KR20170127234A - Automated concentrator for large volume of sample - Google Patents

Abstract

The present invention relates to an automatic pretreatment device for a large-volume sample which uses an ion-exchange resin method to quickly and efficiently complete a pretreatment process of a large-volume sample. The automatic pretreatment device for the large-volume sample comprises: eight columns capable of being filled with an ion-exchange resin; four peristaltic pumps; a flow selection valve (FSV); a flow distribution valve (FDV); a flow distribution block (FDB); and a controller to drive the four peristaltic pumps, outputting a control signal to control drive of the valves. Accordingly, manpower and time are able to greatly be saved.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic pre-

TECHNICAL FIELD The present invention relates to an automatic pretreatment apparatus for a large-volume sample, and more particularly, to an apparatus for quickly and efficiently completing a pretreatment process for a large-capacity sample using ion exchange resin as a basic principle.

Based on Notice No. 2014-12 of the Nuclear Safety Commission, the nuclear facility shall operate an environmental radiation monitoring program. Since radioactivity concentrations in groundwater or sea water are very low, generally large samples (> 40L) should be treated to meet the legal detection limit for alpha / beta nuclides. The pretreatment process for reducing the sample volume is indispensable for the radioactive analysis of a large amount of samples. Conventional pretreatment techniques are performed by precipitation method and ion exchange using the chemical characteristics of the nuclides of interest as shown in FIGS. 1 (a) and 1 The precipitation method can be used to fill a liquid sample of 40 L or more, a stirrer, and a device with a drain pipe separating the sediment and the supernatant. Generally, it takes 4 to 5 days to pretreat the 40 L sample by the precipitation method. The ion exchange resin method is a method in which a nuclide of interest is substituted with an ion exchange resin and then eluted again to reduce the volume of the sample. Compared to the precipitation method, the chemical reaction rate is faster, and the pretreatment time can be relatively short. As shown in Fig. 1 (b), a method of filling a resin into a column is a method which has much room for development of an automated apparatus.

However, there is a problem in that when the analysts do not process the ion exchange resin method automatically, the advantage of the ion exchange resin method is lost in terms of the time required for pretreatment as compared with the precipitation method.

Korea Patent No. 10-0581019

In order to solve the problems of the related art, the present invention provides an automatic pretreatment apparatus for a large-volume sample for rapidly and efficiently completing a pretreatment process of a large-volume sample using an ion exchange resin process as a basic principle. have.

It is also an object of the present invention to provide an automatic pretreatment apparatus for a large-volume sample which can pre-treat eight samples simultaneously for a single nuclide and pre-treat up to four samples simultaneously for two or more nuclides .

The present invention also relates to an automatic preprocessing apparatus for a large-volume sample, which is capable of applying up to two columns applicable to one sample using the sequential separation function and doubling the amount of the sample to be processed, Which has its purpose.

In addition, the present invention provides a large-capacity sample for repeatedly performing a process of supplying a sample, removing unnecessary interfering ions through a rinsing or washing process with respect to the supplied sample, and then extracting only the nuclear species of interest into a liquid state, And an object thereof is to provide an automatic preprocessing apparatus of the present invention. That is, in order to measure a radioactivity concentration with respect to a radionuclide of a sample, a sample in a liquid state is supplied to a chemical reactor so that the liquid core is transformed into a specimen of a solid core of interest, And then transformed into a solid sample by repeatedly supplying the sample to the chemical reactor so as to reduce the volume of the sample.

The automatic pretreatment apparatus for a large volume sample according to an embodiment of the present invention includes a column section 120 having a plurality of columns capable of filling an ion exchange resin; A flow distribution block 125 that allows a uniform amount of reagent to be supplied to the columns of the column part 120 in response to externally input control signals; A peristaltic pump unit 130 driven so that a sample or a reagent is supplied to the columns in order to secure only a nuclear species of interest in response to an externally input control signal; A first valve unit 135 driven to supply a reagent for washing or elution to each of the columns of the column unit 120 in response to a control signal input from the outside; A second valve unit 140 driven to supply a reagent or a sample through the peristaltic pump unit 130 in response to a control signal input from the outside; A third valve unit 145 driven to discard the sample or the washing solution in response to a control signal input from the outside; A fourth valve unit 150 driven to separate and supply the waste solution and the eluting solution that have passed through the columns in response to a control signal input from the outside; And a controller for outputting a control signal to the flow distribution block 125, the peristaltic pump unit 130, the first valve unit 135 to the fourth valve unit 150 in response to an operation start command input according to an operation from the outside, (Not shown).

The third valve unit 145 may further include a collecting unit 160 configured to collect and store the eluting solution eluted by each column of the column unit 120, May be driven to discharge the eluting solution supplied from the column part 120 to the collecting part 160 in response to the control signal of the controller 155. [

As an embodiment related to the present invention, the third valve portion 145 may be driven to continuously supply the sample passed through the column of the column portion 120 in response to the control signal of the controller 155 to the next column.

As an embodiment related to the present invention, a column holder 175 may be provided in which columns of the column section 120 are fitted and engaged.

As an embodiment related to the present invention, the column holders 175 of the column rest 170 are provided on the front and rear surfaces of the column rest 170, and the sizes of the respective column holders 175 provided on the front and rear surfaces may be different.

The present invention has the effect of making it possible to complete the pretreatment process of a large capacity sample quickly and efficiently by using the ion exchange resin method as a basic principle, thereby saving manpower and time.

In addition, the present invention has the effect of being able to pre-treat eight samples simultaneously for a single nuclide and to pre-treat a maximum of four samples simultaneously for two or more nuclides, thereby saving manpower and time .

In addition, the present invention makes it possible to apply up to two columns that can be applied per sample by using the sequential separation function, thereby enlarging the processable sample volume up to twice, thereby greatly reducing manpower and time There is an effect to be able to do.

In addition, the present invention has an effect to be utilized for daily monitoring purposes of the environment around a nuclear power plant.

Further, the present invention has an effect of being utilized for the purpose of environmental monitoring of the medium / low level waste repository.

The present invention also relates to a process for converting a liquid sample into a solid sample by feeding it into a chemical reactor and converting the solid sample into a liquid and then feeding it back to the chemical reactor to transform it into a solid sample It is possible to reduce the volume of the test piece by performing it repeatedly.

1 is a view for explaining a conventional pretreatment technique.
2 is a block diagram for explaining a configuration of an automatic preprocessing apparatus for a large volume sample according to the present invention.
3 is a schematic diagram of Fig.
4 is a view for explaining the appearance of an automatic preprocessing apparatus for a large-volume sample according to the present invention.
5 is an exploded view of Fig.
6 is a flowchart illustrating an operation of the controller of FIG.
FIG. 7 is a user interface screen for controlling the operation state of the automatic preprocessing apparatus of the large-capacity sample provided by the controller of FIG. 2 or providing operational state information.
FIG. 8 is an application example of an automatic preprocessing apparatus for a large-capacity sample according to the present invention.

It is noted that the technical terms used in the present invention are used only to describe specific embodiments and are not intended to limit the present invention. In addition, the technical terms used in the present invention should be construed in a sense generally understood by a person having ordinary skill in the art to which the present invention belongs, unless otherwise defined in the present invention, Should not be construed to mean, or be interpreted in an excessively reduced sense. In addition, when a technical term used in the present invention is an erroneous technical term that does not accurately express the concept of the present invention, it should be understood that technical terms can be understood by those skilled in the art. In addition, the general terms used in the present invention should be interpreted according to a predefined or prior context, and should not be construed as being excessively reduced.

Furthermore, the singular expressions used in the present invention include plural expressions unless the context clearly dictates otherwise. In the present invention, terms such as "comprising" or "comprising" and the like should not be construed as encompassing various elements or various steps of the invention, Or may further include additional components or steps.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings, wherein like reference numerals refer to like or similar elements throughout the several views, and redundant description thereof will be omitted.

2 is a block diagram for explaining a configuration of an automatic preprocessing apparatus for a large volume sample according to the present invention. 3 is a schematic diagram of Fig. 4 is a view for explaining the appearance of an automatic preprocessing apparatus for a large-volume sample according to the present invention. 5 is an exploded view of Fig.

As shown in FIG. 2, the automatic preprocessing apparatus 100 for a large volume sample to which the present invention is applied includes a sample storage unit 110 including a plurality of sample storage containers for storing a sample, a plurality of reagent storage units A column section 120 comprising a plurality of columns capable of filling the ion exchange resin and a reagent storage section 115 made up of containers in which a uniform amount of reagent is supplied to the column section 120), a peristaltic pump unit (130) driven to supply a sample or a reagent to the columns in order to secure only nuclear species of interest in response to a control signal of the controller (155) And a first valve unit 135 driven to supply a reagent for washing or elution stored in a reagent storage container of the reagent storage unit 115 to each of the columns of the column unit 120 in response to a control signal of the controller 155 And a control signal of the controller 155 A second valve unit 140 driven to supply a reagent or a sample through the peristaltic pump unit 130 in response to a control signal from the control unit 155 and a third valve unit 145 A fourth valve unit 150 driven to supply the waste solution and the eluting solution that have passed through the columns separately in response to the control signal of the controller 155, A controller 155 for outputting control signals to the block 125, the peristaltic pump unit 130, the first valve unit 135 to the fourth valve unit 150, And a collecting unit 160 composed of a plurality of collectors for storing and storing the eluted solution.

That is, only the nuclear species of interest are collected in the collector of the collecting unit 160. And the waste ions are discharged to the outside through a discharge pipe (see FIG. 3).

The washing solution and the eluting solution are stored in the reagent storage container of the reagent storage part 115. The washing solution and the elution solution are supplied by the first valve part 135 which is the flow rate distribution valve depending on the nuclides to be extracted . That is, the first valve unit 135 controls the washing solution in accordance with the control signal of the controller 155 through the first valve unit 140, the interlocking pump unit 130, and the column unit 120 ) So that the elution solution for eluting the nuclide of interest is supplied. The eluting solution is also supplied through the same path as that for which the washing solution is supplied.

The second valve unit 140 is provided between the two flow distribution blocks 125 and the two peristaltic pump units 130. The second valve unit 140 is disposed between the peristaltic pump unit 130 and four columns of the column 120, Respectively. That is, a total of three second valve units 140 are provided, and each of the second valve units 140 includes as many valves as the number of columns connected thereto.

The second valve unit 140 provided between the column 120 and the peristaltic pump unit 130 is connected to the third valve unit 145. The first valve unit 140 and the second valve unit 145 are connected to each other through a first column section 3 valve portion 145 to pass through the secondary column portion.

3, each of the peristaltic pumps is provided with two channels, and the second valve unit 140 is controlled to control the sample storage unit 110 And the sample or reagent of the reagent storage container 115 are supplied to the column.

The third valve portion 145 and the fourth valve portion 150 are provided in a line connecting the column of the column portion 120 and the collector of the collecting portion 160 in a one-to-one manner and a line connected to a discharge pipe discharging the same to the outside. That is, the third valve portion 145 and the fourth valve portion 150 are arranged such that the respective columns of the column portion 120 are connected one-to-one to the collector of the collecting portion 160 in response to the control of the controller 155 (see FIG. 2) Or operate so that each column of column portions 120 is connected to a discharge tube.

As described above, the peristaltic pump unit 130 has two channels per pump. Since the peristaltic pump unit 130 needs to flow the sample or the reagent into the column of the column 120 at a desired flow rate, the peristaltic pump unit 130 not only has good reproducibility of the flow rate, So that the difference in flow rate between the two is not greatly increased. The difference in flow rate between the pumps is directly related to the quality of the tubing used as well as the mechanical properties of the pump. The tubing used in the present invention is an E-3603 model (1/8 "in inner diameter, 1/4" in outer diameter, 1/16 "thick, Tygon) and can deliver 100 ml per minute. The reproducibility of the flow rate variation within 10% was confirmed even if the flow rate difference between the pumps was within 5% and used for more than 6 months. Since a large volume of sample is to be treated, the flow rate through which the sample is passed through the ion exchange resin column is an important criterion for determining the time required for the pretreatment. Since the sample flows through each column through the pump, it can be flowed at a flow rate of 100 ml / min. As a result, the completion speed of the nuclide of interest is shortened.

A flow pipe is provided between the second valve unit 140 and the peristaltic pump unit 130. The inner surface of the flow tube is oxidized by passing the nuclide, The separating performance may be reduced. Therefore, an anti-oxidation coating layer, which is an anti-oxidation coating layer, may be formed on the inner surface of the flow tube (tube).

Here, the first valve 135, the third valve 145 and the fourth valve 150 are flow rate distribution valves, and the second valve 140 is a flow rate selection valve.

The third valve unit 145 is driven to discharge the eluting solution supplied from the column unit 120 to the collecting unit 160 in response to the control signal from the controller 155.

The third valve portion 145 is driven to continuously supply the sample passed through the column of the column portion 120 to the next column in response to the control signal of the controller 155. [

The controller 155 provides the panel through the user interface screen of FIG. 8 so that the type, the input amount, and the input time of the washer solution can be determined and input or input. The controller 155 receives the set or input values through the user interface screen, And generates and provides a control signal for controlling the valve unit and the peristaltic pump unit.

FIG. 4 is a view for explaining the appearance of the automatic preprocessing apparatus for a large volume sample according to the present invention. The column holder 175 is provided at a position opposite to the upper and lower sides of the column holder 170, The upper and lower ends of the column are fixed to the column holder 170, and the column is fixed to the column holder 170.

4, the column holder 170 is provided so as to be detachable from the automatic preprocessing apparatus, and the columns of the column section 120 are fitted to the column holder 170, The column holder 175 is provided. Particularly, the column holder 175 is provided on the front and rear surfaces of the column holder 170, and the column holders 175 are configured to have different sizes so that the columns of different sizes can be joined. The column size was Φ 15 (internal diameter) × L 600 mm (volume: 100 ml), Φ 25 (internal diameter) × L 600 mm (volume: 300 ml), Φ 55 : 1200 ml) can be utilized. The column holder 175 may be formed on the front and rear surfaces of the column holder 170 to separate the column holder 170 from the column holder 170, After that, the column can be changed to a different size.

The operation state of the automatic preprocessing apparatus of the large-capacity sample having the above-described structure will now be described.

6 is a flowchart illustrating an operation of the controller of FIG. FIG. 7 is a user interface screen for controlling the operation state of the automatic preprocessing apparatus of the large-capacity sample provided by the controller of FIG. 2 or providing operational state information. FIG. 8 is an application example of an automatic preprocessing apparatus for a large-capacity sample according to the present invention.

As shown in FIG. 6, when the operation start command input from the outside is input, the controller 155 determines whether or not an automatic pre-processing command is sequentially included in the operation start command If it is determined that the number of columns has been inputted (S120), if the automatic preprocessing command is included in step S110, the following steps are sequentially performed for the corresponding columns in step S120. . For each column, resin optimization (conditioning, S130) is performed, sample loading (S140) is performed, washing of the interfering ions (S150), elution of only the nuclear species of interest (S160) , And then the column clean-up (S170) is performed when all processes are completed.

The reagent used in step S130, which is a resin optimization process, and step S150, which is a process of removing an interfering ion, can be designed to use up to six reagents depending on the nuclide of interest.

On the other hand, if the automatic preprocessing command is not included sequentially in step S110, the following processes are simultaneously performed for a total of eight columns. That is, resin optimization (S130) is performed for each of the eight columns, sample loading S140 is performed, washing of the interfering ions (S150), elution of only the nuclear species of interest (S160) Then, after all processes are completed, a clean-up (S170) is performed.

As described above, the automatic preprocessing apparatus for a large-capacity sample according to the present invention can pre-treat 1 to 8 samples at the same time or sequentially separate two nuclides among 1 to 4 samples. In addition, the control algorithm for performing the automatic sequencing protocol of the large volume sample applied to the present invention was developed based on the algorithm of the automatic sequencing apparatus (Patent Application No. 10-2014-129176).

The controller 155 of the automatic preprocessing apparatus 100 of the large-volume sample operated according to the operation flowchart shown in FIG. 6 provides the user interface screen shown in FIG.

That is, the controller 155 is a panel capable of performing a pump calibration operation as shown in FIG. 7 (a), a calibration (calibration) a user interface screen divided into execution panels for processing actual samples as shown in FIG. 7 (c), so that the operator can easily set the conditions, and confirms the set conditions on the screen In addition, the automatic pretreatment process of a large sample can be confirmed on the screen. And the user interface screen is designed so that columns 1 to 8 can be operated separately and the selection of the sequential function can be selected.

[Application example of the automatic preprocessing apparatus of the large capacity sample of the present invention]

Suppose that liquid samples such as groundwater or seawater are pretreated for Sr and I purposes. Sr is cation exchange resin and I is anion exchange resin. In the case of the single nuclide pretreatment, the sample may be supplied to one column as shown in Fig. 8 (a). When the two nuclides are sequentially separated, as shown in FIG. 8 (b), the sample may be configured to pass through two columns successively. If the radioactivity concentration is so low that a larger amount of sample is required than expected, the sample may be processed such that the column filled with the same kind of resin is continuously passed through as shown in FIG. 8 (c). In this case, the volume of the sample that can be treated can be doubled.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or essential characteristics thereof. Therefore, the embodiments disclosed in the present invention are intended to illustrate rather than limit the scope of the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments. The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

100: Large sample automatic pretreatment device
110: sample storage part 115: reagent storage part
120: Column part 125: Flow distribution block
130: peristaltic pump unit 135: first valve unit
140: second valve part 145: third valve part
150: fourth valve part 155: controller
160: Collecting section

Claims (5)

A column portion 120 comprising a plurality of columns capable of filling an ion exchange resin;
A flow distribution block 125 for supplying a uniform amount of reagent to each column of the column part 120 in response to a control signal input from the outside;
A peristaltic pump unit 130 driven so that a sample or a reagent is supplied to the columns in order to secure only a nuclear species of interest in response to a control signal input from the outside;
A first valve part 135 driven to supply a reagent for washing or elution to the columns in response to a control signal input from the outside;
A second valve unit 140 driven to supply a reagent or a sample through the peristaltic pump unit 130 in response to a control signal input from the outside;
A third valve unit 145 driven to discard the sample or the washing solution in response to a control signal input from the outside;
A fourth valve unit 150 driven to separate and supply the waste solution and the eluting solution that have passed through the columns in response to a control signal input from the outside; And
And outputs control signals to the flow distribution block 125, the peristaltic pump unit 130, the first valve unit 135 to the fourth valve unit 150 in response to an operation start command input from an external operation A controller 155 for outputting;
The automatic pretreatment device for a large volume sample.
The method according to claim 1,
And a collecting unit 160 composed of a plurality of collectors for receiving and storing the eluting solution eluted by each column of the column unit 120,
And the third valve part 145 is driven to discharge the eluting solution supplied from the column part 120 to the collecting part 160 in response to a control signal of the controller 155. [ Automatic preprocessing equipment for samples.
3. The method of claim 2,
And the third valve part 145 is driven to continuously supply the sample passed through the column of the column part 120 to the next column in response to the control signal of the controller 155. [ Device.
The method according to claim 1,
Further comprising a column holder (170) provided with a column holder (175) in which the columns of the column section (120) are fitted and engaged.
5. The method of claim 4,
The column holder 175 of the column rest 170 is provided on the front and rear surfaces of the column rest 170 and the size of each of the column holders 175 provided on the front and rear surfaces is different. Device.

Images