Gas chromatograph equipment

Abstract

To provide a gas chromatography device that can properly determine that the temperature of the entire heating object is stabilized after the heating object within a column oven is cooled to a target temperature after temperature increase analysis.SOLUTION: A gas chromatography device 10, which can implement temperature increase analysis, is configured to, with the completion of the temperature increase analysis, cool an interior of a column oven 16 by a cooling mechanism 40. Also, the gas chromatography device is configured to, when a detection temperature from a temperature sensor 44 detecting the temperature of a heating object 46 reaches a target temperature after the interior of the column oven 16 is cooled, heat the heating object 46 by a heater 42, and with the detection temperature from the temperature sensor 44 reaching the target temperature, determine whether the temperature of the entire heating object 46 is stabilized on the basis of the power consumption of the heater 42.SELECTED DRAWING: Figure 6

Description

[Technical Field]

[0001] The present invention relates to a gas chromatograph apparatus. [Background technology]

[0002] For example, in a gas chromatograph apparatus such as that disclosed in Patent Document 1 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, the sample components separated by the column are detected by a detector, thereby making it possible to perform temperature-programmed analysis. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2017-009459 Summary of the Invention [Problem to be solved by the invention]

[0004] The gas chromatograph can also repeatedly perform temperature-programmed analyses. In this case, after a temperature-programmed analysis, the object to be heated in the column oven is cooled to a target temperature, and after an equilibration time has elapsed, the next temperature-programmed analysis is performed while heating the object to be heated in the column oven again. Examples of the object to be heated include a column and a sample introduction section. The equilibration time is the waiting time until the temperature equilibrates, and can be set in advance as a parameter by the user.

[0005] If the equilibration time is set shorter than appropriate, the next heating analysis will begin before the overall temperature of the heated object has stabilized, which may result in poor analytical results.

[0006] Furthermore, if the equilibration time is set longer than appropriate, the time required to complete the repeated temperature-programmed analyses will be unnecessarily long.

[0007] The present invention has been made in consideration of the above-described circumstances, and aims to provide a gas chromatograph apparatus that can appropriately determine whether the overall temperature of an object to be heated has stabilized after cooling the object to be heated in a column oven to a target temperature following a temperature-programmed analysis. [Means for solving the problem]

[0008] One aspect of the present invention is a gas chromatograph apparatus capable of performing a temperature-programmed analysis, which involves introducing a sample into a column through a sample introduction unit, raising the temperature of the column in a column oven, and detecting sample components separated by the column with a detector. The gas chromatograph apparatus includes 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 upon completion of the temperature-programmed analysis, and heats the heating object using the heater upon the temperature detected by the temperature sensor reaching a target temperature. The determination processing unit determines whether the overall temperature of the heating object has stabilized based on the power consumption of the heater upon the temperature detected by the temperature sensor reaching the target temperature. [Effects of the Invention]

[0009] According to the present invention, after the heating object in the column oven is cooled to the target temperature after the temperature-programmed analysis, it can be appropriately determined that the temperature of the entire heating object has stabilized. [Brief explanation of the drawings]

[0010] [Figure 1] 1 is a schematic diagram showing an example of the configuration of a gas chromatograph apparatus according to an embodiment of the present invention. [Figure 2] FIG. 2 is a block diagram showing an example of the electrical configuration of the gas chromatograph apparatus of the present embodiment. [Figure 3]4 is an example of a graph for explaining a heating process and a cooling process according to the present embodiment. [Figure 4] 1 is an example of a graph for explaining a heat treatment according to the present embodiment. [Figure 5] FIG. 2 is a block diagram specifically showing the electrical configuration of the gas chromatograph apparatus of the present embodiment. [Figure 6] FIG. 4 is a flowchart showing an example of a stabilization process of the CPU according to the present embodiment. [Figure 7] FIG. 10 is a flowchart showing an example of an instruction output process of a CPU according to the present embodiment. DETAILED DESCRIPTION OF THE INVENTION

[0011] 1. Configuration of gas chromatograph equipment 1 is a schematic diagram showing an example of the configuration of a gas chromatograph apparatus 10 according to this embodiment. The gas chromatograph apparatus 10 includes a pre-processing unit 12 and a gas chromatograph unit 14, which are communicatively connected to each other.

[0012] For example, the pre-processing unit 12 and the gas chromatograph unit 14 may be communicatively connected by a wire such as a cable, or may be communicatively connected by infrared communication or short-range wireless communication such as Bluetooth (registered trademark).

[0013] The pretreatment unit 12 holds a plurality of sample containers and includes an automatic sample injection device (not shown) for automatically injecting the liquid sample in the sample containers into the gas chromatograph unit 14. The pretreatment unit 12 can also hold a plurality of reagent containers, and can pretreat the liquid sample using the liquid reagent in the reagent containers, and then inject the pretreated liquid sample into the gas chromatograph unit 14.

[0014] The pretreatment unit 12 is capable of aspirating and injecting liquid through a needle. In the pretreatment unit 12, a pretreated liquid sample can be aspirated through a needle and injected into a sample vaporization chamber 20 in a sample introduction unit 18 (described later) of the gas chromatograph unit 14. In other words, the pretreatment unit 12 can pretreat the liquid sample and supply the pretreated liquid sample to the sample vaporization chamber 20 in the sample introduction unit 18.

[0015] 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, all of which are housed in a housing.

[0016] A sample introduction part 18, a column 22, a fan 24, a detector 26, etc. are provided inside a temperature-controllable column oven 16. Specifically, a part of the sample introduction part 18 and the detector 26 is provided inside the column oven 16.

[0017] The sample introduction part 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 septum (not shown). A sample vaporization chamber 20 is formed inside the sample introduction part 18. The sample vaporization chamber 20 is provided in the column oven 16, just like the sample introduction part 18.

[0018] Furthermore, 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 first heater 42a heats the sample introduction section 18. Therefore, the liquid sample injected into the sample vaporization chamber 20 is vaporized by the heat from the first heater 42a.

[0019] Furthermore, the sample introduction part 18 is provided with a temperature sensor 44. Specifically, the temperature sensor 44 includes a first temperature sensor 44a which is provided in the sample introduction part 18. The temperature of the sample introduction part 18 is detected by this first temperature sensor 44a.

[0020] Furthermore, the sample vaporization chamber 20 is connected to a gas supply channel 28 and a split channel 30. The gas supply channel 28 is a channel for supplying a carrier gas into the sample vaporization chamber 20 of the sample introduction part 18.

[0021] The split flow path 30 is a flow path for discharging a portion of the gas (a mixture of carrier gas and sample gas) in the sample vaporization chamber 20 to the outside at a predetermined split ratio when a carrier gas and a vaporized liquid sample (sample gas) are introduced into the column 22 by the split introduction method.

[0022] For these reasons, the sample introduction section 18 introduces the sample gas into the column 22 together with the carrier gas.

[0023] 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 this second heater 42b.

[0024] Specifically, the fan 24 is rotated as the second heater 42b generates heat. Therefore, the air heated by the second heater 42b circulates within the column oven 16. As a result, the column 22 is heated.

[0025] 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 this second temperature sensor 44b.

[0026] When the sample gas is introduced into the heated column 22, the sample components contained in the sample gas are separated into individual components. The column 22 is a general-purpose column, such as a capillary column.

[0027] The detector 26 is provided to sequentially detect the various components separated by the column 22. The detector 26 is configured by, for example, a flame ionization detector (FID).

[0028] The detector 26 is also 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.

[0029] Furthermore, the detector 26 is 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 this third temperature sensor 44c.

[0030] The column oven 16 is also provided with an air intake flap 34 that opens and closes the air intake port 32 and an exhaust flap 38 that opens and closes the exhaust port 36. When the column 22 is heated, the air intake flap 34 and the exhaust flap 38 are closed.

[0031] On the other hand, when cooling the inside of the column oven 16, the air intake flap 34 and the air exhaust flap 38 are changed from a closed state to an open state. The fan 24 is constantly rotating, and when cooling the inside of the column oven 16, the air taken in through the air intake port 32 removes heat from inside the column oven 16. The air that has removed the heat from inside the column oven 16 is then discharged from the air exhaust port 36.

[0032] From these facts, the fan 24 , the air intake flap 34 and the air exhaust flap 38 can be said to be a cooling mechanism 40 that cools the inside of the column oven 16 .

[0033] The gas chromatograph apparatus 10 described above can perform temperature-programmed analysis, which involves introducing a sample gas into the column 22, raising the temperature of the column 22 in the column oven 16, and detecting the sample components separated by the column 22 with the detector 26.

[0034] The heater 42 can heat the heating object 46 in the column oven 16. The temperature sensor 44 can detect the temperature of the heating object 46 in the column oven 16.

[0035] In this embodiment, the object to be heated 46 includes at least one of the sample introduction part 18, the column 22, and the detector 26. In the example shown in Fig. 2, the sample introduction part 18, the column 22, and the detector 26 are all included in the object to be heated 46. However, the object to be heated 46 is not limited to the sample introduction part 18, the column 22, or the detector 26.

[0036] 2. Electrical configuration of gas chromatograph equipment 2 is a block diagram showing an example of the electrical configuration of the gas chromatograph 10 of this embodiment. As shown in FIG. 2, the gas chromatograph 10 includes a control unit 50, a power control circuit 58, and the like in addition to a cooling mechanism 40, etc.

[0037] The control unit 50, pre-processing unit 12, power control circuit 58, first temperature sensor 44a, second temperature sensor 44b, third temperature sensor 44c, and cooling mechanism 40 are electrically connected to one another via a circuit 60 such as a bus. The power control circuit 58 is also connected to the first heater 42a, second heater 42b, and third heater 42c.

[0038] The control unit 50 is responsible for overall control of the gas chromatograph apparatus 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 that can be directly accessed by the CPU 52.

[0039] The CPU 52 controls each component of the gas chromatograph apparatus 10. The RAM 54 is used as a work area and a buffer area for the CPU 52. The storage unit 56 is a non-volatile memory, and for example, an HDD (Hard Disc Drive) or an SSD (Solid State Drive) is used as the storage unit 56.

[0040] The storage unit 56 stores a control program for controlling each component of the gas chromatograph apparatus 10, data required for executing the control program (execution data), etc. The storage unit 56 may be configured to include the RAM 54.

[0041] The power control circuit 58 is a circuit for supplying power to each of the first heater 42 a, the second heater 42 b, and the third heater 42 c. In other words, the power control circuit 58 is a circuit for controlling each of the first heater 42 a, the second heater 42 b, and the third heater 42 c.

[0042] Although not shown, the gas chromatograph 10 also includes an operation reception unit that receives operations from a user, a display unit that is a general-purpose display, and the like.

[0043] 3. Temperature control of the heated object In the gas chromatograph apparatus 10 of this embodiment, the temperature of the heating object 46 is controlled upon completion of the temperature-programmed analysis. The temperature control of the heating object 46 will be described in detail below. In this embodiment, upon completion of the temperature-programmed analysis, a cooling process is performed. In the cooling process, the inside of the column oven 16 is cooled using the cooling mechanism 40.

[0044] The cooling process cools the sample introduction part 18, the column 22, the detector 26, and the like in the column oven 16. The sample introduction part 18 and the detector 26 are also cooled by the outside air outside the column oven 16 in addition to the cooling mechanism 40.

[0045] In the gas chromatograph apparatus 10 of this embodiment, a heating process is performed after the cooling process. In the heating process, the heating object 46 in the column oven 16 is heated when the temperature detected by the temperature sensor 44 reaches the target temperature after the cooling process.

[0046] Furthermore, the cooling process ends with the start of the heating process. That is, the time during which the cooling process is performed (cooling time) is the time from the completion of the temperature rise analysis until the temperature detected by the temperature sensor 44 reaches the target temperature. Furthermore, during the heating process, the heater 42 is controlled so that the temperature detected by the temperature sensor 44 is maintained at the target temperature.

[0047] In the heating process, for example, when the temperature detected by the first temperature sensor 44a reaches a target temperature, the sample introduction section 18 in the column oven 16 is heated. Control of the second heater 42b based on the temperature detected by the second temperature sensor 44b and control of the third heater 42c based on the temperature detected by the third temperature sensor 44c are similar to those of the first heater 42a, so only the control of the first heater 42a will be described below.

[0048] Furthermore, in this embodiment, a determination process is executed in conjunction with the temperature control of the heating object 46. 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 has stabilized.

[0049] In the determination process, for example, after heating of the sample introduction section 18 is started by a heating process, it is determined whether the temperature of the entire sample introduction section 18 has stabilized based on the power consumption of the first heater 42a. Note that the entire sample introduction section 18 is a concept that includes not only the area around the first temperature sensor 44a but also the position in the sample introduction section 18 that is farthest from the first temperature sensor 44a. The same applies to the column 22 and the detector 26.

[0050] Fig. 3 is an example of a graph for explaining the heating process and cooling process of this embodiment. Fig. 4 is an example of a graph for explaining the heating process of this embodiment. Fig. 4 is an enlarged view of a part of Fig. 3. Figs. 3 and 4 show graphs corresponding to the sample introduction part 18.

[0051] 3 and 4, the dashed line indicates the temperature detected by the first temperature sensor 44a. The dashed line indicates the reference temperature. The reference temperature is the temperature of a portion of the sample introduction section 18 that is distant from the first temperature sensor 44a. The reference temperature was detected by providing an experimental temperature sensor separate from the first temperature sensor 44a. The solid line indicates the duty ratio related to the power consumption of the first heater 42a.

[0052] 3, after the temperature rise analysis is completed, the cooling process and the heating process are carried out in this order. The heating process is started when the temperature detected by the first temperature sensor 44a reaches the target temperature, so immediately after the start of the heating process, the temperature detected by the first temperature sensor 44a is the same as the target temperature.

[0053] Furthermore, 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) in the vicinity of the first temperature sensor 44a in the sample introduction part 18 is stable.

[0054] On the other hand, since the sample introduction part 18 uses many metal components, the temperature of the part of the sample introduction part 18 away from the first temperature sensor 44a gradually decreases due to the outside air outside the column oven 16. Therefore, in the examples shown in Figures 3 and 4, the detected temperature is maintained at the target temperature, while the reference temperature decreases slightly.

[0055] Furthermore, in the heating process, the detected temperature is maintained at the target temperature while heat is being removed from the sample introduction part 18, so the duty ratio related to the power consumption of the first heater 42a increases.

[0056] Furthermore, the duty ratio related to the power consumption of the first heater 42a gradually stabilizes while increasing. This is because the sample introduction part 18 is heated to a degree that stabilizes the overall temperature even if it is affected by the outside air outside the column oven 16. Therefore, in the examples shown in Figures 3 and 4, as the duty ratio related to the power consumption of the first heater 42a stabilizes, the reference temperature also stabilizes.

[0057] Therefore, in the example shown in Figures 3 and 4, when the change in the duty ratio related to the power consumption of the first heater 42a, specifically, the change in the duty ratio over a predetermined period of time, becomes below a threshold value, it can be determined that the overall temperature of the sample introduction section 18 has stabilized.

[0058] The same applies to the case where the column 22 is heated by the second heater 42b or the case where the detector 26 is heated by the third heater 42c during the heat treatment.

[0059] Furthermore, in the above example, it is determined that the overall temperature of the object to be heated 46 is stabilized when the amount of change in the duty ratio related to the power consumption of the heater 42 becomes equal to or less than a threshold value, but it may also be determined that the overall temperature of the object to be heated 46 is stabilized when the duty ratio related to the power consumption of the heater 42 (the duty ratio itself) becomes equal to or greater than a threshold value. Note that 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.

[0060] Also, for example, if 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 overall temperature of the object to be heated 46 has stabilized.

[0061] Furthermore, for example, instead of the duty ratio related to the power consumption of the heater 42, it may be determined that the temperature of the entire object to be heated 46 has stabilized simply based on the power consumption of the heater 42.

[0062] In this embodiment, the equilibration time is the time required from the start of the heating process until it is determined that the temperature of the entire heating object 46 has stabilized. In this way, if it can be determined that the temperature of the entire heating object 46 has stabilized after a temperature rise analysis, the next temperature rise analysis can be performed after the temperature of the entire heating object 46 has stabilized. In other words, in repeated temperature rise analyses, good analysis results can be obtained, while the time required for repeated temperature rise analyses can be prevented from being longer than necessary.

[0063] Furthermore, if it is possible to determine whether the overall temperature of the heating object 46 has stabilized, there is no need to set parameters such as the equilibration time in advance when repeatedly performing temperature rise analysis, which saves unnecessary effort.

[0064] Furthermore, if there are multiple heating objects 46, the next temperature-programmed analysis can be performed after the overall temperature of each heating object 46 has stabilized. For example, if the heating object 46 includes the sample introduction portion 18, the column 22, and the detector 26, particularly good analytical results can be obtained.

[0065] Furthermore, in this embodiment, when temperature rise analysis is repeatedly performed, information about 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 the 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 overall temperature of the heating object 46 has stabilized. Note that the stabilization period can also be said to be the period from the completion of the temperature rise analysis until it is determined that the overall temperature of the heating object 46 has stabilized.

[0066] For example, if the heating object 46 includes the sample introduction part 18, the column 22, and the detector 26, the stabilization period is the period from when the cooling process starts until it is determined that the overall temperatures of the sample introduction part 18, the column 22, and the detector 26 have stabilized. Compared to the column 22 (capillary column), which has a small heat capacity, the sample introduction part 18 and the detector 26 have a large heat capacity and tend to have a long stabilization period.

[0067] In this embodiment, if stabilization period information is stored in the storage unit 56, the preprocessing unit 12 is instructed to start preprocessing of the sample for the next temperature-programmed analysis so that the preprocessing of the sample for the next temperature-programmed analysis is completed at a timing corresponding to the end 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 + equilibration time) stored in the storage unit 56, and after the start of the cooling process, the preprocessing unit 12 is instructed to start preprocessing of the sample for the next temperature-programmed analysis at the time when the waiting time has elapsed. This allows the next temperature-programmed analysis to start simultaneously with the end of the stabilization period. Note that if stabilization period information is not stored in the storage unit 56, the preprocessing unit 12 is instructed to start preprocessing of the sample for the next temperature-programmed analysis as in the conventional method.

[0068] However, the start timing of the next temperature-programmed analysis does not have to be simultaneous with the end timing of the stabilization period, and may be before or after that. In other words, the timing according to the end timing of the stabilization period includes timing before and after that end timing. Therefore, the timing at which pretreatment of the sample for the next temperature-programmed analysis is completed may be before or after the end timing of the stabilization period.

[0069] As described above, when pretreatment is performed on a liquid sample in pretreatment unit 12, the liquid sample is pretreated using a liquid reagent. If the pretreatment of the sample for the next temperature program analysis is completed before the end of the stabilization period, the pretreated liquid sample will remain in a state awaiting the temperature program analysis, which may adversely affect the analysis results.

[0070] On the other hand, if the timing at which pretreatment of the sample for the next heating analysis is completed is after the end of the stabilization period, a waiting time is required between heating analyses after the end of the stabilization period before the next heating analysis is started, which unnecessarily lengthens the time required for repeated heating analyses.

[0071] Therefore, it is preferable that the timing at which the pretreatment of the sample for the next temperature-programmed analysis is completed is synchronized with the end of the stabilization period.

[0072] By storing the stabilization period information in the storage unit 56 in this manner, it is possible to complete the pretreatment of the sample for the next temperature-programmed analysis at a timing corresponding to the end timing of the stabilization period.

[0073] 3. Specific electrical configuration of the gas chromatograph 5 is a block diagram specifically showing the electrical configuration of the gas chromatograph 10 of this embodiment. Note that the storage unit 56 is not shown in FIG.

[0074] The RAM 54 stores execution data that has been read out in advance from the storage unit 56. In addition, when acquired data acquired using devices, sensors, etc. is stored in the storage unit 56, the acquired data is temporarily stored in the RAM 54.

[0075] 5, the RAM 54 stores stabilization period data 62 and instruction data 64. Although not shown in the figure, the RAM 54 also stores data required for controlling various components.

[0076] The stabilization period data 62 is data corresponding to the stabilization period information. The instruction data 64 is data corresponding to an instruction to be output to the preprocessing unit 12.

[0077] A control program (not shown) previously read from the memory unit 56 is stored in the RAM 54, and when the CPU 52 executes the control program, the control unit 50 functions as a temperature control unit 66, a judgment processing unit 70, a memory processing unit 72, and an instruction processing unit 74.

[0078] When the temperature rise analysis is completed, the temperature control unit 66 cools the inside of the column oven 16 using the cooling mechanism 40, and when the temperature detected by the temperature sensor 44 reaches the target temperature, the temperature control unit 66 heats the heating object 46 using the heater 42. The temperature control by the temperature control unit 66 is performed by PID (Proportional Integral Differential) control.

[0079] 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 object to be heated 46 has stabilized based on the power consumption of the heater 42.

[0080] 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.

[0081] The instruction processing unit 74 instructs the pre-processing unit 12 to start pre-processing of the sample for the next temperature rise analysis so that the pre-processing of the sample for the next temperature rise analysis is completed at a timing corresponding to the end timing of the stabilization period.

[0082] 4. Flow 6 is a flow chart showing an example of the temperature rise analysis process of the CPU 52 of this embodiment. The temperature rise analysis process is started, for example, in response to the gas chromatograph apparatus 10 receiving an operation to start the temperature rise analysis.

[0083] In step S1, a temperature-programmed analysis is carried out, and in step S2, the inside of the column oven 16 is cooled.

[0084] In step S3, it is determined whether the temperature detected by the temperature sensor 44 has reached the target temperature. If the result in step S3 is "NO," 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 result in step S3 is "YES," that is, if the temperature detected by the temperature sensor 44 has reached the target temperature, the process proceeds to step S4.

[0085] In step S4, the heating object 46 in the column oven 16 is heated, and in step S5, it is determined whether the overall temperature of the heating object 46 has stabilized based on the power consumption of the heater 42. If step S5 returns "NO," that is, if the overall temperature of the heating object 46 has not stabilized, the process returns to step S4. On the other hand, if step S5 returns "YES," that is, if the overall temperature of the heating object 46 has stabilized, the process proceeds to step S6.

[0086] 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.

[0087] In step S8, it is determined whether this is the last temperature rise analysis among the repeatedly performed temperature rise analyses. If "NO" in step S8, that is, if this is not the last temperature rise analysis, the process returns to step S1. On the other hand, if "YES" in step S8, that is, if this is the last temperature rise analysis, the temperature rise analysis process ends.

[0088] 7 is a flowchart showing an example of instruction output processing by the CPU 52 of this embodiment. The instruction output processing is started, for example, in response to the gas chromatograph apparatus 10 receiving an operation to start a temperature-programmed analysis.

[0089] 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.

[0090] In step S11, the stabilization period data 62 is referenced, and in step S12, it is determined whether it is time to issue an instruction to the pre-processing unit 12. If the answer is "NO" in step S12, that is, if it is not time 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 time to issue an instruction to the pre-processing unit 12, in step S13, the pre-processing unit 12 is instructed to pre-process the liquid sample.

[0091] In step S14, it is determined whether the previous instruction to the pre-processing unit 12 is the last instruction. If the answer is "NO" in step S14, that is, if the previous instruction to the pre-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 previous instruction to the pre-processing unit 12 is the last instruction, the instruction output process ends.

[0092] It should be noted that the order in which the steps in the flow charts shown in the above-described embodiments are processed can be changed as appropriate, provided that the same results are obtained.

[0093] Furthermore, the electrical configurations and the like shown in the above-described embodiments are merely examples and can be modified as appropriate in actual products. For example, although the present embodiment exemplifies a case in which a liquid sample is used as the sample, the form of the sample is not particularly limited as long as the sample can be introduced through the sample introduction section 18. For example, when a gas sample is used as the sample, the pretreatment section 12 is configured to pretreat the gas sample and supply the pretreated gas sample to the sample introduction section 18. In such a case, the sample introduction section 18 is of a type suitable for gas samples, specifically, a type that does not have a sample vaporization chamber 20.

[0094] 5. Aspects It will be appreciated by those skilled in the art that the exemplary embodiments described above are examples of the following aspects.

[0095] (Item 1) A gas chromatograph apparatus according to one aspect comprises: A gas chromatograph apparatus capable of performing temperature-programmed analysis, which is an analysis in which a sample is introduced into a column through a sample introduction section, and sample components separated by the column are detected by a detector while the temperature of the column is increased in a column oven, a heater that heats an object to be heated in the column oven; a cooling mechanism for cooling the inside of the column oven; a temperature sensor that detects the temperature of the object to be heated; a temperature control unit that cools the inside of the column oven using the cooling mechanism when the temperature rise analysis is completed, and heats the heating object using the heater when the temperature detected by the temperature sensor reaches a target temperature; The heating device may further include a determination processing unit that determines whether the temperature of the entire object to be heated has stabilized based on the power consumption of the heater when the temperature detected by the temperature sensor reaches the target temperature.

[0096] According to the gas chromatograph apparatus described in paragraph 1, after a temperature-programmed analysis, the object to be heated in the column oven is cooled to a target temperature, and then it is possible to appropriately determine whether the temperature of the entire object to be heated has stabilized based on the power consumption of the heater. This allows the next temperature-programmed analysis to be performed after the temperature of the entire object to be heated has stabilized. Furthermore, if the next temperature-programmed analysis can be performed after the temperature of the entire object to be heated has stabilized, good analytical results can be obtained in repeated temperature-programmed analyses, while preventing the time required for repeated temperature-programmed analyses from being longer than necessary.

[0097] (Item 2) In the gas chromatograph apparatus according to item 1, The heating device may further include a memory processing unit that stores information about a stabilization period, which is the period from when cooling by the cooling mechanism begins until when the judgment processing unit judges that the temperature of the entire object to be heated has stabilized.

[0098] According to the gas chromatograph apparatus described in paragraph 2, it is possible to store information about the stabilization period. Furthermore, if information about the stabilization period can be stored, that information can be used in the next temperature-programmed analysis.

[0099] (Item 3) In the gas chromatograph apparatus according to item 2, a pretreatment section that pretreats a sample and supplies the pretreated sample to the sample introduction section; The apparatus may further include an instruction processing unit that instructs the pre-processing unit to start pre-processing of the sample for the next temperature rise analysis so that the pre-processing of the sample for the next temperature rise analysis is completed at a timing corresponding to the end timing of the stabilization period.

[0100] According to the gas chromatograph apparatus described in paragraph 3, the pretreatment of the sample for the next temperature-programmed analysis is completed at a timing corresponding to the end of the stabilization period, thereby minimizing the waiting time between the completion of the pretreatment of the sample and the start of the temperature-programmed analysis of that sample. This effectively prevents the time required for repeated temperature-programmed analyses from becoming longer than necessary. Furthermore, since the pretreated sample is prevented from remaining in a state waiting for the temperature-programmed analysis, better analysis results can be obtained.

[0101] (Item 4) In the gas chromatograph apparatus according to any one of items 1 to 3, The determination processing unit may determine that the temperature of the entire object to be heated has stabilized when a change in a duty ratio related to power consumption of the heater becomes equal to or less than a threshold value.

[0102] According to the gas chromatograph device described in paragraph 4, it is possible to appropriately determine that the overall temperature of the object to be heated has stabilized based on the fact that the amount of change in the duty ratio related to the power consumption of the heater has become equal to or less than a threshold value.

[0103] (Item 5) In the gas chromatograph apparatus according to any one of items 1 to 3, The determination processing unit may determine that the temperature of the entire object to be heated has stabilized when a duty ratio related to the power consumption of the heater is equal to or greater than a threshold value.

[0104] According to the gas chromatograph device described in paragraph 5, it is possible to appropriately determine that the temperature of the entire object to be heated has stabilized based on whether the duty ratio related to the power consumption of the heater has reached a threshold value or more.

[0105] (Item 6) In the gas chromatograph apparatus according to any one of Items 1 to 5, The object to be heated may include at least one of the sample introduction section, the column, and the detector.

[0106] According to the gas chromatograph apparatus described in item 6, it is possible to appropriately determine whether the overall temperature of at least one of the sample introduction part, the column, and the detector has stabilized after the temperature-programmed analysis. [Explanation of symbols]

[0107] 10 Gas chromatograph 12 Pretreatment section 16 Column oven 18 Sample introduction section 22 Columns 26 detector 40 Cooling mechanism 42 Heater 44 Temperature Sensor 46 Heating object 56 Memory section 66 Temperature control unit 70 Judgment processing unit 72 Memory Processing Unit 74 Instruction processing section

Claims

1. A gas chromatograph apparatus capable of performing temperature-programmed analysis, which is an analysis in which a sample is introduced into a column through a sample introduction section, and sample components separated by the column are detected by a detector while the temperature of the column is increased in a column oven, a heater that heats an object to be heated in the column oven; a cooling mechanism for cooling the inside of the column oven; a temperature sensor that detects the temperature of the object to be heated; a temperature control unit that, upon completion of the temperature-programmed analysis, executes a cooling process to cool the inside of the column oven using the cooling mechanism, and, upon the temperature detected by the temperature sensor reaching a target temperature after the cooling process, executes a heating process to heat the heating object using the heater; a determination processing unit that determines whether the temperature of the entire object to be heated has stabilized based on the power consumption of the heater when the temperature detected by the temperature sensor reaches the target temperature after the cooling process.

2. 2. The gas chromatograph apparatus according to claim 1, further comprising a memory processing unit that stores information about a stabilization period, which is a period from when the cooling process is started by starting cooling using the cooling mechanism until when the determination processing unit determines that the temperature of the entire object to be heated has stabilized.

3. a pretreatment section that pretreats a sample and supplies the pretreated sample to the sample introduction section; 3. The gas chromatograph apparatus according to claim 2, further comprising an instruction processing unit that instructs the preprocessing unit to start preprocessing of the sample for the next programmed temperature analysis so that the preprocessing of the sample for the next programmed temperature analysis is completed at a timing corresponding to an end timing of the stabilization period.

4. 4. The gas chromatograph apparatus according to claim 1, wherein the determination processor determines that the temperature of the entire object to be heated is stable when a change in a duty ratio related to power consumption of the heater becomes equal to or less than a threshold value.

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

6. The gas chromatograph apparatus according to claim 1 , wherein the object to be heated includes at least one of the sample introduction section, the column, and the detector.

Images