CN109580761A - One kind being suitable for the device and method of the absolute micro-zone in situ analysis of hafnium (oxygen) isotope and uranium lead age - Google Patents
One kind being suitable for the device and method of the absolute micro-zone in situ analysis of hafnium (oxygen) isotope and uranium lead age Download PDFInfo
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Abstract
The invention discloses a kind of device and methods of absolute micro-zone in situ analysis for being suitable for hafnium (oxygen) isotope and uranium lead age.The device includes laser ablation plasma system, quality sorting device, U-Pb Isotope Dating analysis system and Hf isotope analysis system.Zircon sample is by after laser ablation, it is transferred in plasma and is ionized, the sample of ionization enters in quality sorting device, the lightweight component containing Hf and the heavy mass component containing U-Pb are isolated under the deflecting action in magnetic field in quality sorting device, counterweight mass part carries out the analysis of U-Pb Isotope Dating, carries out Hf isotope or oxygen isotope analysis to lightweight part.
Description
Technical field
The invention belongs to geological sample analysis Instrument technology fields, and in particular to one kind is suitable for hafnium (oxygen) isotope and uranium
The device and method of the absolute micro-zone in situ analysis of lead age.
Background technique
Zircon is a kind of common accessory mineral in nature, with extremely low Gibbs energy, with particularly stable crystalline substance
Body structure so that it is easy to crystallize in various geological environments, and is fully preserved, is prevalent in deposition, rock
In slurry and metamorphic rock.In traditional sense, zircon has common lead content low, rich in the radioactive elements such as U, Th, ion diffusion speed
The features such as rate is low, and closure temperature is high is therefore widely used in petrology, mineralogy and geochemical investigation, especially closely
Over a little years, based on fine zircon mineral research, carry out relevant isotope work, zircon has become geology research
In one of ideal object.
Zircon U-Pb Age is one of the important method for obtaining the geologic body age, is contained by the uranium lead in analysis sample
It measures, and the age of geologic body is calculated according to its half-life period.Uranium element has 3 kinds of isotopes in nature, respectively238U、235U
With234U, wherein238U and235U can be decayed into over time206Pb and207Pb.Lead element has isotope in 4 in nature,
Respectively204Pb、206Pb、207Pb and208Pb。232Th is decayed into208Pb.Only204Pb is non-radioactivity genesis.If there is one
Kind mineral, U and Th is absorbed when being formed strongly, without absorbing lead, then can pass through the phase of this two groups of elements in measurement sample
Abundance is further calculated from sample closing to the time currently undergone.Its calculation formula is as follows:
206Pb*=238U(eλ238t-1)
207Pb*=235U(eλ235t-1)
207Pb*/206Pb*=1/137.88 (eλ235t-1)/(eλ238t-1)
Therefore for each geological sample, three independent ages can be obtained simultaneously, and if three ages are in error
It is consistent in range, it can be said that bright mineral are after its formation, U-Pb system be it is closed, i.e., U-Pb isotopic age is harmonious
, any one of this 3 ages can represent the age of mineral formation.Otherwise its U-Pb body since mineral formation has been illustrated
System is open or once in open state, or since common lead deduction is improper, U-Pb isotopic age is to discord
, the correct mineral formation age could be obtained by needing to carry out internal calibrations.With207Pb*/235U is abscissa, with206Pb*
/238U is on the X-Y scheme of ordinate, and different age values constitutes a harmonious line or is consistent curve.For same closing
System utilizes207Pb*/235U and206Pb*/238Age value obtained by U in error range should be consistent, and can fall on consistent line.If
After U-Pb System forming, the loss of lead or the acquisition of uranium occurred, drop point can constitute one below consistent line on the diagram
Straight line, referred to as discordia.Discordia and consistent line have 2 intersection points, and upper intersection point represents sample and forms age, lower intersection point table
Show the time that late events occur.Therefore Zircon U-Pb Age be geological sample determine the most frequently used and most important method in year it
One.
Hf is High field side injection identical with Ti, Zr, has 6 isotopes in nature, and abundance is respectively,174Hf
(0.162%),176Hf (5.206%),177Hf (18.606%),178Hf (27.297%),179Hf (13.629%), with180Hf
(35.100%).Hf and Zr is present in the mineral lattice of zircon in isomorph, other opposite mineral, and Hf content is high in zircon
(close to 1%), this provides guarantee to obtain high-precision Hf isotope ratio Value Data；Its Lu/Hf value is extremely low simultaneously, by176Lu
What decay was formed176Hf ratio is very low, and the influence of the Hf isotopics after being formed to zircon is little, and the Hf of such zircon is same
Position element composition substantially represents initial Hf isotopics when zircon crystallization.In addition zircon chemical property is stablized, have very
High Hf isotope closure temperature, can retain the same position initial Hf well experienced the high grade metamorphisms such as granulite facies
Element composition, therefore the Hf in zircon is very suitable for petrogenetic Hf Isotope Research.In recent years, Hf isotope application solves
Related important geological problem.Such as Griffin passes through the Hf isotope to zircon in Hua Nanping pool and Tonglu I I type granite body
Research finds that the Hf isotopics of the zircon of different stages of growth are different, and their microelement is formed there is also difference,
Disclose this 2 I I type granite bodies has the magma more than 2 kinds of separate sources that union dyeing has occurred in forming process.The equal utilization of Wang
Hf isotope in zircon has inquired into restriction of the mantle magma to the Peraluminous granite origin cause of formation.Bennet et al (1993) and
The Hf isotope in-situ test of the application zircon such as McCulloch et al (1994) successfully solves whether Early Archaean is deposited
The super depleted mantle the problem of.The U-Pb age of the REE feature of detrital zircon and its original position, Hf isotopics are surveyed in sedimentary rock
Determine to be recognized by the Hf isotope of multiple groups zircon by the powerful tool as research deposit parent rock and crustal evolution
Know its evolutionary process.
Currently, the common method of zircon U-Pb geochronology has: isotopic dilution-thermal ionization mass spectrometry (tims) (ID-TIMS), two
Secondary ion mass spectrography (SIMS) and laser ablation Plasma Mass Spectrometry (LA-ICP-MS).Other than Thermal Ionization Mass Spectrometry,
Obtain the analysis result of micro-zone in situ.
Since Hf has very high ionization energy, the thermal ionization mass spectrometry (tims) analysis of Hf isotope is extremely difficult.It is fast in recent years
The multiple-collector plasma source mass spectrometry instrument (MC-ICPMS) that speed grows up combines the high ionization temperature and magnetic-type of plasma
The advantage of multiple collector mass analyzer, completely can be with traditional thermal ionization in terms of the accuracy of isotope analysis and accuracy
Mass spectrum compares favourably, while being aided with laser microprobe sampling system, and LA-MC-ICPMS to a certain extent can also be as ion probe matter
Spectrum equally realizes high-precision isotope and the elemental analysis of micro-zone in situ.
But it, can not be in former test position because LA-ICP-MS needs biggish denudation, therefore after completing U-Pb test
Carry out Hf isotope analysis in situ.Now in order to which the U-Pb isotopic age and Hf isotope that obtain zircon micro-zone in situ are believed
Breath, generally using SIMS recycle after U-Pb isotope analysis LA-MC-ICPMS same position or different location into
Row Hf isotope analysis.Or micro-zone in situ analysis is carried out to variable grain using LA-ICPMS and LA-MC-ICPMS.It is resulting
Though age data and Hf isotopic data are micro-zone in situ, it is not the same position, is not absolute microcell
Information in situ leaves uncertainty for the geologic interpretation in later period.
Summary of the invention
The object of the present invention is to provide the absolute micro-zone in situ point for being suitable for hafnium isotope or oxygen isotope and uranium lead age
The device and method of analysis, after the present invention carries out laser ablation to sample and ionized by plasma, using the matter of special designing
It measures sorter and Pre-sorting is carried out to ion, ion beam effectively can be divided into high quality number (containing U-Pb) with low quality number (containing Hf
With two sections of O), and resulting two sections of ions are analyzed using corresponding analysis method, effectively obtain absolute micro-zone in situ
Hf isotope or oxygen isotope information and high-precision U-Pb age.
The device of the absolute micro-zone in situ analysis for being suitable for hafnium isotope or oxygen isotope and uranium lead age of the invention,
It is characterised in that it includes laser ablation plasma system, quality sorting device, U-Pb Isotope Dating analysis system and the same position Hf
Plain analysis system；
The sample export of laser ablation plasma system is connected with the sample inlet of quality sorting device, quality sorting device tail
End is equipped with 2 sample exports, i.e. the first sample export and the second sample export, the first sample export and Hf isotope analysis system
Sample inlet be connected, the second sample export is connected with the sample inlet of U-Pb Isotope Dating analysis system；
The quality sorting device includes the magnet on the inside or outside of sorting chamber and sorting cavity wall, and magnet is used in sorting chamber
Interior generation magnetic field space, sorting chamber front end are equipped with sample inlet, and tail end is equipped with 2 sample exports, i.e. the first sample export and the
Two sample exports；The magnetic field space is that the plasma sample for entering sample inlet separates under the deflecting action in magnetic field
Lightweight component containing Hf and O and the heavy mass component containing U-Pb out, weight mass component enter the second sample export, lightweight
Component enters the first sample port.
The laser ablation plasma system is to degrade zircon sample, and be transferred in plasma and carry out
Ionization, then give through ion transmission channel to the sample inlet of quality sorting device.
The U-Pb Isotope Dating analysis system is preferably level four bars mass spectrograph.
The Hf isotope analysis system preferably more receives magnetic-type mass spectrograph
The sorting chamber is horn-like in sample inlet end is small, sample export end is big, the isotope that can be measured simultaneously
Maximum relative mass deviation is 17%-40%, can effectively by mass number be 190 or less (containing Hf and O) and mass number be 190 with
The ion of upper (containing U-Pb) is divided into two sections.
It is preferred that being also connected between the sample export of laser ablation plasma system and the sample inlet of quality sorting device
Tertiary focusing component is connected with the second focusing block between the second sample export and U-Pb Isotope Dating analysis system, first
The first focusing block is connected between sample export and Hf isotope analysis system, the focusing block is gathered to ion
Coke, to be analyzed.
It is also connected with electrostatic analyzer between the first focusing block and Hf isotope analysis system, can effectively make low quality
Several ions carries out Voice segment.
The laser ablation plasma system includes the connected laser ablation device of sequence, plasma device and the
Three focusing blocks.Laser ablation plasma system be zircon sample is degraded, and be transferred in plasma device into
Row ionization.
A second object of the present invention is to provide a kind of absolute microcell for being suitable for hafnium (oxygen) isotope and uranium lead age is former
The method of position analysis, method includes the following steps:
Zircon sample is transferred in plasma and is ionized by after laser ablation, and the sample of ionization enters quality
In sorter, the lightweight component containing Hf and O is isolated under the deflecting action in magnetic field in quality sorting device and containing U-Pb's
Weight mass component, counterweight mass part carry out the analysis of U-Pb Isotope Dating, carry out Hf isotope to lightweight part or oxygen is same
Position element analysis.
The counterweight mass part, which carries out the analysis of U-Pb Isotope Dating, to be analyzed with level four bars mass spectrograph.
Described to lightweight part progress Hf isotope or oxygen isotope analysis carried out with the magnetic-type mass spectrographs that receive more
Analysis.
It is preferred that zircon sample is transferred in plasma and is ionized by after laser ablation, the sample of ionization is through poly-
It is defocused to enter in quality sorting device, the lightweight group containing Hf and O is isolated under the deflecting action in magnetic field in quality sorting device
Divide and the heavy mass component containing U-Pb, counterweight mass part carry out U-Pb Isotope Dating with level four bars mass spectrograph after over-focusing
Analysis receives magnetic-type spectrometer analysis Hf isotope or oxygen isotope with after over-focusing to lightweight part more.
The present invention is to degrade sample, and ionized by carrier gas transfer into plasma with laser, is led to
It crosses the magnetic field in quality sorting device to sort the ion of entrance at high quality number part and low quality number part, which is to have
The small very big design in outlet of entrance, the maximum relative mass deviation for the isotope that can be measured simultaneously is 17%-40%, can be effective
Be 190 or less (lightweight parts) by mass number and ion that mass number is 190 or more (weight mass fraction) is divided into two sections, institute
The focusing block stated further is focused to two sections of ions after separating, and is carried out corresponding detector and is analyzed, described
Level four bars mass spectrograph be that the ion of counterweight mass component is analyzed, obtain high-precision U-Pb age, more reception magnetic
Formula mass spectrograph is analyzed the ion of lightweight component, and high-precision Hf isotope or oxygen isotope are obtained.
After plasma enters the magnetic field of sorter, initial velocity having the same, therefore in the case where magnetic field is fixed,
Ion deflection radius in magnetic field only has relationship with its quality, and the element that can be analyzed as needed carries out the magnetic force size in magnetic field
It is corresponding to adjust.It is 190 or less (lightweight parts) and mass number is 190 or more as plasma can be divided into mass number
Two sections of ion (weight mass fraction).Described adjusts the magnetic force size in magnetic field accordingly, if it is electromagnet,
Magnetic field size can be changed by adjusting the voltage of load.
Beneficial effects of the present invention are as follows:
Two components required for the present invention can effectively split into the micro-zone in situ information of laser ablation, make full use of
Resulting substance is degraded in original position, and can obtain the multipacket message of same position according to actual needs.And because being able to achieve while measuring,
Signal is not lost, so high-precision result can also be obtained.Hf isotope or O isotope etc. to obtain absolute in-situ micro area show
Track information and U-Pb age provide important technical method.
Detailed description of the invention:
Fig. 1 is the knot of the device of the absolute micro-zone in situ analysis for being suitable for hafnium (O) isotope and uranium lead age of the invention
Structure schematic diagram；Wherein 1, laser ablation plasma system；2, quality sorting device；3, level four bars mass spectrograph；4, electrostatic analyzer；
5, receive magnetic-type mass spectrograph more；6, the sample export of laser ablation plasma system；7, the sample inlet of quality sorting device；8,
First sample export；9, the second sample export；10, sorting chamber；11, the first focusing block；12, the second focusing block；13, laser
Degrade device；14, plasma device；15, tertiary focusing component；16, magnet.
Specific embodiment:
The following examples are further illustrations of the invention, rather than limiting the invention.
Embodiment 1:
As shown in Figure 1, the dress of the absolute micro-zone in situ analysis for being suitable for hafnium (O) isotope and uranium lead age of the present embodiment
Set, including laser ablation plasma system 1, quality sorting device 2, level four bars mass spectrograph 3, electrostatic analyzer 4 and receive magnetic
Formula mass spectrograph 5；
The sample export 6 of the laser ablation plasma system is connected with the sample inlet 7 of quality sorting device, quality
Sorter tail end is equipped with 2 sample exports, i.e. the first sample export 8 and the second sample export 9, and the first sample export 8, first is poly-
Burnt component 11, electrostatic analyzer 4 are sequentially connected more with the magnetic-type mass spectrographs 5 that receive；Second sample export 9, the second focusing block 12,
The sample inlet sequence of level four bars mass spectrograph 3 is connected；
The quality sorting device includes the magnet 16 on the outside of sorting chamber 10 and sorting chamber, and magnet in sorting chamber for producing
Raw magnetic field space, 10 front end of sorting chamber are equipped with sample inlet 7, and tail end is equipped with 2 sample exports, i.e. the first sample export 8 and the
Two sample exports 9；The magnetic field space is that the plasma sample for entering sample inlet divides under the deflecting action in magnetic field
The lightweight component containing Hf and O and the heavy mass component containing U-Pb are separated out, weight mass component enters the second sample export 9, gently
Mass component enters the first sample port 8.
The laser ablation plasma system includes the connected laser ablation device 13 of sequence, plasma device 14
With tertiary focusing component 15, laser ablation plasma system is to degrade zircon sample, and be transferred to plasma dress
It is ionized in setting, then is sent by ion transmission channel to the sample inlet of quality sorting device after the aggregation of tertiary focusing component.
The sorting chamber is horn-like in sample inlet end is small, sample export end is big, the isotope that can be measured simultaneously
Maximum relative mass deviation is 17%-40%, can be effectively 190 or less (the lightweight components containing Hf) and quality by mass number
Number is that the ion isolation of 190 or more (the heavy mass components containing U-Pb) forms 2 sections.
The present embodiment also provides a kind of side of absolute micro-zone in situ analysis for being suitable for hafnium (oxygen) isotope and uranium lead age
Method, comprising the following steps:
Zircon sample is transferred in plasma device and is ionized by after the laser ablation of laser ablation device, from
The sample of sonization enters in quality sorting device after the focusing of tertiary focusing component, in quality sorting device under the deflecting action in magnetic field
The lightweight component containing Hf and O and the heavy mass component containing U-Pb are isolated, lightweight component enters the first sample export 8,
Weight mass component enters the second sample port 9, and lightweight component is analyzed after the focusing of the first focusing block 11 through electrostatic analyzer 4
After enter back into the magnetic-type mass spectrographs 5 that receive more and carry out Hf isotopes or oxygen isotope analysis, and weight mass component is focused by second
Component 12 enters after assembling carries out the analysis of U-Pb Isotope Dating in level four bars mass spectrograph.
From the above, it can be seen that the present invention can effectively by the micro-zone in situ information of laser ablation split into required for two
Component makes full use of original position to degrade resulting substance, and can obtain the multipacket message of same position according to actual needs.And because of energy
It realizes while measuring, signal is not lost, so high-precision result can also be obtained.For the Hf isotope for obtaining absolute in-situ micro area
Or the trace informations such as oxygen isotope and U-Pb age provide important technical method.
Claims (10)
1. the device that one kind is suitable for the absolute micro-zone in situ analysis of hafnium (oxygen) isotope and uranium lead age, which is characterized in that packet
Include laser ablation plasma system, quality sorting device, U-Pb Isotope Dating analysis system and Hf isotope analysis system；
The sample export of laser ablation plasma system is connected with the sample inlet of quality sorting device, and quality sorting device tail end is set
There are 2 sample exports, i.e. the first sample export and the second sample export, the sample of the first sample export and Hf isotope analysis system
Product entrance is connected, and the second sample export is connected with the sample inlet of U-Pb Isotope Dating analysis system；
The quality sorting device includes the magnet on the inside or outside of sorting chamber and sorting cavity wall, and magnet in sorting chamber for producing
Raw magnetic field space, sorting chamber front end are equipped with sample inlet, and tail end is equipped with 2 sample exports, i.e. the first sample export and the second sample
Product outlet；The magnetic field space is to isolate the plasma sample of sample inlet entrance under the deflecting action in magnetic field to contain
There are the lightweight component of Hf and O and the heavy mass component containing U-Pb, lightweight component enters the first sample export, weight mass component
Into the second sample port.
2. the apparatus according to claim 1, which is characterized in that the U-Pb Isotope Dating analysis system is level four bars
Mass spectrograph.
3. the apparatus according to claim 1, which is characterized in that the Hf isotope analysis system is more reception magnetic-type matter
Spectrometer.
4. device according to claim 1,2 or 3, which is characterized in that the sorting chamber small, sample in sample inlet end
Big horn-like in outlet end.
5. the apparatus according to claim 1, which is characterized in that in the sample export and matter of laser ablation plasma system
It measures and is also connected with tertiary focusing component, the second sample export and U-Pb Isotope Dating analysis system between the sample inlet of sorter
Between be connected with the second focusing block, be connected with the first focusing block between the first sample export and Hf isotope analysis system.
6. device according to claim 5, which is characterized in that between the first focusing block and more reception magnetic-type mass spectrographs
Also it is connected with electrostatic analyzer.
7. the apparatus according to claim 1, which is characterized in that the laser ablation plasma system includes sequence phase
Laser ablation device, plasma device and tertiary focusing component even.
8. the method that one kind is suitable for the absolute micro-zone in situ analysis of hafnium (oxygen) isotope and uranium lead age, which is characterized in that should
Method the following steps are included:
Zircon sample is transferred in plasma and is ionized by after laser ablation, and the sample of ionization enters quality sorting
In device, the lightweight component containing Hf and O and the heavy containing U-Pb are isolated under the deflecting action in magnetic field in quality sorting device
Component is measured, counterweight mass part carries out the analysis of U-Pb Isotope Dating, carries out Hf isotope or O isotope point to lightweight part
Analysis.
9. according to the method described in claim 8, it is characterized in that, the counterweight mass part carries out U-Pb Isotope Dating
Analysis is analyzed with level four bars mass spectrograph, and described is to use to lightweight part progress Hf isotope or O isotope analysis
The magnetic-type mass spectrographs that receive are analyzed more.
10. according to the method described in claim 8, it is characterized in that, zircon sample is transferred to plasma by after laser ablation
In ionized, after the sample line focus of ionization enter quality sorting device in, in quality sorting device magnetic field deflection make
The lightweight component containing Hf and O and the heavy mass component containing U-Pb are isolated under, counterweight mass part is used after over-focusing
Level four bars mass spectrograph carries out the analysis of U-Pb Isotope Dating, receives magnetic-type mass spectrograph point with after over-focusing to lightweight part more
Analyse Hf isotope or oxygen isotope.
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| CN116840334A (en) * | 2023-07-03 | 2023-10-03 | 中国地质科学院地质研究所 | In-situ joint measurement analysis method for silicon oxygen isotope micro-region of ion probe |
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| 江宗耀: "电子电离源的研制及其在新型杂化串联质谱仪中的应用", 《中国优秀硕士学位论文全文数据库》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116840334A (en) * | 2023-07-03 | 2023-10-03 | 中国地质科学院地质研究所 | In-situ joint measurement analysis method for silicon oxygen isotope micro-region of ion probe |
| CN116840334B (en) * | 2023-07-03 | 2023-12-22 | 中国地质科学院地质研究所 | In-situ joint measurement analysis method for silicon oxygen isotope micro-region of ion probe |
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