Gas chromatography device

Abstract

A gas chromatograph is provided, which can appropriately determine whether the temperature of the entire heating object is stable after cooling the heating object in the column oven to the target temperature after the temperature rise analysis. In the gas chromatograph (10) capable of performing the temperature rise analysis, the column oven (16) is cooled by a cooling mechanism (40) as the temperature rise analysis is completed. In addition, after the column oven (16) is cooled, when the detected temperature of the temperature sensor (44) for detecting the temperature of the heating object (46) reaches the target temperature, the heating object (46) is heated by a heater (42). As the detected temperature of the temperature sensor (44) reaches the target temperature, it is determined whether the temperature of the entire heating object (46) is stable based on the power consumption of the heater (42).

Description

Technical Field

[0001] The invention relates to a gas chromatography device. Background Art

[0002] For example, in a gas chromatograph such as disclosed in Patent Document 1 listed below, a sample is introduced into a column from a sample vaporization chamber, and while the temperature of the column is increased in a column oven, sample components separated by the column are detected by a detector, thereby enabling temperature increase analysis.

[0003] Prior art literature

[0004] Patent Literature

[0005] Patent Document 1: Japanese Patent Application Publication No. 2017-009459 Summary of the invention

[0006] Problem that the invention aims to solve

[0007] The gas chromatograph can also repeatedly perform temperature analysis. In this case, after the temperature analysis, the heating object in the column oven is cooled to the target temperature, and after the equalization time, the next temperature analysis is performed while the heating object in the column oven is heated again. As an example of the heating object, a column and a sample introduction part can be cited. The equalization time is the waiting time until the temperature is equalized, and can be pre-set by the user as a parameter.

[0008] When the equalization time is set shorter than the appropriate time, the next temperature increase analysis will be started before the temperature of the entire heating object is stabilized, so that a good analysis result may not be obtained.

[0009] Furthermore, when the equalization time is set longer than an appropriate time, the time required to complete the repeated temperature rise analysis becomes unnecessarily long.

[0010] The present invention has been made in view of the above-mentioned actual situation, and an object thereof is to provide a gas chromatograph capable of appropriately determining whether the temperature of the entire heating object has stabilized after cooling the heating object in a column oven to a target temperature after temperature analysis.

[0011] Solutions for solving problems

[0012] The present invention is a gas chromatograph capable of performing temperature rise analysis, wherein the temperature rise analysis is the following analysis: a sample is introduced into a column from a sample introduction portion, the temperature of the column is raised in a column oven, and a sample component separated by the column is detected by a detector, wherein the gas chromatograph comprises a heater, a cooling mechanism, a temperature sensor, a temperature control unit, and a determination processing unit. The heater heats a heating object in the column oven. The cooling mechanism cools the inside of the column oven. The temperature sensor detects the temperature of the heating object. The temperature control unit cools the inside of the column oven using the cooling mechanism as the temperature rise analysis is completed, and heats the heating object using the heater as the temperature detected by the temperature sensor reaches a target temperature. The determination processing unit determines whether the temperature of the heating object as a whole is stable based on the power consumption of the heater as the temperature detected by the temperature sensor reaches the target temperature.

[0013] Effects of the Invention

[0014] According to the present invention, after the heating object in the column oven is cooled to the target temperature after the temperature increase analysis, it is possible to appropriately determine whether the temperature of the entire heating object has stabilized. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic diagram showing an example of the structure of the gas chromatograph according to the present embodiment.

[0016] Figure 2 This is a block diagram showing an example of the electrical configuration of the gas chromatograph according to the present embodiment.

[0017] Figure 3 This is an example of a graph for explaining the heating process and the cooling process in this embodiment.

[0018] Figure 4 This is an example of a graph for explaining the heating process according to the present embodiment.

[0019] Figure 5 This is a block diagram specifically showing the electrical configuration of the gas chromatograph according to the present embodiment.

[0020] Figure 6 This is a flowchart showing an example of the CPU stabilization process according to the present embodiment.

[0021] Figure 7 This is a flowchart showing an example of instruction output processing of the CPU according to the present embodiment. DETAILED DESCRIPTION

[0022] 1. Structure of gas chromatography device

[0023] Figure 1 1 is a schematic diagram showing an example of the structure of the gas chromatograph 10 according to the present embodiment. The gas chromatograph 10 includes a pre-processing unit 12 and a gas chromatograph 14, and the pre-processing unit 12 and the gas chromatograph 14 are connected to each other in a communicable manner.

[0024] For example, the preprocessing unit 12 and the gas chromatograph unit 14 may be connected to each other in a communicative manner via a wired method such as a cable, or may be connected to each other in a communicative manner via infrared communication or short-distance wireless communication such as Bluetooth (registered trademark).

[0025] The pre-processing unit 12 includes an automatic sample injection device (not shown) for automatically injecting liquid samples in the sample containers into the gas chromatograph unit 14 while holding a plurality of sample containers. In addition, the pre-processing unit 12 can also hold a plurality of reagent containers, and after the liquid samples are pre-processed using the liquid reagents in the reagent containers, the pre-processed liquid samples can be injected into the gas chromatograph unit 14.

[0026] The pre-processing unit 12 can perform aspiration and injection of liquid by means of a needle. The pre-processing unit 12 can aspirate a pre-processed liquid sample by means of a needle and inject the liquid sample into a sample vaporization chamber 20 in a sample introduction unit 18 described later of the gas chromatograph unit 14. In other words, the pre-processing unit 12 can perform pre-processing on the liquid sample and supply the pre-processed liquid sample to the sample vaporization chamber 20 in the sample introduction unit 18.

[0027] The gas chromatograph section 14 includes a column oven 16 , a sample introduction section 18 , a column 22 , a fan 24 , a detector 26 , and the like, which are accommodated in a casing.

[0028] A sample introduction unit 18 , a column 22 , a fan 24 , a detector 26 , etc. are provided in a temperature-adjustable column oven 16 . Specifically, the sample introduction unit 18 and the detector 26 are partially provided in the column oven 16 .

[0029] The sample introduction section 18 is a sample introduction unit (SPL) for introducing a carrier gas and a sample gas into the column 22, and is provided with a diaphragm (not shown). In addition, a sample vaporization chamber 20 is formed inside the sample introduction section 18. The sample vaporization chamber 20 is provided in the column oven 16 in the same manner as the sample introduction section 18.

[0030] In addition, a heater 42 is provided in the sample introduction section 18. Specifically, a first heater 42a included in the heater 42 is provided in the sample introduction section 18. The sample introduction section 18 is heated by the first heater 42a. Therefore, the liquid sample injected into the sample vaporization chamber 20 is vaporized by the heat from the first heater 42a.

[0031] The sample introduction part 18 is further provided with a temperature sensor 44. Specifically, a first temperature sensor 44a included in the temperature sensor 44 is provided in the sample introduction part 18. The temperature of the sample introduction part 18 is detected by the first temperature sensor 44a.

[0032] In addition, the gas supply flow path 28 and the branch flow path 30 are communicated with the sample vaporization chamber 20. The gas supply flow path 28 is a flow path for supplying a carrier gas into the sample vaporization chamber 20 of the sample introduction section 18.

[0033] The split flow path 30 is a flow path for discharging a portion of the gas (mixed gas of carrier gas and sample gas) in the sample vaporization chamber 20 to the outside at a predetermined split ratio when the carrier gas and the vaporized liquid sample (sample gas) are introduced into the normal column 22 by split flow introduction.

[0034] Thus, the sample gas is introduced into the column 22 together with the carrier gas through the sample introduction section 18 .

[0035] In addition, a heater 42 is provided in the column oven 16. Specifically, a second heater 42b included in the heater 42 is provided in the column oven 16. The column 22 is heated by the second heater 42b.

[0036] Specifically, the fan 24 rotates as the second heater 42b generates heat. Therefore, the air heated by the second heater 42b circulates in the column oven 16. Thus, the column 22 is heated.

[0037] In addition, a temperature sensor 44 is provided in the column oven 16. Specifically, a second temperature sensor 44b included in the temperature sensor 44 is provided in the column oven 16. The temperature of the column 22 is detected by the second temperature sensor 44b.

[0038] When a sample gas is introduced into the heated column 22, sample components contained in the sample gas are separated into different components. The column 22 is a general-purpose column, such as a capillary column.

[0039] The detector 26 is provided to sequentially detect the components separated by the column 22. The detector 26 is constituted by, for example, a hydrogen flame ionization detector (FID).

[0040] In addition, the detector 26 is provided with a heater 42. Specifically, a third heater 42c included in the heater 42 is provided in the detector 26. The detector 26 is heated by the third heater 42c.

[0041] The detector 26 is further provided with a temperature sensor 44. Specifically, a third temperature sensor 44c included in the temperature sensor 44 is provided in the detector 26. The temperature of the detector 26 is detected by the third temperature sensor 44c.

[0042] The column oven 16 also includes a gas supply damper 34 for opening and closing the gas supply port 32 and an exhaust damper 38 for opening and closing the exhaust port 36. When the column 22 is heated, the gas supply damper 34 and the exhaust damper 38 are closed.

[0043] On the other hand, when cooling the inside of the column oven 16, the air supply damper 34 and the exhaust damper 38 are changed from the closed state to the open state. The fan 24 is always rotating, and when cooling the inside of the column oven 16, the heat in the column oven 16 is taken away by the air taken in from the air supply port 32. In addition, the air from which the heat in the column oven 16 is taken away is exhausted from the exhaust port 36.

[0044] Therefore, the fan 24 , the air supply damper 34 , and the exhaust damper 38 can be said to be a cooling mechanism 40 that cools the inside of the column oven 16 .

[0045] The gas chromatograph 10 can perform temperature-elevation analysis in which a sample gas is introduced into the column 22 , the temperature of the column 22 is increased in the column oven 16 , and the sample components separated by the column 22 are detected by the detector 26 .

[0046] In addition, the heating object 46 in the column oven 16 can be heated by the heater 42 . Furthermore, the temperature of the heating object 46 in the column oven 16 can be detected by the temperature sensor 44 .

[0047] In this embodiment, the heating object 46 includes at least one of the sample introduction section 18, the column 22, and the detector 26. Figure 2 In the example shown, the sample introduction section 18 , the column 22 , and the detector 26 are all included in the heating object. However, the heating object 46 is not limited to the sample introduction section 18 , the column 22 , or the detector 26 .

[0048] 2. Electrical structure of gas chromatography device

[0049] Figure 2 1 is a block diagram showing an example of the electrical structure of the gas chromatograph 10 according to the present embodiment. Figure 2 As shown, the gas chromatograph 10 includes a control unit 50, a power control circuit 58, and the like in addition to the cooling mechanism 40, and the like.

[0050] In addition, the control unit 50, the pre-processing unit 12, the power control circuit 58, the first temperature sensor 44a, the second temperature sensor 44b, the third temperature sensor 44c, and the cooling mechanism 40 are electrically connected to each other via a bus or other circuit 60. In addition, the power control circuit 58 is connected to the first heater 42a, the second heater 42b, and the third heater 42c.

[0051] The control unit 50 is responsible for overall control of the gas chromatograph 10. The control unit 50 includes a CPU (Central Processing Unit) 52. The control unit 50 also includes a RAM (Random Access Memory) 54 and a storage unit 56 to which the CPU 52 can directly access.

[0052] The CPU 52 controls each component of the gas chromatograph 10. The RAM 54 is used as a work area and a buffer area of ​​the CPU 52. The storage unit 56 is a nonvolatile memory, and for example, a HDD (Hard Disc Drive) or an SSD (Solid State Drive) is used as the storage unit 56 .

[0053] The storage unit 56 stores a control program for controlling each component of the gas chromatograph 10 and data (execution data) necessary for executing the control program. The storage unit 56 may include the RAM 54.

[0054] The power control circuit 58 is a circuit for supplying power to each of the first heater 42a, the second heater 42b, and the third heater 42c. In other words, the power control circuit 58 is a circuit for controlling each of the first heater 42a, the second heater 42b, and the third heater 42c.

[0055] Although not shown in the figure, the gas chromatograph 10 further includes an operation receiving unit for receiving an operation from a user, a display unit as a general-purpose display, and the like.

[0056] 3. Temperature control of heated objects

[0057] In the gas chromatograph 10 of the present embodiment, the temperature of the heating object 46 is controlled as the temperature increase analysis is completed. The temperature control of the heating object 46 is described in detail below. In the present embodiment, the cooling process is performed as the temperature increase analysis is completed. In the cooling process, the cooling mechanism 40 is used to cool the inside of the column oven 16.

[0058] The cooling process cools the sample introduction unit 18, the column 22, the detector 26, etc. in the column oven 16. The sample introduction unit 18 and the detector 26 are cooled by the cooling mechanism 40 and by the outside air outside the column oven 16.

[0059] The gas chromatograph 10 of the present embodiment performs a heating process after the cooling process. In the heating process, the heating object 46 in the column oven 16 is heated as the temperature detected by the temperature sensor 44 reaches the target temperature after the cooling process.

[0060] In addition, the cooling process ends with the start of the heating process. That is, the time for implementing the cooling process (cooling time) is the time from the completion of the temperature rise analysis until the detection temperature of the temperature sensor 44 reaches the target temperature. And, during the heating process, the heater 42 is controlled so that the detection temperature of the temperature sensor 44 is maintained at the target temperature.

[0061] In the heating process, for example, as the temperature detected by the first temperature sensor 44a reaches the target temperature, the sample introduction section 18 in the column oven 16 is heated. The control of the second heater 42b based on the temperature detected by the second temperature sensor 44b and the control of the third heater 42c based on the temperature detected by the third temperature sensor 44c are the same as those of the first heater 42a, and therefore, only the control of the first heater 42a will be described below.

[0062] Furthermore, in the present embodiment, the determination process is executed while the temperature control of the heating object 46 is executed. In the determination process, after the heating process is started, that is, when the temperature detected by the temperature sensor 44 reaches the target temperature, it is determined based on the power consumption of the heater 42 whether the temperature of the heating object 46 is stable.

[0063] In the determination process, for example, after the heating of the sample introduction section 18 is started by the heating process, it is determined whether the temperature of the entire sample introduction section 18 is stable based on the power consumption of the first heater 42a. The entire sample introduction section 18 is a concept that includes not only the periphery of the first temperature sensor 44a but also the position of the sample introduction section 18 farthest from the first temperature sensor 44a. This is also the same for the column 22 and the detector 26.

[0064] Figure 3 This is an example of a graph for explaining the heating process and the cooling process in this embodiment. Figure 4 This is an example of a chart for explaining the heating process of this embodiment. Figure 4 Yes Figure 3 A diagram obtained by enlarging a portion of Figure 3and Figure 4 A graph corresponding to the sample introduction section 18 is shown.

[0065] exist Figure 3 and Figure 4 In FIG. 1 , the dotted line indicates the detected temperature of the first temperature sensor 44a. In addition, the single-point chain line indicates the reference temperature. The reference temperature is the temperature of the portion of the sample introduction portion 18 away from the first temperature sensor 44a. The reference temperature is detected by providing a temperature sensor for experiment separately from the first temperature sensor 44a. The solid line is the duty cycle related to the power consumption of the first heater 42a.

[0066] like Figure 3 As shown, after the temperature rise analysis is completed, cooling and heating are performed in sequence. The heating process starts when the temperature detected by the first temperature sensor 44a reaches the target temperature, so the temperature detected by the first temperature sensor 44a is the same as the target temperature immediately after the heating process starts.

[0067] In the heating process, the first heater 42a is controlled so that the temperature detected by the first temperature sensor 44a is maintained at the target temperature. Therefore, the temperature (detected temperature) near the first temperature sensor 44a of the sample introduction section 18 is stabilized.

[0068] On the other hand, since many metal components are used in the sample introduction part 18, the temperature of the portion of the sample introduction part 18 away from the first temperature sensor 44a is gradually lowered by the external air outside the column oven 16. Figure 3 and Figure 4 In the example shown, the probe temperature is maintained at the target temperature, but the reference temperature is slightly reduced.

[0069] Furthermore, during the heating process, although the heat of the sample introduction section 18 is taken away, the detected temperature is intended to be maintained at the target temperature, and therefore the duty ratio associated with the power consumption of the first heater 42 a increases.

[0070] Furthermore, the duty ratio related to the power consumption of the first heater 42a increases but gradually stabilizes. This is because the sample introduction section 18 is heated to a level where the overall temperature is stable even if it is affected by the outside air outside the column oven 16. Figure 3 and Figure 4 In the example shown, as the duty ratio related to the power consumption of the first heater 42 a becomes stable, the reference temperature also becomes stable.

[0071] Therefore, in Figure 3 and Figure 4In the example shown, when the duty ratio change amount related to the power consumption of the first heater 42 a , specifically, the duty ratio change amount within a predetermined time becomes equal to or less than a threshold value, it can be determined that the temperature of the entire sample introduction section 18 is stable.

[0072] In addition, these cases can be said to be the same also in the case where the column 22 is heated by the second heater 42 b and in the case where the detector 26 is heated by the third heater 42 c during the heating process.

[0073] Furthermore, in the above example, when the amount of change in the duty ratio related to the power consumption of the heater 42 becomes less than the threshold value, it is determined that the temperature of the entire heating object 46 is stable, but it is also possible to determine that the temperature of the entire heating object 46 is stable when the duty ratio related to the power consumption of the heater 42 (the duty ratio itself) becomes more than the threshold value. The duty ratio related to the power consumption of the heater 42 is, for example, the duty ratio of the voltage applied to the heater 42.

[0074] Alternatively, for example, when the duty ratio related to the power consumption of the heater 42 is equal to or greater than a first threshold value and the amount of change in the duty ratio is equal to or less than a second threshold value, it may be determined that the temperature of the entire heating object 46 is stable.

[0075] Furthermore, for example, whether the temperature of the entire heating object 46 is stable may be determined based simply on the power consumption of the heater 42 instead of the duty ratio related to the power consumption of the heater 42 .

[0076] The time from the start of the heating process until the temperature of the entire heating object 46 is determined to be stable is the equalization time of the present embodiment. In this way, if it can be determined that the temperature of the entire heating object 46 is stable after the temperature increase analysis, the next temperature increase analysis can be performed after the temperature of the entire heating object 46 is stable. That is, in repeated temperature increase analysis, good analysis results can be obtained, and the time required for repeated temperature increase analysis can be suppressed from being unnecessarily prolonged.

[0077] Furthermore, if it is possible to determine whether the temperature of the entire heating object 46 is stable, it is not necessary to set parameters such as the equalization time in advance even when the temperature rise analysis is repeated, thereby saving unnecessary effort.

[0078] Furthermore, when there are a plurality of heating objects 46, the next temperature increase analysis can be performed after the temperature of the entire heating objects 46 stabilizes. For example, if the heating objects 46 include the sample introduction section 18, the column 22, and the detector 26, particularly good analysis results can be obtained.

[0079] Furthermore, in the present embodiment, when the temperature rise analysis is repeatedly performed, information on the stabilization period immediately after the first temperature rise analysis (stabilization period information) may be stored in the storage unit 56. The stabilization period is a period from the start of the cooling process, that is, from the start of cooling by the cooling mechanism 40 until it is determined that the temperature of the entire heating object 46 is stabilized. In addition, the stabilization period can also be said to be a period from the completion of the temperature rise analysis until it is determined that the temperature of the entire heating object 46 is stabilized.

[0080] For example, if the heated object 46 includes the sample introduction part 18, the column 22, and the detector 26, the stabilization period is a period from the start of the cooling process until it is determined that the overall temperature of the sample introduction part 18, the column 22, and the detector 26 is stabilized. The sample introduction part 18 and the detector 26 have a larger heat capacity than the column 22 (capillary column) having a smaller heat capacity, and thus the stabilization period tends to be longer.

[0081] In the present embodiment, when the stabilization period information is stored in the storage unit 56, the preprocessing unit 12 is instructed to start preprocessing the sample related to the next temperature rise analysis, so that the preprocessing of the sample related to the next temperature rise analysis is completed at a timing corresponding to the end timing of the stabilization period. Specifically, the waiting time is calculated by subtracting the time required for preprocessing (preprocessing time) from the stabilization period (cooling time + equalization time) stored in the storage unit 56, and the preprocessing unit 12 is instructed to start preprocessing the sample related to the next temperature rise analysis at a timing after the waiting time has passed after the cooling process starts. In this way, the next temperature rise analysis can be started simultaneously with the end timing of the stabilization period. In addition, when the stabilization period information is not stored in the storage unit 56, the preprocessing unit 12 is instructed to start preprocessing the sample related to the next temperature rise analysis in the same manner as before.

[0082] However, the start timing of the next temperature rise analysis and the end timing of the stabilization period are not limited to being simultaneous, and the start timing of the next temperature rise analysis may be before or after the end timing of the stabilization period. That is, the timing corresponding to the end timing of the stabilization period includes the timing before or after the end timing. Therefore, the timing for completing the pretreatment of the sample related to the next temperature rise analysis may also be the timing before or after the end timing of the stabilization period.

[0083] When the pretreatment unit 12 performs pretreatment on the liquid sample, the liquid sample is pretreated using the liquid reagent as described above. If the timing of completing the pretreatment of the sample related to the next temperature rise analysis is earlier than the end timing of the stabilization period, the liquid sample that has been pretreated directly becomes a state of waiting for the temperature rise analysis, which may have an adverse effect on the analysis result.

[0084] On the other hand, if the timing for completing the pretreatment of the sample related to the next temperature increase analysis is later than the end timing of the stabilization period, a standby time is required from the end of the stabilization period until the start of the next temperature increase analysis during the temperature increase analysis, so the time spent on repeated temperature increase analysis becomes unnecessarily long.

[0085] Therefore, it is preferable that the timing of completing the pre-processing of the sample related to the next temperature increase analysis is synchronized with the timing of ending the stabilization period.

[0086] If the stabilization period information is stored in advance in the storage unit 56 in this manner, the preprocessing of the sample related to the next temperature increase analysis can be completed at a timing corresponding to the end timing of the stabilization period.

[0087] 3. Specific electrical structure of gas chromatography device

[0088] Figure 5 is a block diagram specifically showing the electrical structure of the gas chromatograph 10 according to the present embodiment. Figure 5 In the figure, the storage unit 56 is omitted.

[0089] The RAM 54 stores the execution data read in advance from the storage unit 56. When the acquired data acquired using the device, sensor, etc. is stored in the storage unit 56, the acquired data is temporarily stored in the RAM 54.

[0090] exist Figure 5 In the example shown, the stabilization period data 62 and the instruction data 64 are stored in the RAM 54. Although not shown in the figure, the RAM 54 also stores data and the like necessary for controlling various components.

[0091] The stabilization period data 62 is data corresponding to the stabilization period information. The instruction data 64 is data corresponding to the instruction output to the pre-processing unit 12.

[0092] The RAM 54 stores a control program (not shown) read in advance from the storage unit 56 . When the CPU 52 executes the control program, the control unit 50 functions as a temperature control unit 66 , a determination processing unit 70 , a storage processing unit 72 , and an instruction processing unit 74 .

[0093] The temperature control unit 66 cools the inside of the column oven 16 using the cooling mechanism 40 as the temperature rise analysis is completed, and heats the heating object 46 using the heater 42 as the temperature detected by the temperature sensor 44 reaches the target temperature. The temperature control performed by the temperature control unit 66 is performed by PID (Proportional Integral Differential) control.

[0094] When the temperature detected by the temperature sensor 44 reaches the target temperature, the determination processing unit 70 determines whether the temperature of the entire heating object 46 is stable based on the power consumption of the heater 42 .

[0095] When the temperature rise analysis is repeatedly performed, the storage processing unit 72 stores the stabilization period information related to the first temperature rise analysis as the stabilization period data 62 .

[0096] The instruction processing unit 74 instructs the preprocessing unit 12 to start preprocessing the sample for the next temperature increase analysis so that the preprocessing of the sample for the next temperature increase analysis is completed at the timing corresponding to the end timing of the stabilization period.

[0097] 4. Process

[0098] Figure 6 2 is a flowchart showing an example of the temperature increase analysis process of the CPU 52 of the present embodiment. For example, the temperature increase analysis process is started in response to the gas chromatograph 10 accepting an operation for starting the temperature increase analysis.

[0099] In step S1 , temperature rise analysis is performed, and in step S2 , cooling of the column oven 16 is performed.

[0100] In step S3, it is determined whether the temperature detected by the temperature sensor 44 has reached the target temperature. If the answer is "No" in step S3, that is, if the temperature detected by the temperature sensor 44 has not reached the target temperature, the process returns to step S2. On the other hand, if the answer is "Yes" in step S3, that is, if the temperature detected by the temperature sensor 44 has reached the target temperature, the process proceeds to step S4.

[0101] In step S4, the heating object 46 in the column oven 16 is heated, and in step S5, it is determined whether the temperature of the entire heating object 46 is stable based on the power consumption of the heater 42. If the answer is "No" in step S5, that is, if the temperature of the entire heating object 46 is not stable, the process returns to step S4. On the other hand, if the answer is "Yes" in step S5, that is, if the temperature of the entire heating object 46 is stable, the process proceeds to step S6.

[0102] In step S6, it is determined whether the stabilization period data 62 is stored. If the answer is "No" in step S6, that is, if the stabilization period data 62 is not stored, the stabilization period data 62 is stored in step S7, and the process proceeds to step S8. On the other hand, if the answer is "Yes" in step S6, that is, if the stabilization period data 62 is stored, the process proceeds to step S8.

[0103] In step S8, it is determined whether this is the last temperature rise analysis in the repeated temperature rise analysis. If the answer is "No" in step S8, that is, if it is not the last temperature rise analysis, the process returns to step S1. On the other hand, if the answer is "Yes" in step S8, that is, if it is the last temperature rise analysis, the temperature rise analysis process ends.

[0104] Figure 7 2 is a flowchart showing an example of the instruction output process of the CPU 52 of the present embodiment. For example, the instruction output process is started in response to the gas chromatograph 10 accepting an operation for starting temperature increase analysis.

[0105] In step S10, it is determined whether the stabilization period data 62 is stored. If the answer is "No" in step S10, that is, if the stabilization period data 62 is not stored, the process proceeds to step S12. On the other hand, if the answer is "Yes" in step S10, that is, if the stabilization period data 62 is stored, the process proceeds to step S11.

[0106] In step S11, the stabilization period data 62 is referred to, and in step S12, it is determined whether it is the timing to issue an instruction to the pre-processing unit 12. If the answer is "No" in step S12, that is, if it is not the timing to issue an instruction to the pre-processing unit 12, the process returns to step S12. On the other hand, if the answer is "Yes" in step S12, that is, if it is the timing to issue an instruction to the pre-processing unit 12, the pre-processing unit 12 is instructed to perform pre-processing on the liquid sample in step S13.

[0107] In step S14, it is determined whether the instruction previously issued by the forward processing unit 12 is the last instruction. If the answer is "No" in step S14, that is, if the instruction previously issued by the forward processing unit 12 is not the last instruction, the process returns to step S10. On the other hand, if the answer is "Yes" in step S14, that is, if the instruction previously issued by the forward processing unit 12 is the last instruction, the instruction output process ends.

[0108] In addition, regarding each step of the flowchart shown in the above-mentioned embodiment, the order of performing the processing can be changed as appropriate as long as the same result can be obtained.

[0109] In addition, the electrical structure and the like shown in the above-mentioned embodiment are only examples, and can be appropriately changed in actual products. For example, in this embodiment, the case where a liquid sample is used as a sample is cited as an example, but as long as the sample can be introduced from the sample introduction part 18, the form of the sample is not particularly limited. For example, in the case where a gas sample is used as a sample, the pretreatment part 12 is configured to perform pretreatment on the gas sample and supply the pretreated gas sample to the sample introduction part 18. In addition, in such a case, the sample introduction part 18 uses an introduction part suitable for the type of gas sample, specifically, an introduction part of a type that does not form the sample vaporization chamber 20.

[0110] 5. Method

[0111] It will be understood by those skilled in the art that the above-mentioned multiple exemplary embodiments are specific examples of the following aspects.

[0112] (Item 1) A gas chromatograph according to one embodiment is capable of performing temperature-raising analysis, wherein a sample is introduced into a column from a sample introduction portion, the temperature of the column is raised in a column oven, and sample components separated by the column are detected by a detector. The gas chromatograph may also include:

[0113] A heater for heating a heating object in the column oven;

[0114] A cooling mechanism for cooling the column oven;

[0115] a temperature sensor for detecting the temperature of the heating object;

[0116] a temperature control unit that cools the inside of the column oven using the cooling mechanism as the temperature rise analysis is completed, and heats the heating object using the heater as the temperature detected by the temperature sensor reaches a target temperature; and

[0117] A determination processing unit determines whether the temperature of the entire heating object is stable based on the power consumption of the heater when the temperature detected by the temperature sensor reaches the target temperature.

[0118] According to the gas chromatograph apparatus described in the first item, after the heating object in the column oven is cooled to the target temperature after the temperature rise analysis, it is possible to appropriately determine whether the temperature of the entire heating object is stable based on the power consumption of the heater. As a result, the next temperature rise analysis can be performed after the temperature of the entire heating object is stable. In addition, if the next temperature rise analysis can be performed after the temperature of the entire heating object is stable, good analysis results can be obtained in repeated temperature rise analysis, and the time required for repeated temperature rise analysis can be prevented from being unnecessarily prolonged.

[0119] (Item 2) In the gas chromatography apparatus described in Item 1, it may be that:

[0120] A storage processing unit is further provided for storing information on a stabilization period, which is a period from when cooling by the cooling mechanism is started until when the determination processing unit determines that the temperature of the entire heating object is stabilized.

[0121] According to the gas chromatograph described in the second aspect, it is possible to store information on the stabilization period. Furthermore, if it is possible to store information on the stabilization period, the information can be used for the next temperature increase analysis.

[0122] (Item 3) In the gas chromatograph described in Item 2, it may further include:

[0123] a pre-processing unit that pre-processes the sample and supplies the pre-processed sample to the sample introduction unit; and

[0124] The instructing processing unit instructs the preprocessing unit to start preprocessing the sample related to the next temperature increase analysis so that the preprocessing of the sample related to the next temperature increase analysis is completed at a timing corresponding to an end timing of the stabilization period.

[0125] According to the gas chromatograph apparatus described in the third item, since the pretreatment of the sample related to the next temperature rise analysis is completed at the timing corresponding to the end timing of the stabilization period, the waiting time from the completion of the pretreatment of the sample to the start of the temperature rise analysis of the sample can be suppressed to a minimum. As a result, it is possible to effectively prevent the time required for repeated temperature rise analysis from being unnecessarily prolonged. In addition, since it is possible to prevent the sample that has been subjected to pretreatment from directly entering a state of waiting for temperature rise analysis, a better analysis result can be obtained.

[0126] (Item 4) In the gas chromatograph described in any one of Items 1 to 3, it may be that:

[0127] The determination processing unit determines that the temperature of the entire heating object is stable if the amount of change in the duty ratio related to the power consumption of the heater becomes equal to or less than a threshold value.

[0128] According to the gas chromatograph apparatus described in the fourth aspect, it is possible to appropriately determine that the temperature of the entire heating object is stable based on the fact that the amount of change in the duty ratio related to the power consumption of the heater becomes equal to or less than the threshold value.

[0129] (Item 5) In the gas chromatograph described in any one of Items 1 to 3, it may be that:

[0130] The determination processing unit determines that the temperature of the entire heating object is stable when the duty ratio related to the power consumption of the heater is equal to or larger than a threshold value.

[0131] According to the gas chromatograph apparatus described in the fifth aspect, it is possible to appropriately determine that the temperature of the entire heating object is stable based on the fact that the duty ratio related to the power consumption of the heater becomes equal to or larger than the threshold value.

[0132] (Item 6) In the gas chromatograph described in any one of Items 1 to 5, it may be that:

[0133] The heating object includes at least one of the sample introduction section, the column, and the detector.

[0134] According to the gas chromatograph as described in item 6, after the temperature increase analysis, it is possible to appropriately determine whether the overall temperature of at least one of the sample introduction part, the column, and the detector is stable.

[0135] Description of Reference Numerals

[0136] 10: gas chromatograph; 12: pre-processing unit; 16: column oven; 18: sample introduction unit; 22: column; 26: detector; 40: cooling mechanism; 42: heater; 44: temperature sensor; 46: heating object; 56: storage unit; 66: temperature control unit; 70: determination processing unit; 72: storage processing unit; 74: indication processing unit.

Claims

1. A gas chromatograph capable of performing temperature-raising analysis, wherein a sample is introduced into a column from a sample introduction portion, the temperature of the column is raised in a column oven, and sample components separated by the column are detected by a detector, the gas chromatograph comprising: A heater for heating a heating object in the column oven; A cooling mechanism for cooling the column oven; a temperature sensor for detecting the temperature of the heating object; a temperature control unit that cools the inside of the column oven using the cooling mechanism as the temperature rise analysis is completed, and heats the heating object using the heater as the temperature detected by the temperature sensor reaches a target temperature; and A determination processing unit determines whether the temperature of the entire heating object is stable based on the power consumption of the heater when the temperature detected by the temperature sensor reaches the target temperature.

2. The gas chromatography apparatus according to claim 1, wherein: A storage processing unit is further provided for storing information on a stabilization period, which is a period from when cooling by the cooling mechanism is started until when the determination processing unit determines that the temperature of the entire heating object is stabilized.

3. The gas chromatography apparatus according to claim 2, wherein: Also available: a pre-processing unit that pre-processes the sample and supplies the pre-processed sample to the sample introduction unit; and The instructing processing unit instructs the preprocessing unit to start preprocessing the sample related to the next temperature increase analysis so that the preprocessing of the sample related to the next temperature increase analysis is completed at a timing corresponding to an end timing of the stabilization period.

4. The gas chromatography apparatus according to claim 1, wherein: The determination processing unit determines that the temperature of the entire heating object is stable if the amount of change in the duty ratio related to the power consumption of the heater becomes equal to or less than a threshold value.

5. The gas chromatography apparatus according to claim 1, wherein: The determination processing unit determines that the temperature of the entire heating object is stable when the duty ratio related to the power consumption of the heater is equal to or larger than a threshold value.

6. The gas chromatography apparatus according to any one of claims 1 to 5, wherein: The heating object includes at least one of the sample introduction section, the column, and the detector.

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