CN114018678A - Device and method for purifying and separating copper isotopes in soil - Google Patents
Device and method for purifying and separating copper isotopes in soil Download PDFInfo
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- CN114018678A CN114018678A CN202111422611.1A CN202111422611A CN114018678A CN 114018678 A CN114018678 A CN 114018678A CN 202111422611 A CN202111422611 A CN 202111422611A CN 114018678 A CN114018678 A CN 114018678A
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a device and a method for purifying and separating copper isotopes in soil, which comprises a reagent bottle, a filling column, an upper panel, a pressure-resistant glass cover, a bearing panel and a vacuum pump, wherein the top end of the filling column is connected with the reagent bottle through a guide pipe and a quantitative six-way valve, anion exchange resin is filled in the filling column, the bottom end of the filling column is connected with the top end of a two-way valve arranged on the upper panel, the bottom end of the two-way valve is connected with a drainage pipe, the pressure-resistant glass cover is arranged at the bottom of the upper panel, the bearing panel is arranged in the pressure-resistant glass cover, the drainage pipe is arranged in the pressure-resistant glass cover, a sample pipe for containing eluent flowed down by the drainage pipe is arranged on the bearing panel, the pressure-resistant glass cover is connected with the vacuum pump through a pipeline, and a pressure control valve is arranged on the pipeline; the invention establishes the method for purifying the copper isotope in the soil, simplifies the pretreatment process of the copper isotope in the soil and greatly improves the pretreatment efficiency. The establishment of the method is beneficial to researching the migration and transformation process of the copper element in the soil and analyzing the source of the copper element.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a device and a method for purifying and separating copper isotopes in soil.
Background
Copper is one of the main transition metal elements in nature, on one hand, it is used as a necessary trace element in the human body to participate in metabolic cycle, and on the other hand, it is often existed in various environmental media such as rocks, minerals, soil and organisms in different valence states (0, +1, +2) in the natural environment, and it is widely involved in various biochemical and geochemical processes. Copper is found in nature65Cu and63two stable isotopes of Cu, 30.826% and 69.174% of total copper, respectively. The copper isotope in nature has obvious fractionation phenomenon, and the research on the composition of the copper isotope provides new clues and evidences for showing various geological actions in nature and researching the cause and distribution rule of ore deposit. In the research, the copper isotope composition in the soil has important significance in environmental science and the interaction between the earth and the biosphere.
The rapid development of copper isotope research in the above scientific research field benefits from the improvement of the analysis technology, and the key point lies in the application of a multi-receiving plasma mass spectrometer (MC-ICP-MS). However, because of the complex chemical composition of the soil sample, the direct copper isotope test on various samples by using MC-ICP-MS can generate strong allomone interference and mass discrimination effect, such as the possibility of existence of (A) in the copper isotope determination process23Na40Ar)+、(25Mg40Ar)+、(64ZnH) + isoallotrope interferes, thereby affecting the accurate determination of the copper isotopic composition. Therefore, it is particularly important to obtain pure Cu components by chemical purification and separation before copper isotope determination using a multiple-reception plasma mass spectrometer. At present, the purification and separation of Cu are realized by manually passing through ion exchange resin, and no commercial device for purifying and separating copper isotopes in soil exists.
Disclosure of Invention
The invention aims to provide a device and a method for purifying and separating copper isotopes in soil, which are used for solving the problems in the prior art, developing a set of device for purifying the copper isotopes, establishing a method for purifying the copper isotopes in the soil, simplifying the pretreatment process of the copper isotopes in the soil and greatly improving the pretreatment efficiency. The establishment of the method is beneficial to researching the migration and transformation process of the copper element in the soil and analyzing the source of the copper element.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a device for purifying and separating copper isotopes in soil, which comprises a reagent bottle, a filling column, an upper panel, a pressure-resistant glass cover, a receiving panel and a vacuum pump, wherein the reagent bottle comprises a reagent bottle A filled with a mixed solution of hydrochloric acid and hydrogen peroxide and a reagent bottle B filled with ultrapure water, the top end of the filling column is connected with the reagent bottle A and the reagent bottle B through a guide pipe and a quantitative six-way valve, anion exchange resin is filled in the filling column, the bottom end of the filling column is connected with the top end inlet of a two-way valve arranged on the upper panel, the bottom end outlet of the two-way valve is connected with a drainage pipe, the pressure-resistant glass cover is arranged at the bottom of the upper panel, the receiving panel is arranged in the pressure-resistant glass cover, the drainage pipe is arranged in the pressure-resistant glass cover, and a sample pipe for containing eluent flowed down by the drainage pipe is arranged on the receiving panel, the pressure-resistant glass cover is further connected with the vacuum pump through a pipeline, and a pressure control valve is arranged on the pipeline.
Preferably, the quantitative six-way valve comprises a six-way valve and three quantitative rings installed on the six-way valve, two reagent inlets of the six-way valve are respectively connected with the reagent bottle a and the reagent bottle B, three reagent outlets of the six-way valve are respectively connected with the three quantitative rings, the three quantitative rings are connected with the conduit at the top end of the filling column, and the volumes of the three quantitative rings are respectively 3mL, 5mL and 10 mL; and the waste liquid outlet of the six-way valve is connected with a waste liquid collecting bottle through a conduit.
Preferably, a piston head is installed at the top of the filling column, two ends of the piston head are respectively provided with a thin opening and a thick opening, the thin opening is connected with the conduit, and the diameter of the thin opening is 1.2-2.2 mm; the thick port is connected with the packed column, and the diameter of the thick port is 1-1.5 mm.
Preferably, a plurality of round holes for installing the two-way valve are arranged on the upper panel.
Preferably, the receiving panel is provided with receiving holes which are opposite to the round holes one by one, and the sample tubes are placed on the receiving holes; and supporting legs are arranged at four corners of the bottom of the bearing panel.
Preferably, the upper panel and the receiving panel are made of Teflon, the number of the round holes in the upper panel and the number of the receiving holes in the receiving panel are respectively 4-10, and the aperture is 3-6 mm.
Preferably, the pressure-resistant glass cover is hermetically connected with the upper panel.
Preferably, the conduit is made of corrosion-resistant plastic material, and the diameter of the conduit is 1 mm-2 mm; the drainage tube is made of Teflon and has a diameter of 0.5-1.2 mm.
Preferably, the particle size of the anion exchange resin is 100-200 meshes, and the filling volume is 1.6-2.3 mL.
Based on the device for purifying and separating the copper isotopes in the soil, the invention also provides a method for purifying and separating the copper isotopes, which comprises the following steps:
step one, alternately soaking and cleaning anion exchange resin with nitric acid and ultrapure water, and then filling columns by a wet method;
step two, the packed column is arranged on a two-way valve, the upper end of the packed column is connected to a reagent bottle through a conduit and a quantitative six-way valve, and the reagent bottle A contains HCl and H2O2Reagent A composed of the mixed liquid of (1), reagent bottle B containing reagent B composed of ultrapure water; opening the vacuum pump, keeping the pressure-resistant glass cover in a negative pressure state, and adjusting the tightness of the two-way valve to control the flow rate of the liquid; controlling the reagent and volume flowing into the packed column through the six-way valve and the quantitative ring;
step three, alternately leaching the packed column by using the reagent A and the reagent B respectively, wherein leaching solution directly flows into a pressure-resistant glass cover; opening a piston head of the packed column, and dropwise adding 0.2-1 mL of a sample; eluting matrix elements in the anion exchange resin by using 7-10 mL of the reagent A, and directly flowing eluent into a pressure-resistant glass cover; and finally, eluting the copper element by using 24-30 mL of the reagent A, and carrying the eluent by using a sample tube.
Compared with the prior art, the invention has the following beneficial technical effects:
1. reagent is automatically injected into the filling column, so that labor cost is saved.
2. The whole system is under the negative pressure condition, the time of the solvent flowing through the packed column can be controlled, and the sample preparation time is saved.
3. Meanwhile, 4-10 filling columns can be adopted for purifying and separating samples, and the samples are more efficiently processed. The method develops a device for purifying and separating the copper isotopes in the soil, simplifies the pretreatment process of the copper isotopes in the soil, greatly improves the pretreatment efficiency, and reduces the operation cost and the labor cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and 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 to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for purifying and separating copper isotopes in soil according to the present invention;
in the figure: 1-reagent bottle A, 2-reagent bottle B, 3-quantitative ring, 4-six-way valve, 5-piston head, 6-packed column, 7-anion exchange resin, 8-two-way valve, 9-round hole, 10-drainage tube, 11-sample tube, 12-upper panel, 13-receiving panel, 14-pressure-resistant glass cover, 15-pressure control valve, 16-vacuum pump, 17-waste liquid collecting bottle.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a device and a method for purifying and separating copper isotopes in soil, which aim to solve the problems in the prior art.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The device for purifying and separating copper isotopes in soil in the embodiment comprises a reagent bottle, a filling column 6, an upper panel 12, a pressure-resistant glass cover 14, a receiving panel 13 and a vacuum pump 16, wherein the reagent bottle comprises a reagent bottle A1 filled with a mixed solution of hydrogen chloride and hydrogen peroxide and a reagent bottle B2 filled with ultrapure water, the top end of the filling column 6 is connected with a reagent bottle A1 and a reagent bottle B2 through a guide pipe and a quantitative six-way valve, anion exchange resin 7 is filled in the filling column 6, the bottom end of the filling column 6 is connected with the top end inlet of a two-way valve 8 arranged on the upper panel 12, the bottom end outlet of the two-way valve 8 is connected with a drainage pipe 10, the pressure-resistant glass cover 14 is arranged at the bottom of the upper panel 12, the pressure-resistant glass cover 14 is hermetically connected with the upper panel 12, the receiving panel 13 is arranged in the pressure-resistant glass cover 14, the drainage pipe 10 is arranged on the receiving panel 13 and is provided with a sample pipe 11 for containing eluent flowed down by the drainage pipe 10, the pressure-resistant glass cover 14 is also connected to a vacuum pump 16 via a pipe, on which a pressure control valve 15 is provided.
In the embodiment, the quantitative six-way valve comprises a six-way valve 4 and three quantitative rings 3 arranged on the six-way valve 4, two reagent inlets of the six-way valve 4 are respectively connected with a reagent bottle A1 and a reagent bottle B2, three reagent outlets of the six-way valve 4 are respectively connected with the three quantitative rings 3, the three quantitative rings 3 are connected with a conduit at the top end of the packing column 6 through the three quantitative rings 3, and the volumes of the three quantitative rings 3 are respectively 3mL, 5mL and 10 mL; the waste liquid outlet of the six-way valve 4 is connected with a waste liquid collecting bottle 17 through a conduit; the quantitative ring 3 has a fixed volume, the corresponding quantitative ring 3 is selectively connected according to the requirement, the ring is filled with the reagent with the same volume as the quantitative ring 3, and then the quantitative reagent is conveyed to the filling column 6; excess reagent is discharged through the waste outlet of the six-way valve 4 to the waste collection bottle 17.
In the embodiment, the top of the packed column 6 is provided with a piston head 5, two ends of the piston head 5 are respectively provided with a thin opening and a thick opening, the thin opening is connected with a conduit, and the diameter of the conduit is 1.2-2.2 mm; the thick port is connected with a packed column 6, and the diameter is 1-1.5 mm.
In this embodiment, the upper panel 12 is provided with a plurality of circular holes 9 for installing the two-way valve 8; the bearing panel 13 is provided with bearing holes which are opposite to the round holes 9 one by one, and the sample tubes 11 are placed on the bearing holes; the four corners of the bottom of the bearing panel 13 are provided with supporting legs; the upper panel 12 and the receiving panel 13 are made of Teflon, the number of the round holes 9 on the upper panel 12 and the number of the receiving holes on the receiving panel 13 are 4-10 respectively, and the aperture is 3-6 mm.
In this embodiment, the catheter is made of Teflon (PTFE) and has a diameter of 1mm to 2 mm; the drainage tube 10 is made of Teflon (PTFE) and has a diameter of 0.5-1.2 mm.
In this embodiment, the anion exchange resin 7 has a particle size of 100 to 200 mesh and a filling volume of 1.6 to 2.3 mL.
Based on the device for purifying and separating the copper isotopes in the soil, the embodiment also provides a method for analyzing the copper isotopes in the soil, which comprises the following steps:
1. soil sample digestion: accurately weighing 40-60 mg of ground soil sample into a 15mL beaker, adding 2mL of hydrofluoric acid, 1mL of concentrated nitric acid and 0.5mL of perchloric acid electric heating plates, heating to 120-130 ℃, and keeping for 48-72 hours until the solid sample in the beaker is completely digested, and clarifying the solution; evaporating to dryness at 80-90 ℃ and re-dissolving, repeating the operation for 3 times, and finally dissolving the sample in a mixed solution of a hydrochloric acid solution with the concentration of 8mol/L and a hydrogen peroxide solution with the concentration of 0.001%.
2. The separation and purification process of copper element by adopting the device for purifying and separating copper isotope in soil with the combination of figure 1 is as follows:
step one, AG MP-1M anion exchange resin 7 (the particle size is 100-200 meshes) is alternately soaked and cleaned by 5% nitric acid and ultrapure water, then the AG MP-1M anion exchange resin is loaded into a filling column 6 by a wet method, resin particles are uniform and free of gaps in the filling column 6 by beating in the filling process, and polyethylene sieve plates are respectively filled at the upper end and the lower end of the filling resin to prevent the filling material from moving.
Step two, the filling column 6 is arranged on a two-way valve 8, the two-way valve 8 is arranged on a round hole 9 on an upper panel 12, the upper end of the filling column 6 is connected to a reagent bottle A1 and a reagent bottle B2 through a guide pipe, a quantitative ring 3 and a six-way valve 4, the reagent bottle A1 contains mixed liquid of hydrochloric acid solution with the concentration of 6-8 mol/L and hydrogen peroxide solution with the concentration of 0.001%, and the reagent bottle B2 contains ultrapure water; opening a vacuum pump and a pressure control valve 15, vacuumizing the pressure-resistant glass cover 14 to enable the pressure-resistant glass cover 14 to be in a negative pressure state, and adjusting the tightness of the two-way valve 8 to control the flow speed of liquid in the drainage tube 10; controlling the reagent and volume flowing into the packed column 6 through the six-way valve 4 and the quantitative ring 3;
step three, leaching the packed column 6 by using 5mL of reagent A, 5mL of reagent B, 3mL of reagent A, 3mL of reagent B and 3mL of reagent A in sequence respectively, wherein the leaching solution directly flows into the pressure-resistant glass cover 14; opening a piston head 5 of the filling column 6, and dropwise adding 0.2-1 mL of a sample; leaching matrix elements in the resin by using 7-10 mL of reagent A, and directly flowing eluent into the pressure-resistant glass cover 14; and finally, eluting the copper element by using 24-30 mL of reagent A, and receiving the eluent by using a sample tube 11, wherein the sample tube 11 is placed on a receiving panel 13.
3. And analyzing the recovery rate of the Cu sample purification and separation process with the concentration of 0.5 mu g/g and 2.0 mu g/g by adopting an inductively coupled plasma mass spectrometer (ICP-MS), wherein the recovery rate is 101.2 +/-1.2%.
Compared with the prior art, the device and the method for purifying and separating the copper isotopes in the soil have the following advantages: 1. reagent is automatically injected into the packed column 6, so that the labor cost is saved; 2. the whole system is under the negative pressure condition, the time for the solvent to flow through the packed column 6 can be controlled, and the sample preparation time is saved; 3. meanwhile, 4-10 filling columns 6 can be adopted for purifying and separating samples, and the samples are more efficiently processed. The method develops a device for purifying and separating the copper isotopes in the soil, simplifies the pretreatment process of the copper isotopes in the soil, greatly improves the pretreatment efficiency, and reduces the operation cost and the labor cost.
The principle and the implementation mode of the invention are explained by applying specific examples, and the description of the above examples is only used for helping understanding the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In summary, this summary should not be construed to limit the present invention.
Claims (10)
1. A device for purifying and separating copper isotopes in soil is characterized in that: the device comprises a reagent bottle, a filling column, an upper panel, a pressure-resistant glass cover, a receiving panel and a vacuum pump, wherein the reagent bottle comprises a reagent bottle A filled with a mixed solution of hydrochloric acid and hydrogen peroxide and a reagent bottle B filled with ultrapure water, the top end of the filling column is connected with the reagent bottle A and the reagent bottle B through a guide pipe and a quantitative six-way valve, anion exchange resin is filled in the filling column, the bottom end of the filling column is connected with the top end inlet of a two-way valve arranged on the upper panel, the bottom end outlet of the two-way valve is connected with a drainage pipe, the pressure-resistant glass cover is arranged at the bottom of the upper panel, the receiving panel is arranged in the pressure-resistant glass cover, the drainage pipe is arranged in the pressure-resistant glass cover, the receiving panel is provided with a sample pipe for containing eluent flowing down from the drainage pipe, and the pressure-resistant glass cover is also connected with the vacuum pump through a pipeline, and a pressure control valve is arranged on the pipeline.
2. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: the quantitative six-way valve comprises a six-way valve and three quantitative rings arranged on the six-way valve, two reagent inlets of the six-way valve are respectively connected with the reagent bottle A and the reagent bottle B, three reagent outlets of the six-way valve are respectively connected with the three quantitative rings, the three quantitative rings are connected with a conduit at the top end of the filling column, and the volumes of the three quantitative rings are respectively 3mL, 5mL and 10 mL; and the waste liquid outlet of the six-way valve is connected with a waste liquid collecting bottle through a conduit.
3. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: the top of the filling column is provided with a piston head, two ends of the piston head are respectively provided with a thin opening and a thick opening, the thin opening is connected with the conduit, and the diameter of the thin opening is 1.2-2.2 mm; the thick port is connected with the packed column, and the diameter of the thick port is 1-1.5 mm.
4. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: and the upper panel is provided with a plurality of round holes for installing the two-way valve.
5. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 4, wherein: the bearing panel is provided with bearing holes which are opposite to the round holes one by one, and the sample tubes are placed on the bearing holes; and supporting legs are arranged at four corners of the bottom of the bearing panel.
6. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 5, wherein: the upper panel with accept the panel material and be Teflon, the round hole on the upper panel with accept the quantity of the hole on the panel and be 4 ~ 10 respectively, the aperture is 3 ~ 6 mm.
7. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: the pressure-resistant glass cover is connected with the upper panel in a sealing manner.
8. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: the guide pipe is made of corrosion-resistant plastic materials, and the diameter of the guide pipe is 1 mm-2 mm; the drainage tube is made of Teflon and has a diameter of 0.5-1.2 mm.
9. The apparatus for purifying and separating copper isotopes in soil as claimed in claim 1, wherein: the anion exchange resin has a particle size of 100-200 meshes and a filling volume of 1.6-2.3 mL.
10. A method for purifying and separating copper isotopes is characterized by comprising the following steps:
step one, alternately soaking and cleaning anion exchange resin with nitric acid and ultrapure water, and then filling columns by a wet method;
step two, the packed column is arranged on a two-way valve, the upper end of the packed column is connected to a reagent bottle through a conduit and a quantitative six-way valve, and the reagent bottle A contains HCl and H2O2Reagent A composed of the mixed liquid of (1), reagent bottle B containing reagent B composed of ultrapure water; opening the vacuum pump, keeping the pressure-resistant glass cover in a negative pressure state, and adjusting the tightness of the two-way valve to control the flow rate of the liquid; controlling the reagent and volume flowing into the packed column through the six-way valve and the quantitative ring;
step three, alternately leaching the packed column by using the reagent A and the reagent B respectively, wherein leaching solution directly flows into a pressure-resistant glass cover; opening a piston head of the packed column, and dropwise adding 0.2-1 mL of a sample; eluting matrix elements in the anion exchange resin by using 7-10 mL of the reagent A, and directly flowing eluent into a pressure-resistant glass cover; and finally, eluting the copper element by using 24-30 mL of the reagent A, and carrying the eluent by using a sample tube.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111422611.1A CN114018678A (en) | 2021-11-26 | 2021-11-26 | Device and method for purifying and separating copper isotopes in soil |
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| CN202111422611.1A CN114018678A (en) | 2021-11-26 | 2021-11-26 | Device and method for purifying and separating copper isotopes in soil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117606894A (en) * | 2023-11-27 | 2024-02-27 | 中国地质大学（北京） | Separation and purification and detection method for copper isotopes in geological samples |
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