CN108459070A - A kind of diluent free measures apatite (U-Th)/He and determines year method - Google Patents
A kind of diluent free measures apatite (U-Th)/He and determines year method Download PDFInfo
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- CN108459070A CN108459070A CN201810139733.1A CN201810139733A CN108459070A CN 108459070 A CN108459070 A CN 108459070A CN 201810139733 A CN201810139733 A CN 201810139733A CN 108459070 A CN108459070 A CN 108459070A
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Abstract
A kind of diluent free of present invention offer measures apatite (U Th)/He and determines year method, and the method is first measured and calculated into size, volume and quality to test apatite particle, then tested wherein on gas mass spectrum4The content of He, solution is made with nitric acid sample dissolution again, configure the standard solution of the uranium and thorium of various concentration, test and drawing curve on inductive coupling plasma mass spectrometry, U in solution is calculated in conjunction with working curve, the concentration of Th finally uses the content of the concentration of uranium thorium and the Mass Calculation uranium thorium of particle, and4The content of He calculates the age for obtaining mineral to be measured together, with it is previous determine year method compared with, the present invention solves the restricted problem of diluent；The method calculates through the invention, obtains the age of mineral to be measured, to the research applied to geological process.
Description
Technical field
The invention belongs to mineral isotope chronology technical fields, and in particular to a kind of diluent free measurement apatite (U-
Th)/He determines year method.
Background technology
Apatite (U-Th)/He chronologys are low temperature (heat) Age Datings that fast development is got up in recent decades, by
In its extremely low closure temperature (~75 DEG C) and He spread can simulation, extend middle low temperature thermochronometry significantly (such as40Ar
/39Ar, FT etc.) at a temperature of limit, so that it is had in the great palegeology Study on Problems such as neotectonics, Landform Evolution, the change of circumstances
Have broad application prospects.It is same that the measurement at apatite (U-Th)/He ages will test daughter on inert gas mass spectrograph respectively
Position element (4He test) and on Inductively coupled plasma mass spectrometry parent isotope (238U,232Th).Currently, in apatite (U-
Th in)/He Isotope Datings field, technical staff both domestic and external mainly applies the same position of isotope-dilution analysis test uranium and thorium
Element, this method is in spite of higher precision, but since diluent is mainly derived from foreign countries, it is radioisotopic obtain by
To the limitation of various conditions.The country had established more families (U-Th)/He and has determined year laboratory in succession in recent years, but the valence of diluent
Lattice are expensive and to obtain channel limited, face this problem, are badly in need of a kind of (U-Th)/He age dating methods of diluent free.
Therefore, the above problem present in technology at present, greatly constrains apatite (U-Th)/He dating techniques in geological research
Using.
Invention content
To solve the above-mentioned problems, a kind of diluent free measurement apatite (U-Th)/He of present invention offer determines year method,
The method is first measured and is calculated into size, volume and quality to test apatite particle, is then surveyed on gas mass spectrum
Examination is wherein4The content of He, then solution is made with nitric acid sample dissolution, the uranium of various concentration and the standard solution of thorium are configured, in electricity
Feel test and drawing curve on Coupled Plasma-Mass Spectroscopy, calculates U in solution in conjunction with working curve, the concentration of Th is finally used
The content of the concentration of uranium thorium and the Mass Calculation uranium thorium of particle, and4The content of He calculates the age for obtaining mineral to be measured together；
Further, it the described method comprises the following steps：
Step 1：Selected sample measures size：Selected under 160 times of Stereo microscopes complete crystal form, it is pure, without inclusion enclave
And the apatite particle in crack, take pictures and survey the three-dimensional dimension information of particle；It is calculated according to the shape, size and density of apatite
Its quality；
Step 2：Daughter4The test of He：The platinum cylinder of 1 mm dia of particle in step 1,1 mm length is wrapped up
Sealing, is loaded into Alphachron MK II inert gas mass spectrographs in test sample4He contents；
Step 3：The dissolving of mineral grain：It will be tested in step 24The particle and platinum cylinder of He contents are transferred to molten together
In sample bottle, 25 microlitres of nitric acid sample dissolutions are added, 325 microlitres of Milli-Q pure water are added later；
Step 4：Configure the U of various concentration, Th standard solution；
Step 5：Inductively coupled plasma mass spectrometry is done into mass calibration, best letter is obtained with tuning solution tuning mass spectrograph
Number, the U of various concentration is tested, Th solution makes working curve；
Step 6：Solution survey in step 3 is introduced into Inductively coupled plasma mass spectrometry and is tested, is obtained using in step 5
Working curve calculate apatite particle in uranium and thorium concentration；
Step 7：Utilize the thorium absolute content of the absolute uranium sum of the Mass Calculation of the apatite particle obtained in step 1；
Step 8：The age of apatite particle is calculated using radioactive decay formula；
Further, the radioactive decay formula applied in step 8 is：
Wherein4He,238U,235U,232Th, to correspond to isotopic content, λ in mineral now238, λ235, λ232Respectively238U
,235U,232The decay coefficient of Th, t are accumulated time, correspond to (U-Th)/He ages of mineral；
Further, the concentration of nitric acid described in step 3 is 7mol/L, and the volume of solution is 350 microlitres after dissolving；
Further, 25 microlitres of pipettor described in step 3 is corrected with Milli-Q pure water, the side of correction
Method is to measure the quality of 20 Milli-Q pure water, is averaged later；
Further, the concentration of standard solution described in step 4 is respectively 0ppb, 0.1ppb, 1ppb, 3ppb, 5ppb,
10ppb, 20ppb, 30ppb and 50ppb；
Further, it is 1ppb solution concentration to be tuned described in step 5, and the standard of tuning is238U,232The signal of Th is higher than
60000cps/ppb, oxide yield (156CeO/140Ce) less than 3%, double charge yield (137Ba++/137Ba) it is less than 2%；
Beneficial effects of the present invention are as follows：
1)：With it is previous determine year method compared with, the present invention solves the restricted problem of diluent；
2)：The method calculates through the invention, obtains the age of mineral to be measured, to grinding applied to geological process
Study carefully；
3)：The method of the invention have validity and operability, without diluent can measure apatite (U-Th)/
The He ages；
4)：Method of the present invention greatly reduces cost than diluent method, still can be with although accuracy is relatively low
Obtain the consistent age result of same diluent method.
Description of the drawings
Fig. 1 is photo and dimension measurement result under the microscope of particle of the present invention；
Fig. 2 is that apatite particle of the present invention is transferred to encapsulation schematic diagram in platinum pipe；
Fig. 3 is the flow chart that diluent free of the present invention measures apatite (U-Th)/He aging methods；
Fig. 4 is to measure to obtain the working curve of various concentration standard solution in the specific embodiment of the invention.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.On the contrary, the present invention cover it is any be defined by the claims the present invention spirit and scope on do
Replacement, modification, equivalent method and scheme.Further, in order to make the public have a better understanding the present invention, below to this
It is detailed to describe some specific detail sections in the datail description of invention.It is thin without these for a person skilled in the art
The description of section part can also understand the present invention completely.
The invention will be further described in the following with reference to the drawings and specific embodiments, but not as a limitation of the invention.
Below most preferred embodiment is enumerated for the present invention：
A kind of diluent free of present invention offer measures apatite (U-Th)/He and determines year method, and method is that first will be singled out
Apatite particle take pictures measure size calculating volume (as shown in Figure 1) and granular mass, Zhi Hou under the microscope
It is tested on Alphachron MK II gas mass spectrums4Then solution is made with nitric acid sample dissolution in the content of He；Configuration is different dense
The uranium of degree and the standard solution of thorium the testing and drawing working curve on inductive coupling plasma mass spectrometry (ICP-MS) test to be measured
The solution of grain calculates U in solution, the concentration of Th in conjunction with working curve；Finally use the Mass Calculation uranium of the concentration and particle of uranium thorium
The content of thorium, and4The content of He calculates the age for obtaining mineral to be measured together, to the research applied to geological process.
The method of the invention specifically includes following steps：
Step 1. selected sample measures size：Selected under 160 times of Stereo microscopes complete crystal form, it is pure, without inclusion enclave
And the apatite particle in crack, take pictures and survey the three-dimensional dimension information of particle；According to the shape and size and densitometer of apatite
Calculate its quality；
Step 2. daughter4The test of He：The platinum cylinder of 1 mm dia of particle in step 1,1 mm length is wrapped up
Sealing, is loaded into Alphachron MK II inert gas mass spectrographs in test sample4He contents；
The dissolving of step 3. mineral grain：It will be tested in step 24The particle and platinum cylinder of He contents are transferred to molten together
In sample bottle, nitric acid sample dissolution is added；
Step 4. configures the U of various concentration, Th standard solution；
Inductively coupled plasma mass spectrometry is done mass calibration by step 5., and best letter is obtained with tuning solution tuning mass spectrograph
Number, the U of various concentration is tested, Th solution makes working curve；
Solution survey in step 3 is introduced into Inductively coupled plasma mass spectrometry and tests by step 6., is obtained using in step 5
Working curve calculate apatite particle in uranium and thorium concentration；
Step 7. using the absolute uranium sum of Mass Calculation of the apatite particle obtained in step 1 thorium absolute content；
Step 8. calculates the age of apatite particle using radioactive decay formula, and calculation formula is as follows：
Wherein4He,238U,235U,232Th, to correspond to isotopic content, λ in mineral now238, λ235, λ232Respectively238U
,235U,232The decay coefficient of Th, t are accumulated time, correspond to (U-Th)/He ages of mineral.
With it is previous determine year method compared with, the present invention solves the limitation of diluent；Concentration of nitric acid in step 3 is
7mol/L, the volume of solution is 350 microlitres after dissolving.Concentration of standard solution in step 4 is respectively 0ppb, 0.1ppb, 1ppb,
3ppb, 5ppb, 10ppb, 20ppb, 30ppb, 50ppb.Tuning solution concentration 1ppb in step 5, the standard of tuning are238U
,232The signal of Th be higher than 60000cps/ppb, oxide yield (156CeO/140Ce) less than 3%, double charge yield (137Ba++
/137Ba) it is less than 2%.
This example carries out diluent free measurement apatite (U-Th)/He according to preparation process shown in Fig. 3 and determines year method,
Specific steps include：
(1) preparation of sample：The apatite particle sub-elected through conventional beneficiation flowsheet, under the Stereo microscope of high power
Complete crystal form, pure, without inclusion enclave and crack apatite particle are selected, the rulers such as the length and width of particle are taken pictures and measure
Very little information, as shown in Figure 1；
(2) daughter4The measurement of He contents：By 1 mm dia of the particle in step 1, the platinum cylinder packet of 1 mm length
Wrap up in sealing, as shown in a in Fig. 2, load closely in numbered sample disc as shown in b in Fig. 2, it is lazy in Alphachron MK II
On property mass spectrometer in test sample4He contents；
(3) second step：The dissolving of mineral grain：It will be tested in step 24The particle and platinum cylinder of He contents shift together
Into sample flask, nitric acid sample dissolution is added；
(4) U of various concentration, Th standard solution are configured；
(5) Inductively coupled plasma mass spectrometry is done into mass calibration, optimum signal is obtained with tuning solution tuning mass spectrograph,
The U of various concentration is tested, Th solution makes working curve；
(6) solution survey in step 3 is introduced into Inductively coupled plasma mass spectrometry and is tested, utilize what is obtained in step 5
Working curve, as shown in figure 4, calculating the concentration of uranium and thorium in apatite particle；
(7) the thorium absolute content of the absolute uranium sum of the Mass Calculation of the apatite particle obtained in step 1 is utilized；
It is analyzed by examples detailed above, fully shows the method that diluent free measures (U-Th)/He ages and may be implemented, be
(U-Th)/He age datings of geology mineral and the recovery of low temperature thermal history provide a kind of completely new, reliable means.
Embodiment described above, only one kind of the present invention more preferably specific implementation mode, those skilled in the art
The usual variations and alternatives that member carries out within the scope of technical solution of the present invention should be all included within the scope of the present invention.
Claims (7)
1. a kind of diluent free, which measures apatite (U-Th)/He, determines year method, which is characterized in that the method is first to test phosphorus ash
Stone particle is measured and is calculated into size, volume and quality, is then tested wherein on gas mass spectrum4The content of He, then use
Solution is made in nitric acid sample dissolution, configures the uranium of various concentration and the standard solution of thorium, is surveyed on inductive coupling plasma mass spectrometry
Simultaneously drawing curve is tried, calculates U in solution in conjunction with working curve, the concentration of Th finally uses the matter of the concentration and particle of uranium thorium
Amount calculates the content of uranium thorium, and4The content of He calculates the age for obtaining mineral to be measured together.
2. according to the method described in claim 1, other are characterized in that, the described method comprises the following steps：
Step 1：Selected sample measures size：Selected under 160 times of Stereo microscopes complete crystal form, it is pure, without inclusion enclave and split
The three-dimensional dimension information of particle is taken pictures and surveyed to the apatite particle of gap；Its matter is calculated according to the shape, size and density of apatite
Amount；
Step 2：Daughter4The test of He：The platinum cylinder of 1 mm dia of particle in step 1,1 mm length is wrapped up into sealing,
It is loaded into Alphachron MK II inert gas mass spectrographs in test sample4He contents；
Step 3：The dissolving of mineral grain：It will be tested in step 24The particle and platinum cylinder of He contents are transferred to sample flask together
In, 25 microlitres of nitric acid sample dissolutions are added, 325 microlitres of Milli-Q pure water are added later；
Step 4：Configure the U of various concentration, Th standard solution；
Step 5：Inductively coupled plasma mass spectrometry is done into mass calibration, optimum signal is obtained with tuning solution tuning mass spectrograph,
The U of various concentration is tested, Th solution makes working curve；
Step 6：Solution survey in step 3 is introduced into Inductively coupled plasma mass spectrometry and is tested, the work obtained in step 5 is utilized
The concentration of uranium and thorium in composition line computation apatite particle；
Step 7：Utilize the thorium absolute content of the absolute uranium sum of the Mass Calculation of the apatite particle obtained in step 1；
Step 8：The age of apatite particle is calculated using radioactive decay formula.
3. according to the method described in claim 2, it is characterized in that, the radioactive decay formula applied in step 8 isWherein4He,238U,235U,232Th, for mine now
Isotopic content, λ are corresponded in object238, λ235, λ232Respectively238U,235U,232The decay coefficient of Th, t are accumulated time, are corresponded to
(U-Th)/He ages of mineral.
4. according to the method described in claim 2, it is characterized in that, the concentration of nitric acid described in step 3 is 7mol/L, after dissolving
The volume of solution is 350 microlitres.
5. according to the method described in claim 2, it is characterized in that, 25 microlitres of pipettor described in step 3 is used
Milli-Q pure water is corrected, and the method for correction is to measure the quality of 20 Milli-Q pure water, is averaged later.
6. according to the method described in claim 2, it is characterized in that, the concentration of standard solution described in step 4 is respectively 0ppb,
0.1ppb, 1ppb, 3ppb, 5ppb, 10ppb, 20ppb, 30ppb and 50ppb.
7. according to the method described in claim 2, it is characterized in that, described in step 5 tune solution concentration be 1ppb, tuning
Standard is238U,232The signal of Th be higher than 60000cps/ppb, oxide yield (156CeO/140Ce) it is less than 3%, double charge yield
(137Ba++/137Ba) it is less than 2%.
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| CN113945175A (en) * | 2021-10-14 | 2022-01-18 | 中国地质科学院地质力学研究所 | Rock three-dimensional data acquisition method and device |
| CN114427985A (en) * | 2020-09-30 | 2022-05-03 | 中国石油化工股份有限公司 | Method for selecting and loading apatite mineral particles |
| CN117388043A (en) * | 2023-11-02 | 2024-01-12 | 中国地质科学院地质研究所 | Method for dissolving single-particle sphene and (uranium-thorium)/helium annual method of single-particle sphene |
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| CN113945175A (en) * | 2021-10-14 | 2022-01-18 | 中国地质科学院地质力学研究所 | Rock three-dimensional data acquisition method and device |
| CN117388043A (en) * | 2023-11-02 | 2024-01-12 | 中国地质科学院地质研究所 | Method for dissolving single-particle sphene and (uranium-thorium)/helium annual method of single-particle sphene |
| CN117388043B (en) * | 2023-11-02 | 2024-03-29 | 中国地质科学院地质研究所 | Method for dissolving single-particle sphene and (uranium-thorium)/helium annual method of single-particle sphene |
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