetic Mass Spectrometry (LA-MC-ICP-MS) to control the analysis time at 30 seconds, 12 seconds, 6 seconds and 3 seconds per spot and compare the analysis test results. The result shows that the data spectrogram of the clastic zircon obtained by the analysis time of 3 seconds (-1.8 seconds of signal acquisition and-1.2 seconds of gas background) is basically consistent with the spectrogram of the conventional U-Pb dating year. However, the paper has a problem that 1.1200 dots/hour is a theoretical working efficiency, and the analysis time of the standard substance in the analysis process and the time required for the laser to move to the next sample dot are not considered at all; 2.1200 points/hour is extremely poor, and the 1200 points/hour method is known from the data in the paper206Pb/238The test accuracy of the U age is 0.7-13.6%,207Pb/235the test precision of the U age is 1.2-104.3%; obtained by the 600 o' clock/hour method206Pb/238The test precision of the U age is 0.7-18.0%,207Pb/235the test precision of the U age is 1.0-23.5%; obtained by the 600 o' clock/hour method206Pb/238The test precision of the U age is 0.7-18.0%,207Pb/235the test precision of the U age is 1.0-23.5%; 300 dots/smallObtained by a time method206Pb/238The test accuracy of the U age is 0.7-4.7%,207Pb/235the test precision of the U age is 0.9-20.0%; obtained by the 120 point/hour method206Pb/238The test precision of the U age is 0.6-8.2%,207Pb/235the precision of the U-age test is 0.7-19.8%. Namely, the analysis and test precision of the U-Pb age obtained by the rapid zircon dating technology of the predecessor hardly reaches the data quality requirement of the U-Pb age analyzed by the conventional LA-ICP-MS: the external precision reaches 2-3%.
Referring to FIG. 1, the poor data quality is due to almost all rapid zircon dating techniques, simply reducing the analytical test time from the conventional 60-80 second sampling time to seconds. However, the data processing scheme still adopts the traditional point by point data processing method. In the data processing method of point by point, the average value and uncertainty of the Pb/U ratio are calculated by the arithmetic average value and standard deviation, respectively. When the analysis test time is shortened, the amount of data collected by the mass spectrometer is reduced, and the data of the arithmetic mean and the standard deviation are naturally influenced. It is difficult to obtain good data results.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method overcomes the defects of the prior art and provides a new rapid U-Pb dating method which comprises the adjustment of laser parameters and the improvement of a data processing mode in the sample analysis process.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a zircon U-Pb rapid dating method based on LA-ICP-MS specifically comprises the following steps: step (1): making a target sample comprising a tested sample and a standard sample; (2): selecting points, marking and adjusting laser ablation parameters of the zircon to be detected at the laser software; (3) collecting data: setting the sampling number of each sample to be N according to requirements, and setting laser to automatically and sequentially denudate the 1 st point to the Nth point, wherein the single sampling analysis time is divided into laser denudation time and time for moving the laser to the next analysis point, and the total time is less than 15 seconds; (4) data processing: a single signal of the sample is collected,the single-point sample signal is divided and corrected for background interference, and then is calculated by a linear regression processing method206Pb/238U and207Pb/235the ratio of U; (5) the data of the tested sample was corrected by the standard sample to obtain a weighted average age of zircon U-Pb.
Further, the linear regression processing method specifically includes utilizing a linear regression technique and calculating206Pb/238U and207Pb/235calculating uncertainty of the ratio of U by using an uncertain calculation formula of Excel's LINEST linear regression slope, and using standard sample206Pb/238U and207Pb/235correcting the sample to be measured by the ratio and uncertainty of U206Pb/238U and207Pb/235mass fractionation of the U ratio to obtain the final sample206Pb/238U and207Pb/235u corrects the ratio and uncertainty.
Further, the laser ablation parameter is that each analysis point is ablated by laser for 5-9 seconds, preferably for 7 seconds; the beam spot is 20-40 microns; the frequency is 5-50 Hz; preferably 20 HZ.
The beneficial effects obtained include: (1) the method of the invention improves the U-Pb fixed-year testing efficiency of the traditional LA-ICP-MS zircon from 20 points/hour to 240 points/hour, reduces the analysis time from 60-80 seconds to 5-9 seconds, and improves the analysis efficiency by one order of magnitude. The quality of the denudation substance in unit time is improved, so that the signals of the elements Pb and U to be detected are improved, and the capability of LA-ICP-MS for analyzing low-content substances is improved due to high-frequency denudation; (2) the number of laser pulses is only 100-180 times, which significantly reduces the amount of zircon consumed and the depth of the denudation pits.
Drawings
FIG. 1 shows the raw data of Pb and U signals in U-Pb definite years of conventional LA-ICP-MS zircon (a) and the signal ratio of 207Pb/238U (b)
FIG. 2 is a graph of a signal profile (a) obtained when a zircon standard 91500 was analyzed by LA-ICP-MS and a 206Pb/238U ratio (b) obtained by a linear regression correction scheme.
FIG. 3 shows U-Pb harmonized ages of zircon standard 91500 (left panel) and Rak-17 (right panel) obtained by the protocol of example 1.
Detailed Description
The invention will be further described with reference to the following examples:
the specific test steps of the invention are as follows: (1) starting LA-ICP-MS equipment, and adjusting the instrument to an optimal state through a reference substance; (2) selecting points, marking and adjusting laser ablation parameters of the zircon to be tested at a laser software, wherein each analysis point is subjected to laser ablation for 7 seconds, the beam spot is 20-40 microns, and the frequency is 20 Hz; (3) after the laser point selection is finished, determining the time required for completing all laser analysis points according to the number of analysis points determined by the laser, and then establishing a corresponding analysis method in a mass spectrometer, wherein the time for acquiring data by the analysis method can completely cover the time required for laser analysis; (4) firstly, starting a mass spectrometer to collect data, and then operating a laser ablation system to start automatic sequential ablation; (5) 15 seconds are needed for single laser analysis, wherein 7 seconds of laser ablation is needed, and the laser can move to the next analysis point within 8 seconds, so that the analysis efficiency of 240 points per hour can be completely realized; (6) after the analysis is completed, the original data is analyzed, firstly, the data in the whole file needs to be divided into single sample signals, and the function can be realized by a computer algorithm or a laser ablation log file; (7) the segmented data was first corrected for background interference and then calculated using linear regression techniques (FIG. 2 (b))206Pb/238U and207Pb/235calculating the uncertainty of the ratio by using an uncertain calculation formula of Excel's LINEST linear regression slope; (8) using standards206Pb/238U and207Pb/235correcting the sample to be measured by the ratio and uncertainty of U206Pb/238U and207Pb/235mass fractionation of the U ratio to obtain the final sample206Pb/238U and207Pb/235correcting ratio and uncertainty (an external standard correction method and considering an uncertainty transfer rule); (9) the samples being processed by means of the general software isoplot of geochemistry206Pb/238U and207Pb/235u corrects the ratio, obtains the synergistic age of the sample, or206Pb/238Weighted average age of U.
In the traditional zircon U-Pb analysis, the analysis time is required to be 60-80 seconds, and the ablation pit cannot be too deep so as to avoid the serious down-hole fractionation effect, so that the frequency of laser ablation is in the range of 5-10Hz, and the pulse number of the laser ablation is controlled to be 400-600 times. The research proposes that for the peak-shaped signal, a data processing mode of point by point is not adopted any more, and a linear regression correction technology is adopted to determine the Pb/U ratio.
As shown in FIG. 2, in FIG. 2 (a)206Pb、207Pb and238the complete analysis process for U is only 15 seconds, with the first 5 seconds being the background blank time, and after 7 seconds of laser ablation, the signal intensity can drop to near the blank value at the 15 th second. We took the entire 15 seconds of FIG. 2 (a)238The signal U is taken as the abscissa and,206the signal intensity of Pb as the ordinate makes it possible to obtain a scatter diagram in fig. 2 (b). The data can be found to show good positive correlation arrangement, and the correlation coefficient R20.9981 can be achieved. The slope of the regression line is206Pb/238The ratio of U. By replacing the point by point method with a linear regression method, we can get a more robust element ratio, especially when dealing with peak-shaped signals. By using the slope shown in FIG. 2 (b), the subsequent U-Pb chronological data correction can be performed.
Example 1
In the embodiment, the LA-ICP-MS analysis method is adopted to rapidly analyze 2 international zircon standard substances.
Putting zircon standard substances GJ-1, 91500 and Rak-17 into a laser sample ablation pool, wherein GJ-1 is used as an external standard substance to correct isotope mass fractionation, and 91500 and Rak-17 are used as detected samples to verify data quality; (2) starting LA-ICP-MS equipment, and adjusting the instrument to an optimal state through a reference substance; (3) selecting points, marking and adjusting laser to the zircon to be tested at the laser softwareThe optical ablation parameters comprise that each analysis point is subjected to laser ablation for 7 seconds, the beam spot is 32 microns, the frequency is 20Hz, 20 points (5 minutes) are analyzed for each sample to be detected, and the analysis is carried out twice on GJ-1, wherein the analysis totally comprises 20 91500 and 40 Rak-1; (4) the analysis takes about 17 minutes for 20 91500 samples, 40 Rak-1 samples and 8 GJ-1 samples, and 68 samples, so that an analysis method with data acquisition time of 17-18 minutes is established in a mass spectrometer, and the time for acquiring data can completely cover the time required by laser analysis; (5) firstly, starting a mass spectrometer to collect data, and then operating a laser ablation system to start automatic sequential ablation; (6) after the analysis is finished in 17 minutes, analyzing the original data, and firstly, segmenting the data in a whole file into single sample signals by using professional software; (7) the segmented data is corrected for background interference and then calculated by utilizing a linear regression technology206Pb/238U and207Pb/235calculating the uncertainty of the ratio by using an uncertain calculation formula of Excel's LINEST linear regression slope; (8) using GJ-1 as a standard206Pb/238U and207Pb/235correcting the sample to be measured by the ratio and uncertainty of U206Pb/238U and207Pb/235mass fractionation of the U ratio to obtain the final sample206Pb/238U and207Pb/235correcting ratio and uncertainty (an external standard correction method and considering an uncertainty transfer rule); (9) with reference to FIG. 3, the samples were processed using the general software for geochemistry isoplot206Pb/238U and207Pb/235u corrects the ratio, obtains the synergistic age of the sample, or206Pb/238Weighted average age of U. The resulting sample 91500 was tested in this example for age synergy with Rak-17. 91500 test cooperation age 1065.0 + -3.9 Ma, consistent with recommended value 1064 Ma within error range; the test cooperation age of the Rak-17 is 299.91 +/-0.90 Ma, the deviation is 1.6 percent from the recommended value 295Ma, but the reasonable range of the data error of the LA-ICP-MS is met, and particularly, the Rak-17 is a zircon standard substance with low U and Pb contents, and the annual test difficulty of zircon U-Pb is higher.
In addition, the analysis and test precision of all the analysis test points is less than 3%, and a rapid (240 points/hour) and high-quality U-Pb annual analysis strategy is realized. The technical scheme improves the U-Pb fixed-year testing efficiency of the traditional LA-ICP-MS zircon from 20 points/hour to 240 points/hour, and the testing efficiency is improved by 8 times.
In conclusion, the method greatly improves the annual test efficiency of the LA-ICP-MS zircon U-Pb, and if the annual test cost of the LA-ICP-MS zircon is charged by hours and is about 1800 yuan per hour on average, the new scheme reduces the test cost by 87.5 percent, thereby greatly saving the test cost of relevant basic earth science research, regional geological survey and regional mineral resource exploration in geological industry. The new analysis and test scheme has high efficiency, the data quality is not influenced, and the method can be rapidly popularized in various geological universities and colleges, scientific research institutions and third-party geological analysis and test platforms.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention should still fall within the scope of the patent coverage of the present invention without departing from the technical solution of the present invention.
Claims (8)
1. A zircon U-Pb rapid dating method based on LA-ICP-MS is characterized by comprising the following steps: step (1): making a target sample comprising a tested sample and a standard sample; step (2): selecting points, marking and adjusting laser ablation parameters of the zircon to be detected at the laser software; and (3): collecting data: setting the sampling number of each sample to be N according to requirements, and setting laser to automatically and sequentially denudate the 1 st point to the Nth point, wherein the single sampling analysis time is divided into laser denudation time and time for the laser to move to the next analysis point; and (4): data processing: collecting single sample signal, segmenting the single sample signal, correcting background interference, and performing linear regressionCalculate out206Pb/238U and207Pb/235the ratio of U; and (5): the data of the tested sample was corrected by the standard sample to obtain a weighted average age of zircon U-Pb.
2. A method for rapid dating of U-Pb zircon based on LA-ICP-MS as in claim 1, wherein said single sample analysis time is less than 15 seconds in total.
3. The LA-ICP-MS-based zircon U-Pb rapid dating method as claimed in claim 1, wherein the linear regression processing method specifically comprises using linear regression technique and calculating206Pb/238U and207Pb/235calculating uncertainty of the ratio of U by using an uncertain calculation formula of Excel's LINEST linear regression slope, and using standard sample206Pb/238U and207Pb/235correcting the sample to be measured by the ratio and uncertainty of U206Pb/238U and207Pb/235mass fractionation of the U ratio to obtain the final sample206Pb/238U and207Pb/235u corrects for the ratio and uncertainty values.
4. A method for rapid dating of zircon U-Pb based on LA-ICP-MS as claimed in claim 1, wherein said laser ablation parameters are laser ablation for 5-9 seconds per analysis point; the beam spot is 20-40 microns; the frequency is 5-50 Hz.
5. A method for rapid dating of zircon U-Pb based on LA-ICP-MS as in claim 4, wherein said laser ablation time per analysis point is 7 seconds.
6. A method of LA-ICP-MS based zircon U-Pb rapid dating according to claim 5, wherein 5 seconds before the laser ablation time is background blank time.
7. A method for rapid dating of zircon U-Pb based on LA-ICP-MS as claimed in claim 4, wherein said laser ablation parameter has a frequency of 20 Hz.
8. A method for rapid dating of zircon U-Pb based on LA-ICP-MS as claimed in claim 1, wherein said segmentation method is realized by computer algorithm or log file by laser ablation to segment the data in a whole file into single sample signal.
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| CN113791131A (en) * | 2021-08-19 | 2021-12-14 | 核工业北京地质研究院 | Method for constructing age three-dimensional distribution image of zircon secondary ion mass spectrum |
| CN114295598A (en) * | 2021-12-21 | 2022-04-08 | 中国地质大学（武汉） | Method for distinguishing type of zircon original rock by applying zircon lattice damage |
| CN116297465A (en) * | 2023-05-25 | 2023-06-23 | 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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| 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 |
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Cited By (7)
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| CN113791131A (en) * | 2021-08-19 | 2021-12-14 | 核工业北京地质研究院 | Method for constructing age three-dimensional distribution image of zircon secondary ion mass spectrum |
| CN114295598A (en) * | 2021-12-21 | 2022-04-08 | 中国地质大学（武汉） | Method for distinguishing type of zircon original rock by applying zircon lattice damage |
| CN116429488A (en) * | 2023-03-24 | 2023-07-14 | 西藏巨龙铜业有限公司 | Method for inverting in-situ micro-regional chronology history of heterogeneous mineral and application |
| CN116429488B (en) * | 2023-03-24 | 2023-10-31 | 西藏巨龙铜业有限公司 | Method for inverting in-situ micro-regional chronology history of heterogeneous mineral and application |
| CN116297465A (en) * | 2023-05-25 | 2023-06-23 | 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 |
| 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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