KR20220007465A - Particulate sample fixing apparatus for multi-purpose analysis - Google Patents

Abstract

According to the present invention, a sample fixing device comprises: a base unit having a base opening that is an opening opened in a vertical direction; and a wall unit protruding upwardly from the base unit so as to surround a receiving area, which is a vertically open area located on an upper side of the base opening. The base unit has a locking unit positioned on an inner side compared to the wall unit when viewed from the bottom and configured to define the base opening so that a sample, inserted downward into the receiving area, does not pass downward through the base opening and a sample is seated.

Description

Particulate sample fixing device for multipurpose analysis {PARTICULATE SAMPLE FIXING APPARATUS FOR MULTI-PURPOSE ANALYSIS}

The present invention relates to a fixing device for fixing a particulate sample for multi-purpose analysis.

The environmental sample analysis method, introduced by the International Atomic Energy Agency (IAEA) for the purpose of strengthening nuclear safety measures, is an analysis method that detects unauthorized nuclear activities such as nuclear weapons development by precisely analyzing nuclear materials in samples collected from the environment. Among these analysis methods, the FT-TIMS (Fission Track - Thermal Ionization Mass Spectroscopy) method, which is a key analysis method, is more precise and accurate than other analysis methods, but the analysis procedure is complicated and takes a lot of time to analyze. There are also downsides to it. If North Korea's denuclearization proceeds in the future, the IAEA environmental sample analysis method is highly likely to be used as a key analysis method for related sample analysis.

The FT-TIMS particle analysis method is a method of measuring the isotope ratio of individual particles with a thermo-ionization mass spectrometer (TIMS) by selecting nuclear material particles from among the particles recovered from the environment using the fission track method. It is difficult to shorten the mass analysis time because the isotope ratio measurement by the mass spectrometer depends on the analysis equipment, but it is possible to simplify the analysis method for the reduction of the analysis time in the nuclear material particle selection process. In order to improve the efficiency of environmental sample analysis, it is necessary to develop a sample preparation method that can be applied not only to the FT-TIMS particle analysis method but also to other analysis methods without special pretreatment.

1 is a diagram illustrating a situation in which particles are collected from an environmental sample. 2 is a view sequentially showing a conventional preparation process for making a collected particulate sample to be used for analysis using FT.

Referring to the drawings, in order to collect particles from the environmental sample (ES), a syringe filter (F) connected to a pump may be used. The syringe filter F includes a membrane filter inside, so that particles of the environmental sample ES sucked by the pump are filtered by the membrane filter. After separating the membrane filter from the syringe filter (F), it is dissolved as shown in (a) of FIG. 2, and spread on the quartz glass plate 1012 as shown in FIG.

A nuclear fission track detector 1013 made of polycarbonate is overlapped on the particle layer 1011, and one end is taped with an adhesive tape 1014, as shown in FIG. 1013) is prepared in the form of a fixed sample 101. The fixed sample 101 is pressed between polyethylene plates in a container made of polyethylene plates as shown in FIG. to keep

The sample 101 is irradiated with neutrons. After the neutrons are irradiated, the detector 1013 is chemically treated with a strong base solution (C), etc. as shown in FIG. 2(e) with one end of the detector 1013 connected to the particle layer 1011. Since the quartz glass plate 1012 or the particle layer 1011 should not come into contact with the solution C provided for chemical treatment, only the detector 1013 is erected in the vertical direction and immersed in the solution C while the quartz glass plate 1012 and the particle layer ( 1011) may be used as a separate mechanism to be located on the outside of the solution (C).

After the chemical treatment of the detector 1013 is completed, the detector 1013 is seated on the particle layer 1011 in its original state. Thereafter, the positions of the fission track (T) and the particle (P), which can be confirmed in FIG. After separating a part of the displayed particle layer 1011 to prepare a sample for mass spectrometry, a nuclide can be identified using TIMS.

In order to chemically process only the detector 1013 after neutron irradiation as described above, a specially manufactured instrument must be used, and then only the detector 1013 must be cleaned in order to return the detector 1013. Analysis, etc. There are factors that prevent the process from proceeding quickly. In addition, when returning the detector 1013, in order to accurately match the fission track T and the particle P corresponding thereto, the detector 1013 must be accurately returned to the original position. Therefore, it is not easy to simply return the detector 1013 .

The present invention has been devised to solve such problems, and an object of the present invention is to provide a fixing device for easily selecting a particulate sample for analysis from a nuclear fission track.

A sample holding device according to an embodiment of the present invention includes: a base having a base opening that is an opening that is opened in a vertical direction; and a wall portion protruding upward from the base to surround a receiving area that is an area open in the vertical direction located above the base opening, wherein the base includes a sample inserted downward into the receiving area through the base opening. It has a locking part which is located inside the wall part and defines the base opening when viewed along the downward direction so that the sample is seated so as not to pass downward.

Accordingly, it is possible to fix the particulate sample to be analyzed for multi-purpose analysis so that it can be easily selected.

The sample can be easily removed from the sample holder.

1 is a diagram illustrating a situation in which particles are collected from an environmental sample.
2 is a view sequentially showing a conventional preparation process for making a collected particulate sample to be used for analysis using FT.
3 is a perspective view of a sample holding device according to an embodiment of the present invention.
4 is a longitudinal cross-sectional view of a sample holding device according to an embodiment of the present invention.
5 is a longitudinal cross-sectional view illustrating a state in which a sample is disposed in a sample holding device according to an embodiment of the present invention.
6 is a perspective view of a sample holding device according to another embodiment of the present invention.
7 is a diagram illustrating a situation in which a detector used in a sample fixing device according to an embodiment of the present invention is post-processed.
8 is a diagram illustrating a situation in which particles to be analyzed are detected using the sample fixing device according to an embodiment of the present invention.
9 is a view showing a sample with a detector removed in the state of FIG. 8 .

Hereinafter, some embodiments of the present invention will be described in detail with reference to exemplary drawings. In adding reference numerals to the components of each drawing, it should be noted that the same components are given the same reference numerals as much as possible even though they are indicated on different drawings. In addition, in describing the embodiment of the present invention, if it is determined that a detailed description of a related known configuration or function interferes with the understanding of the embodiment of the present invention, the detailed description thereof will be omitted.

In addition, in describing the components of the embodiment of the present invention, terms such as first, second, A, B, (a), (b), etc. may be used. These terms are only for distinguishing the elements from other elements, and the essence, order, or order of the elements are not limited by the terms. When it is described that a component is "connected", "coupled" or "connected" to another component, the component may be directly connected or connected to the other component, but another component is between each component. It will be understood that may also be "connected", "coupled" or "connected".

3 is a perspective view of a sample holding device 1 according to an embodiment of the present invention. 4 is a longitudinal cross-sectional view taken along line A-A' of the sample holding device 1 according to an embodiment of the present invention. 5 is a longitudinal cross-sectional view showing a state in which the sample S is disposed in the sample holding device 1 according to an embodiment of the present invention.

Referring to the drawings, the sample holding device 1 according to an embodiment of the present invention is a device capable of fixing the sample S in an easy state for neutron irradiation and analysis without taping, and includes a base 11 and a wall ( 12) is included. The base portion 11 and the wall portion 12 may be made of polyethylene or ABS resin to minimize the influence of neutron irradiation, but the material constituting the sample holding device 1 is not limited thereto.

base (11)

The base 11 constitutes the lower end of the sample holding device 1, but is a part on which the sample S is seated. The base 11 may include a perimeter 111 and a catching portion 112 protruding inward from the perimeter 111 when the perimeter 111 is viewed from above, and the engaging portion 112 . It has a base opening 110 that is surrounded by and opened along the vertical direction.

From the peripheral portion 111, a wall portion 12, which will be described later, is formed to protrude upward. Accordingly, the engaging portion 112 protruding inward from the peripheral portion 111 may be naturally located on the inner side of the wall portion 12 when viewed downwardly. The locking part 112 may form the base opening 110 having an area smaller than the area of the sample S so that the sample S does not pass downward through the opening. Therefore, when the sample (S) is inserted downwardly from the upper side of the wall part (12), the edge of the sample (S) may be seated on the engaging part (112). Since the locking part 112 defines the base opening 110 , the sample S may not fall downward through the base opening 110 by being caught in the locking part 112 .

The base 11 may be formed in a predetermined rectangular plate shape with an open center. Since the wall part 12 protrudes upward from the perimeter 111 forming the perimeter of the base part 11, the perimeter may be formed along the predetermined rectangle when viewed downward. The base opening 110 may also have a rectangular shape when viewed along the lower side. The base opening 110 may have a rectangular shape having a size smaller than the predetermined rectangular size. However, the base 11 , the wall 12 , and the base opening 110 may have other polygonal shapes when viewed downward, which can be appropriately deformed according to the shape of the sample S.

The peripheral portion 111 may further protrude outward from the wall portion 12 when viewed downwardly.

wall (12)

The wall part 12 is a component that can be fixed so that the sample S does not deviate in a horizontal direction. A receiving area 120 that is an area open in the vertical direction located above the base opening 110 may be formed, and the wall part 12 protrudes upward from the base 11 to surround the receiving area 120 . . That is, the receiving area 120 is defined by the wall portion 12 and is opened up and down. The base opening 110 is disposed below the receiving area 120 . The sample S may be inserted into the receiving area 120 downward through the upper opening located on the upper side of the receiving area 120 , and the periphery thereof may be seated on the upper surface of the locking part 112 .

The wall part 12 may be formed along the perimeter of a predetermined rectangle surrounding the base opening 110 when viewed along the downward direction. Specifically, the wall portion 12 includes two barrier portions 121 respectively formed along two long sides of the predetermined rectangle and two short wall portions 122 respectively formed along two short sides of the predetermined rectangle. can do. The long side is a relatively long side among the sides of the rectangle, and the short side is a relatively short side among the sides of the rectangle. The two barrier parts 121 are disposed to be spaced apart from each other with the base opening 110 therebetween, and the two end wall parts 122 are also disposed to be spaced apart from each other with the base opening 110 therebetween. Both ends of the two barrier portions 121 meet the opposite ends of the two end wall portions 122 to form a predetermined rectangular shape.

Since the wall portion 12 is formed as described above, the side shape of the receiving area 120 may be formed like the side shape of a rectangular parallelepiped. A cross-sectional area of a cross-section of the receiving region 120 formed by the wall portion 12 cut in a plane perpendicular to the vertical direction may be similar to the area of the sample S. Therefore, when stacked, the sample S formed like a rectangular parallelepiped can be easily inserted into the receiving area 120 , seated on the base 11 , and fixed by the wall 12 . In order to form the sample S, a quartz glass plate G having a particle layer PL formed on its upper surface is inserted downward into the receiving region 120 to be seated on the protrusion, and the detector D is further placed in the receiving region 120 The sample S can be formed by inserting it to settle on the particle layer PL. At this time, the positions of the particle layer PL and the detector D are fixed by the wall portion 12 without taping, and the sample S is placed in a situation where neutron irradiation is possible. In addition, the detector (D) and the quartz glass plate (G) can be easily removed from the sample holding device (1).

another embodiment

6 is a perspective view of a sample holding device 2 according to another embodiment of the present invention.

According to another embodiment of the present invention, the base portion 21 of the sample holding device 2 is formed in the same manner as in the first embodiment, and the wall portion 22 has the base opening 210 when viewed along the downward direction as described above. It may constitute a part of the perimeter of a predetermined rectangle surrounding the . That is, in one embodiment and another embodiment, the wall parts 12 and 22 may constitute at least a part of the perimeter of the predetermined rectangle when viewed along the downward direction. In a modified example of another embodiment, a part of the barrier part 221 is opened or a part of the end wall part 222 is opened so that the sample S is fixed and the sample S is easily gripped at the same time.

In another embodiment, the two barrier portions 221 and the two end wall portions 222 do not meet each other. Accordingly, in the portion where the perimeter of the above-described predetermined rectangle passes where the barrier portion 221 and the end wall portion 222 do not meet each other, the side opening opened in the horizontal direction between the barrier portion 221 and the end wall portion 222 . (23) is formed.

The two barrier portions 221 and the two end wall portions 222 do not reach the vertices of the predetermined rectangle. Accordingly, the side opening 23 may be formed in a portion corresponding to the vertex of a predetermined rectangle. Since the rectangle has four vertices, four side openings 23 can be formed as shown.

Since the side opening 23 is formed, when a sample S having an area larger than the cross-sectional area of the receiving region 220 is inserted into the receiving region 220 , each of the barrier portions 221 and the end wall portions 222 are separated from each other. It can be deformed while being pushed outward, thereby preventing damage to the sample (S). Although this deformation is possible, the wall part 22 may be formed of a material having elasticity so that it can return to its original shape.

7 is a diagram illustrating a situation in which the detector D used in the sample holding device 1 according to an embodiment of the present invention is post-processed.

5, a quartz glass plate G on which a particle layer PL is laminated is inserted into the sample holding device 1 according to an embodiment of the present invention as shown in FIG. The sample (S) can be configured by being seated on the (PL). The sample S may be irradiated with neutrons while the sample S is fixed by the sample fixing device 1 . After neutrons are irradiated to the sample S, the detector D may be lifted upward to separate it from the particle layer PL and the sample fixing device 1 . When transporting the detector (D) and the quartz glass plate (G), an adsorption head that adsorbs using negative pressure can be used.

Referring to the drawings, the detector (D) separated from the sample holding device (1) according to an embodiment of the present invention may be immersed in a solution (C) for chemical treatment. In this case, unlike the conventional preparation process described in FIG. 2 , a separate instrument is not required, and only the detector (D) can be immersed in the solution (C) to perform chemical treatment. Therefore, in a situation where the same volume of the solution (C) is present, when the sample fixing device 1 according to the embodiment of the present invention is used, a larger amount of the detectors (D) can be simultaneously processed, so that the analysis proceeds more quickly This is possible.

8 is a diagram illustrating a situation in which an analyte particle P is detected using the sample fixing device 1 according to an embodiment of the present invention. 9 is a view showing the sample S with the detector D removed in the state of FIG. 8 .

After the chemical treatment is completed, the detector D may be seated again on the particle layer PL as shown in FIG. 8 , and the portion where the fission track T is formed may be marked M with a laser or the like. Since the detector D is stacked on the particle layer PL, the marked portion M may be formed on both the detector D and the particle layer PL. Since the nuclear fission track T is formed around the particles P of the particles P of the particle layer PL, which react by the irradiated neutrons to form the nuclear fission track T, the portion where the nuclear fission track T is formed When indicated (M), the position of the reacting particle P in the particle layer PL is displayed (M), and the position can be grasped. When the detector (D) is separated and inserted into the sample holding device (1) as it is, the positional relationship that the detector (D) had relative to the particle layer (PL) before the separation of the detector (D) is changed to the detector (D) ) may be maintained as it is when seated on the particle layer PL again. Therefore, both the chemical treatment of the detector (D) and the alignment of the detector (D) are made easily, enabling rapid analysis.

As shown in FIG. 9, with the detector (D) separated, the marked (M) part of the particle layer (PL) was selected and removed to make a sample (S) for mass spectrometry, and mass spectrometry was performed and it was located in the marked (M) part. It is possible to identify the nuclide of the particle (P). Since it is very easy to separate the detector D from the particle layer PL and the quartz glass plate G on which the particle layer PL is formed from the sample holding device 1, it is possible to proceed quickly with analysis.

In an embodiment of the present invention, the sample (S) and the analysis process have been described with reference to the case of using FT-TIMS as an example. The analysis may be performed using the same or sized sample holding device 1 .

In the above, even though it has been described that all components constituting the embodiment of the present invention operate by being combined or combined into one, the present invention is not necessarily limited to this embodiment. That is, within the scope of the object of the present invention, all the components may operate by selectively combining one or more. In addition, terms such as "comprises", "comprises" or "have" described above mean that the corresponding component may be inherent, unless otherwise specified, excluding other components. Rather, it should be construed as being able to further include other components. All terms, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs, unless otherwise defined. Terms commonly used, such as those defined in the dictionary, should be interpreted as being consistent with the contextual meaning of the related art, and are not interpreted in an ideal or excessively formal meaning unless explicitly defined in the present invention.

The above description is merely illustrative of the technical spirit of the present invention, and various modifications and variations will be possible without departing from the essential characteristics of the present invention by those skilled in the art to which the present invention pertains. Accordingly, the embodiments disclosed in the present invention are not intended to limit the technical spirit of the present invention, but to explain, and the scope of the technical spirit of the present invention is not limited by these embodiments. The protection scope of the present invention should be construed by the following claims, and all technical ideas within the scope equivalent thereto should be construed as being included in the scope of the present invention.

1, 2: Sample holding device
11, 21: base
12, 22: wall
23: side opening
110, 210: basal opening
111: circumference
112: locking part
121, 221: barrier part
122, 222: single wall part
120, 220: Receiving area
101, S: sample
1011, PL: particle layer
1012, G: quartz glass plate
1013, D: detector
1014: tape
C: solution
ES : Environmental sample
F : syringe filter
M: mark
P: particle
T: fission track

Claims (7)

a base having a base opening that is an opening in the vertical direction; and
and a wall portion protruding upward from the base to surround a receiving area that is an area open in the vertical direction located above the base opening,
The base part is positioned inside the wall part when viewed from the bottom and defines the base opening so that the sample inserted downward into the receiving area does not pass downward through the base opening and the sample is seated. A sample holder having a portion. According to claim 1,
Wherein the wall portion constitutes at least a part of the perimeter of the predetermined rectangle when viewed along the downward direction, the sample holding device. 3. The method of claim 2,
The wall portion includes two barrier portions respectively formed along two long sides of the predetermined rectangle, and two short wall portions respectively formed along two short sides of the predetermined rectangle,
The two barrier portions and the two end wall portions do not meet each other, sample holding device. 4. The method of claim 3,
The two barrier portions and the two end wall portions do not reach the vertices of the predetermined rectangle. 3. The method of claim 2,
When viewed along the downward direction, the base opening, the sample holding device having a rectangular shape having a size smaller than the predetermined rectangular size. According to claim 1,
Connecting the two different parts of the locking part, the sample holding device comprising a rib disposed in the base opening. The method of claim 1,
The base part and the wall part are made of polyethylene or ABS resin, the sample holding device.

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