CN113390702A - Radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device - Google Patents

Radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device Download PDF

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CN113390702A
CN113390702A CN202110603186.XA CN202110603186A CN113390702A CN 113390702 A CN113390702 A CN 113390702A CN 202110603186 A CN202110603186 A CN 202110603186A CN 113390702 A CN113390702 A CN 113390702A
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extraction
liquid
collected liquid
activity measurement
module
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CN113390702B (en
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陆地
胡建文
杜瑶芳
王伟
尚迪
张晓影
邓宛梅
王海涛
胡克
赵钰玲
赵克明
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Beijing Labtech Instruments Co ltd
Yantai Customs Technical Center
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Beijing Labtech Instruments Co ltd
Yantai Customs Technical Center
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/405Concentrating samples by adsorption or absorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16Measuring radiation intensity
    • G01T1/167Measuring radioactive content of objects, e.g. contamination
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16Measuring radiation intensity
    • G01T1/18Measuring radiation intensity with counting-tube arrangements, e.g. with Geiger counters
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01TMEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16Measuring radiation intensity
    • G01T1/20Measuring radiation intensity with scintillation detectors
    • G01T1/204Measuring radiation intensity with scintillation detectors the detector being a liquid
    • G01T1/2042Composition for liquid scintillation systems
    • G01T1/2047Sample preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • General Health & Medical Sciences (AREA)
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  • Analytical Chemistry (AREA)
  • Immunology (AREA)
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  • High Energy & Nuclear Physics (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides a radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device which comprises a mobile mechanical arm, a shifting column, an extraction device, a pipettor, a sample loading module, a collection module, a collected liquid transverse conveying module, a concentration drying device and an activity measurement device, wherein an extraction column support of the extraction device can transversely slide along a sliding guide assembly under the driving of the shifting column. The radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device can automatically and sequentially complete the solid-phase extraction, sample preparation and activity measurement of radioactive strontium, solves the problem that the radioactive strontium solid-phase extraction, sample preparation and activity measurement need to be respectively carried out in independent instruments in the prior art, avoids the accident that sample pollution and loss are possibly caused in the sample transfer process, greatly improves the sample pretreatment efficiency, is simple to operate, can improve the working efficiency and the experimental precision, and reduces the labor intensity of experimenters.

Description

Radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device
Technical Field
The invention belongs to a sample pretreatment and analysis technology, and particularly relates to a measuring device integrating radioactive strontium solid-phase extraction, sample preparation and activity measurement functions.
Background
Solid phase extraction is a common sample pretreatment technology, and is to pass a sample solution through an ion exchange column or an extraction column, and purify and separate a sample by utilizing the distribution effect of a separated substance between a liquid phase and a solid phase, so as to realize the separation and purification of an element to be detected and other elements in the sample. The technology is widely applied in the fields of biology, food, medicine, environment, nuclide and the like.
In the analysis of radionuclide strontium, a sample solution is usually extracted, then the collected extract is concentrated and dried to prepare a sample, and finally the dried sample is fixed on a measurement tray of a low background beta measurement device to perform strontium activity (namely the activity of strontium) measurement and analysis.
In the prior art, because the research and development and the use of equipment for radioactive strontium separation and analysis are less, the extraction, sample preparation and activity measurement of radioactive strontium are mainly and respectively operated in independent instruments, and no integrated and automatic equipment capable of realizing the rapid separation, sample preparation, detection and analysis of the radioactive strontium in the whole process exists in the market. The extraction steps are complicated, the flow is long, and a large amount of analysis time is occupied; meanwhile, when the extract is concentrated, the extract is heated and concentrated through a water bath or an oil bath and dried in an electric heating plate, the heating time is long, and the extract is easy to lose in the transfer process; the dried sample needs to be additionally transferred to a measuring tray of a low background beta measuring device for strontium activity measurement and analysis; the whole process needs manual operation, the requirements on the operation capacity and the energy of experimenters are high, and sample pollution and loss accidents can be caused in the sample transfer process.
Therefore, it is necessary to develop an integrated device for solid-phase extraction, sample preparation and activity measurement of radioactive strontium, improve the working efficiency and experimental precision of radioactive strontium treatment and measurement, and reduce the labor intensity of experimenters.
Disclosure of Invention
The invention provides an integrated device for radioactive strontium solid-phase extraction, sample preparation and activity measurement, which can solve the problems of low working efficiency, low experimental precision and high labor intensity of experimenters caused by the fact that the radioactive strontium solid-phase extraction, the sample preparation and the activity measurement are respectively operated in independent instruments in the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that the radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device comprises:
the mobile mechanical arm comprises a transverse moving module and a vertical moving module, wherein the vertical moving module is arranged on the transverse moving module and can move transversely along with the transverse moving module;
the shifting column is arranged on the vertical moving module;
the extraction device comprises an extraction column, an extraction column bracket and a sliding guide assembly, wherein the extraction column is arranged on the extraction column bracket, and the extraction column bracket can transversely slide along the sliding guide assembly under the driving of the toggle column;
the pipettor is arranged on the vertical moving module;
the sample loading module comprises a sample container for containing a sample to be tested;
a collection module comprising a collection fluid container for collecting collection fluid output by the extraction column when the extraction column is slid to a collection position;
the collected liquid transverse conveying module comprises a transverse moving part, a collected liquid conveying part and an electric driving part, wherein the collected liquid conveying part is fixedly connected with the transverse moving part into a whole, the electric driving part is used for driving the transverse moving part to transversely move, a collected liquid containing part is arranged on the collected liquid conveying part, and the collected liquid conveying part can move to the collected liquid containing part at least to be located at a collected liquid adding position and a collected liquid concentrating and drying position under the driving of the transverse moving part;
a concentrated drying device arranged at the collected liquid concentrated drying position and used for concentrating and drying the collected liquid when the collected liquid accommodating part added with the collected liquid moves to the collected liquid concentrated drying position;
and the activity measuring device is used for measuring the activity of the sample formed after concentration and drying.
The collection liquid lateral transportation module is located extraction device reaches concentrated drying device's below, and it still includes the casing, lateral shifting part reaches electric drive part all establishes in the casing, be formed with on the roof of casing with the liquid feeding that the liquid feeding position corresponds dodge the hole and with the concentrated stoving that the concentrated stoving position corresponds dodges the hole, concentrated drying device is located the top in hole is dodged in concentrated stoving.
The extraction device is located one side of the concentration drying device, the concentration drying device comprises an evaporation lamp and a lampshade covering the evaporation lamp on the periphery, and a heat insulation plate is surrounded on the inner side of a circumferential side plate of the lampshade.
A heat dissipation hole is formed in the top plate of the lampshade.
Under the drive of the transverse moving component, the collected liquid accommodating part can also move to a measuring position, the measuring position is positioned in the activity measuring device, and an avoiding space for avoiding the transverse movement of the collected liquid conveying component is formed on a shell of the activity measuring device.
The integrated device further comprises:
the automatic liquid adding device comprises an injection pump, a corrosion-resistant three-way electromagnetic valve, a multi-connection electromagnetic valve, a buffer tube, a buffer reagent container for containing buffer reagents and a plurality of extraction reagent containers for containing the extraction reagents respectively, wherein the output end of the injection pump is connected with a first interface of the corrosion-resistant three-way electromagnetic valve, a second interface of the corrosion-resistant three-way electromagnetic valve is connected with a buffer reagent pipeline inserted into the buffer reagent container, a third interface of the corrosion-resistant three-way electromagnetic valve is connected with an interface at one end of the buffer tube, an interface at the other end of the buffer tube is connected with an input interface of the multi-connection electromagnetic valve, an output interface of the multi-connection electromagnetic valve is connected with a liquid transfer device, and the extraction reagent containers are connected with different interfaces of the multi-connection electromagnetic valve through extraction reagent pipelines respectively.
Each extraction reagent container and each buffer reagent container are provided with a cover body, a buffer reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of each buffer reagent container, the buffer reagent pipeline is inserted into the buffer reagent container through the buffer reagent pipeline insertion opening, an extraction reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of each extraction reagent container, the extraction reagent pipeline is inserted into the extraction reagent container through the extraction reagent pipeline insertion opening, a gas inlet pipeline is inserted into each gas pipeline insertion opening, and an electromagnetic valve is arranged on each gas inlet pipeline.
The integrated device further comprises:
the cleaning module is at least used for cleaning the pipettor, and a plurality of cleaning grooves are arranged on the cleaning module and are arranged along the transverse direction.
The integrated device further comprises:
and the waste liquid tank is used for collecting the waste liquid output by the extraction column when the extraction column slides to a waste liquid collecting position, the waste liquid tank and the collecting module are transversely arranged, and a liquid inlet of the waste liquid tank is communicated with a liquid outlet of the cleaning tank through a pipeline.
The integrated device further comprises an air exhaust device.
Compared with the prior art, the invention has the following advantages and positive effects: the radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device can complete the solid-phase extraction, sample preparation and activity measurement of radioactive strontium in sequence, solves the problem that the radioactive strontium solid-phase extraction, sample preparation and activity measurement need to be carried out in independent instruments in the prior art, avoids the accidents of sample pollution and loss possibly caused in the sample transfer process, greatly improves the sample pretreatment efficiency, is simple to operate, can improve the working efficiency and the experimental precision, and reduces the labor intensity of experimenters.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a front perspective view of an integrated radioactive strontium solid-phase extraction, sample preparation and activity measurement apparatus according to an embodiment of the present invention;
FIG. 2 is an enlarged view of portion A of FIG. 1;
fig. 3 is a front perspective view of the integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement without the front side plate of the outer body according to the embodiment of the present invention;
fig. 4 is a rear perspective view of an integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to an embodiment of the present invention;
FIG. 5 is a schematic view of an embodiment of an extraction rack according to the present invention;
fig. 6 is a front perspective view of the integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement in the embodiment of the present invention without a concentrating and drying apparatus;
FIG. 7 is a perspective view of the collected liquid lateral transfer device of the embodiment of the present invention with a portion of the housing omitted;
FIG. 8 is a perspective view of the concentrating and drying apparatus according to the embodiment of the present invention;
FIG. 9 is a sectional view of the concentrating and drying apparatus according to an embodiment of the present invention;
FIG. 10 is a perspective view of a collection fluid delivery assembly in an embodiment of the present invention;
FIG. 11 is a perspective view of the assembly of the collecting liquid conveying member and the activity measuring device (without the housing) according to the embodiment of the present invention;
FIG. 12 is a schematic diagram of the structure of an automatic liquid adding device in the embodiment of the present invention;
FIG. 13 is a perspective view of a cleaning module in an embodiment of the invention.
Reference numerals: 100. moving the mechanical arm; 110. a transverse moving module; 120. a vertical moving module; 200. shifting the column; 300. an extraction device; 310. an extraction column; 320. an extraction column support; 330. a sliding guide assembly; 331. supporting the side plates; 332. a slide rod; 400. a pipettor; 410. a bubble sensor; 500. a sample loading module; 510. a sample container; 520. a sample container holder; 600. a collection module; 610. a collection liquid container; 620. a collection fluid container support; 700. a collecting liquid transverse conveying module; 710. a lateral moving member; 720. a collected liquid conveying member; 721. a collected liquid accommodating portion; 730. a housing; 731. liquid adding avoiding holes; 732. concentrating, drying and avoiding holes; 740. a photoelectric switch; 800. a concentration drying device; 810. an evaporation lamp; 820. a lamp shade; 821. heat dissipation holes; 822. a through hole; 830. a heat insulating plate; 900. an activity measuring device; 1000. an automatic liquid adding device; 1010. an injection pump; 1020. a corrosion-resistant three-way electromagnetic valve; 1030. a concatemer solenoid valve; 1040. a buffer tube; 1050. a buffer reagent container; 1060. a buffer reagent line; 1070 an extraction reagent line; 1080. an air intake line; 1090. an electromagnetic valve; 1100. a cleaning module; 1110. a cleaning tank; 1200. a waste liquid tank; 1300. a peristaltic pump; 1400. an air exhaust device; 1500. an argon bottle; 1600. a flow meter; 1700. a housing.
Detailed Description
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Referring to fig. 1 to 7, the integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement in this embodiment includes a mobile robot arm 100, a toggle column 200, an extraction apparatus 300, a pipette 400, a sample loading module 500, a collection module 600, a transverse collection liquid conveying module 700, a concentration drying apparatus 800 and an activity measurement apparatus 900, and further includes a housing 1700, where at least the mobile robot arm 100, the toggle column 200, the extraction apparatus 300, the pipette 400, the sample loading module 500, the collection module 600, the transverse collection liquid conveying module 700 and the concentration drying apparatus 800 are disposed in the housing 1700.
As shown in fig. 1 and 3, the mobile robot 100 includes a transverse moving module 110 and a vertical moving module 120, the vertical moving module 120 is disposed on the transverse moving module 110, and is particularly disposed on a transverse moving component of the transverse moving module 110, so that the vertical moving module 120 can move transversely with the transverse moving module 110 (particularly with the transverse moving component of the transverse moving module 110), and the mobile robot 100 can be an existing two-axis moving module.
As shown in fig. 1 and 2, the toggle column 200 is disposed on the vertical moving module 120, and particularly on the vertical moving component of the vertical moving module 120, so as to be vertically movable along with the vertical moving component of the vertical moving module 120, and meanwhile, since the vertical moving module 120 as a whole can be horizontally movable along with the horizontal moving component of the horizontal moving module 110, the toggle column 200 can be both horizontally movable and vertically movable; the number of the toggle columns 200 is two in this embodiment, and the toggle columns are arranged at intervals along the longitudinal direction, specifically, are vertically arranged in a short shaft shape, and are inserted into the vertically movable component of the vertically movable module 120 in an inserting manner.
As shown in fig. 1, fig. 2 and fig. 5, the extraction apparatus 300 comprises an extraction column 310, an extraction column holder 320 and a sliding guide assembly 330, wherein the extraction column 310 is disposed on the extraction column holder 320, and the extraction column holder 320 can slide along the sliding guide assembly 330 in the transverse direction under the driving of the toggle column 200; the sliding guide assembly 330 specifically includes two supporting side plates 331 disposed opposite to each other and two sliding rods 332 located at top ends of the supporting side plates 331, the sliding rods 332 are cylindrical rods disposed horizontally, the two sliding rods 332 are disposed in parallel along a longitudinal direction, the extraction column bracket 320 is T-shaped and supported on the two sliding rods 332, the extraction column 310 is an existing extraction column, a vertical accommodating hole is formed in the extraction column bracket 320, and the extraction column 310 is placed in the accommodating hole. When the moving arm 100 moves the column 200 to the position of the column holder 320, it can move the column holder 320 to slide along the slide rod 332, so as to change the position of the column 310.
As shown in fig. 1 and 2, the pipetter 400 is also disposed on the vertical movement module, specifically, on the vertical movement component of the vertical movement module 120, so as to be vertically movable with the vertical movement component of the vertical movement module 120, and meanwhile, since the vertical movement module 120 as a whole can be horizontally movable with the horizontal movement component of the horizontal movement module 110, the pipetter 400 can be moved both horizontally and vertically; the pipette 400 is used at least to add a sample to be tested or an extraction reagent to the extraction column 310 and to transfer a collected liquid after extraction.
As shown in fig. 1 and 2, the loading module 500 includes a sample container 510, which in this embodiment further includes a sample container holder 520, the sample container 510 is used for holding a sample to be tested, and the sample container holder 520 is used for supporting and placing the sample container 510.
As shown in fig. 1 and 2, the collection module 600 includes a collection liquid container 610, and in this embodiment, a collection liquid container support 620, wherein the collection liquid container 610 is used for collecting the collection liquid output by the extraction column 310, i.e., the solution in which the strontium obtained by leaching is dissolved, when the extraction column 310 slides to the collection position, and the collection liquid container support 620 is used for supporting and placing the collection liquid container 610.
As shown in fig. 1, 3, 6, 7 and 10, the collected liquid transverse conveying module 700 includes a transverse moving component 710, a collected liquid conveying component 720 fixedly connected with the transverse moving component 710 into a whole, and an electric driving component (not shown) for driving the transverse moving component 710 to transversely move, a collected liquid accommodating portion 721 is disposed on the collected liquid conveying component 720, and the collected liquid conveying component 720 is driven by the transverse moving component 710 to move at least to the collected liquid accommodating portion 721 to be at a collected liquid charging position and a collected liquid concentrating and drying position. The collected liquid containing part 721 is used for containing the collected liquid to be concentrated and dried, and is specifically a groove structure, and the collected liquid can be directly placed in the groove structure, or a tray is placed in the groove structure, and the collected liquid is placed in the tray, and the collected liquid is usually 3 mL. When the collected liquid containing portion 721 is located at the collected liquid adding position, the liquid transferring device 400 is driven by the moving mechanical arm 100 to move to the position of the collected liquid container 610, the collected liquid in the collected liquid container 610 is sucked and then moved to the collected liquid adding position of the collected liquid containing portion 721, the collected liquid is added into the collected liquid containing portion 721, and then the collected liquid conveying component 720 is driven by the transverse moving component 710 to move to the collected liquid concentrating and drying position for concentrating, drying and sample preparation, i.e. sample preparation.
And a concentration drying device 800 provided at the collected liquid concentration drying position for concentrating and drying the collected liquid when the collected liquid containing part 721 to which the collected liquid is added moves to the collected liquid concentration drying position.
Activity measuring device 900 for carry out the activity measurement to the sample that forms after the concentration is dried, its activity measuring device such as specifically can select for use low background beta measuring device, liquid scintillation measuring device or Cerenkov count measuring device, it is low background beta measuring device in this embodiment, uses with flowmeter 1600 in the cooperation argon gas cylinder 1500, and argon gas cylinder 1500 passes through the gas cylinder solid fixed ring to be fixed in the curb plate outside of shell 1700.
When the radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device of this embodiment is used for pretreatment of a sample to be tested containing radioactive strontium, firstly, the pipettor 400 first sucks leacheate (ethanol) and adds the leacheate into the extraction column 310, the extraction column 310 is subjected to activation pretreatment, then the sample to be tested and a reagent for extraction are sequentially sucked and added into the extraction column 310 for solid-phase extraction, waste liquid formed by extraction is discharged from the extraction column 310, the extracted radioactive strontium is adsorbed on a resin material in the extraction column 310, then the pipettor 400 sucks eluent and adds the eluent into the extraction column 310 to dissolve the radioactive strontium adsorbed on the resin material in the extraction column 310, so that collection liquid is formed, and the collection liquid is output to the collection liquid container 610 of the collection module 600 through the extraction column 310; then, the liquid transfer device 400 sucks the collected liquid in the collected liquid container 610 and then moves to the collected liquid adding position where the collected liquid accommodating portion 721 is located, the collected liquid is added into the collected liquid accommodating portion 721, then the collected liquid conveying component 720 is driven by the transverse moving component 710 to move to the collected liquid concentration drying position for concentration, drying and sample preparation, namely sample preparation, and the prepared sample is transferred to the activity measuring device 900 for activity measurement and analysis. The position change of the pipettor 400 is realized by the driving of the mobile mechanical arm 100, similarly, the position change of the extraction column 310 is realized by the driving of the mobile mechanical arm 100 and the movement of the toggle column 200, and the position change of the collected liquid conveying part 720 is realized by the collected liquid transverse conveying module 700.
Further, the collected liquid transverse conveying module 700 is located below the extraction device 300 and the concentration and drying device 800, so that when the collected liquid accommodating portion 721 is driven by the transverse moving component 710 to move to the lower portion of the extraction column 310, the collected liquid in the extraction column 310 can directly flow into the collected liquid accommodating portion 721 under the action of gravity, and meanwhile, the collected liquid accommodating portion 721 can also be driven by the transverse moving component 710 to move to the lower portion of the concentration and drying device 800, and concentration and drying are performed by the concentration and drying device 800. The collecting liquid transverse conveying module 700 is positioned below the extraction device 300 and the concentration drying device 800, so that the structure is compact, and the occupied space is saved. The transverse collected liquid conveying module 700 in this embodiment further includes a housing 730, the transverse moving component 710 and the electric driving component are both disposed inside the housing 730, a liquid adding avoiding hole 731 corresponding to the liquid adding position and a concentrated drying avoiding hole 732 corresponding to the concentrated drying position are formed on a top plate of the housing 730, and the concentrated drying device 800 is located above the concentrated drying avoiding hole 732. Thus, the collected liquid in the extraction column 310 falls into the collected liquid accommodating part 721 through the liquid adding avoiding hole 731 under the action of gravity, and then when the collected liquid accommodating part 721 is driven by the transverse moving part 710 to move to the lower part of the concentrating and drying device 800, the heat generated by the concentrating and drying device 800 concentrates and dries the collected liquid in the collected liquid accommodating part 721 through the concentrating and drying avoiding hole 732.
As shown in fig. 7, a photoelectric switch 740 is further disposed in the collecting liquid transverse conveying module 700 to detect the position of the collecting liquid container 721 moving to the liquid adding position and the concentrated drying position, when the photoelectric switch 740 detects that the collecting liquid container 721 moves to the liquid adding position, the collecting liquid transverse conveying module 700 stops working, the extraction column 310 is driven by the toggle column 200 to move to the liquid adding position to add liquid into the collecting liquid container 721, after the liquid adding is completed, the collecting liquid transverse conveying module 700 continues working, so that when the collecting liquid container 721 moves to the concentrated drying position, the collecting liquid transverse conveying module 700 stops working, and the concentrated drying device 800 concentrates and dries the collecting liquid in the collecting liquid container 721.
Preferably, referring to fig. 8 and 9 in conjunction with fig. 1 to 3 and 5, the extraction device 310 is located at one side of the concentrated drying device 800 to reduce the distance between the feeding position and the concentrated drying position, thereby further making the structure compact. The concentrating and drying device 800 includes an evaporation lamp 810 and a lamp cover 820 covering the periphery of the evaporation lamp 810, the inner side of the circumferential side plate of the lamp cover 820 is surrounded by a heat insulation plate 830, and a through hole 822 corresponding to the concentrating and drying avoiding hole 732 is formed on the bottom plate of the lamp cover 820. Specifically, the evaporation lamp 810 is an infrared quartz heating bulb, the filament is a thickened tungsten filament, high-purity negative-pressure nitrogen is filled in the lamp to prevent splashing, and a nano protective film is arranged on the surface of quartz glass, so that accurately controlled energy radiation can be provided, and the evaporation lamp has the advantages of explosion prevention, high heat conduction speed, good thermal stability, corrosion resistance and the like, and greatly improves the concentration and drying efficiency of a sample; the heat insulating plate 830 may be a vacuum formed alumina ceramic plate having excellent heat insulating property, and may prevent heat from being radiated around the evaporation lamp 810 to affect the column temperature of the extraction column 310 located at one side of the concentration drying apparatus 800.
Further, as shown in fig. 8, heat dissipation holes 821 are formed on the top plate of the lamp housing 820, the heat dissipation holes 821 are distributed at four corners of the top plate for dissipating the excessive heat, and a large heat dissipation space is disposed at the top of the lamp housing 820 for dissipating the heat quickly, and protecting the evaporation lamp 810, thereby prolonging the service life.
In order to further improve the automation degree of the integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement in this embodiment, improve the working efficiency, and reduce sample pollution and loss possibly caused by the sample transfer process, in this embodiment, under the driving of the lateral moving component 710, the collecting liquid accommodating portion 721 can also be moved to the measurement position, the measurement position is located in the activity measurement apparatus 900, and an avoiding space 910 for avoiding the lateral movement of the collecting liquid conveying component 720 is formed on the housing of the activity measurement apparatus 900. Specifically, as shown in fig. 1, 3 and 11, the activity measuring device 900 is disposed at one side of the concentration and drying device 800, and the extraction device 300, the concentration and drying device 800 and the activity measuring device 900 are disposed in the horizontal direction in sequence to accommodate the horizontal movement of the collected liquid conveying component 720. Like this the collecting fluid on collecting fluid container portion 721 carries out concentrated stoving system appearance after, can continue to drive by lateral shifting part 710 and remove to the measuring position in activity measuring device 900, carry out the activity measurement and analysis to the sample after the concentrated stoving by activity measuring device 900, then this embodiment has realized the solid phase extraction, the automatic transfer of sample between concentrated stoving system appearance and the three process of activity measurement, need not artifical the participation, the degree of automation of whole integrated device has been improved greatly, work efficiency, and effectively reduce sample pollution and the loss that the sample transfer process probably caused.
Also, in order to improve the automation degree and the working efficiency of the whole integrated device, the integrated device in this embodiment further comprises an automatic liquid adding device 1000. Referring to fig. 4 and 12, the automatic liquid adding apparatus 1000 includes an injection pump 1010, a corrosion-resistant three-way electromagnetic valve 1020, a multi-union electromagnetic valve 1030, a buffer tube 1040, a buffer reagent container 1050 for containing buffer reagents, and a plurality of extraction reagent containers (not shown) for containing respective extraction reagents, an output end of the injection pump 1010 is connected to a first interface of the corrosion-resistant three-way electromagnetic valve 1020, a second interface of the corrosion-resistant three-way electromagnetic valve 1020 is connected to a buffer reagent tube 1060 inserted into the buffer reagent container 1500, a third interface of the corrosion-resistant three-way electromagnetic valve 1020 is connected to an interface at one end of the buffer tube 1040, an interface at the other end of the buffer tube 1040 is connected to an input interface of the multi-union electromagnetic valve 1030, an output interface of the multi-union electromagnetic valve 1030 is connected to a pipette 400, and the respective extraction reagent containers are connected to different interfaces of the multi-union electromagnetic valve 1030 through extraction reagent tubes 1070. The buffer reagent is a non-corrosive reagent, the buffer reagent pipeline 1060, the extraction reagent pipeline 1070 and other related pipelines are made of anti-corrosion materials such as PTFE, and the injection pump 1010 is internally provided with a stepping motor and a control circuit board, so that the volume and the flow rate of the reagent can be accurately controlled.
When extracting reagents are added into the pipette 400, the third interface of the corrosion-resistant three-way electromagnetic valve 1020 is closed, the first interface and the second interface are opened, the piston rod of the injection pump 1010 is positioned at the foremost end (namely, the output end), the injection pump 1010 works, and the piston rod of the injection pump 1010 retreats, so that the buffer reagents in the buffer reagent container 1050 are sucked into the injection pump 1010; then the second interface of the corrosion-resistant three-way electromagnetic valve 1020 is closed, the first interface and the third interface are opened, the injection pump 1010 works, and the piston rod of the injection pump 1010 is pushed forwards, so that the buffer reagent in the injection pump 1010 is pushed into the buffer tube 1040; then the second interface of the corrosion-resistant three-way electromagnetic valve 1020 keeps a closed state, the piston rod of the injection pump 1010 retreats, the buffer reagent is sucked into the injection pump 1010 again, and simultaneously the solvent in one of the extraction reagent containers is sucked into the buffer tube 1040 through the extraction reagent pipeline 1070 and the corresponding interface of the concatemer electromagnetic valve 1030; the valve between the concatemer solenoid valve 1030 and the pipette 400 is opened, the valve between the concatemer solenoid valve 1030 and the extraction reagent line 1070 is closed, and the piston rod of the syringe pump 1010 is pushed forward again, so that the buffer reagent in the syringe pump 1010 enters the buffer tube 1040 again, and the extraction reagent in the buffer tube 1040 is pushed into the pipette 400.
For example, if the volume of the buffer tube 1040 of buffer solvent or extraction reagent drawn into the buffer tube 1040 each time is 10mL, the volume of the extraction solvent drawn into the buffer tube 1040 each time is 10mL, and the volume of the buffer tube 1040 is 10.510mL, an air lock may be formed between the buffer reagent and the extraction reagent during the process that the piston rod of the syringe pump 1010 is retracted and the buffer reagent is drawn into the syringe pump 1010 again while the solvent in one of the extraction reagent containers is drawn into the buffer tube 1040, so as to prevent the buffer reagent and the extraction reagent from mixing with each other and entering the syringe pump 1010.
Since multiple reagents are usually required for radioactive strontium solid-phase extraction, each extraction reagent container is connected to different interfaces of the concatemer solenoid valve 1030 through the extraction reagent pipeline 1070, so that the effect of reagent switching can be achieved, only one reagent is added into the extraction column 310 by the pipettor 400 each time, and the operations are repeated when the reagents are switched. Through setting up automatic liquid feeding device 1000, can replace artifical with the liquid feeding rifle absorb different kinds of reagent, through high accuracy syringe pump and corrosion-resistant three-way solenoid valve 1020, concatemer solenoid valve 1030 switches can be extracted with reagent from different reagent bottles according to setting for the velocity of flow, the volume is inhaled in buffer tube 1040, in reagent propelling movement in buffer tube 1040 reaches pipettor 400 again, also can absorb the sample to be measured in sample container 510 to pipettor 400 pipeline through pipettor 400, realize automatic liquid feeding, get the liquid operation, the experiment precision has been improved. Meanwhile, the automatic liquid adding device 1000 in the embodiment can ensure that only the buffer reagent enters and exits the injection pump 1010, the buffer reagent is a non-corrosive reagent, such as water, the reagent for extraction (usually, an acid-containing reagent) only enters the buffer tube 1040 and does not enter the injection pump 1010, on one hand, the corrosion of the reagent for extraction on the injection pump 1010 can be avoided, on the other hand, the cavity of the injection pump 1010 is larger than the inner diameters of the extraction reagent pipeline 1070 and the buffer tube 1040, the volume is larger, if the reagent for extraction enters the injection pump 1010, the reagent is easy to remain, the reagent loss is caused, and the corrosion to the injection pump 1010 is aggravated.
The pipette 400 is provided with a bubble sensor 410 for detecting whether continuous bubbles exist in a communication pipeline between the pipette and the concatemer solenoid valve 1030, so as to determine whether the sample in the sample container 510 is completely sucked when the liquid is taken from the loading module 500, thereby performing a complete loading operation.
Furthermore, each extraction reagent container and each buffer reagent container 1050 are provided with a cover body, a buffer reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of the buffer reagent container 1050, the buffer reagent pipeline 1060 is inserted into the buffer reagent container 1050 through the buffer reagent pipeline insertion opening, an extraction reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of the extraction reagent container, the extraction reagent pipeline is inserted into the extraction reagent container through the extraction reagent pipeline insertion opening, an air inlet pipeline 1080 is inserted into each gas pipeline insertion opening, and an electromagnetic valve 1090 is arranged on each air inlet pipeline 1080. The lid can guarantee the sealed of buffer reagent container 1050 and extraction reagent container respectively, and outer pressure balance in the container when air inlet pipe 1080 guarantees outside outflow buffer reagent or extraction with reagent guarantees that buffer reagent or extraction flow out smoothly with reagent.
Because pipettor 400 not only will be used for absorbing different solvents for extraction, buffer reagent, still can absorb the sample that awaits measuring, for avoiding cross contamination between different liquid, integrated device is still including wasing module 1100 in this embodiment, at least, be used for wasing pipettor 400, refer to fig. 13, combine fig. 1 to 3 and fig. 6 simultaneously, be equipped with a plurality of washing tanks 1110 on the washing module 1100, a plurality of washing tanks 1110 are along transverse arrangement, then pipettor 400 changes the transverse position along transverse movement under the drive that removes arm 100, vertical migration transform height position, can realize that it washs in different washing tanks 1110, set up a plurality of washing tanks 1110, ensure the cleaning performance of pipettor 400 inside and outside wall.
In addition, as shown in fig. 1 to fig. 3 and fig. 6, the integrated apparatus of the present embodiment further includes a waste liquid tank 1200 for collecting waste liquid output by the extraction column 310 when the extraction column 310 slides to the waste liquid collecting position, which is arranged with the collecting module 600 along the transverse direction at intervals, and a liquid inlet of the waste liquid tank 1200 is communicated with a liquid outlet of the cleaning tank 1110 through a pipeline. Because the sample that contains radioactive strontium can produce the waste liquid after the reextraction, need discharge the waste liquid from extraction column 310, then collect the radioactive strontium who adsorbs on the column wall again, waste liquid groove 1200 then can be convenient for the waste liquid to collect, waste liquid groove 1200 position is the waste liquid collection position promptly, extraction column support 320 can be shifted the drive of post 200 down along sliding guide assembly 330 horizontal slip to waste liquid collection position, even make extraction column 310 reach the waste liquid collection position, discharge the waste liquid that the extraction formed into in waste liquid groove 1200. Meanwhile, the liquid outlet of the cleaning tank 1110 is communicated with the liquid inlet of the waste liquid tank 1200, the liquid in the cleaning tank 1110 can flow into the waste liquid tank 1200 for uniform treatment, the liquid outlet of the waste liquid tank 1200 can be further communicated with the waste liquid barrel, the waste liquid drives the peristaltic pump 1300 to operate through the stepping motor, the waste liquid in the waste liquid tank 1200 can be discharged into the waste liquid barrel, the peristaltic pump 1300 can realize positive and negative operation, the stepping motor is matched with a driver, the system parameters above the driver can be adjusted, and the waste liquid speed can be adjusted and controlled by adjusting the system parameters above the driver.
In addition, the integrated device of this embodiment is further provided with an exhaust device 1400, such as an exhaust fan, etc., as shown in fig. 4, which can automatically exhaust acid gas.
In this embodiment, the main components, such as the extraction column holder 320, the sample loading module 500, the collection module 600, the cleaning module 1100, the waste liquid tank 1200, etc., are made of PTFE, and all have corrosion resistance, so that replacement is substantially avoided. The main body shell of the activity analysis and measurement device 900 is made of metal tungsten and has the characteristic of radiation resistance.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The utility model provides a radioactivity strontium solid-phase extraction, sample preparation and activity measurement integrated device which characterized in that includes:
the mobile mechanical arm comprises a transverse moving module and a vertical moving module, wherein the vertical moving module is arranged on the transverse moving module and can move transversely along with the transverse moving module;
the shifting column is arranged on the vertical moving module;
the extraction device comprises an extraction column, an extraction column bracket and a sliding guide assembly, wherein the extraction column is arranged on the extraction column bracket, and the extraction column bracket can transversely slide along the sliding guide assembly under the driving of the toggle column;
the pipettor is arranged on the vertical moving module;
the sample loading module comprises a sample container for containing a sample to be tested;
a collection module comprising a collection fluid container for collecting collection fluid output by the extraction column when the extraction column is slid to a collection position;
the collected liquid transverse conveying module comprises a transverse moving part, a collected liquid conveying part and an electric driving part, wherein the collected liquid conveying part is fixedly connected with the transverse moving part into a whole, the electric driving part is used for driving the transverse moving part to transversely move, a collected liquid containing part is arranged on the collected liquid conveying part, and the collected liquid conveying part can move to the collected liquid containing part at least to be located at a collected liquid adding position and a collected liquid concentrating and drying position under the driving of the transverse moving part;
a concentrated drying device arranged at the collected liquid concentrated drying position and used for concentrating and drying the collected liquid when the collected liquid accommodating part added with the collected liquid moves to the collected liquid concentrated drying position;
and the activity measuring device is used for measuring the activity of the sample formed after concentration and drying.
2. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1, wherein,
the collection liquid lateral transportation module is located extraction device reaches concentrated drying device's below, and it still includes the casing, lateral shifting part reaches electric drive part all establishes in the casing, be formed with on the roof of casing with the liquid feeding that the liquid feeding position corresponds dodge the hole and with the concentrated stoving that the concentrated stoving position corresponds dodges the hole, concentrated drying device is located the top in hole is dodged in concentrated stoving.
3. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1 or 2,
the extraction device is located one side of the concentration drying device, the concentration drying device comprises an evaporation lamp and a lampshade covering the evaporation lamp on the periphery, and a heat insulation plate is surrounded on the inner side of a circumferential side plate of the lampshade.
4. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 3, wherein,
a heat dissipation hole is formed in the top plate of the lampshade.
5. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1, wherein,
under the drive of the transverse moving component, the collected liquid accommodating part can also move to a measuring position, the measuring position is positioned in the activity measuring device, and an avoiding space for avoiding the transverse movement of the collected liquid conveying component is formed on a shell of the activity measuring device.
6. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1, further comprising:
the automatic liquid adding device comprises an injection pump, a corrosion-resistant three-way electromagnetic valve, a multi-connection electromagnetic valve, a buffer tube, a buffer reagent container for containing buffer reagents and a plurality of extraction reagent containers for containing the extraction reagents respectively, wherein the output end of the injection pump is connected with a first interface of the corrosion-resistant three-way electromagnetic valve, a second interface of the corrosion-resistant three-way electromagnetic valve is connected with a buffer reagent pipeline inserted into the buffer reagent container, a third interface of the corrosion-resistant three-way electromagnetic valve is connected with an interface at one end of the buffer tube, an interface at the other end of the buffer tube is connected with an input interface of the multi-connection electromagnetic valve, an output interface of the multi-connection electromagnetic valve is connected with a liquid transfer device, and the extraction reagent containers are connected with different interfaces of the multi-connection electromagnetic valve through extraction reagent pipelines respectively.
7. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 6, wherein,
each extraction reagent container and each buffer reagent container are provided with a cover body, a buffer reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of each buffer reagent container, the buffer reagent pipeline is inserted into the buffer reagent container through the buffer reagent pipeline insertion opening, an extraction reagent pipeline insertion opening and a gas pipeline insertion opening are formed in the cover body of each extraction reagent container, the extraction reagent pipeline is inserted into the extraction reagent container through the extraction reagent pipeline insertion opening, a gas inlet pipeline is inserted into each gas pipeline insertion opening, and an electromagnetic valve is arranged on each gas inlet pipeline.
8. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1, further comprising:
the cleaning module is at least used for cleaning the pipettor, and a plurality of cleaning grooves are arranged on the cleaning module and are arranged along the transverse direction.
9. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 8, further comprising:
and the waste liquid tank is used for collecting the waste liquid output by the extraction column when the extraction column slides to a waste liquid collecting position, the waste liquid tank and the collecting module are transversely arranged, and a liquid inlet of the waste liquid tank is communicated with a liquid outlet of the cleaning tank through a pipeline.
10. The integrated apparatus for solid-phase extraction of radioactive strontium, sample preparation and activity measurement according to claim 1, wherein,
the integrated device further comprises an air exhaust device.
CN202110603186.XA 2021-05-31 2021-05-31 Radioactive strontium solid-phase extraction, sample preparation and activity measurement integrated device Active CN113390702B (en)

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