CN115963164A - Preparation method and application of massive olivine iron isotope composition standard sample - Google Patents
Preparation method and application of massive olivine iron isotope composition standard sample Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a massive olivine iron isotope composition standard sample, wherein the preparation method of the olivine iron isotope composition standard sample comprises the following preparation steps: crushing olivine to obtain coarse olivine; grinding the olivine coarse body, and drying to obtain olivine powder; tabletting the olivine powder to obtain an olivine blank; and sintering the blank in a protective gas to obtain a standard sample consisting of the blocky olivine iron isotope. The invention provides a micro-area iron isotope composition standard sample which is prepared under the condition of not introducing a binder, can be used for olivine micro-area in-situ iron isotope analysis, has uniform components, is easy to store and is suitable for long-term use.
Description
Technical Field
The invention relates to the technical field of micro-area in-situ metal stable isotope analysis and test, in particular to a preparation method and application of a standard sample consisting of blocky olivine iron isotopes.
Background
Olivine is one of the main minerals that make up the earth's mantle, and is also the earliest crystalline product formed by magnesium-rich magma when it reaches the surface. Olivine is therefore commonly used as a geochemical and petro-chemical tracer of the physicochemical processes that take place during the formation or ascent of the magma. The structural information and the chemical components of the olivine can be used for deducing the components of the original rock pulp, and the component bands of the olivine also record important information such as the evolution process of the rock pulp in different periods and the change of the environment in the ascending eruption process of the rock pulp. Compositional banding in olivine crystals is evidence of changes in the chemical or physical conditions of the magma system, which exist in the evolution process including melt composition, oxygen fugacity, pressure, volatile content. Therefore, the research on olivine has important significance on the inference of original magma, magma evolution and time scale process, and the element and isotope composition characteristics play an important role in the aspects of inverting the material composition, properties, long-term evolution process and the like of the mantle of the rock circle. With the progress of analytical techniques and the development of emerging research approaches, accurate determination of olivine iron isotopes becomes possible. The olivine iron isotope geochemical characteristics have important significance for researching the iron isotope fractionation behaviors in the magma process (such as partial melting, mantle regeneration, magma differentiation and the like), understanding the magma action and mantle action process of the earth, tracing the material source and the mineralization process of the magma type ore deposit and the like.
The laser ablation plasma mass spectrum is one of important means for in-situ isotope analysis of mineral microcells, has the advantages of high spatial resolution, small sample consumption, low pollution risk, rapidness, economy and the like, and can obtain isotope information on the scale of the mineral microcells. However, since the isotope analysis by laser ablation plasma mass spectrometry is a relative method, i.e. analysis is performed by comparing the ratio of isotopes in the sample to be detected and the standard sample, the lack of the olivine solid standard sample with uniform iron isotope composition and matched matrix directly restricts the application of laser ablation plasma mass spectrometry to the accurate analysis of the olivine micro-zone in-situ iron isotope.
Generally, a standard sample for laser ablation plasma mass spectrometry isotope analysis testing is prepared, natural minerals are selected from the nature and crushed into small samples, the small samples are embedded in resin, and a finished product is prepared after grinding and polishing and uniformity inspection and analysis fixed value. However, olivine in nature has complex and various components, poor uniformity and consistency, small sample amount meeting requirements, and cannot be popularized and used for a long time.
Traditionally, the method for preparing a solid standard sample with relatively uniform components for micro-area analysis is a powder tabletting method, which is to directly compress a powder sample into tablets, is simple, convenient, efficient and rapid, but the sample is easy to loosen and cannot be stored for a long time, and in the laser ablation process, the beam spot, energy and frequency of laser have large influence on the sample, so that the iron isotope analysis error is large, and the analysis requirements of high precision and high accuracy cannot be met. In order to improve the defects of loose and low compactness of the pressed sample, a binder is usually introduced into the system to improve the strength of the pressed tablet. However, the binder used in the method is mostly organic and cannot be removed, which changes the matrix component of olivine and is easy to introduce new impurities; furthermore, the pressed sheet prepared by the method still has the defects of easy moisture absorption, incapability of polishing and washing, and difficult long-term storage and use.
The melting method is also a commonly used method for preparing a solid standard sample, but is mainly used for element content analysis, and because the molten standard substance is difficult to ensure that the internal and external temperatures are completely consistent in the cooling and solidifying processes, the solidifying time of each area is different, so that the iron isotope is significantly fractionated, and a sample with uniform iron isotope is difficult to obtain. Moreover, during the melting and cooling process, the oxidation of ferrous iron in the olivine is easy to occur, so that the phase of the olivine is changed fundamentally.
Therefore, the development of a standard sample suitable for micro-area analysis, which is homogeneous in composition, easy to store and suitable for long-term use, will be a key research goal in the art.
Disclosure of Invention
The invention mainly aims to provide a preparation method and application of a massive olivine iron isotope composition standard sample, and aims to prepare a standard sample which is used for olivine micro-area in-situ iron isotope composition analysis, has uniform components, is easy to store and is suitable for long-term use under the condition of not introducing a binder.
In order to achieve the purpose, the invention provides a preparation method of a massive olivine iron isotope composition standard sample, which comprises the following preparation steps:
s1: coarse crushing olivine to obtain coarse olivine;
s2: grinding the olivine coarse body, and drying to obtain olivine powder;
s3: tabletting the olivine powder to obtain an olivine blank;
s4: and sintering the blank in a protective gas to obtain a standard sample consisting of the blocky olivine iron isotope.
Optionally, the step S2 includes adding absolute ethanol, isopropanol or n-butanol to the olivine coarse body, grinding, and drying to obtain olivine powder.
Optionally, in step S2, the grinding time is 9 to 11h.
Optionally, in step S2, the drying temperature is 70 to 110 ℃.
Optionally, in step S3, the pressure during tabletting is 4 to 6MPa.
Optionally, in the step S4, the sintering temperature is 1000 to 1300 ℃; and/or the heating speed is 1-3 ℃/min.
Optionally, the sintering time in step S4 is 4 to 6 hours.
Optionally, in step S4, the shielding gas is argon with a volume fraction of not less than 99.999%; and/or the protective gas is nitrogen with the volume fraction of not less than 99.999%.
In addition, the invention also provides application of the massive olivine iron isotope composition standard sample, which is prepared by the preparation method of the massive olivine iron isotope composition standard sample and is used for quantitative analysis of the olivine iron isotope by laser ablation plasma mass spectrometry.
In the technical scheme provided by the invention, the olivine powder is directly sintered by adopting an atmosphere tube furnace without introducing a binder in the tabletting process, the prepared iron isotope standard sample is an olivine block, is compact and difficult to damage, has the hardness higher than 370HV, has the hardness similar to that of glass, compact internal structure, high strength and uniform iron isotope composition, and delta is large in size, difficult to damage and stable in quality 56 The 2-time standard deviation (2 SD) of Fe is less than 0.1 per mill, the requirement of laser ablation plasma mass spectrum olivine iron isotope quantitative analysis is met, and compared with a sample prepared by a powder pressing cake method, the sample can be washed and polished by water, is not easy to absorb moisture and is convenient to store.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other relevant drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of an embodiment of a method for preparing a standard sample of the isotopic composition of massive olivine iron according to the present invention;
fig. 2 is X-ray diffraction patterns of the iron isotope composition standard samples of the blocky olivine prepared in examples 1 to 5 of the present invention and the samples of the blocky olivine prepared in comparative examples 1 to 3;
FIG. 3 is a SEM image of a standard sample of the isotopic composition of massive olivine iron prepared in example 3 of the present invention;
fig. 4 is a result of micro-domain in situ iron isotope composition analysis of the bulk olivine iron isotope composition standard samples prepared in examples 1 to 5 of the present invention and the bulk olivine sample prepared in comparative example 1.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between the various embodiments may be combined with each other, but must be based on the realization of the capability of a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Generally, a standard sample for laser ablation plasma mass spectrometry isotope analysis testing is prepared, natural minerals are selected from the nature and crushed into small samples, the small samples are embedded in resin, and a finished product is prepared after grinding and polishing and uniformity inspection and analysis fixed value. However, in nature, olivine has complex and various components, poor uniformity and consistency, and small sample size meeting requirements, so that the olivine cannot be popularized and used for a long time.
Traditionally, the method for preparing a solid standard sample with relatively uniform components for micro-area analysis is a powder tabletting method, which is to directly compress a powder sample into tablets, is simple, convenient, efficient and rapid, but the sample is easy to loosen and cannot be stored for a long time, and in the laser ablation process, the beam spot, energy and frequency of laser have large influence on the sample, so that the iron isotope analysis error is large, and the analysis requirements of high precision and high accuracy cannot be met. In order to improve the defects of loose and low compactness of the pressed sample, a binder is usually introduced into the system to improve the strength of the pressed tablet. However, the binder used in the method is mostly organic and cannot be removed, which changes the matrix component of olivine and is easy to introduce new impurities; furthermore, the pressed sheet prepared by the method still has the defects of easy moisture absorption, incapability of polishing and washing, and difficult long-term storage and use.
The melting method is also a commonly used method for preparing a solid standard sample, but is mainly used for element content analysis, and because the molten standard substance is difficult to ensure that the internal and external temperatures are completely consistent in the cooling and solidifying process, the solidifying time of each area is different, so that the iron isotope is significantly fractionated, and a sample with uniform iron isotope is difficult to obtain. Moreover, during the melting and cooling process, the oxidation of ferrous iron in the olivine is easy to occur, so that the phase of the olivine is changed fundamentally.
In view of the above, the invention provides a method for preparing a massive olivine iron isotope composition standard sample, the massive olivine iron isotope composition standard sample prepared by the method has uniform distribution of iron isotope composition, and the sample is easy to store and suitable for long-term use; with reference to the flow chart of fig. 1, the method for preparing a massive olivine iron isotope composition standard sample includes the following steps:
step S1, coarse crushing the olivine to obtain the coarse olivine.
Before the step S1, the olivine needs to be selected, and when the olivine is selected, the olivine with uniform texture and uniform color distribution is preferably selected as a sample, the content of impurity minerals of the olivine with uniform texture and uniform color distribution is low or zero, and the sample is made of the olivine, so that the interference on the test result is small, and the test result is more reliable.
When step S1 is performed, specifically, the following steps may be performed: selecting olivine with uniform texture and color distribution, crushing the olivine into blocks of olivine blocks, selecting high-purity olivine blocks, and coarsely crushing the olivine blocks to 200 meshes to obtain coarse samples of olivine.
And S2, grinding the olivine coarse body, and drying to obtain olivine powder.
In this step, the grinding mode is not limited, and this embodiment adopts wet ball milling to obtain olivine powder, which is more efficient, the ground powder has more uniform texture and takes less time, but slurry with uniform composition can be obtained, and the particles of the slurry are mainly round particles rather than flaky particles, which is beneficial for rapid flow of the slurry, so as to obtain uniform-texture olivine powder. In the process of wet ball milling, the added grinding aid, such as water or an organic solvent, can facilitate the grinding of the olivine coarse sample and prevent the grinding materials from adhering to the grinding balls, thereby improving the grinding efficiency.
When step S2 is performed, the following steps may be performed: putting the olivine coarse bodies, the small ball milling beads and the large ball milling beads into a ball milling tank, adding an organic solvent until the olivine coarse bodies, the small ball milling beads and the large ball milling beads are submerged, grinding for 9-11 h, drying at the temperature of 70-110 ℃, and obtaining more uniform olivine powder under the conditions.
It should be noted that, in step S2, the organic solvent is not limited, and may be any one of absolute ethyl alcohol, isopropyl alcohol, or n-butyl alcohol, and the purpose of adding the organic solvent is to improve the dispersibility of the coarse olivine sample, avoid the coarse olivine sample from being coagulated into blocks during grinding, accelerate the grinding effect, and meanwhile, the organic solvent is required to have strong volatility, so that the ball-milled powder is easier to dry.
In some embodiments, the diameter of the large ball milling beads is 4 to 5mm, the diameter of the small ball milling beads is 1.5 to 2mm, and the material of the ball milling beads is not limited. As a preferred embodiment of this embodiment, the material of the ball-milling beads is an agate material, and the ball-milling beads made of the agate material are harder, so as to avoid introducing impurities during the milling process. The diameter of the small agate sphere is 2mm, the diameter of the large agate sphere is 5mm, and the selection is more beneficial to grinding the olivine coarse body.
In some embodiments, the mass ratio of the natural olivine coarse body to the large ball grinding beads to the small ball grinding beads is (0.5-1) to (1.5-2), i.e. 1.5-3 kg of large ball grinding beads and 1.5-3 kg of small ball grinding beads are added to 1kg of the coarse sample of the olivine. As a preferred example of this embodiment, 2kg of small agate spheres and 2kg of large agate spheres need to be added to each 1kg of olivine coarse sample, and it should be noted that, in this embodiment, the mass ratio of the single large ball milling beads to the single small ball milling beads is 1:1. with the proportion, the obtained olivine powder is more uniform.
In some embodiments, the particle size of the olivine powder is mainly 0.5 to 4 μm, and the above particle size range value is favorable for fully and uniformly mixing the olivine powder, so that the iron isotope composition distribution of the finally obtained standard sample is more uniform.
S3: and tabletting the olivine powder to obtain an olivine blank.
In step S3, during the process of tabletting the olivine powder by using the powder direct tabletting process, no binder is added, the pressure selected during tabletting is 4 to 6MPa, preferably 4MPa, and the blank obtained under the conditions has uniform texture and smooth surface.
And S4, sintering the blank in protective gas to obtain a standard sample consisting of the blocky olivine iron isotope.
In step S4, in order to avoid the oxidation reaction between the sample and oxygen during sintering, it is necessary to perform sintering in the presence of a shielding gas, which is usually argon or nitrogen, and preferably, the volume fraction of argon or nitrogen is not less than 99.999%, so as to prevent the oxidation of ferrous iron in olivine into ferric iron during sintering.
In some embodiments, an atmosphere tube furnace sintering method is adopted, the temperature rising speed is high, the olivine blank is not sintered into a traditional molten glass state, the uniformity and the stability of the iron isotope standard sample are improved to the maximum extent under the condition of keeping the property of the sample, the storage is easy, the analysis error of the olivine iron isotope caused by the looseness of the iron isotope standard sample in the laser ablation process is reduced, and the accuracy of iron isotope analysis is ensured.
The olivine powder is directly sintered by an atmosphere tube furnace without introducing a binder in the tabletting process, the prepared iron isotope standard sample is an olivine block, is compact and difficult to damage, has the hardness higher than 370HV, has the hardness similar to that of glass, compact internal structure, high strength and difficult to damage, has uniform iron isotope composition, delta 56 The 2-time standard deviation (2 SD) of Fe is less than 0.1 per mill, the requirement of laser ablation plasma mass spectrum olivine iron isotope quantitative analysis is met, and compared with a sample prepared by a powder pressing cake method, the sample can be washed and polished by water, is not easy to absorb moisture and is convenient to store.
When step S4 is performed, the following steps may be specifically performed: and putting the blank into an alumina crucible, putting the alumina crucible into a tube furnace, pumping out air in the furnace, introducing argon, heating to 1000-1300 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 4-6 h, so that the prepared massive olivine iron isotope composition standard sample is compact, difficult to damage and high in hardness under the conditions.
Further, in order to ensure that the homogeneity and the hardness of the massive olivine iron isotope composition standard sample are better, the sintering temperature of the atmosphere tube furnace is 1300 ℃, and the sintering time of the atmosphere tube furnace is 4 hours.
In some embodiments, after placing the green body into the tube furnace, the tube furnace is evacuated for 15min in order to keep the oxygen fugacity in the tube furnace low.
In addition, the invention also provides application of the massive olivine iron isotope composition standard sample, which is prepared by the preparation method of the massive olivine iron isotope composition standard sample and is used for quantitative analysis of the olivine iron isotope by laser ablation plasma mass spectrometry. The application of the iron isotope standard sample has all the beneficial effects of the iron isotope standard sample, and is not repeated herein.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
(1) Coarsely crushing the olivine coarse gravel, selecting high-purity olivine minerals, and crushing into powder of 80 μm to obtain olivine coarse powder;
(2) Putting the olivine coarse body, the small agate sphere and the large agate sphere into an agate ball milling tank according to the weight ratio of 1.5.
(3) Weighing a certain amount of olivine powder, filling into a tablet press, and pressing under 4MPa to obtain an olivine blank;
(4) And (3) filling the pressed blank body in a crucible, heating to 1200 ℃ in a tube furnace in an atmosphere of normal-pressure inert gas at the heating rate of 3 ℃/min, and preserving heat for 4 hours to obtain an iron isotope standard sample.
Example 2
(1) Coarsely crushing the olivine coarse gravel, selecting high-purity olivine mineral, and crushing to powder of 60 μm to obtain olivine coarse powder;
(2) Putting the olivine crude sample, the small agate spheres and the large agate spheres into an agate ball milling tank according to the weight ratio of 1.
(3) Weighing a certain amount of olivine powder, filling the olivine powder into a tablet press, and pressing the olivine powder into tablets under the pressure of 5MPa to obtain olivine blanks;
(4) And (3) filling the pressed blank body in a crucible, heating to 1200 ℃ by a tube furnace in an atmosphere of normal-pressure inert gas at the heating rate of 1 ℃/min, and preserving heat for 5 hours to obtain the iron isotope standard sample.
Example 3
(1) Coarsely crushing the olivine coarse gravel, selecting high-purity olivine mineral, and crushing to 74 μm powder to obtain olivine coarse body;
(2) Putting the olivine rough sample, the small agate spheres and the large agate spheres into an agate ball milling tank according to the weight ratio of 1.5.
(3) Weighing a certain amount of olivine powder, filling the olivine powder into a tablet press, and pressing the olivine powder into tablets under the pressure of 4MPa to obtain olivine blanks;
(4) And (3) filling the pressed blank body in a crucible, heating to 1300 ℃ by a tube furnace in an atmosphere of normal-pressure inert gas at the heating rate of 2 ℃/min, and preserving heat for 4h to obtain the iron isotope standard sample.
The scanning electron microscope results of the surface and internal cross section of the obtained massive olivine iron isotope composition standard sample are shown in fig. 3, and it can be seen from the figure that the inside of the olivine standard sample is in fine round-like grain close packing, which shows that the sintered body is dense, and the particles are not completely melted but are fused and cemented among the particles.
Example 4
(1) Coarsely crushing the olivine coarse gravel, selecting high-purity olivine minerals, and crushing into powder of 80 μm to obtain olivine coarse powder;
(2) Putting the olivine rough sample, the small agate spheres and the large agate spheres into an agate ball milling tank according to the weight ratio of 1.8.
(3) Weighing a certain amount of olivine powder, filling into a tablet press, and pressing under the pressure of 6MPa to obtain an olivine blank;
(4) And (3) filling the pressed blank body in a crucible, heating to 1300 ℃ by a tube furnace in an atmosphere of normal-pressure inert gas at the heating rate of 2 ℃/min, and preserving heat for 6 hours to obtain the iron isotope standard sample.
Example 5
(1) Coarsely crushing the olivine coarse gravel, selecting high-purity olivine minerals, and crushing to 100 μm powder to obtain olivine coarse powder;
(2) Placing the olivine crude sample, the small agate spheres and the large agate spheres into an agate ball milling tank according to the weight ratio of 1.5.
(3) Weighing a certain amount of olivine powder, filling the olivine powder into a tablet press, and pressing the olivine powder into tablets under the pressure of 4MPa to obtain olivine blanks;
(4) And (3) filling the pressed blank body in a crucible, heating to 1000 ℃ by using a tube furnace in the atmosphere of normal-pressure inert gas at the heating rate of 3 ℃/min, and preserving heat for 4h to obtain the iron isotope standard sample.
Comparative example 1
The conditions were kept the same as in example 3, except that only steps (1), (3) and (4) were carried out.
Comparative example 2
The sintering temperature in step (4) was changed to 900 ℃, and other conditions were kept the same as in example 3.
Comparative example 3
The sintering temperature was changed to 1400 ℃ in step (4), and other conditions were kept consistent with example 3.
Performance test
(1) Phase test
Phase tests were performed by X-ray diffraction (XRD) on the sintered tablets of the standard block-shaped olivine samples prepared in examples 1 to 5 and the olivine samples prepared in comparative examples 1 to 5, and the test results are shown in table 1.
TABLE 1 test results
| Phase test results | Appearance of the sample | |
| Example 1 | No change, high diffraction peak intensity | High compactness and uneasy damage |
| Example 2 | No change, and large diffraction peak intensity | High compactness and uneasy damage |
| Example 3 | No change, and large diffraction peak intensity | High compactness and uneasy damage |
| Example 4 | No change, and large diffraction peak intensity | High compactness and uneasy damage |
| Example 5 | No change, high diffraction peak intensity | High compactness and uneasy damage |
| Comparative example 1 | No change, and large diffraction peak intensity | High compactness and uneasy damage |
| Comparative example 2 | No change, high diffraction peak intensity | Loose and easily damaged |
| Comparative example 3 | Is not seen to changeHigh diffraction peak intensity | Local melting appears and dark patches appear |
From table 1, fig. 2, it can be derived: the phase of the bulk olivine iron isotope composition standard samples prepared in examples 1 to 5 was not changed, and the phase of the olivine samples prepared in comparative examples 1 to 3 was not changed, indicating that the manner of solid phase sintering under protective gas did not affect the phase of the samples.
(2) Hardness test
The hardness test was performed on the massive olivine iron isotope composition standard samples prepared in examples 1 to 5 by a vickers hardness tester, and the test results are shown in table 2.
TABLE 2 test results
| D1(um) | D2(um) | DAvg(um) | Hardness Value (HV) | |
| Example 1 | 52.78 | 46.76 | 49.77 | 374.32 |
| Practice ofExample 2 | 50.98 | 48.20 | 49.59 | 377.05 |
| Example 3 | 53.75 | 46.15 | 49.95 | 371.62 |
| Example 4 | 51.58 | 47.60 | 49.59 | 377.05 |
| Example 5 | 53.39 | 45.79 | 49.59 | 377.05 |
From table 2 it can be derived: the hardness of the bulk olivine iron isotope composition standard samples prepared in examples 1 to 5 is higher than 370HV. The massive olivine standard sample prepared by the preparation method provided by the invention has the advantages of high hardness, approximate hardness to glass, compact internal structure, high strength and difficult damage.
And the comparative example 2 has insufficient sintering temperature, low overall density and looseness, and is broken after being taken out of a sintering instrument. Comparative example 5 the sintering temperature was too high and dark spots caused by partial melting of the surface of the sample appeared.
(3) Homogeneity of iron isotope composition
The uniformity of the iron isotope composition in the bulk olivine iron isotope composition standard samples prepared in examples 1 to 5 and the uniformity of the iron isotope composition in the olivine sample of comparative example 1 was examined by uniform spot distribution analysis on an olivine sintered plate by laser ablation plasma mass spectrometry, wherein the uniformity was determined by two-fold standard deviation (2 SD), and the test results are shown in table 3.
TABLE 3 test results
| δ 56 Fe | |
| Example 1 | 0.02±0.06‰ |
| Example 2 | 0.02±0.08‰ |
| Example 3 | -0.02±0.07‰ |
| Example 4 | -0.02±0.07‰ |
| Example 5 | 0.01±0.07‰ |
| Comparative example 1 | 0.01±0.76‰ |
From table 3 and fig. 4, it can be seen that: iron isotope composition of standard sample iron isotope group of massive olivine prepared in examples 1 to 5Become uniform, δ 56 The 2SD of Fe is less than 0.1 per mill, the homogeneity of the iron isotope composition of the olivine standard sample of the comparative example 1 is poor, and the olivine standard sample is not suitable for being used as a standard sample.
In conclusion, the hardness of the massive olivine iron isotope composition standard sample prepared by the preparation method provided by the invention is higher than 370HV, the sample is similar to glass hardness, the internal structure is compact, the strength is high, the sample is not easy to break, the iron isotope composition is uniform, and the delta is 56 The 2-time standard deviation (2 SD) of Fe is less than 0.1 per thousand, meets the requirement of laser ablation plasma mass spectrum iron isotope quantitative analysis, and is suitable for being used as a standard sample for testing the composition of the in-situ iron isotope in the olivine micro-area.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.
Claims (10)
1. A preparation method of a massive olivine iron isotope composition standard sample is characterized by comprising the following steps:
s1: coarse crushing olivine to obtain coarse olivine;
s2: grinding the olivine coarse body, and drying to obtain olivine powder;
s3: tabletting the olivine powder to obtain an olivine blank;
s4: and sintering the blank in a protective gas to obtain a standard sample consisting of the blocky olivine iron isotope.
2. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S1:
the particle size of the olivine coarse body is less than or equal to 100 μm.
3. The method for preparing the standard sample of isotopic composition of massive olivine iron as set forth in claim 1, wherein the step S2 comprises:
and adding absolute ethyl alcohol or isopropanol or n-butanol into the olivine coarse body, grinding, and drying to obtain olivine powder with the particle size of 0.5-4 μm.
4. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S2:
the grinding time is 9-11 h.
5. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S2:
the drying temperature is 70-110 ℃.
6. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S3:
the pressure intensity during tabletting is 4-6 MPa.
7. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S4:
the sintering temperature is 1000-1300 ℃; and/or the presence of a gas in the gas,
the heating rate is 1-3 ℃/min.
8. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S4:
the sintering time is 4-6 h.
9. The method for preparing the massive olivine iron isotope composition standard sample according to claim 1, wherein in step S4:
the protective gas is argon with the volume fraction not less than 99.999%; and/or the presence of a gas in the gas,
the protective gas is nitrogen with the volume fraction not less than 99.999%.
10. Use of a massive olivine iron isotope composition standard sample prepared by the method for preparing a massive olivine iron isotope composition standard sample according to any of claims 1 to 9 for quantitative analysis of an olivine iron isotope by laser ablation plasma mass spectrometry.
Priority Applications (1)
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