Measurement cell and method of manufacturing the same

Abstract

To provide a measurement cell which makes it easier to convey a measurement target sample and enables more accurate measurement of the measurement target sample.SOLUTION: A measurement cell for holding a target sample for Raman measurement is provided, the measurement cell comprising a base having a sample placement portion, or a recess for placing a sample, a lid for closing an open face of the sample placement portion, fastening members for fastening the lid to the base, a suction line connected to the sample placement portion of the base and to a suction device for sucking air out of the sample placement portion, and a valve provided in the suction line.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present disclosure relates to a measurement cell that holds a sample to be measured in Raman measurement, and a method for producing the measurement cell. [Background technology]

[0002] One method for analyzing components involves irradiating a sample to be measured with measurement light of a specific wavelength and measuring Raman scattered light. Patent Document 1 describes a container for holding a sample to be measured. Patent Document 1 describes a closed observation container (measurement cell) that includes a flat observation container body having a first recess formed in the center and a second recess formed at the bottom of the first recess, an observation window material that is housed in the first recess and covers the top of the second recess, thereby forming a sample chamber in the second recess, and a lid member that has a through-hole formed in the center through which the sample chamber can be seen and that covers the outer peripheral edge of the observation window material and the outer peripheral surface of the observation container body. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Patent No. 5779963 Summary of the Invention [Problem to be solved by the invention]

[0004] The components of the sample held in the measurement cell may change depending on the measurement target. If the components change when the measurement is performed, the measurement accuracy will decrease. Furthermore, there is a need to be able to handle cases where the sample is collected at different locations and the sample is measured at different locations, or where it takes time from collection to measurement.

[0005] The present disclosure is intended to solve the above-mentioned problems, and aims to provide a measurement cell and a method for creating a measurement cell that can easily transport a sample to be measured and can more accurately measure the sample to be measured. [Means for solving the problem]

[0006] In order to achieve the above-mentioned object, the measurement cell of the present disclosure is a measurement cell that holds a sample to be measured in Raman measurement, and includes a base having a sample placement section that is a recess on which the sample is placed, a lid that closes the open surface of the sample placement section, a fastening member that fastens the base and the lid, a suction line that is connected to the sample placement section of the base and connects to a suction device that sucks air from the sample placement section, and a valve that is arranged on the suction line.

[0007] The presently disclosed method for creating a measurement cell is a method for creating a measurement cell that holds a sample to be measured for Raman measurement, and includes the steps of placing the sample in a sample placement section at the base of the measurement cell, and sucking air out of the sample placement section. [Effects of the Invention]

[0008] According to the present disclosure, the sample to be measured can be easily transported, and the sample to be measured can be measured more accurately. [Brief explanation of the drawings]

[0009] [Figure 1] FIG. 1 is a schematic diagram showing an example of a measurement system including a measurement cell according to this embodiment. [Figure 2] FIG. 2 is a perspective view showing an example of a measurement cell. [Figure 3] FIG. 3 is a front view showing the base of the measurement cell. [Figure 4] FIG. 4 is a front view showing the lid of the measurement cell. [Figure 5] FIG. 5 is a perspective view showing the surface of the lid of the measurement cell that comes into contact with the base. [Figure 6] FIG. 6 is a flowchart showing an example of a measurement method using a measurement cell. [Figure 7] FIG. 7 is a perspective view showing another example of the measurement cell. [Figure 8]FIG. 8 is a perspective view showing another example of the measurement cell. [Figure 9] FIG. 9 is a front view showing another example of the measurement cell. [Figure 10] FIG. 10 is an explanatory diagram illustrating an example of a sample supply method. DETAILED DESCRIPTION OF THE INVENTION

[0010] Preferred embodiments of the present disclosure will be described in detail below with reference to the drawings. Note that the present disclosure is not limited to these embodiments, and when there are multiple embodiments, the present disclosure also includes configurations that combine the embodiments. Furthermore, the components in the embodiments include those that can be easily imagined by a person skilled in the art, those that are substantially identical, and those that are within the so-called equivalent range.

[0011] FIG. 1 is a schematic diagram showing an example of a measurement system including a measurement cell according to this embodiment. The measurement cell (vacuum cell for Raman measurement) according to this embodiment irradiates a measurement light of a predetermined wavelength onto a sample to be measured, and measures the Raman scattered light generated in the sample to measure the components of the sample. The measurement system 1 measures the sample to be measured, which is obtained from a measurement object holding facility 2. The measurement object holding facility 2 is not particularly limited, and can be various facilities such as a factory, chemical plant, power plant, research institute, etc. The measurement object sample is also not particularly limited. The measurement system 1 collects the sample from the measurement object holding facility 2.

[0012] The measurement system 1 includes a measurement device 4, a suction device 6, an inert gas supply device 8, and a measurement cell 10. In the measurement cell 10, a sample collected at the measurement target holding facility 2 is placed at a predetermined position. The configuration of the measurement cell 10 will be described later.

[0013] The measuring device 4 measures the components of a sample using Raman spectroscopy. The measuring device 4 irradiates the sample in the measuring cell 10 with measurement light and measures the generated Raman scattered light. The measuring device 4 measures the components of the sample based on the wavelength and intensity of the Raman scattered light.

[0014] The suction device 6 suctions gas from the measurement cell 10. The suction device 6 is, for example, a rotary pump. In this embodiment, the pressure inside the measurement cell 10 is reduced by reducing the gas in the measurement cell 10, thereby approaching a vacuum state. The inert gas supply device 8 supplies an inert gas to the measurement cell 10, creating an inert gas atmosphere inside the measurement cell 10.

[0015] The measurement cell will be described with reference to Figs. 2 to 5. Fig. 2 is a perspective view showing an example of a measurement cell. Fig. 3 is a front view showing the base of the measurement cell. Fig. 4 is a front view showing the lid of the measurement cell. Fig. 5 is a perspective view showing the surface of the lid of the measurement cell that contacts the base. The measurement cell 10 has a base 12, a lid 14, a fastening member 16, a suction line 18, an air supply line 20, an on-off valve 22, an on-off valve 24, and a seal portion 26.

[0016] The base 12 is plate-shaped, in this embodiment, a disk-shaped plate, and is formed with a sample placement section 30, a screw hole 32, and a groove 34. The sample to be measured is placed in the sample placement section 30. The sample placement section 30 is a recess formed in the base 12, having a bottom surface, side surfaces, and an open top surface. The screw hole 32 is formed on the surface of the base 12 on which the sample placement section 30 is formed. In this embodiment, the screw holes 32 are arranged at four locations at 90-degree intervals on a circle of a predetermined radius centered on the center of the disk of the base 12. The groove 34 is located on the same surface as the sample placement section 30, and is a ring-shaped groove formed around the entire outer periphery of the sample placement section 30, at a position closer to the center than the screw hole 32 on the outer side of the sample placement section 30. The groove 34 is shallower than the sample placement section 30. A seal member 26 is inserted into the groove 34.

[0017] The lid 14 covers the exposed surface of the sample placement section 30 of the base 12. The lid 14 has a window 40, a hole 42, and a groove 44. The window 40 is located at the center of the lid 14, in a position that allows the area of ​​the sample placement section 30 where the sample is placed to be visible when the lid 14 is fixed to the base 12. The window 40 is made of a material that transmits the measurement light and Raman scattered light of the measurement device 4. The window 40 is made of transparent resin, glass, or the like. The hole 42 is a through-hole formed in the lid 14. In this embodiment, the hole 42 is located at four positions that overlap with the screw holes 32 of the base 12 and are spaced 90 degrees apart on a circle of a predetermined radius centered on the center of the base 12. The groove 44 is disposed on the surface facing the base 12, and is a ring-shaped groove formed around the entire outer periphery of the sample placement section 30 at a position closer to the center than the outer hole 42 of the sample placement section 30 when the sample placement section 30 is fixed to the base 12. The groove 44 is a shallow groove. The seal member 26 is inserted into the groove 44.

[0018] Fastening members 16 fasten lid portion 14 to base portion 12. Fastening members 16 are, for example, screws, and are arranged in four locations in this embodiment. By attaching and detaching fastening members 16, it is possible to switch between a state in which lid portion 14 is fastened to base portion 12 and a state in which lid portion 14 and base portion 12 are separated.

[0019] The suction line 18 is a conduit connected to the sample placement section 30. In this embodiment, the conduit is an opening on the side surface of the disk of the base 12 and connected to the sample placement section 30, but the path is not particularly limited. The suction line 18 can be connected to the suction device 6. The on-off valve 22 is a valve that opens and closes the suction line 18. In this embodiment, the valve of the suction line 18 is the on-off valve 22, but the suction line 18 may be any valve that prevents outside air from flowing into the sample placement section 30, and may be, for example, a check valve that allows fluid to flow only in the direction of discharging the fluid in the sample placement section 30 to the outside and prevents fluid from flowing in the opposite direction.

[0020] The gas supply line 20 is a conduit connected to the sample placement section 30. In this embodiment, the conduit opens on the side surface of the disk of the base 12 and connects to the sample placement section 30, but the path is not particularly limited. The gas supply line 20 can be connected to an inert gas supply device 8. The on-off valve 22 is a valve that opens and closes the gas intake line 20.

[0021] The seal portion 26 seals between the base portion 12 and the lid portion 14. The seal portion 26 separates the area surrounded by the sample placement portion 30 and the lid portion 14 from the outside area. The seal portion 26 is, for example, an O-ring, and is inserted into the grooves 34, 44. Note that the grooves 34, 44 may be provided on only one side.

[0022] Next, a measurement method using a measurement cell will be described with reference to Fig. 6. Fig. 6 is a flowchart showing an example of a measurement method using a measurement cell. The processing in Fig. 6 may be performed by an operator or automatically using a conveying machine or the like. In the following, the processing will be described assuming that it is performed by the measurement system 1.

[0023] The measurement system 1 acquires a sample from the facility that has the measurement target (step S12). If the measurement target is a substance stored at a predetermined location, the measurement system 1 collects the stored substance at a predetermined value. If the measurement target is a foreign substance contained in a liquid flowing through a pipe, the measurement system 1 collects a substance captured by a filter in the pipe.

[0024] Next, the measurement system 1 places the sample in the sample placement section (step S14). That is, the sample acquired from the measurement target facility is placed in the sample placement section. The measurement system 1 places the lid section on the base and fastens them with a fastening member (step S16). That is, the open part of the sample placement section is closed with the lid section 14, and the fastening member 16 tightly attaches the lid section 14 to the base section 12. The gap between the base section 12 and the lid section 14 is sealed with the seal section 26.

[0025] The measurement system 1 connects the suction device and the inert gas supply device (step S18). That is, the suction device 6 is connected to the suction line 18, and the inert gas supply device 8 is connected to the gas supply line 20. The connection of the lines and each part may be performed between steps S12 and S16.

[0026] The measurement system 1 supplies an inert gas while sucking air from the sample placement section (step S20). That is, the gas in the sample placement section 30 is replaced with an inert gas to create an inert gas atmosphere. The measurement system 1 stops the supply of the inert gas and continues sucking air from the sample placement section (step S22). That is, the gas in the sample objective 30 is reduced to reduce the pressure. The measurement system 1 closes the on-off valve (step S24). After reducing the pressure to a predetermined level, the measurement system 1 closes the on-off valves 22 and 24 to maintain the pressure and atmosphere in the sample placement section 30. The measurement system 1 measures the measurement cell with a measurement device (step S26).

[0027] The measurement cell 10 of this embodiment is provided with a suction line 18, which reduces the pressure in the sample placement section 30, thereby reducing changes in the atmosphere in which the sample is placed. This suppresses changes in the sample placed in the measurement cell 10, allowing accurate measurement of the measurement target using Raman spectroscopy. For example, oxidation can be suppressed even when the sample is made of a material that is easily oxidized. Furthermore, deterioration of the sample can be suppressed even when the measurement device 4 is located in a different location from the measurement target holding facility 2 and it takes time from sample collection to measurement.

[0028] To suppress oxidation, alcohol is preferably used as a sample collection method. Specifically, the filter on which the sample has been collected is immersed in a solvent capable of removing water, and the sample adhering to the filter is dispersed in ethanol. It is desirable to dissolve the filter in an organic solvent capable of dissolving the filter before solvent dispersion. The sample is re-collected after removing the solvent from the solvent in which the sample was dispersed. The sample in the solvent is placed in the sample placement section 30, and the atmosphere is replaced with an inert gas, after which it is aspirated. This prevents the sample from coming into contact with oxygen, thereby suppressing oxidation.

[0029] Measurement system 1 is 10 -5It is preferable to reduce the pressure to atmospheric pressure or less. The measurement cell 10 has an airtight mechanism that can maintain the above degree of vacuum. By maintaining the measurement cell 10 at a degree of vacuum within the above range, deterioration of the sample can be suppressed.

[0030] The measurement cell 10 is provided with a suction line 18 and an air supply line 20, and by making each line detachable from the suction device 6 and the inert gas supply device 8, the measurement cell 10 can be made smaller and easier to transport.

[0031] The measurement cell 10 is provided with an air supply line 20, which allows the air in the sample placement section 30 to be replaced with the desired component. In this embodiment, an inert gas is supplied, but a line for supplying a liquid may also be used. By filling the sample placement section 30 with a liquid and sucking the internal fluid through the suction line 18, deterioration of the sample in the sample placement section 30 can be suppressed. Furthermore, if the sample is liquid, the measurement cell 10 can also supply the liquid through the air supply line 20. Furthermore, the measurement cell 10 can be suitably transported even when the measurement target holding facility 2 and the measurement device 4 are separated from each other, and deterioration of the sample during transport can be suppressed.

[0032] Although the measuring cell 10 of this embodiment is provided with one suction line 18 and one gas supply line 20, it is sufficient to have at least one suction line 18. For example, two suction lines 18 may be provided.

[0033] Next, another example of the measurement cell will be described with reference to Fig. 7. Fig. 7 is a perspective view showing another example of the measurement cell. The measurement cell 10a shown in Fig. 7 has a sample adhering material 70 and a spacer 72 in addition to the configuration of each part of the measurement cell 10 shown in Fig. 2. The other configurations are the same as those of each part of the measurement cell 10.

[0034] The sample attachment 70 is a filter that collects a sample at the measurement target holding facility 2. The sample attachment 70 is placed, for example, in a pipe at a predetermined position in the measurement target holding facility 2 to capture foreign matter contained in the fluid flowing through the pipe. The sample attachment 70 is made of a porous material. The spacer 72 is placed in the sample placement section 30. The spacer 72 is ring-shaped, with a hollow center of the disk of the base 12. The spacer 72 is placed between the sample attachment 70 and the lid 14. By sandwiching the sample attachment 70 between the bottom surface of the sample placement section 30 and the spacer 72, the position of the sample attachment 70 in the depth direction of the sample placement section 30 is fixed at a predetermined position, thereby improving measurement accuracy and stabilizing the sample, making it easier to transport. The spacer 72 has holes formed therein that communicate with the suction line 18 and the air supply line 20.

[0035] The measurement cell 10a can stably hold the sample to be measured by placing the spacer 72 in the sample placement section 30. In this embodiment, the atmosphere on the surface of the sample-adhered object 30 can be stabilized by sandwiching the sample-adhered object 70 between the spacer 72 and the bottom surface of the sample-adhered object 30, but the sample-adhered object 70 may also be sandwiched between the lid section 14 and the spacer 72.

[0036] Next, another example of the measurement cell will be described with reference to Fig. 8. Fig. 8 is a perspective view showing another example of the measurement cell. The measurement cell 10b shown in Fig. 8 has an attachment 80 in addition to the configuration of each part of the measurement cell 10 shown in Fig. 2. The other configurations are the same as those of each part of the measurement cell 10.

[0037] The attachment 80 has a disk shape that can be detachably placed on the sample placement section 30. The attachment 80 has a recess 82. The recess 82 is a depression in which a sample can be placed. The attachment 80 is formed with a through-hole that connects the suction line 18 to the recess 82, and a through-hole that connects the air supply line 20 to the recess 82.

[0038] The measurement cell 10b allows a sample to be placed in a predetermined position on the sample placement section 30 by placing the sample on an attachment 80 that can be attached to and detached from the sample placement section 30. This improves measurement accuracy and stabilizes the sample, making it easier to transport. Furthermore, the sample can be collected in a recess 82, which is a smaller depression than the sample placement section 30, making it possible to suitably measure even trace amounts of sample. The attachment 80 is suitable for use when the sample is a powder. Furthermore, the attachment 80 can fill the space within the sample placement section 30, making it easier to replace the air with an inert gas or reduce the pressure.

[0039] Next, another example of the measurement cell will be described with reference to Figures 9 and 10. Figure 9 is a front view showing another example of the measurement cell. Figure 10 is an explanatory diagram showing an example of a sample supply method. The measurement cell 10c shown in Figures 9 and 10 has a sample supply path 90, a sealing plug 94, and a sample injection device 96 in addition to the configuration of each part of the measurement cell 10 shown in Figure 2. The other configurations are the same as those of each part of the measurement cell 10.

[0040] The sample supply path 90 is a conduit that opens into the side surface of the base 12 and is connected to the sample placement section 30. A sealing plug 94 is placed at the end of the sample supply path 90 that opens into the side surface of the base 12. The sealing plug 94 closes the sample supply path 90. A sample injection device 96 is detachably connected to the sealing plug 94. The sample injection device 96 stores a sample mixed with a liquid and supplies the sample together with the liquid to the sample supply path 90. The measurement cell 10c is configured so that the sample supplied to the sample supply path 90 reaches the sample placement section 30.

[0041] The measurement cell 10c is supplied with a sample through the sample supply path 90 and placed in the sample placement section 30. This allows the measurement cell 10c to supply a sample to the sample placement section 30 without opening or closing the lid 14 relative to the base 12. This eliminates the need to remove and fasten the fastening member 16, simplifying the work. Furthermore, by providing a sealing plug 94, the sample placement section 30 can be disconnected from the outside, and the interior can be depressurized by sucking in a fluid using the suction line 18.

[0042] [Effects of this embodiment] The present disclosure has the following features, but is not limited to the following. (1) A measurement cell that holds a sample to be measured for Raman measurement, the measurement cell having: a base having a sample placement section that is a recess on which the sample is placed; a lid that closes the open surface of the sample placement section; a fastening member that fastens the base and the lid; a suction line that is connected to the sample placement section of the base and connects to a suction device that sucks air from the sample placement section; and a valve that is arranged on the suction line.

[0043] (2) The measurement cell according to (1), further comprising a sealing member for sealing between the base and the lid.

[0044] (3) The measurement cell according to (1) or (2), wherein the cover serves as a window that transmits measurement light for Raman measurement and Raman scattered light from the sample.

[0045] (4) A measurement cell according to any one of (1) to (3), which has a spacer that is placed in the sample placement section and maintains the depthwise position of the sample placement section of the filter on which the sample is placed.

[0046] (5) The measurement cell according to any one of (1) to (3), which has an attachment that is placed on the sample placement section and has a recess formed therein for holding the sample.

[0047] (6) A measurement cell described in any one of (1) to (5), which has an air supply line connected to the sample placement section of the base and connected to an inert gas supply device that supplies inert gas to the sample placement section, and an on-off valve that opens and closes the air supply line.

[0048] (7) The measurement cell according to any one of (1) to (6), further comprising a sample supply line formed in the base for supplying a sample to the sample placement section.

[0049] (8) A method for creating a measurement cell that holds a sample to be measured for Raman measurement, the method comprising the steps of placing the sample in a sample placement section at the base of the measurement cell, and sucking air out of the sample placement section.

[0050] (9) A method for preparing a measurement cell according to (8), in which a sample collection device that has collected a sample to be measured is immersed in alcohol, the sample is dispersed in the alcohol, and the sample together with the dispersed alcohol is placed in the sample placement section. [Explanation of symbols]

[0051] 1. Measurement System 2. Facilities subject to measurement 4. Measuring equipment 6 Suction device 8. Inert gas supply equipment 10. Measurement cell 12 base 14 Lid 16 Fastening members 18 Suction line 20 Air supply line 22, 24 On-off valve 26 Seal part 30 Sample placement section 32 screw holes 34 Groove 40 Window 42 holes

Claims

1. A measurement cell that holds a sample to be measured for Raman measurement, a base having a sample placement portion which is a recess on which a sample is placed; a lid portion that closes the open surface of the sample placement portion; a fastening member that fastens the base and the lid; a suction line connected to the sample placement portion of the base and connected to a suction device that suctions air from the sample placement portion; a valve disposed in the suction line.

2. 2. The measurement cell according to claim 1, further comprising a sealing member for sealing between the base and the lid.

3. 2. The measurement cell according to claim 1, wherein the lid portion is a window portion that transmits measurement light for Raman measurement and Raman scattered light from a sample.

4. 2. The measurement cell according to claim 1, further comprising a spacer that is placed on the sample placement section and that maintains the position of the sample placement section of the filter in the depth direction, on which the sample is placed.

5. 2. The measurement cell according to claim 1, further comprising an attachment that is placed on the sample placement section and has a recess formed therein for holding the sample.

6. an air supply line connected to the sample placement portion of the base and connected to an inert gas supply device that supplies an inert gas to the sample placement portion; 2. The measurement cell according to claim 1, further comprising an on-off valve that opens and closes the gas supply line.

7. 2. The measurement cell according to claim 1, further comprising a sample supply line formed in the base for supplying a sample to the sample placement portion.

8. A measurement cell preparation method for preparing a measurement cell holding a sample to be measured by Raman measurement, comprising: placing a sample on a sample placement portion at a base of the measurement cell; and a step of sucking air from the sample placement portion.

9. 9. A method for preparing a measurement cell according to claim 8, wherein a sample collecting device that has collected a sample to be measured is immersed in alcohol to disperse the sample in the alcohol, and the sample together with the dispersed alcohol is placed in the sample placement section.

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