JP2023027924A - Microsample retainer - Google Patents

Abstract

To provide a microsample retainer that collects and transports a microsample, and hardly loses or changes it in quality during transportation.SOLUTION: A microsample retainer 1 for collecting, transporting, and measuring a microsample comprises: a base 3 having a retaining surface 12 that can retain the microsample; a thin film layer 6 formed on the retaining surface 12 and composed of one or more kinds of rare metals selected from among rare metals such as gold and indium; and a container 7 connected to a portion different from the retaining surface 12 of the base 3. An adhesive material 5 is affixed on the retaining surface 12, and a thin film layer 6 is formed on the affixed adhesive material 5. The microsample retainer 1 also comprises the container 7, and a lid body 10 that can internally store the base 3 and the thin film layer 6 in collaboration with the container 7.SELECTED DRAWING: Figure 1

Description

TECHNICAL FIELD The present invention relates to a micro-sample holder for collecting and carrying a micro-sample, and a method of using the same.

Conventionally, in the preliminary stage of analyzing a minute sample (hereinafter referred to as a minute sample), the minute sample is collected, transported, and before reaching the place to be analyzed, the minute sample is lost, contaminated, or deteriorated. I have something to do.

For example, a micro sample may be picked up with tweezers, placed in a petri dish, and lost before the micro sample placed in the petri dish is transported to a destination. Also, when the petri dish is opened, dust may enter, making it unclear whether the sample is the sample to be analyzed or some other foreign matter. In addition, although a minute sample is sometimes wrapped in a medicine-wrapping paper, it may flow out through the gaps in the medicine-wrapping paper and be lost during transportation.

If Cellotape (registered trademark) is used as an adhesive material when collecting a minute sample, the components of the Cellotape may be detected during measurement, or the detected component may be misidentified due to the presence of the Cellotape adhesive. In addition, when the petri dish is opened, the microsample may break, the microsample may be broken by fragments, or the microsample may be worn or scratched.

For example, the probe described in Patent Document 1 is known as a probe for collecting a minute sample. This device has a local heating mechanism capable of locally heating only the tip of the probe.
However, there is no known micro-sample holder that collects and transports micro-samples, prevents them from being lost during transport, maintains the state of the micro-samples as they were before collection, and maintains an environment that prevents deterioration.

Japanese Patent Application Laid-Open No. 2008-003016

Solves the problem of minimizing the risk of loss, contamination, deterioration, etc. of microsamples during the pre-analytical stage of microsample collection, storage, transport, and delivery to the analysis room. are required to do so.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a holder for micro-samples which is difficult to be lost or degraded while collecting and transporting micro-samples.

A micro-sample holder of the present invention is a holder for collecting, transporting, and measuring a micro-sample, and comprises a base (3, 23) having a holding surface (12) capable of holding a micro-sample. and one or more rare metal materials (6, 24) selected from rare metals such as gold and indium formed on the holding surface, and a holder body ( 7) and a configuration including.

According to this micro-sample holder, when the base is pressed against a micro-sample to be analyzed such as a foreign substance, a thin film layer or a rare metal material having properties such as adhesion of the rare metal formed on the holding surface of the base is formed on the holding surface of the base. A micro sample is embedded and held in the . Therefore, the micro sample can be transported to the destination while being protected by being embedded in the rare metal thin film layer or the rare metal material. Therefore, it is difficult to lose it, it is difficult to be contaminated or deteriorated, it can be safely delivered to the analysis room, and it is difficult to misidentify the component detection at the time of analysis.

Further, a method of using a micro sample holder of the present invention is a method of using a micro sample holder for collecting, transporting, and measuring a micro sample, wherein the holding surface is pressed against the target sample. , embedding and holding the target sample in the thin film layer; moving the holder body to a target location; and measuring the target sample without separating it from the thin film layer.

Therefore, according to the micro-sample holder of the present invention, the micro-sample is collected, stored, transported, and held until the micro-sample is reached at the destination such as an analysis room in the stage prior to analysis of the micro-sample. Since the micro sample is held without separation on the thin film layer formed on the holding surface of the base, problems such as loss, contamination, or deterioration can be prevented.

The base of the micro-sample holder of the present invention is, for example, beads.
The adhesive material of the micro-sample holder of the present invention is, for example, a grip sheet.

The gold deposited on the adhesive material of the micro-sample holder of the present invention has a thickness of, for example, 200-300 Å.

A micro sample holder of the present invention is a holder for collecting, transporting, and measuring a micro sample, and comprises a collection part (22) containing indium (24) and a handle (25) connected to the collection part. ) and a cap (26) that covers the collecting portion.

The micro sample holder of the present invention comprises a base, a grip sheet, and gold. The base has a height effect. The grip sheet has a sticky effect. Gold is conductive. Furthermore, since gold does not absorb infrared rays during measurement, it has the effect of preventing the wavelength of the grip sheet from being detected.

Since the micro-sample holder of the present invention contains indium, the micro-sample can be embedded in the metal for measurement.

Gold and indium are rare metals (rare metals) and do not become contaminants to be detected. Also, gold and indium are soft metals. Gold and indium rarely contaminate during extraction, transport, or measurement.
Lead is excluded from the thin film layer because it becomes a foreign substance that is a detection target.

As an example, when collecting a minute sample adhering to the copy drum of a copier, the minute sample holder of the present invention can be used to detect dot imprints in printing and foreign matter displayed in images. It is also possible to

If it is rusted or corroded, it is also possible to check and detect the presence or absence of foreign matter that affects rust or corrosion.

1 is a perspective view of a micro-sample holder according to a first embodiment; FIG. FIG. 2 is a cross-sectional view of the micro-sample holder according to the first embodiment; Infrared absorption spectrum showing experimental data by the ATR method using a micro-sample holder to which only a grip sheet is attached. Infrared absorption spectrum showing experimental data by the ATR method using the grip sheet according to the first embodiment and the gold vapor-deposited micro-sample holder. FIG. 10 is an infrared absorption spectrum showing experimental data of hair by the ATR method using the micro-sample holder according to the first embodiment; FIG. FIG. 4 is a perspective view of a micro-sample holder according to a second embodiment; FIG. 10 is a perspective view of a collecting part and a fixing jig of the micro-sample holder according to the second embodiment; Infrared absorption spectrum showing experimental data of cellulose by the ATR method using the micro-sample holder according to the second embodiment. Infrared absorption spectrum showing experimental data of an eraser by the ATR method using the micro-sample holder according to the second embodiment.

BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the present invention will be described below with reference to the drawings.

(First embodiment)
A micro sample holder according to a first embodiment of the present invention will be described with reference to FIGS. 1 to 5. FIG.
The micro sample holder of the first embodiment is the
, 7, 8, 9, and 10.

As shown in FIGS. 1 and 2, the micro-sample holder 1 includes a container 7 corresponding to the main body of the holder, and a lid 10 that can be fitted to the container 7 .

For the container 7, for example, a clear case can be used. The clear case is transparent, and the beads 3 corresponding to the base inside, the grip sheet 5 corresponding to the adhesive material, and the thin film layer 6 made of gold can be seen from the outside. As this container 7, a clear case for storing free silicic acid measurement samples can be used. The container 7 is, for example, 35 mm long, 35 mm wide and 15 mm high with the lid 10 attached.

FIG. 1 shows the micro sample holder when the container 7 is not covered with the lid 10 . FIG. 2 shows a hypothetical micro-sample holder in which the container 7 and the lid 10 are separated. When the lid is closed, the top surface 13 of the container 7 and the bottom surface 14 of the lid 10 are brought together.

The cubic base 3 has a holding surface 12 whose lower surface is joined to the upper surface of the bottom plate 8 of the container 7 and which can hold a minute sample. The lower surface of the base 3 that is different from the holding surface 12 is joined to the upper surface of the container 7 .

For the base 3, for example, beads for handicrafts, which are cubes with a side of 7 mm, can be used. In the base, the collecting surface corresponding to the holding surface 12 is higher than the container wall (top surface 13 of the side plate 9 to be described later). Moreover, the base used is one in which the lid body 10 does not come into contact with the collecting surface.
The adhesive material 5 attached to the holding surface 12 of the base 3 is a grip sheet. For the grip sheet, for example, HG70-58 manufactured by Micro Support Co., Ltd. is used. A grip sheet is a non-conducting thin adhesive tape.

The thin film layer 6 is made of gold, and the grip sheet 5 attached to the holding surface 12 of the base 3 is vapor-deposited with 200 to 300 Å of gold, for example. Gold reflects infrared light. Only the infrared absorption spectrum of the minute sample captured by the stickiness of the grip sheet is detected. Furthermore, during the measurement, the grip sheet does not detect the wavelength.
At this time, if a large amount of gold is vapor-deposited, the stickiness of the grip sheet is lost. In addition, if the amount of deposited gold is small, the wavelength due to the grip sheet will be detected during measurement.

The lid 10 is attachable to and detachable from the container 7 and can cooperate with the container 7 to protect and manage the base 3 and the thin film layer 6 .

The container 7 is composed of a square bottom plate 8 and side plates 9 rising from the four sides of the bottom plate 8. The holding surface 12 of the base 3 joined to the upper surface 11 of the bottom plate 8 is level with the top surface 13 of the side plate 9. is higher than The outer wall of the side plate 9 of the container 7 corresponds to the grip. The operator's hand grips the outer wall of the side plate 9 of the container 7 when collecting the minute sample. At this time, the holding surface 12 of the base 3 is provided at a level (position) that protrudes from the level of the top surface 13 of the side plate 9 corresponding to the grip portion held by hand.

As a result, when the base 3 is pressed against a micro sample to be analyzed such as a foreign substance, the micro sample is embedded in the thin film layer 6 formed on the holding surface 12 of the base 3 and having characteristics such as adhesiveness of the rare metal. retained. Therefore, the micro sample can be transported to the destination while being embedded and protected in the rare metal thin film layer 6 . Therefore, it is difficult to lose, difficult to be contaminated or degraded, it can be safely delivered to an analysis room, and misidentification of component detection is less likely to occur during analysis.
(Example of usage)

Next, an experimental example of analysis using the micro sample holder of the present invention is shown below.
The micro-sample holder 1 can be used as a collection kit for analytical instruments, for example, infrared spectroscopy, scanning electron microscope SEM, or electron probe microanalyzer EPMA.

Sampling of the micro-sample holder 1 is performed by removing the lid 10 of the container 7 of the collection kit, and directly touching the surface of the sample (micro-sample), which is a foreign substance, with the feeling of pressing a stamp. A grip sheet 5 forming a thin layer 6 of gold is pressed against. Then, the target sample is embedded in the grip sheet 5 and held. Thereafter, the lid 10 is attached to the container 7, the target sample is stored, and the container 7 is moved to the destination analysis room.

The micro sample holder 1 is analyzed by removing the cover 10 of the sampling kit, placing the sample on the FT-IR stage, determining the sample position and aperture size, and pressing a prism against it for measurement. Since the grip sheet is a hard type, it can only be pushed into a small depth. Auto measurement is also possible. At this time, the measurement can be performed even if the aperture diameter is made wider than the object.

In the analysis of minute samples, minute means 1 mm or less. The foreign matter is minute and has a three-dimensional shape, a film shape, a particle shape, or the like.

(experimental data)
Next, FIG. 3 to FIG. 5 show experimental data using the micro-sample holder in the ATR method.

The micro sample holder includes, for example, resin beads 3 as a base, a grip sheet 5 as an adhesive, gold as a thin film layer, a clear case as a container, and a transparent lid.

Experimental data 1 is experimental data with an aperture size of 100 μm×100 μm, and as shown in FIG. . According to this experimental data 1, the wavelength of the grip sheet was detected.

Experimental data 2 has an aperture size of 100 μm×100 μm, and as shown in FIG. It is experimental data using a holder. According to this experimental data 2, since gold absorbs infrared rays, the wavelength of the grip sheet 5 as shown in FIG. 3 was not detected, resulting in a blank.

From this, it was found that when an adhesive material, which is a grip sheet, is attached to a base, which is a bead, and gold is vapor-deposited thereon, it functions as a micro-sample holder for an analytical instrument.

Experimental data 3 has an aperture size of 400 μm×200 μm, and as shown in FIG. of wavelengths are detected.
Comparing FIG. 5 with FIG. 4, it is clear from the comparison with the blank shown in FIG. 4 that the wavelength of the hair shown in FIG. 5 is detected.

(Second embodiment)
A second embodiment of the present invention will be described with reference to FIGS. 6 to 9. FIG.

The micro sample holder of the second embodiment corresponds to the inventions described in claims 1, 5, 7, 11, 12, and 13 of the scope of claims.

As shown in FIG. 6, the micro-sample holder 21 includes a handle 25 corresponding to a pen-shaped holder main body and a cylindrical cap 26 with a bottom that can be attached to and detached from the handle 25 .
FIG. 6 shows a state in which a cap 26 corresponding to a lid body is removed from a cylindrical handle 25. As shown in FIG.
A sample container 23 corresponding to a base is connected to one end 251 of the handle 25 via the connecting portion 34 . The sample container 23 is made of aluminum, for example, and has a T-shaped longitudinal section.

The connecting portion 34 includes a mounting portion for the sample container 23, a fitting portion for holding the mounting portion between one end 251 of the handle 25, and one end 251 of the handle 25 and the sample container 23. It has a spring mechanism that does not. The state shown in FIG. 6 shows a state in which the handle 25 and the sample container 23 are engaged and fixed.

The sample container 23 is provided at a position protruding from the grip portion 252 held by hand, and the holding surface 12 of the sample container 23 is formed on the protruding position side.

The holding surface 12 of the sample container 23 has a plate member 24 made of indium on the side opposite to the handle 25 . A plate member 24 made of indium and a sample container 23 constitute a sampling section 22 . The collection part 22 is connected to one end 251 of the handle 25 .

A cap 26 corresponding to a lid is a cylindrical cap with a bottom similar to the cap of an art knife. By inserting the opening 27 into the handle 25 in the direction of arrow 31 shown in FIG. The cap 26 is attachable/detachable with respect to the handle 25 .

A plate member 24 made of indium is fixed to the holding surface 12 . A plate member 24 made of indium can hold a minute sample embedded therein.

Indium is used because indium is flexible at room temperature, plastically deforms when foreign matter is pressed against it, traps foreign matter, does not cause chemical reaction with trapped foreign matter, and is resistant to deterioration. be.

(When collecting)
To collect (sampling) a micro-sample using the micro-sample holder 21, remove the cap 26 of the collection kit, and directly apply the micro-sample to the surface to which the micro-sample as the object is attached, as if pressing a pencil. is pressed to embed the minute sample in the plate material 24 made of indium of the sample container 23 .

(during transportation)
Next, with the micro sample embedded in the plate material 24 made of indium, the handle 25 with the cap 26 fitted in the direction of the arrow 31 so as to protect the micro sample captured in the sample container 23 by the sampling part 22 is brought to the destination. For example, move to an analysis room. At this time, since it is a holder in the form of a pen-type holder, it can be carried in a pocket.

(at the time of analysis)
A method for analyzing the micro sample holder 21 is to remove the cap 26 of the micro sample holder 21 shown in FIG. Next, the sample container 23 corresponding to the base is sandwiched between fixing jigs (clips) 28 and the fixing jigs 28 are placed on the mounting table 32 . Here, the fixing jig 28 is of a form capable of maintaining the holding surface of the sample container horizontally.

Next, observation of the minute sample held in the sample container 23 or FT-IR ATR measurement is performed.

As shown in FIG. 7, the sampling part 22 of the micro-sample holder 21 has a sampling jig attached to a portion corresponding to, for example, the blade of an art knife, and is kept horizontal during observation or measurement. It is fixed by a fixing jig 28 . The picking part 22 is sandwiched between the fixing jigs 28 .

(experimental data)
8 and 9 show experimental data using the micro-sample holder 21 shown in FIG. 6 in the ATR method.

Experimental data 4, as shown in FIG. 8, in the ATR method, when the aperture size is 100 μm × 100 μm, and the micro sample is cellulose, the micro sample holder is used to measure with an analytical instrument. of wavelengths were detected.

Experimental data 5, as shown in FIG. 9, in the ATR method, when the aperture size is 100 μm×100 μm and the micro-sample object is an eraser, the micro-sample holder is used to measure with an analytical instrument. of wavelengths were detected.

(Other embodiments)
The grip sheet 5 as the adhesive material and the gold thin film layer 6 used in the first embodiment may be made of an indium plate according to the present invention.

In the first embodiment, the top surface 13 of the container 7 and the bottom surface 14 of the lid 10 are flat. It is good also as an uneven surface which carries out.
In the first embodiment, a clear case is used for the container 7, but a non-transparent holder main body may be used in the present invention.
The base of the present invention may not be beads and may be made of other materials.
The adhesive material of the present invention does not have to be a grip sheet, and may be another adhesive material.

In the second embodiment, the sample container corresponding to the base is made of aluminum and has a T-shaped longitudinal section. However, in the present invention, the material and shape of the base are not limited to these. is.
In the present invention, the indium plate member 24 formed on the holding surface 12 of the sample container 23 of the second embodiment may be replaced with an adhesive material such as a grip sheet and a thin gold layer formed thereon.
The base of the present invention has a holding surface capable of fixing a rare metal such as indium.

Although clips were used as the fixing jigs used in the second embodiment, fixing jigs other than clips may be used in the present invention.

Gold and indium in the above embodiments may be one or more rare metals selected from other rare metals.

As described above, the present invention is not limited to the above-described embodiments, and can be implemented in various forms without departing from the gist of the present invention.

1 micro sample holder,
3 beads (base),
5 grip sheet (adhesive material),
6 thin film layer,
7 container (main body of holder),
8 bottom plate,
9 side plate (gripping portion),
10 lid,
11 upper surface 12 holding surface,
21 micro sample holder,
22 sampling unit,
23 sample container (base),
24 plate material made of indium,
25 handle (holder main body),
26 cap (cover),
28 clip (fixing jig),
34 connecting part,
251 one end,
252 gripper;

A micro-sample holder of the present invention is a holder for collecting, transporting, and measuring a micro-sample, and comprises a base (3, 23) having a holding surface (12) capable of holding a micro-sample. and gold formed on the holding surface via an adhesive material (5) , or one or more metal materials (6, 24) selected from rare metals formed on the holding surface, and the base a holder body (7, 25) connected to a portion different from the holding surface ; and a rare metal material such as gold or indium, which is detachable from the holder body and cooperates with the holder body. and a lid body (10, 26) capable of storing the .

Indium is a rare metal and does not become a foreign substance to be detected. Also, gold and indium are soft metals. Gold and indium rarely contaminate during extraction, transport, or measurement.
Lead is excluded from the thin film layer because it becomes a foreign substance that is a detection target.

(First embodiment)
A micro sample holder according to a first embodiment of the present invention will be described with reference to FIGS. 1 to 5. FIG.
The micro sample holder of the first embodiment corresponds to the inventions described in claims 1, 2, 3, 6, 7, 8, 9 and 10 of the scope of claims.

The micro-sample holder of the second embodiment corresponds to the inventions described in claims 1, 4, 7, 11, 12, and 13 of the scope of claims.

Claims (14)

A holder for collecting, transporting, and measuring minute samples,
a base (3, 23) having a holding surface (12) capable of holding a minute sample;
one or more rare metal materials (6, 24) selected from rare metals such as gold and indium, which are formed on the holding surface;
and a holder main body (7, 25) connected to a portion of the base different from the holding surface. an adhesive material (5) attached to the holding surface;
A micro-sample holder according to claim 1, further comprising a thin film layer made of said one or more kinds of rare metal materials formed on said adhered adhesive material. 3. The micro-sample holder according to claim 2, wherein the adhesive material is a grip sheet. 3. The micro sample holder according to claim 2, wherein said thin film layer is gold. 2. A lid body (10, 26) according to claim 1, which is detachable from said holder body and capable of storing said base and said one or more rare metal materials in cooperation with said holder body. Micro sample holder. The holder main body is composed of a square bottom plate (8) and side plates (9) rising from the four sides of the bottom plate. 4. The holder for a micro sample according to claim 3, which is higher than the level of the top surface (13) of said side plate. 2. The micro-sample holder according to claim 1, wherein said holder main body comprises a hand-operated grip for pressing said micro-sample against said one or more kinds of rare metal materials when collecting said micro-sample. 2. A micro sample holder according to claim 1, wherein said holder main body is made of transparent resin. 2. The micro-sample holder according to claim 1, wherein said base is a bead. 3. The micro-sample holder according to claim 2, wherein said thin film layer is a gold material having a thickness of 200-300 Å. The holder body is a pen-shaped holder body (25) that connects the base to one end (251), and cooperates with the one end of the pen-shaped holder body to accommodate the base and the one kind of 2. A micro sample holder according to claim 1, wherein said one end is provided with a detachable bottomed cylindrical cap (26) capable of storing said rare metal material. 12. The micro-sample holder according to claim 11, further comprising a connecting portion (34) that allows the base and the one end of the pen-shaped holder body to be detachably connected. 13. The micro sample holder according to claim 11 or 12, wherein said pen-shaped holder main body has a hand grip portion (252) for pressing said micro sample against said one or more kinds of rare metal materials when collecting said micro sample. . A method of using the micro sample holder according to claim 1 for collecting, transporting, and measuring a micro sample,
a step of operating the holder body to press the holding surface against a minute sample;
a step of holding a minute sample in one or more rare metal materials selected from rare metals such as gold and indium;
moving the holder body to a destination;
and measuring the minute sample without separating the minute sample from the one or more rare metal materials.

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