An automated combined sample preparation device and method for iron-55 and nickel-63

Abstract

The application relates to an automatic combined sample preparation device and method of iron-55 and nickel-63, which comprises a pretreatment device, a first separation device, a second separation device, a liquid transfer device and a control device; the pretreatment device is used for concentrating and constant-volume treatment of a sample to be treated to obtain a first sample to be treated; the liquid transfer device is used for transferring the first sample to be treated in the pretreatment device to the first separation device and transferring liquid reagents to the pretreatment device, the first separation device and the second separation device; the first separation device is used for separating the first sample to be treated, concentrating a first effluent and performing pH adjustment treatment, and processing a first desorption liquid into a first sample; the second separation device is used for separating the first effluent after treatment and processing a second desorption liquid into a second sample; and the control device is electrically connected with the pretreatment device, the first separation device, the second separation device and the liquid transfer device respectively. The application can continuously prepare samples of iron and nickel.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of radiation environment monitoring, and particularly relates to an automatic combined sample preparation device and method for iron-55 and nickel-63. BACKGROUND

[0002] Iron and nickel are widely used as metal materials in various components of a reactor, and the corresponding activated products exist in radioactive solid waste and waste water generated by the reactor, and iron-55 and nickel-63 are radioactive nuclides with relatively large discharge amounts in liquid effluent of a nuclear power plant, and are conventional monitoring items of the radioactive liquid effluent.

[0003] In the related art, iron-55 and nickel-63 are prepared separately, and there are many separate sample preparation processes, which also wastes materials, and needs to be prepared manually by high-level operation technicians, which is high in labor cost and low in efficiency. The above problems need to be solved urgently. SUMMARY

[0004] The present application discloses an automatic combined sample preparation device and method for iron-55 and nickel-63, and aims to solve the technical problems in the prior art.

[0005] The present application adopts the following technical solutions:

[0006] In a first aspect, the present application provides an automatic combined sample preparation device for iron-55 and nickel-63, comprising: a pretreatment device, a first separation device, a second separation device, a liquid transfer device, and a control device;

[0007] The pretreatment device is used to concentrate and constant-volume the sample to be treated to obtain a first sample to be treated;

[0008] The liquid transfer device is used to transfer the first sample to be treated in the pretreatment device to the first separation device, and transfer liquid reagents to the pretreatment device, the first separation device, and the second separation device, wherein the liquid reagents at least include a dissolution reagent, a first elution reagent, a first desorption reagent, a second elution reagent, a pH adjustment reagent, a second desorption reagent, and a constant-volume reagent;

[0009] The first separation device is used to separate the first sample to be treated into a first effluent, a first elution liquid, and a first desorption liquid, and perform pH adjustment processing on the first effluent after concentration, and the first separation device is also used to process the first desorption liquid into a first sample;

[0010] The second separation device is used to separate the first effluent after processing to obtain a second effluent, a second elution liquid, and a second desorption liquid, and the second separation device is also used to process the second desorption liquid into a second sample;

[0011] The control device is electrically connected to the pretreatment device, the first separation device, the second separation device and the liquid injection device respectively.

[0012] In a second aspect, the application also provides an automated combined sample preparation method of iron-55 and nickel-63, comprising the following steps:

[0013] A sample to be treated is injected into the pretreatment device, and then the pH value is adjusted to less than 2, and then iron-55 carriers, nickel-63 carriers and counter carriers are injected, and after stirring, the sample is concentrated to near dryness, and then a hydrochloric acid solution of a first concentration is injected into the liquid injection device to obtain a first sample to be treated;

[0014] The first sample to be treated is introduced into the first separation device to obtain a first effluent, and then the liquid injection device injects a first elution reagent into the first separation device to obtain a first eluate, and then the liquid injection device injects a first desorption reagent into the first separation device to obtain a first desorption liquid, and the first desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected into the first desorption liquid through the liquid injection device to prepare a first sample rich in iron-55;

[0015] The first separation device evaporates the first effluent to near dryness, and then adds a dissolving reagent into the first effluent through the liquid injection device, stirs uniformly, and adds a pH adjusting reagent to pH=9 to obtain the adjusted first effluent;

[0016] The first effluent is introduced into the second separation device to obtain a second effluent, and then a second elution reagent is injected into the second separation device through the liquid injection device to obtain a second eluate, and then a second desorption reagent is injected into the second separation device to obtain a second desorption liquid; the second desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected to obtain a second sample rich in nickel-63.

[0017] The technical solution adopted by the application can achieve the following beneficial effects:

[0018] The application mainly provides an automated combined sample preparation device of iron-55 and nickel-63, which can automatically prepare samples of iron-55 and nickel-63, simplify the sample preparation process, improve the sample preparation efficiency, reduce labor costs and save raw materials. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the embodiments of the application, the following will briefly introduce the drawings needed to be used in the embodiment description, which constitutes a part of the application. The schematic embodiments of the application and their description and explanation do not constitute an improper limitation on the application. In the drawings:

[0020] Figure 1 Fig. 1 is a structural schematic diagram of an automatic combined sample preparation device for Fe-55 and Ni-63 according to the present application;

[0021] Figure 2 Fig. 2 is a structural schematic diagram of an automatic combined sample preparation device for Fe-55 and Ni-63 according to the present application;

[0022] Figure 3 Fig. 3 is a structural schematic diagram of a liquid transfer device according to the present application.

[0023] BRIEF DESCRIPTION OF DRAWINGS

[0024] 1. pre-treatment device; 11. first conveying device; 12. first container; 13. first heater; 2. first separation device; 21. first separation column; 22. first multi-way valve; 23. second container; 24. second heater; 25. third container; 26. third heater; 27. second conveying device; 28. third conveying device; 29. first liquid scintillator vial; 210. first waste vial; 3. second separation device; 31. fourth conveying device; 32. second separation column; 33. second multi-way valve; 34. fourth container; 35. fourth heater; 36. second waste vial; 37. fifth conveying device; 38. second liquid scintillator vial; 4. liquid transfer device; 41. first multi-interface communicator; 411. first inner mounting disc; 412. first outer mounting disc; 413. first outer passage; 4131. first outer outlet passage; 4132. first outer inlet passage; 414. first inner passage; 42. communicating tube; 43. conveying pump; 44. second multi-interface communicator; 441. second inner mounting disc; 442. second outer mounting disc; 443. second outer passage; 4431. second outer inlet passage; 4432. second outer outlet passage; 444. second inner passage; 5. control device. DETAILED DESCRIPTION

[0025] In order to make the objectives, technical solutions and advantages of the present application clearer, the technical solutions of the present application will be described below in connection with specific embodiments of the present application and corresponding drawings. In the description of the present application, it should be noted that the term "or" is generally used in the sense of including "and / or" unless the context clearly indicates otherwise.

[0026] Unless expressly stated to the contrary, numerical parameters in the specification and accompanying claims are approximations. Although the numerical parameters are approximations, the numerical values set forth in the specific description are reported as precisely as possible. Any numerical value, however, can contain certain errors associated with the standard variation found in their respective testing measurements.

[0027] Also, the word "comprising" does not exclude the presence of elements or steps other than those listed in a claim. The word "first", "second", "third" and the like in the description do not necessarily mean "first", "second", "third" etc. in a strict sense, but are used to differentiate one element from another, and should be interpreted as a distinction in order.

[0028] In addition, unless specifically described or necessary in sequence, the order of the steps described above is not limited to the above list, and can be changed or rearranged according to the desired design. And the above examples can be mixed and used with each other or with other examples based on design and reliability considerations, that is, the technical features in different examples can be freely combined to form more examples.

[0029] Obviously, the described embodiments are only a part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0030] To solve the problems in the prior art, the embodiments of the present application provide an automatic combined sample preparation device for iron-55 and nickel-63 and a method.

[0031] Embodiment 1

[0032] The present embodiment provides an automatic combined sample preparation device for iron-55 and nickel-63, as shown in Figure 1As shown, it comprises: a pretreatment device 1, a first separation device 2, a second separation device 3, a liquid transfer device 4 and a control device 5; the pretreatment device 1 is used for concentrating and constant volume of the sample to be treated to obtain a first sample to be treated; the liquid transfer device 4 is used for transferring the first sample to be treated in the pretreatment device 1 to the first separation device 2, and transferring liquid reagents to the pretreatment device 1, the first separation device 2 and the second separation device 3, the liquid reagents at least including a dissolution reagent, a first elution reagent, a first desorption reagent, a constant volume reagent, a second elution reagent, a pH adjusting reagent and a second desorption reagent; the first separation device 2 is used for separating the first sample to be treated into a first effluent, a first eluent and a first desorption liquid, and performing pH adjustment treatment on the first effluent after concentration; the first separation device 2 is also used for processing the first desorption liquid into a first sample (i.e. a liquid sample rich in iron-55); the second separation device 3 is used for separating the processed first effluent to obtain a second effluent, a second eluent and a second desorption liquid, and processing the second desorption liquid into a second sample (i.e. a liquid sample rich in nickel-63); and the control device 5 is electrically connected to the pretreatment device 1, the first separation device 2, the second separation device 3 and the liquid transfer device 4 respectively to control their working or non-working.

[0033] The automatic combined sample preparation device for iron-55 and nickel-63 can automatically prepare samples of iron-55 and nickel-63, simplify the sample preparation process, improve the sample preparation efficiency, reduce the labor cost and save raw materials.

[0034] In some preferred embodiments, the pretreatment device 1 comprises a first conveying device 11, a first container 12 and a first heater 13; the discharge port of the first conveying device 11 communicates with the feed port of the first container 12, and the first conveying device 11 is electrically connected to the control device 5; the discharge port of the first container 12 communicates with the feed port of the liquid transfer device 4; the first heater 13 is used for heating the first container 12 and is electrically connected to the control device 5; based on the control of the first conveying device 11 and the first heater 13 by the control device 5, the automatic injection of the material is realized, and the sample to be treated is concentrated and constant volume by heating, which on the one hand realizes the preparation of the iron-55 and nickel-63 samples by the cooperation of the first separation device 2 and the second separation device 3, and on the other hand reduces the liquid amount in the subsequent process; in the second aspect, the accurate control of the sample system (i.e. the content of each component) and the accurate control of the sample volume are realized.

[0035] Preferably, the control device 5 is also used for detecting the near-dry state of the material in the first container 12; the detection of the near-dry state can include various ways. For example, the model can be trained by a network model to enable the model to identify the near-dry state. The monitoring can also be completed by other ways, which are not exemplified one by one in the embodiments of the present disclosure.

[0036] Preferably, the first conveying device 11 is an injection pump, and the number is one or more, for conveying the sample to be processed, concentrated nitric acid, iron-55 carrier, nickel-63 carrier and counter carrier; alternatively, the sample to be processed, concentrated nitric acid, iron-55 carrier, nickel-63 carrier and counter carrier can be conveyed by one first conveying device 11 or by multiple first conveying devices 11 respectively.

[0037] Specifically, when starting processing, the control device 5 controls the first conveying device 11 to feed, and sequentially adds the sample to be processed, iron-55 carrier, nickel-63 carrier and counter carrier into the first container 12 in sequence, and then stirs uniformly, and the control device 5 controls the first heater 13 to work to heat the first container 12, evaporates the liquid in the first container 12 to near dryness, and then the control device 5 controls the liquid injection device 4 to inject a constant volume of reagent (hydrochloric acid of the first concentration) into the first container 12 to obtain the first sample to be processed.

[0038] In some preferred embodiments, the first separation device 2 comprises a first separation column 21, a first multi-way valve 22, a second container 23, a second heater 24, a third container 25, a third heater 26 and a second conveying device 27; the feeding port of the first separation column 21 is communicated with the discharging port of the liquid injection device 4, and the discharging port is communicated with the feeding port of the first multi-way valve 22; the first multi-way valve 22 comprises a plurality of discharging ports, which are respectively communicated with the feeding ports of the second container 23 and the third container 25; the feeding port of the second container 23 is communicated with the discharging port of the second conveying device 27, and the discharging port is communicated with the feeding port of the second separation device 3, and the feeding port of the second container 23 is communicated with the discharging port of the liquid injection device 4; the feeding port of the third container 25 is communicated with the discharging port of the liquid injection device 4; the second heater 24 is used for heating the second container 23; the third heater 26 is used for heating the third container 25; the control device 5 is electrically connected with the first multi-way valve 22, the second heater 24, the third heater 26 and the second conveying device 27; based on the control of the control device 5 on the first multi-way valve 22, the second heater 24, the third heater 26 and the second conveying device 27, the automatic sample preparation is realized, and the efficiency of sample preparation is improved.

[0039] Preferably, the second conveying device 27 is an injection pump, for conveying ammonium citrate with pH=9 and ammonia water; alternatively, the second conveying device 27 is a pump group composed of multiple injection pumps or a multi-channel injection pump or a combination of a single-channel injection pump and a multi-channel injection pump; or, the second conveying device 27 is integrated in the liquid injection device 4, that is, the liquid injection device 4 is used to convey ammonium citrate with pH=9 and ammonia water.

[0040] Preferably, the first separation device 2 further comprises a third conveying device 28 and a first liquid scintillation vial 29; the third conveying device 28 is used to convey the liquid in the third container 25 to the first liquid scintillation vial 29; the control device 5 is electrically connected to the third conveying device 28.

[0041] Preferably, the first separation device 2 further comprises a first waste liquid vial 210; the feed inlet of the first waste liquid vial 210 is communicated with the discharge outlet of the first multi-way valve 22.

[0042] Preferably, the first separation column 21 is an anion exchange resin column; for example, a funnel glass piston type ion exchange column with strong basic anion exchange resin, with a specification of 13x10x200mm.

[0043] Preferably, the first multi-way valve 22 has three discharge outlets, each of which is communicated with the feed inlet of the second container 23, the third container 25 and the first waste liquid vial 210.

[0044] Specifically, the working process of the first separation device 2 is as follows: the control device 5 controls the liquid transfer device 4 to convey the first sample to be treated in the pretreatment device 1 to the first separation column 21; the first multi-way valve 22 opens the discharge outlet corresponding to the second container 23, so that the first effluent enters the second container 23; the control device 5 controls the liquid transfer device 4 to inject the first elution reagent into the first separation column 21; the first multi-way valve 22 opens the discharge outlet corresponding to the first waste liquid vial 210, so that the first eluate flows into the first waste liquid vial 210 for collection; the control device 5 controls the liquid transfer device 4 to inject the first desorption reagent into the first separation column 21; the first multi-way valve 22 opens the discharge outlet corresponding to the third container 25, so that the first desorption liquid flows into the third container 25; the control device 5 controls the third heater 26 to start heating, so that the liquid in the third container 25 is evaporated to near dryness; then, the control device 5 controls the liquid transfer device 4 to inject the constant volume reagent into the third container 25, to obtain the first sample rich in iron-55; the control device 5 controls the third conveying device 28 to convey the liquid to the first liquid scintillation vial 29; the control device 5 controls the second heater 24 to evaporate the first effluent in the second container 23 to near dryness; then, the liquid transfer device 4 injects the dissolving reagent into the second container 23; after stirring, the control device 5 controls the second conveying device 27 to inject the pH adjusting reagent into the second container 23, to obtain the treated first effluent; thus, without the need for on-site supervision, the sample of iron-55 to be analyzed is prepared and stored in the first liquid scintillation vial 29, which only needs to be taken to the liquid scintillation counter for direct measurement.

[0045] In some preferred embodiments, the second separation device 3 comprises a fourth conveying device 31, a second separation column 32, a second multi-way valve 33, a fourth container 34, a fourth heater 35 and a second waste liquid bottle 36; the feeding port of the fourth conveying device 31 is communicated with the first separation device 2, and the discharging port is communicated with the feeding port of the second separation column 32; the discharging port of the second separation column 32 is communicated with the feeding port of the second multi-way valve 33; the second multi-way valve 33 has a plurality of discharging ports, which are respectively communicated with the feeding ports of the fourth container 34 and the second waste liquid bottle 36; the feeding port of the fourth container 34 is communicated with the discharging port of the liquid transfer device 4; the fourth heater 35 is used for heating the fourth container 34; the control device 5 is electrically connected with the fourth conveying device 31, the second multi-way valve 33 and the fourth heater 35; based on the control of the control device 5 on the fourth conveying device 31, the second multi-way valve 33 and the fourth heater 35, the automation of the separation and sample preparation process is realized, and the efficiency of sample preparation is improved.

[0046] Preferably, the second separation column 32 is a nickel specific resin column, such as an ion exchange column with nickel specific resin, with a specification of 9x7x50mm.

[0047] Preferably, the second separation device 3 further comprises a fifth conveying device 37 and a second liquid scintillation vial 38; the fifth conveying device 37 is used for conveying the liquid in the fourth container 34 to the second liquid scintillation vial 38; and the control device 5 is electrically connected with the fifth conveying device 37.

[0048] Specifically, the working process of the second separation device 3 is as follows: the control device 5 controls the fourth conveying device 31 to convey the first effluent obtained by processing the first separation device 2 to the second separation column 32, and separates through the second separation column 32, at the same time, the second multi-way valve 33 is switched to the discharging port communicated with the second waste liquid bottle 36, and the second effluent is conveyed to the second waste liquid bottle 36, then the control device 5 controls the liquid transfer device 4 to inject the second elution reagent into the second separation column 32, and the obtained second elution liquid is conveyed to the second waste liquid bottle 36; then the second multi-way valve 33 is switched to the discharging port communicated with the fourth container 34, then the control device 5 controls the liquid transfer device 4 to inject the second desorption reagent into the second separation column 32, and the obtained second desorption liquid is conveyed to the fourth container 34, the control device 5 controls the fourth heater 35 to heat the fourth container 34 to near dryness of the second desorption liquid, then the liquid transfer device 4 injects the constant volume reagent into the fourth container 34, and the second sample of nickel-63 is obtained.

[0049] In some preferred embodiments, the first heater 13, the second heater 24 and the third heater 26 are all electric heating jackets, preferably electric heating jackets with magnetic stirring function; the first container 12, the second container 23, the third container 25 and the fourth container 34 are reagent bottles matched therewith.

[0050] In some preferred embodiments, asFigure 2 and 3 As shown in the figure, the liquid transfer device 4 comprises a first multi-port connector 41, a connecting pipe 42, a delivery pump 43 and a second multi-port connector 44; the first multi-port connector 41 has a plurality of first inlets and a first outlet; the first outlet can selectively communicate with one of the first inlets; each first inlet is used to communicate with different external liquid reagents; the second multi-port connector 44 has a second inlet and a plurality of second outlets; the second inlet can selectively communicate with one of the second outlets; each second outlet is used to communicate with the pretreatment device 1, the first separation device 2 and the second separation device 3; one end of the connecting pipe 42 communicates with the first outlet, and the other end communicates with the second inlet; the delivery pump 43 is arranged in the connecting pipe 42 and used to deliver materials from the first multi-port connector 41 to the second multi-port connector 44; based on forming a plurality of inlets in the first multi-port connector 41 to input different liquid reagents and forming a plurality of outlets in the second multi-port connector 44 to deliver the liquid reagents into different containers, the structure is simple, and multiple material delivery and multiple container output are realized.

[0051] Preferably, the connecting pipe 42 is a rubber pipe; the delivery pump 43 is a peristaltic pump, and is driven by a stepping motor or a servo motor.

[0052] In some preferred embodiments, the first multi-port connector 41 comprises a first inner mounting disc 411 and a first outer mounting disc 412; the first outer mounting disc 412 is arranged around the outer periphery of the first inner mounting disc 411 and has a plurality of first outer channels 413, that is, the first outer mounting disc 412 has a circular ring structure, and the first inner mounting disc 411 is inside the circular ring; the first inner mounting disc 411 has a first inner channel 414; one of the plurality of first outer channels 413 is a first outer outlet channel 4131, and the others are first outer inlet channels 4132; each first outer inlet channel 4132 has one end arranged close to the outer periphery of the first outer mounting disc 412 to form a plurality of first inlets, and the other end is used to abut and communicate with one end of the first inner channel 414; the other end of the first inner channel 414 communicates with one end of the first outer outlet channel 4131; the other end of the first outer outlet channel 4131 forms the first outlet; the first outer mounting disc 412 and the first inner mounting disc 411 can rotate relative to each other, so that one end of the first inner channel 414 can abut and communicate with one end of each first outer inlet channel 4132 in turn, and the other end of the first inner channel 414 remains abutting and communicating with the first outer outlet channel 4131; based on this, a structure of one outlet corresponding to a plurality of inlets is formed, and the structure is simple and convenient to switch.

[0053] Preferably, the first inner mounting disc 411 and the first outer mounting disc 412 rotate relative to each other by a servo motor, for example, the servo motor drives the first inner mounting disc 411 to rotate.

[0054] Preferably, the first inner channel 414 is a hose, one end of which is in communication with the first outer inlet channel 4131 and is fixed in position, and the other end can rotate to change the orientation with the first inner mounting disc 411 to be in communication with different first outer inlet channels 4132.

[0055] Preferably, the end of the first outer inlet channel 4132 in communication with the first inner channel 414 is elastically abutted and sealed;

[0056] Preferably, the first outer inlet channel 4132 and the first outer outlet channel 4131 are both rigid pipes.

[0057] Alternatively,

[0058] The second multi-interface communication device 44 comprises a second inner mounting disc 441 and a second outer mounting disc 442; the second outer mounting disc 442 is arranged around the outer periphery of the second inner mounting disc 441 and has a plurality of second outer channels 443; the second inner mounting disc 441 can rotate relative to each other and has a second inner channel 444; one of the plurality of second outer channels 443 is a second outer inlet channel 4431, and the rest are second outer outlet channels 4432; each second outer outlet channel 4432 has one end arranged close to the outer periphery of the second outer mounting disc 442 to form a plurality of second outlet ports, and the other end is used to be in communication with one end of the second inner channel 444; the other end of the second inner channel 444 is in communication with one end of the second outer outlet channel 4432; the other end of the second outer inlet channel 4431 forms a second inlet port; the second outer mounting disc 442 and the second inner mounting disc 441 can rotate relative to each other, so that one end of the second inner channel 444 can be in communication with one end of each second outer outlet channel 4432 in turn, and the other end of the second inner channel 444 remains in communication with one end of the second outer inlet channel 4431. Based on this, a structure of one inlet port corresponding to multiple outlet ports is formed, and the structure is simple and convenient to switch.

[0059] Preferably, the second inner mounting disc 441 and the second outer mounting disc 442 are relatively rotated by a servo motor, for example, the servo motor drives the second inner mounting disc 441 to rotate.

[0060] Preferably, the second inner channel 444 is a hose, one end of which is in communication with the second outer inlet channel 4131 and is fixed in position, and the other end can rotate to change the orientation with the second inner mounting disc 441 to be in communication with different second outer outlet channels 4132.

[0061] Preferably, the end of the second outer outlet channel 4132 in communication with the second inner channel 444 is elastically abutted and sealed;

[0062] Preferably, the second outer inlet channel 4431 and the second outer outlet channel 4432 are both rigid pipes.

[0063] In some preferred embodiments, the control unit 16 can also control a mechanical device such as a mechanical arm to transfer the first liquid scintillation vial 29 to the liquid scintillation counter for measurement when the measurement condition of the Fe-55 sample in the first liquid scintillation vial 29 is met after one round of automated sample preparation, and then take it out after the measurement is completed and obtain the result, generate a log and record.

[0064] In some preferred embodiments, various problems that may occur in mechanical design, such as component acid resistance, resin treatment degree, cross-contamination prevention, etc., can be solved by using polytetrafluoroethylene pipelines, sample collection vials, etc. to achieve the purpose of automatic pretreatment-sample preparation-analysis-recording in the embodiments of the present disclosure. The sample preparation and analysis efficiency can be improved, the manual operation steps can be reduced, the labor cost can be reduced, and the raw materials can be saved.

[0065] The device of the present application can realize the processing flow of automatic pretreatment-sample preparation-analysis-recording, accurately control the liquid volume by positive pressure sampling, avoid cross-contamination by independent valves, control the on-off of the injection pump by the control device 5 to realize the quantitative addition of reagents and the control of the flow rate through the column, and all operations are controlled on the liquid crystal screen of the control device 5.

[0066] Example 2

[0067] The present embodiment provides an automatic combined sample preparation method for Fe-55 and Ni-63, comprising the following steps:

[0068] S1. Inject the sample to be treated into the pretreatment device 1, and then adjust the pH value to less than 2, preferably by concentrated nitric acid; then inject the Fe-55 carrier, the Ni-63 carrier and the counter carrier Co, Zn, Cs carrier, stir uniformly, evaporate and concentrate to near dryness, and then inject the constant volume reagent by the liquid transfer device 4 to obtain the first sample to be treated;

[0069] Specifically, the amount of the sample to be treated injected is 20ml-1L;

[0070] Preferably, considering that the carrying capacity of the resin is limited in the subsequent treatment process, the weight of each carrier also has corresponding requirements, the Fe-55 carrier and the Ni-63 carrier are each 5mg, and the counter carrier Co, Zn, Cs carrier is each 1mg,

[0071] Preferably, the constant volume reagent is 7mol / L hydrochloric acid, and the injection amount is 15mL;

[0072] Further preferably, the constant volume reagent can be injected at a first preset flow rate, and the first preset flow rate can be 0.5mL / min, 0.4mL / min, etc.

[0073] Specifically, at the beginning of the process, the control device 5 controls the first conveying device 11 to feed the sample to be treated, and sequentially adds the iron-55 carrier, the nickel-63 carrier and the counter carrier into the first container 12, and then stirs them uniformly. The control device 5 controls the first heater 13 to work, and heats the first container 12 to evaporate the liquid in the first container 12 to near dryness. Then, the control device 5 controls the liquid transfer device 4 to inject the hydrochloric acid solution of the first concentration into the first container 12 to obtain the first sample to be treated.

[0074] S2. The first sample to be treated is introduced into the first separation device 2 to obtain the first effluent. Then, the liquid transfer device 4 injects the first elution reagent into the first separation device 2 to obtain the first eluate. Then, the liquid transfer device 4 injects the first desorption reagent into the first separation device 2 to obtain the first desorption liquid. The first desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected into the first desorption liquid by the liquid transfer device 4 to obtain the sample rich in iron;

[0075] Preferably, the first elution reagent is 30 mL of 4 mol / L hydrochloric acid.

[0076] Preferably, the first desorption reagent is 40 mL of 0.1 mol / L hydrochloric acid.

[0077] Preferably, the constant volume reagent is 0.1 mol / L hydrochloric acid, and the specific injection amount can be determined according to the actual situation.

[0078] Preferably, the first desorption reagent can be performed at a second preset flow rate, which can also be set according to the actual situation, and is controlled by the control device 5. Preferably, the second preset flow rate is 0.5 mL / min, which is conducive to improving the adsorption and desorption effect and improving the overall recovery rate.

[0079] S3. The first separation device 2 evaporates the first effluent to near dryness, and then adds a dissolution reagent into the first effluent by the liquid transfer device 4, stirs them uniformly, and adds a pH adjusting reagent to pH=9 to obtain the treated first effluent.

[0080] Preferably, the dissolution reagent is 1 mol / L hydrochloric acid, and the specific injection amount can be determined according to the actual situation.

[0081] Preferably, the pH adjusting reagent includes 1 mol / L citric acid amine (C6H 17 N3O7) and ammonia water (NH4OH).

[0082] Specifically, the first separation device 2 works as follows: the control device 5 controls the liquid transfer device 4 to transfer the first sample to be treated in the pretreatment device 1 to the first separation column 21, the first multi-way valve 22 opens the outlet corresponding to the second container 23, so that the first effluent enters the second container 23; the control device 5 controls the liquid transfer device 4 to inject the first elution reagent into the first separation column 21, the first multi-way valve 22 opens the outlet corresponding to the first waste liquid bottle 210, so that the first eluate flows into the first waste liquid bottle 210 for collection; the control device 5 controls the liquid transfer device 4 to inject the first desorption reagent into the first separation column 21, the first multi-way valve 22 opens the opening corresponding to the third container 25, so that the first desorption liquid flows into the third container 25; the control device 5 controls the third heater 26 to start heating, evaporating the liquid in the third container 25 to near dryness, and then stops heating, and then the control device 5 controls the liquid transfer device 4 to inject a constant volume reagent into the third container 25 to obtain a liquid sample of iron-55; the third transfer device 28 is controlled to transfer to the first liquid scintillation bottle 29; the control device 5 controls the second heater 24 to work, evaporating the first effluent in the second container 23 to near dryness, and then the liquid transfer device 4 injects a dissolving reagent into the second container 23, and after stirring uniformly, the control device 5 controls the second transfer device 27 to inject a pH adjusting reagent into the second container 23 to obtain the treated first effluent.

[0083] S4. The first effluent is introduced into the second separation device 3 to obtain a second effluent, then a second elution reagent is injected into the second separation device 3 through the liquid transfer device 4 to obtain a second eluate, and then a second desorption reagent is injected into the second separation device 3 to obtain a second desorption liquid; the second desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected to obtain a sample rich in nickel.

[0084] Preferably, the second elution reagent is citric acid amine with pH = 9.

[0085] Preferably, the second desorption reagent is 3 mol / L nitric acid, and the amount of addition can be 30 mL.

[0086] Preferably, the constant volume reagent is 0.1 mol / L hydrochloric acid, and the specific injection amount can be determined according to the actual situation.

[0087] Specifically, the second separation device 3 works as follows: the control device 5 controls the fourth conveying device 31 to convey the first effluent obtained by the first separation device 2 to the second separation column 32, and separates through the second separation column 32, at the same time, the second multi-way valve 33 is switched to the outlet communicating with the second waste liquid bottle 36, and the second effluent is conveyed to the second waste liquid bottle 36, then the control device 5 controls the liquid injection device 4 to inject the second elution reagent into the second separation column 32, and the obtained second elution liquid is conveyed to the second waste liquid bottle 36; then the second multi-way valve 33 is switched to the outlet communicating with the fourth container 34, then the control device 5 controls the liquid injection device 4 to inject the second desorption reagent into the second separation column 32, and the obtained second desorption liquid is conveyed to the fourth container 34, the control device 5 controls the fourth heater 35 to heat the fourth container 34 to near dryness of the second desorption liquid, then the liquid injection device 4 injects a constant volume reagent into the fourth container 34, and the liquid sample of nickel-63 is obtained.

[0088] The automatic combined sample preparation method of iron-55 and nickel-63 can realize the pretreatment, sample preparation and analysis of iron-55 and nickel-63 in the whole process, can reduce the manual operation process, reduce the labor cost, improve the processing efficiency, and can save raw materials and improve the processing efficiency.

[0089] Experimental example

[0090] The 50 mL wastewater sample is separated and purified by using the device, and the obtained sample is measured by using a low-level liquid scintillation spectrometer, and the measurement results of iron-55 and nickel-63 in the sample are 0.25 Bq / L and 1.27 Bq / L. The sample preparation method and device can be well used for sample measurement.

[0091] The embodiments of the present application are described above in combination with the drawings, but the present application is not limited to the above specific embodiments, and the above specific embodiments are only illustrative but not limiting, and those skilled in the art can make many forms under the inspiration of the present application without departing from the purpose of the present application and the scope protected by the claims, which all belong to the protection of the present application.

Claims

1. An automated combined sample preparation device for iron-55 and nickel-63, characterized in that, The application relates to a sample pretreatment and separation device and a control method thereof. The device comprises a pretreatment device, a first separation device, a second separation device, a liquid injection device and a control device. The pretreatment device is used for concentrating and constant-volume processing of a sample to be processed to obtain a first sample to be processed. The liquid injection device is used for transporting the first sample to be processed in the pretreatment device to the first separation device and transporting liquid reagents to the pretreatment device, the first separation device and the second separation device, wherein the liquid reagents at least include a dissolving reagent, a first elution reagent, a first desorption reagent, a second elution reagent, a pH adjusting reagent, a second desorption reagent and a constant-volume reagent. The first separation device is used for separating the first sample to be processed into a first effluent, a first elution liquid and a first desorption liquid, and performing pH adjustment processing on the first effluent after concentration; and the first separation device is also used for processing the first desorption liquid into a first sample. The second separation device is used for separating the first effluent after processing to obtain a second effluent, a second elution liquid and a second desorption liquid, and processing the second desorption liquid into a second sample. The control device is electrically connected to the pretreatment device, the first separation device, the second separation device and the liquid injection device respectively.

2. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 1, characterized in that The pretreatment device comprises a first conveying device, a first container and a first heater. The discharge port of the first conveying device is communicated with the feeding port of the first container, and the first conveying device is electrically connected to the control device. The discharge port of the first container is communicated with the feeding port of the liquid injection device, and the feeding port is communicated with the discharge port of the liquid injection device. The first heater is used for heating the first container and is electrically connected to the control device.

3. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 1, characterized in that The first separation device comprises a first separation column, a first multi-way valve, a second container, a second heater, a third container, a third heater and a second conveying device. The feeding port of the first separation column is communicated with the discharge port of the liquid injection device, and the discharge port is communicated with the feeding port of the first multi-way valve. The first multi-way valve comprises a plurality of discharge ports, which are respectively communicated with the feeding ports of the second container and the third container. The feeding port of the second container is communicated with the discharge port of the second conveying device, the discharge port is communicated with the feeding port of the second separation device, and the feeding port of the second container is communicated with the discharge port of the liquid injection device. The feeding port of the third container is communicated with the discharge port of the liquid injection device. The second heater is used for heating the second container. The third heater is used for heating the third container. The control device is electrically connected to the first multi-way valve, the second heater, the third heater and the second conveying device.

4. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 3, characterized in that The first separation device further comprises a third conveying device and a first liquid scintillation vial. The third conveying device is used for transporting liquid in the third container to the first liquid scintillation vial. The control device is electrically connected to the third conveying device.

5. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 3, characterized in that The first separation device further comprises a first waste liquid vial. The feeding port of the first waste liquid vial is communicated with the discharge port of the first multi-way valve.

6. The automated combined sample preparation device for iron-55 and nickel-63 of claim 1, wherein, The second separation device comprises a fourth conveying device, a second separation column, a second multi-way valve, a fourth container, a fourth heater and a second waste liquid bottle; The feeding port of the fourth conveying device is communicated with the first separation device, and the discharging port is communicated with the feeding port of the second separation column; The discharging port of the second separation column is communicated with the feeding port of the second multi-way valve; The second multi-way valve has a plurality of discharging ports, which are respectively communicated with the feeding ports of the fourth container and the second waste liquid bottle; The feeding port of the fourth container is communicated with the discharging port of the liquid transfer device; The fourth heater is used for heating the fourth container; The control device is electrically connected with the fourth conveying device, the second multi-way valve and the fourth heater.

7. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 6, characterized in that The second separation device further comprises a fifth conveying device and a second liquid scintillation bottle; The fifth conveying device is used for conveying the liquid in the fourth container to the second liquid scintillation bottle; and the control device is electrically connected with the fifth conveying device.

8. The automated combined sample preparation device for iron-55 and nickel-63 of claim 1, wherein, The liquid transfer device comprises a first multi-interface communicator, a communicating pipe, a conveying pump and a second multi-interface communicator; The first multi-interface communicator has a plurality of first feeding ports and a first discharging port; the first discharging port can be selectively communicated with one of the first feeding ports; Each of the first feeding ports is used for communicating with different external liquid reagents; The second multi-interface communicator has a second feeding port and a plurality of second discharging ports; the second feeding port can be selectively communicated with one of the second discharging ports; Each of the second discharging ports is used for being communicated with the pretreatment device, the first separation device and the second separation device; One end of the communicating pipe is communicated with the first discharging port, and the other end is communicated with the second feeding port; The conveying pump is arranged in the communicating pipe and is used for conveying materials from the first multi-interface communicator to the second multi-interface communicator.

9. The automated combined sample preparation device for iron-55 and nickel-63 according to claim 8, characterized in that The first multi-interface communicator comprises a first inner mounting disc and a first outer mounting disc; The first outer mounting disc is arranged around the outer periphery of the first inner mounting disc and has a plurality of first outer channels; The first inner mounting disc has a first inner channel; One of the plurality of first outer channels is a first outer discharging channel, and the others are first outer feeding channels; Each first outer feeding channel has one end arranged close to the outer periphery of the first outer mounting disc to form a plurality of first feeding ports, and the other end is used for being butted and communicated with one end of the first inner channel; The other end of the first inner channel is communicated with one end of the first outer discharging channel; The other end of the first outer discharging channel forms the first discharging port; The first outer mounting disc and the first inner mounting disc can be rotated relative to each other, so that one end of the first inner channel can be butted and communicated with each first outer feeding channel one by one, and the other end of the first inner channel remains butted and communicated with the first outer discharging channel; Alternatively, The second multi-interface communicator comprises a second inner mounting disc and a second outer mounting disc; The second outer mounting disc is arranged around the outer periphery of the second inner mounting disc and has a plurality of second outer channels; The second inner mounting disc has a second inner channel; One of the second outer channels is a second outer feeding channel, and the rest are second outer discharging channels; Each second outer discharging channel is arranged near the outer periphery of the second outer mounting disc, and forms a plurality of second discharging ports at one end, and is used for being connected with one end of the second inner channel at the other end; The other end of the second inner channel is connected with one end of the second outer discharging channel; The other end of the second outer feeding channel forms the second feeding port; The second outer mounting disc and the second inner mounting disc can rotate relative to each other, so that one end of the second inner channel can be connected with one end of each second outer discharging channel in sequence, and the other end of the second inner channel is kept connected with one end of the second outer feeding channel.

10. An automated combined sample preparation method for iron-55 and nickel-63, characterized in that, The method comprises the following steps: A pretreatment device is injected with a sample to be treated, and then the pH value is adjusted to less than 2, and then an iron-55 carrier, a nickel-63 carrier and a counter carrier are injected, stirred uniformly, evaporated and concentrated to near dryness, and then a hydrochloric acid solution of a first concentration is injected through a liquid injection device to obtain a first sample to be treated; The first sample to be treated is introduced into a first separation device to obtain a first effluent, and then a first elution reagent is injected into the first separation device through a liquid injection device to obtain a first elution liquid; then, a first desorption reagent is injected into the first separation device through the liquid injection device to obtain a first desorption liquid, the first desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected into the first desorption liquid through the liquid injection device to obtain a first sample rich in iron-55; The first separation device evaporates the first effluent to near dryness, and then adds a dissolving reagent into the first effluent through the liquid injection device, stirs uniformly, and adds a pH adjusting reagent to obtain an adjusted first effluent with a pH value of 9; The first effluent is introduced into a second separation device to obtain a second effluent, and then a second elution reagent is injected into the second separation device through the liquid injection device to obtain a second elution liquid, and then a second desorption reagent is injected into the second separation device to obtain a second desorption liquid; the second desorption liquid is evaporated to near dryness, and then a constant volume reagent is injected to obtain a second sample rich in nickel-63.

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