Gas preparation device for odor evaluation

Abstract

This odor evaluation gas preparation device is provided with: a gas chromatograph (1) having a separation column (10) for separating a plurality of components contained in a gas to be analyzed; a time interval detection unit (2) that detects a time interval during which each of the plurality of components comes out of the separation column; a gas recovery unit (5) for recovering, into a sampling bag, a component gas containing all or part of the plurality of components discharged from the separation column; a gas introduction unit (56) that introduces a dilution gas into the sampling bag under predetermined gas introduction conditions; a flow rate information acquisition unit (14) that acquires flow rate information of the component gas; a time range setting unit (63, 65, 66) that sets a time range in which the gas recovery unit recovers the component gas with reference to the time interval; a total volume setting unit (63, 65, 66) that sets the total volume of the component gas collected into the sampling bag and the dilution gas introduced into the sampling bag; and a condition determination unit (62) that determines the gas introduction condition on the basis of the flow rate information, the time range, and the total volume.

Description

Technical Field

[0001] This invention relates to a gas preparation apparatus for evaluating the odor (stench, aroma) of various substances. Background Technology

[0002] Fragrances added to food, beverages, cosmetics, detergents, etc., are sometimes made by mimicking the aromas emitted by natural products such as flowers, herbs, and fruits (natural fragrances). Most natural fragrances are complex scents composed of a variety of ingredients, and the variety of scents produced depends on the types and proportions of the ingredients. However, not all components of a natural fragrance contribute to the formation of that scent; some contribute very little or nothing at all. In the field of fragrance development, there is a need to identify which components in natural fragrances contribute to scent formation and which do not.

[0003] The omission test is one method for identifying whether a component in a natural fragrance contributes to aroma formation. In the omission test, an omission gas is prepared by removing any component from the target gas. The omission gas is then compared to the target gas in terms of odor. Based on the similarity of their odors, the similarity is used to evaluate whether the removed component contributes to aroma formation.

[0004] For example, the aforementioned missing gas test can be performed efficiently using the odor evaluation device described in Patent Document 1. The odor evaluation device described in Patent Document 1 includes: a gas chromatograph having a separation column for separating the analyte gas; a gas recovery unit that, by passing the analyte gas through the separation column multiple times, recovers a gas containing all components exiting the separation column (full-component gas) and a gas from which a predetermined component has been removed (missing gas) into different sampling bags; an odor detection port for performing sensory evaluation by smelling the recovered gas in each sampling bag; and an odor sensor for detecting the odor of the recovered gas in each sampling bag. Then, based on the results of the sensory evaluation or the detection results of the odor sensor, an index value representing the similarity between the full-component gas and the missing gas is calculated.

[0005] In the aforementioned odor evaluation device, to prevent highly adsorbable components of the analyte gas from adhering to the flow path from the separation column to the gas recovery unit, a dilution gas is introduced into the flow path at a certain flow rate (pressure) while the separation column and the gas recovery unit are connected. Thus, while the gas containing the components from the separation column passes through the aforementioned flow path, the dilution gas is recovered into the sampling bag via the same flow path. With this configuration, the sampling bag contains the gas containing the components from the separation column, and an amount of dilution gas corresponding to the amount of the gas. The gas recovered into the sampling bag serves as the odor evaluation gas, used for sensory evaluation or odor detection using an odor sensor.

[0006] Existing technical documents Patent documents Patent Document 1: Japanese Patent Application Publication No. 2022-73441 Summary of the Invention The technical problem that the invention aims to solve Sensory evaluation using an odor detection port is performed by releasing the components contained in the gas recovered into the sampling bag through the odor detection port, and then having multiple evaluators sequentially smell the odor. Therefore, for sensory evaluation to be conducted, the sampling bag needs to be filled with a sufficiently large amount of gas. However, in the aforementioned conventional odor evaluation apparatus, since the amount of gas recovered into the sampling bag depends on the amount of gas containing the components exiting the separation column (or the duration of the gas flow through the aforementioned flow path), sensory evaluation can sometimes be difficult to perform, depending on the circumstances.

[0007] The problem this invention aims to solve is to easily prepare any amount of odor evaluation gas.

[0008] Solution to the above technical problems The odor evaluation gas preparation apparatus of the present invention, which was made to solve the above-mentioned problems, comprises: A gas chromatograph has a separation column that separates multiple components contained in an odorous analyte gas in the time direction; The time interval detection unit detects the time interval of each of the plurality of components as it exits the separation column; The gas recovery unit, by passing the analyte gas through the separation column, recovers all or part of the component gas containing the plurality of components exiting the separation column into the sampling bag; The gas inlet section introduces dilution gas into the sampling bag under predetermined gas inlet conditions; The flow information acquisition unit acquires flow information as information about the flow rate of the component gas exiting the separation column; The time range setting unit is used to set the time range for the gas recovery unit to recover the component gas by referring to the time ranges of each of the plurality of components detected by the time range detection unit; A total volume setting unit is used to set the total volume of the component gas recovered into the sampling bag and the dilution gas introduced into the sampling bag by the gas inlet unit; and The condition determination unit determines the gas introduction conditions of the gas introduction unit based on the flow information acquired by the flow information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit.

[0009] Invention Effects According to the present invention, odor evaluation gas of any volume can be easily prepared. Attached Figure Description

[0010] 【 Figure 1 A schematic structural diagram of a gas preparation apparatus for odor evaluation according to an embodiment of the present invention.

[0011] 【 Figure 2 [Image showing an example of a gas preparation condition setting screen on the display unit.]

[0012] 【 Figure 3 The flowchart shows the steps of the gas preparation condition setting unit in determining the conditions for introducing the dilution gas.

[0013] 【 Figure 4 This graph shows an example of the relationship between the pressure and flow rate of the dilution gas introduced through the gas inlet. Detailed Implementation

[0014] Hereinafter, an odor evaluation device as an embodiment of the present invention will be described with reference to the accompanying drawings.

[0015] <Structure of the Odor Evaluation Device> Figure 1 This is a schematic structural diagram of the odor evaluation device involved in this embodiment. The odor evaluation device in this embodiment is generally composed of a gas chromatography section (GC section) 1, a mass spectrometry section (MS section) 2, an odor measurement section 3, interface sections 41 and 42, and a gas recovery section 5.

[0016] The GC unit 1 includes: a chromatographic column 10 for separating the components contained in the target gas; a column oven 11 housing the chromatographic column 10; a sample injection unit 12 located at the inlet of the chromatographic column 10; a flow path switching unit 13 located at the outlet of the chromatographic column 10; and a GC control unit 14 for controlling these units.

[0017] MS unit 2 includes: a vacuum container 20; an ion source 21 for ionizing component molecules in a gas containing components from the chromatographic column 10 introduced from GC unit 1; an ion optical system 22 for transporting the generated ions; a quadrupole mass filter 23 as a mass separation unit for separating ions according to mass number; an ion detector 24 for detecting mass-separated ions; and an MS control unit 25 for controlling these units.

[0018] The interface section 41 is provided between the GC section 1 and the MS section 2, and includes a heater 411 that maintains the pipeline at a high temperature in order to prevent components in the gas from being captured (adsorbed) in the flow path.

[0019] The gas recovery unit 5 is disposed between the GC unit 1 and the odor measurement unit 3, and includes: an autosampler 54, equipped with a means for mounting multiple sampling bags 511 ( Figure 1 The image shows an installation port 51 for 12 sampling bags 511, an inlet / outlet port 52 for allowing gas to enter and exit the sampling bags 511 installed on the installation port 51, a first flow path switching unit 53 for switching the flow path between the inlet / outlet port 52 and the installation port 51, a second flow path switching unit 55 for switching the flow path between the inlet / outlet port 52 and the odor measuring unit 3 and the GC unit 1, a gas inlet unit 56 for introducing dilution gas in the flow path 7 between the flow path switching unit 13 and the second flow path switching unit 55, and upstream of the second flow path switching unit 55, and a gas recovery control unit 57 for controlling the first flow path switching unit 53, the second flow path switching unit 55 and the gas inlet unit 56.

[0020] An interface section 42 is provided on the flow path 7 between the GC section 1 and the gas recovery section 5, and includes a heater 421 for heating the flow path 7 to, for example, approximately 250°C. Furthermore, the inlet / outlet 52, the first flow path switching section 53, and the second flow path switching section 55 are also heated to, for example, approximately 250°C by heaters (not shown). Thus, the high-temperature gas containing components exiting the chromatographic column 10 is introduced into the gas recovery section 5 at its original temperature and recovered into the sampling bag 511 along with the dilution gas.

[0021] Furthermore, an odor detection port (not shown) is connected to the mounting port 51 of each sampling bag 511. This allows for sensory evaluation through human olfaction. For example, when comparing the odor of the gas recovered into the sampling bag 511 (the odor evaluation gas described later) with the gas to be analyzed, it is preferable to use the three-point comparison method, which is one of the sensory evaluation methods.

[0022] The odor measuring unit 3 comprises the following components: an inlet 31 for drawing in gas (the odor evaluation gas described later) recovered into the sampling bag 511; a dilution unit 32 for diluting the drawn-in odor evaluation gas; a concentration unit 33 for concentrating the drawn-in gas; and a sensor unit 34, which contains multiple odor sensors 341 with different response characteristics. Figure 1 The sensor unit 34 contains only one component (only one is shown in the image), used to measure odor evaluation gas containing various odor components; a pump 35, used to draw the odor evaluation gas into the sensor unit 34; an A / D converter 36, used to convert the detection signal generated by the odor sensor 341 into a digital signal; a signal processing unit 37, used to analyze and process the digitized detection signal; and an odor measurement control unit 39, used to control the overall operation of the odor measurement unit 3. The dilution unit 32, for example, consists of a syringe and its drive unit, which dilutes the odor evaluation gas using the syringe and sometimes also acts as a pump to push the gas into the sensor unit 34.

[0023] Odor sensor 341 is typically a metal oxide semiconductor sensor whose resistance varies with the odor component. However, it can also be a conductive polymer sensor, or a sensor based on other detection mechanisms, such as a sensor with a gas adsorption film formed on the surface of a quartz crystal oscillator or surface acoustic wave (SAW) device.

[0024] The signal processing unit 37 and the odor measurement and control unit 39 are configured around the personal computer 6. In addition to the above-mentioned components, the personal computer 6 also includes the following functional units: a data processing unit 61 for analyzing and processing signals acquired by the ion detector 24 of the MS unit 2; a central control unit 62 for comprehensively controlling the control units 14, 25, 39, and 57; a gas preparation condition setting unit 63 for setting the conditions for preparing the gas for odor evaluation; and a storage unit 64. The personal computer 6 is connected to an input unit 65 (such as a keyboard and mouse) and a display unit 66. Furthermore, in this embodiment, when recovering gas into the sampling bag 511, the GC unit 1, MS unit 2, and gas recovery unit 5 operate in conjunction. When the odor of the gas recovered into the sampling bag 511 is measured by the odor measurement unit 3, the gas recovery unit 5 functions as an autosampler, and the gas recovery unit 5 and the odor measurement unit 3 operate in conjunction.

[0025] Furthermore, although this embodiment describes that the GC unit 1, MS unit 2, odor measurement unit 3, and gas recovery unit 5 are controlled by different control units respectively, it is also possible, for example, that the GC unit 1 and MS unit 2 are controlled by a common control unit, and the odor measurement unit 3 and gas recovery unit 5 are controlled by a common control unit.

[0026] In the odor measurement unit 3, the composition of the gas is measured as follows: When the target gas is introduced into the sensor unit 34, the components in the target gas come into contact with multiple odor sensors 341, and each odor sensor 341 outputs its own different detection signal in parallel. This detection signal is sampled by the A / D conversion unit 36, digitized, and input to the signal processing unit 37. The signal processing unit 37 acquires one detection data point from each odor sensor 341 for each target gas. Therefore, for example, if the sensor unit 34 has 10 odor sensors 341, 10 detection data points will be obtained by measuring a certain target gas. Since the 10 odor sensors 341 each have different response characteristics, a 10-dimensional odor space can be envisioned with the outputs of these 10 odor sensors 341 as axes in different directions. The state where the outputs of all odor sensors 341 are zero is the origin of this odor space.

[0027] In the aforementioned odor space, the 10 detection data points can be positioned as a measurement point. Here, when considering the odor vector with the origin of the aforementioned odor space as the starting point and the measurement point as the ending point, the length of the odor vector corresponds to the "odor intensity" (i.e., the concentration of odor components in the target gas), and the direction of the odor vector corresponds to the "odor property." That is, if the direction of the odor vector obtained by measuring one target gas is close to the direction of the odor vector obtained by measuring another target gas, they can be considered to belong to similar types of odors; conversely, if the directions of the vectors differ greatly, they can be considered to belong to distant types of odors. Therefore, as an indicator of the similarity of the directions of two vectors, the angle θ between the two vectors can be used, and the similarity of the "odor property" can be determined based on this angle θ. For example, the similarity rate when the two odor vectors coincide (have the same direction) (i.e., when θ=0) is set to 100%, and the similarity rate is set to 0% when the angle θ is above a predetermined value α. Then, within the range of angle θ from 0 to α, the similarity rate is determined according to this angle θ.

[0028] Furthermore, since the output level of the odor sensor 341 is almost linear with respect to the concentration of the target gas (the concentration of the odor component), the direction of the odor vector remains constant regardless of the concentration of the same odor. Therefore, the angle θ between the two odor vectors also remains constant regardless of the concentration, thus allowing for accurate differentiation of the differences in odor properties between multiple target gases.

[0029] On the other hand, when the output of the odor sensor 341 relative to the concentration of odor components is non-linear, even for the same odor, the direction of the odor vector will change with concentration, making it difficult to accurately distinguish the differences in odor properties between multiple target gases. In this case, when measuring the target gas, feedback control can be performed on the dilution unit 32 and the concentration unit 33 based on the output values ​​of each odor sensor 341, thereby adjusting the concentration of the target gas introduced into the sensor unit 34 to always be a suitable concentration. Specifically, the detection signal obtained from the odor sensor 341 is located as a measurement point in the aforementioned odor space, an odor vector is created with the origin as the starting point and the measurement point as the ending point, and the length of the vector is calculated. Then, to make the length a predetermined value, the dilution rate in the dilution unit 32 or the concentration rate in the concentration unit 33 is controlled.

[0030] <Basic Operation of Odor Evaluation Device> Next, the basic operation of the odor evaluation device in this embodiment will be explained.

[0031] When various actions of using the odor evaluation device are instructed to be performed via the input unit 65, the GC control unit 14, MS control unit 25, odor measurement control unit 39, and gas recovery control unit 57, under the control of the central control unit 62, respectively control the GC unit 1, MS unit 2, odor measurement unit 3, and gas recovery unit 5.

[0032] Then, when the analyte gas, which has an odor and is extracted from a gaseous, liquid, or solid sample, is introduced into the sample injection unit 12 in a gaseous or liquid state, it is introduced into the chromatographic column 10 through the sample introduction unit 121. Furthermore, if the analyte gas is introduced in a liquid state, after being vaporized in the sample introduction unit 121, it is propelled by the carrier gas and introduced into the chromatographic column 10 from the sample introduction unit 121. The components contained in the analyte gas are separated during passage through the chromatographic column 10 and exit the column 10 at staggered times. After passing through the flow path switching unit 13, the components exiting the chromatographic column 10 are introduced into the MS unit 2 through the interface unit 41, or into the gas recovery unit 5 through the interface unit 42. Additionally, the GC control unit 14 acquires information such as the pressure at the carrier gas injection port (sample injection unit 12), the pressure at the carrier gas flow path switching unit 13, the dimensions of the separation column (length, inner diameter), and the temperature of the column oven 11, and calculates and stores the flow rate of the carrier gas (hereinafter referred to as the component gas) containing the components exiting the chromatographic column 10 based on this information. That is, in this embodiment, the GC control unit 14 is equivalent to the traffic information acquisition unit of the present invention.

[0033] When investigating the time interval during which each component of the analyte gas exits the chromatographic column 10, all components exiting the chromatographic column 10 are introduced into the MS unit 2. Therefore, from the start of introducing the analyte gas into the chromatographic column 10 until all components exit the chromatographic column 10, the flow path switching unit 13 is set to connect the GC unit 1 and the MS unit 2. As a result, the components exiting the chromatographic column 10 are sequentially introduced into the MS unit 2.

[0034] The components introduced into the MS unit 2 are ionized in the ion source 21 under the control of the MS control unit 25, and only ions with a specific mass number selected by the quadrupole mass filter 23 reach the ion detector 24. Then, mass scans are repeatedly performed in the quadrupole mass filter 23 within a predetermined mass range, and a detection signal as raw mass spectrometry data is obtained in the ion detector 24 for each scan.

[0035] The detection signal obtained from the ion detector 24 is processed by the data processing unit 61, and a mass spectrum with mass number as the horizontal axis and signal intensity as the vertical axis is repeatedly created. Furthermore, a total ion chromatogram (TIC) is created by focusing on time as the horizontal axis and signal intensity as the vertical axis, without considering mass number. Alternatively, a mass chromatogram can be created by focusing on a specific mass number and using time as the horizontal axis and signal intensity as the vertical axis. Creating a TIC is sufficient for detecting the time interval from which each component exits the chromatographic column 10, but a mass spectrum or mass chromatogram can also be created as needed. The TIC data created by the data processing unit 61 is stored in the data processing unit 61. Furthermore, the data processing unit 61 extracts peaks from the created TICs and stores information about those peaks (peak intensity, peak area, peak width (time range), etc.). In this embodiment, the MS unit 2 corresponds to the time interval detection unit of the present invention. Additionally, the term "time interval" here refers to the time range during which a certain component is detected by the MS unit 2.

[0036] In preparing a gas for evaluating the odor of components contained in the analyte gas (hereinafter referred to as odor evaluation gas), all or part of the components exiting the chromatographic column 10 are introduced into the gas recovery unit 5. That is, under the control of the GC control unit 14 and the gas recovery control unit 57, the drive motor of the flow path switching unit 13, the first flow path switching unit 53, and the second flow path switching unit 55 are switched between a state where the GC unit 1 is connected to the MS unit 2 and a state where the GC unit 1 is connected to the gas recovery unit 5. Furthermore, when the GC unit 1 is connected to the gas recovery unit 5, a dilution gas flows through the gas inlet unit 56 into the flow path 7 between the flow path switching unit 13 and the second flow path switching unit 55. As a result, the component gas exiting the chromatographic column 10 and the dilution gas are recovered together into the sampling bag 511 to prepare the odor evaluation gas. As the dilution gas, an odorless or nearly odorless gas that does not affect the odor of each component introduced into the gas recovery unit 5 is used, such as nitrogen or helium.

[0037] In this embodiment, a portion of the conditions for preparing the gas for odor evaluation are set by the user. The gas preparation condition setting unit 63 displays a gas preparation condition setting screen on the display unit 66 for the user to set these conditions, and receives input from the user through the input unit 65. Figure 2 This is an example of a gas preparation condition setting screen 661. Furthermore, it is assumed that the time intervals during which each component of the analyte gas exits the chromatographic column 10 have been investigated before the user sets these conditions.

[0038] like Figure 2 As shown, the gas preparation condition setting screen 661 includes a TIC 662 created by the data processing unit 61 and a table 663 displaying the destination of the components exiting the chromatographic column 10. Furthermore, the table 663 includes a gas recovery time range display area 6631, a gas destination display area 6632, and an input field 6633 for setting the position of the sampling bag 511 for introducing the odor evaluation gas.

[0039] In the gas preparation condition setting screen 661, the user first sets the gas recovery time range for recovering the components (component gases) from the chromatographic column 10 to the sampling bag 511. The gas recovery time range is set, for example, by the user using a mouse to specify any time range on the TIC 662. Alternatively, the data processing unit 61 can automatically divide the entire time range of the TIC 662 into multiple segments, and the user can select the segmented time range on the TIC 662 by using a mouse or similar means.

[0040] When a gas recovery time range is set in TIC 662, its start and end points are displayed in the gas recovery time range display area 6631 of Table 663. Simultaneously, the word "FAS," indicating that the component gas from column 10 is introduced into gas recovery unit 5, is displayed in the gas introduction destination display area 6632. At this time, the start and end points of the remaining time range outside the set gas recovery time range in the entire time range of TIC 662 are also displayed in the gas recovery time range display area 6631. The word "MS," indicating that the component from column 10 is introduced into MS unit 2 (rejected), is displayed in the gas introduction destination display area 6632 corresponding to this remaining time range. When multiple time ranges for recovering components from column 10 are set on TIC 652, each time a new time range is set, its start and end points are displayed in the gas recovery time range display area 6631, and the start and end points of the remaining time ranges are updated.

[0041] Next, the user sets the position of the sampling bag 511 for recovering the component gas. The position of the sampling bag 511 is set, for example, by entering the number assigned to the mounting port (port) 51 to which the sampling bag 511 is connected in the input field 6633 of the table 663 using the keyboard.

[0042] When the sampling bag 511 is positioned, the gas preparation condition setting unit 63 displays a table 664 on the gas preparation condition setting screen 661. This table 664 includes an input field 6641 for setting the volume of the gas (component gas and dilution gas) introduced into the sampling bag. The user can, for example, input any volume into the input field 6641 using the keyboard to set the total volume of the component gas and dilution gas introduced into the sampling bag (the volume of the odor evaluation gas). The volume of the odor evaluation gas is preferably set to approximately 0.5L to 10L so that one or more people can perform sensory evaluations of the odor evaluation gas.

[0043] The settings described above (the gas recovery time range for the component gas extracted from the chromatographic column 10, the position of the sampling bag 511 for recovering the component gas, and the volume of the odor evaluation gas introduced into the sampling bag 511) are stored in the gas preparation condition setting unit 63. In this embodiment, the display unit 66 (gas preparation condition setting screen 661), the input unit 65, and the gas preparation condition setting unit 63 function as the time range setting unit and total volume setting unit of the present invention.

[0044] The gas preparation condition setting unit 63 also determines the conditions for the gas introduction unit 56 to introduce dilution gas into the sampling bag 511 based on the settings in the gas preparation condition setting screen 661. Figure 3This is a flowchart showing the steps of the gas preparation condition setting unit 63 in determining the conditions for introducing dilution gas.

[0045] First, the gas preparation condition setting unit 63 reads and obtains the flow rate of the component gas introduced into the gas recovery unit 5 from the chromatographic column 10 within the set gas recovery time range from the GC control unit 14 (step S101). Furthermore, the gas preparation condition setting unit 63 calculates the time during which the GC unit 1 and the gas recovery unit 5 are in communication based on the set gas recovery time range (step S102). Alternatively, step S101 can be performed after step S102.

[0046] Subsequently, the gas preparation condition setting unit 63 calculates the volume of the component gas recovered into the sampling bag 511 based on the flow rate of the component gas obtained in step S101 and the aforementioned time calculated in step S102 (step S103). Then, by subtracting the volume of the component gas from the set volume of the odor evaluation gas, the volume of the dilution gas introduced into the sampling bag 511 is calculated (step S104). Furthermore, by dividing this volume by the time calculated in step S102, the flow rate of the dilution gas introduced into the sampling bag 511 is calculated (step S105).

[0047] In this embodiment, the dilution gas flowing from the gas inlet 56 and the component gas flowing from the chromatographic column 10 are introduced into the sampling bag 511 through the flow path 7. Therefore, the flow rate of the dilution gas flowing from the gas inlet 56 varies depending on the flow rate of the component gas flowing from the chromatographic column 10 and the pressure of the dilution gas introduced into the gas inlet 56. Therefore, the relationship between the pressure and flow rate of the dilution gas under a certain component gas flow rate condition has been investigated in advance, and the formula representing this relationship is stored in advance in the storage unit 64 of the computer 6. Figure 4 This is an example of a graph showing the relationship between the pressure and flow rate of the dilution gas. The gas preparation condition setting unit 63 reads the relationship between the pressure and flow rate of the dilution gas from the storage unit 64, and calculates the pressure when the gas inlet unit 56 introduces the dilution gas by substituting the flow rate of the dilution gas calculated in step S105 (step S106).

[0048] Through the above steps, the pressure of the dilution gas introduced into the gas inlet unit 56 is determined. The gas preparation condition setting unit 63 displays the determined pressure in table 664. Furthermore, the gas preparation condition setting unit 63 creates a method file and saves it in the storage unit 64. This method file records the settings made by the user on the gas preparation condition setting screen 661, and the pressure of the dilution gas introduced based on those settings. Based on the created method file, the central control unit 62 comprehensively controls the GC control unit 14, the MS control unit 25, and the gas recovery control unit 57.

[0049] in addition, Figure 2 The following settings are shown: Components exiting the chromatographic column 10 in time ranges T2 and T6 as shown in TIC662 are recovered into sampling bag 511 connected to port 2, and components exiting the chromatographic column 10 in time range T4 are recovered into sampling bag 511 connected to port 3. Components exiting the chromatographic column 10 in both time ranges are recovered into sampling bag 511 connected to port 2. In this case, when the user first sets the time range T2 on the gas preparation condition setting screen 661, the gas preparation condition setting unit 63 considers the components (component gas) exiting the separation column within time range T2 as being recovered into sampling bag 511, and calculates the pressure when introducing dilution gas through steps S101 to S106. Then, when the user sets the time range T6, the gas preparation condition setting unit 63 again executes the processing of steps S101 to S106. At this time, in step S104, the gas preparation condition setting unit 63 calculates the volume of dilution gas to be introduced into the sampling bag, taking into account the volume of component gas recovered into the sampling bag 511 during time range T2. That is, the volume of dilution gas to be introduced into the sampling bag 511 is calculated by subtracting the volumes of component gas recovered into the sampling bag 511 during time range T2 and time range T6 from the set volume of odor evaluation gas. This updates the pressure when introducing the dilution gas. In this embodiment, the gas preparation condition setting unit 63 functions not only as part of the time range setting unit and total volume setting unit of the present invention, but also as the condition determination unit of the present invention.

[0050] Since the dilution gas serves to clean the flow path within the gas recovery unit 5, the gas inlet 56 preferably allows the dilution gas to flow through the flow path 7 in either the case where the component gas from the GC unit 1 is flowing through the flow path 7 or not. However, it is also possible to allow the dilution gas to flow through the flow path 7 only when the component gas from the GC unit 1 is flowing through the flow path 7, or even to prevent the dilution gas from flowing through the flow path 7 when the component gas exiting the chromatographic column 10 is introduced into the gas recovery unit 5.

[0051] When the component gas is introduced into the gas recovery unit 5, without allowing the dilution gas to flow through it, the gas introduction unit 56 can also allow the dilution gas to flow through the flow path 7 and into the sampling bag 511 after the component gas has been recovered to the sampling bag 511. In this case, the introduction time of the dilution gas into the sampling bag 511 can be set independently of the time it takes for the component gas to be recovered to the sampling bag 511. Alternatively, the introduction time can be determined by the gas preparation condition setting unit 63. For example, when the user sets the pressure for introducing the dilution gas into the gas introduction unit 56 on the gas preparation condition setting screen 661, the gas preparation condition setting unit 63 calculates the flow rate of the dilution gas based on the relationship between the pressure and flow rate of the dilution gas. Furthermore, the gas preparation condition setting unit 63 calculates the volume of the dilution gas introduced into the sampling bag 511 in the same manner as in steps S101 to S104. Then, the introduction time of the dilution gas is calculated by dividing the volume of the dilution gas by the flow rate of the dilution gas. Similarly, when the user sets the introduction time of the dilution gas in the gas inlet 56, the gas preparation condition setting unit 63 can also determine the pressure of the dilution gas when the gas inlet 56 introduces the dilution gas based on the volume of the dilution gas introduced into the sampling bag and the relationship between the flow rate and pressure of the dilution gas.

[0052] Furthermore, the dilution gas can also be introduced directly into the autosampler 54 from the gas inlet 56 without passing through the flow path 7. In this case, the GC control unit 14 (flow rate information acquisition unit) acquires information such as the pressure at the carrier gas injection port (sample injection unit 12) and the flow path switching unit 13, the dimensions (length, inner diameter) of the chromatographic column 10, and the temperature of the column oven 11, as well as the pressure information of the component gas at the second flow path switching unit 55, and calculates and stores the flow rate of the component gas introduced into the autosampler 54 based on this information. The dilution gas can be introduced into the autosampler 54 from the gas inlet 56 when the GC unit 1 and the gas recovery unit 5 are in communication, or it can be introduced after the component gas is recovered to the sampling bag 511. When the dilution gas is introduced when the GC unit 1 and the gas recovery unit 5 are in communication, it can be introduced into the autosampler 54 in a manner similar to that of the GC unit 1 and the gas recovery unit 5. Figure 3 The conditions for introducing the dilution gas are determined in the same manner as shown in the flowchart. When the dilution gas is introduced after the component gas has been recovered into sampling bag 511, the conditions for introducing the dilution gas can be determined in the same manner as the steps described in paragraph 0046 of the international publication.

[0053] Through the above steps, by introducing the gas to be analyzed into the chromatographic column 10, the odor evaluation gas containing all or part of the components coming out of the chromatographic column 10 is recovered into a predetermined sampling bag 511 in a predetermined volume.

[0054] The odor evaluation gas recovered in the sampling bag 511 is used for measurement or sensory evaluation by the odor measurement unit 3. When the odor evaluation gas is used for measurement by the odor measurement unit 3, the flow paths of the first and second flow path switching units 53 and 55 are switched under the control of the gas recovery control unit 57. Under the control of the odor measurement control unit 39, the odor evaluation gas is sequentially drawn from the sampling bag 511 into the sensor unit 34 by the pump 35. As a result, the components contained in the odor evaluation gas come into contact with multiple odor sensors 341, causing each odor sensor 341 to output a detection signal.

[0055] Furthermore, when the odor evaluation gas is used for sensory evaluation, multiple odor evaluation supervisors perform odor identification through multiple odor detection ports (not shown) connected to the mounting ports 51 of each sampling bag 511. Sensory evaluation can also be performed after the gas is collected in the sampling bag 511. Since the volume of the odor evaluation gas can be appropriately set according to the volume of the sampling bag 511, a suitable amount of odor evaluation gas can be prepared for sensory evaluation. Furthermore, it is possible to prevent gas from being introduced into the sampling bag 511 and exceeding the volume of the sampling bag 511.

[0056] (Variation example) The present invention is not limited to the above embodiments and can be modified appropriately.

[0057] For example, in the above embodiment, the operator uses a keyboard or the like to input the volume of the odor evaluation gas recovered to the sampling bag 511 in the gas preparation condition setting screen 661. However, the volume of the odor evaluation gas can also be pre-stored in the storage unit 64 in association with the type of sampling bag 511, and the volume of the odor evaluation gas can be set by selecting the type of sampling bag 511 that recovers the odor evaluation gas.

[0058] Furthermore, in the above embodiments, it was explained that by passing the analyte gas through the chromatographic column 10 once, components exiting the column 10 within non-overlapping time ranges were recovered into different sampling bags 511. However, it is also possible, for example, to pass the analyte gas through the chromatographic column 10 multiple times, recovering components exiting the column 10 within the same time range into different sampling bags 511. In this case, by making the volume of odor evaluation gas recovered into each sampling bag 511 different, multiple odor evaluation gases with different concentrations can be prepared for a specific component.

[0059] [plan] It will be apparent to those skilled in the art that the above exemplary embodiments are specific examples of the following schemes.

[0060] (Item 1) An odor evaluation gas preparation apparatus according to one aspect of the present invention comprises: A gas chromatograph has a separation column that separates multiple components contained in an odorous analyte gas in the time direction; The time interval detection unit detects the time interval of each of the plurality of components as it exits the separation column; The gas recovery unit, by passing the analyte gas through the separation column, recovers all or part of the component gas containing the plurality of components exiting the separation column into the sampling bag; The gas inlet section introduces dilution gas into the sampling bag under predetermined gas inlet conditions; The flow information acquisition unit acquires flow information as information about the flow rate of the component gas exiting the separation column; The time range setting unit is used to set the time range for the gas recovery unit to recover the component gas by referring to the time ranges of each of the plurality of components detected by the time range detection unit; A total volume setting unit is used to set the total volume of the component gas recovered into the sampling bag and the dilution gas introduced into the sampling bag by the gas inlet unit; and The condition determination unit determines the gas introduction conditions of the gas introduction unit based on the flow information acquired by the flow information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit.

[0061] According to the odor evaluation gas preparation apparatus mentioned in item 1, when the time range for recovering component gas and the total volume of component gas and dilution gas recovered into the sampling bag are set, the introduction conditions when introducing dilution gas are automatically determined, so any amount of odor evaluation gas can be easily prepared.

[0062] (Item 2) In the odor evaluation gas preparation apparatus mentioned in Item 1, It includes a storage unit that stores a formula relating the flow rate and pressure of the dilution gas introduced by the gas inlet. When the separation column and the sampling bag are in communication, the gas inlet introduces the dilution gas into the flow path connecting the separation column and the sampling bag. The condition determination unit calculates the flow rate of the dilution gas introduced by the gas introduction unit based on the flow rate information acquired by the flow rate information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit, and determines the pressure when the dilution gas is introduced by the gas introduction unit based on the calculated flow rate and the relationship.

[0063] According to the odor evaluation gas preparation apparatus mentioned in item 2, since the pressure of the conditions for introducing dilution gas is automatically determined, any amount of odor evaluation gas can be easily prepared.

[0064] (Item 3) In the odor evaluation gas preparation apparatus mentioned in Item 1, After the gas recovery unit recovers the component gas into the sampling bag, the gas inlet unit introduces the dilution gas into the sampling bag. The condition determination unit determines the volume of the dilution gas introduced by the gas introduction unit based on the flow information acquired by the flow information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit.

[0065] According to the odor evaluation gas preparation apparatus mentioned in item 3, even if the amount of odor evaluation gas is adjusted after the component gas is recovered into the sampling bag, since the volume of the dilution gas, which is a condition for introducing dilution gas, is automatically determined, any amount of odor evaluation gas can be easily prepared.

[0066] (Item 4) In any of the odor evaluation gas preparation apparatuses mentioned in Items 1 through 3, The gas recovery unit, by passing the analyte gas multiple times through the separation column, recovers various component gases containing the same components exiting the separation column into different sampling bags. The volume setting unit sets different total volumes for each of the different sampling bags.

[0067] According to the odor evaluation gas preparation apparatus mentioned in item 4, multiple odor evaluation gases of different concentrations can be prepared for a certain component.

[0068] Explanation of reference numerals in the attached figures 1…GC Department 10… chromatographic column 12…Sample injection section 13… Flow path switching section 14…GC Control Department 2…MS Department 25…MS Control Department 3…Odor Measurement Department 31…suction port 34… Sensor Unit 341…Odor Sensor 36…A / D Conversion Section 37…Signal Processing Department 39…Odor Measurement and Control Department 41, 42… Interface Section 411, 421… heaters 5…Gas Recovery Unit 51…Installation Port 511…sampling bag 52…Import / Export Port 53…First Flow Path Switching Unit 54…Automatic Sampler 55…Second Flow Path Switching Unit 56…Gas Inlet Section 57…Gas Recovery Control Department 6… Personal Computers 61…Data Processing Department 62…Central Control Department 63…Gas Preparation Condition Setting Section 64… Storage Department 65… Input Section 66… Display Department 661… Gas preparation condition setting screen 662…TIC Tables 663, 664...

Claims

1. A gas preparation apparatus for odor evaluation, characterized in that, have: A gas chromatograph has a separation column that separates multiple components contained in an odorous analyte gas in the time direction; The time interval detection unit detects the time interval of each of the plurality of components as it exits the separation column; The gas recovery unit, by passing the analyte gas through the separation column, recovers all or part of the component gas containing the plurality of components exiting the separation column into the sampling bag; The gas inlet section introduces dilution gas into the sampling bag under predetermined gas inlet conditions; The flow information acquisition unit acquires flow information as information about the flow rate of the component gas exiting the separation column; The time range setting unit is used to set the time range for the gas recovery unit to recover the component gas by referring to the time ranges of each of the plurality of components detected by the time range detection unit; The total volume setting unit is used to set the total volume of the component gas recovered into the sampling bag and the dilution gas introduced into the sampling bag by the gas inlet unit; as well as The condition determination unit determines the gas introduction conditions of the gas introduction unit based on the flow information acquired by the flow information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit.

2. The gas preparation apparatus for odor evaluation according to claim 1, characterized in that, It includes a storage unit that stores a formula relating the flow rate and pressure of the dilution gas introduced by the gas inlet. When the separation column and the sampling bag are in communication, the gas inlet introduces the dilution gas into the flow path connecting the separation column and the sampling bag. The condition determination unit calculates the flow rate of the dilution gas introduced by the gas introduction unit based on the flow rate information acquired by the flow rate information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit, and determines the pressure when the dilution gas is introduced by the gas introduction unit based on the calculated flow rate and the relationship.

3. The gas preparation apparatus for odor evaluation according to claim 1, characterized in that, After the gas recovery unit recovers the component gas into the sampling bag, the gas inlet unit introduces the dilution gas into the sampling bag. The condition determination unit determines the volume of the dilution gas introduced by the gas introduction unit based on the flow information acquired by the flow information acquisition unit, the time range set by the time range setting unit, and the total volume set by the total volume setting unit.

4. The gas preparation apparatus for odor evaluation according to claim 1, characterized in that, The gas recovery unit, by passing the analyte gas multiple times through the separation column, recovers various component gases containing the same components exiting the separation column into different sampling bags. The volume setting unit sets different total volumes for each of the different sampling bags.

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