Gas chromatograph analysis system, gas chromatograph analysis apparatus, and control method
The gas chromatographic analysis system addresses the efficiency reduction in sample desorption by controlling carrier gas pressure during desorption, enhancing sample introduction and peak shape in the chromatogram.
Patent Information
- Application Number
- PCT/JP2024/020338
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-07-31
- Filing Date
- 2024-06-04
- Publication Date
- 2025-02-06
AI Technical Summary
The efficiency of desorption of sample gas in gas chromatography using solid phase microextraction is reduced when a large amount of sample gas is adsorbed or when the sample gas has a strong interaction with the adsorption section, leading to decreased sample introduction into the separation column and broadened chromatogram peaks.
A gas chromatographic analysis system that controls the supply pressure of carrier gas during the desorption period, initially setting it to a higher pressure (e.g., 250 kPa) to enhance desorption efficiency and then reducing it to a lower pressure (e.g., 100 kPa) after the desorption is complete, to maintain peak shape and sample introduction efficiency.
This approach effectively suppresses the reduction in desorption efficiency, ensuring a higher amount of sample gas is introduced into the separation column and maintaining the sharpness of chromatogram peaks, even for weakly retained components.
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Figure JP2024020338_06022025_PF_FP_ABST
Abstract
Description
Gas chromatograph analysis system, gas chromatograph analysis device, and control method
[0001] The present disclosure relates to a gas chromatograph analysis system, a gas chromatograph analysis apparatus, and a control method.
[0002] Conventionally, solid phase microextraction (SPME) has been used as a method for introducing a sample gas into a gas chromatograph. Patent Document 1 (JP 2020-165847 A) describes introducing beef volatile components into a gas chromatograph using solid phase microextraction.
[0003] In Patent Document 1, beef as a sample and an adsorption unit (SPME) are stored in a container, and the container is heated at 200°C for 15 minutes, causing the beef's volatile components to be adsorbed onto the adsorption unit. The adsorption unit, which has adsorbed the beef's volatile components, is then inserted into a sample vaporization chamber of a gas chromatograph. The adsorption unit is heated in the sample vaporization chamber, causing the sample gas adsorbed onto the adsorption unit to desorb. The desorbed sample gas is then introduced into a separation column, where it is detected by a detection device for each component.
[0004] Japanese Patent Application Laid-Open No. 2020-165847
[0005] When introducing a sample gas using this solid-phase microextraction method, if a large amount of sample gas is adsorbed to the adsorption unit, or if a sample gas that has a strong interaction with the adsorption unit is adsorbed to the adsorption unit, the desorption efficiency of the sample in the sample vaporization chamber may decrease.When the desorption efficiency decreases, the amount of sample gas introduced into the separation column per unit time becomes small, which can result in broad peak shapes in the chromatogram detected by the detection device.
[0006] The present disclosure has been made to solve the above-mentioned problems, and its purpose is to provide a technology that suppresses a decrease in desorption efficiency when a sample is desorbed from an adsorption section in a gas chromatographic analysis system in which a sample gas is introduced by solid-phase microextraction.
[0007] According to one aspect of the present disclosure, a gas chromatograph analysis system separates components in a sample gas introduced by solid-phase microextraction. The gas chromatograph analysis system includes a gas chromatograph device that separates the components in the sample gas introduced by solid-phase microextraction, and a control device that controls the gas chromatograph device. The gas chromatograph device includes a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted, a gas supply source that supplies a carrier gas to the sample vaporization chamber, a regulator that regulates the amount of carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas, a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber, and a detection device that detects the components in the sample gas that has passed through the separation column. The control device controls the regulator to maintain a supply pressure of a first pressure during a desorption period in which the sample gas is desorbed from the adsorption unit, and controls the regulator to maintain a supply pressure of a second pressure lower than the first pressure after the desorption period ends.
[0008] According to one aspect of the present disclosure, a gas chromatograph apparatus separates components in a sample gas introduced therein by solid-phase microextraction, and includes: a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted; a gas supply source that supplies a carrier gas to the sample vaporization chamber; an adjusting device that adjusts the amount of carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas; a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber; and a detection device that detects the components in the sample gas that has passed through the separation column. The adjusting device applies a first supply pressure to the carrier gas during a desorption period in which the sample gas is desorbed from the adsorption unit, and applies a second supply pressure to the carrier gas after the desorption period ends, the second supply pressure being lower than the first pressure.
[0009] According to one aspect of the present disclosure, there is provided a method for controlling a gas chromatograph that separates components in a sample gas introduced therein by solid-phase microextraction. The gas chromatograph includes a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted, a gas supply source that supplies a carrier gas to the sample vaporization chamber, a regulator that regulates the amount of carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas, a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber, and a detector that detects components in the sample gas that has passed through the separation column. The control method includes, as processing executed by a computer that controls the gas chromatograph, controlling the regulator so that the supply pressure is a first pressure during a desorption period in which the sample gas is desorbed from the adsorption unit, and controlling the regulator so that the supply pressure is a second pressure lower than the first pressure after the desorption period ends.
[0010] According to the present disclosure, in a gas chromatographic analysis system in which a sample gas is introduced by solid-phase microextraction, it is possible to suppress a decrease in desorption efficiency when the sample is desorbed from an adsorption unit.
[0011] It is a diagram showing a schematic configuration of a gas chromatograph analysis system according to the present embodiment. It is a diagram for explaining adsorption and desorption of a sample to an adsorption unit. It is a diagram showing a flowchart for increasing the supply pressure of a carrier gas during thermal desorption. It is a timing chart showing the supply pressure and the column oven temperature in the present embodiment.
[0012] [Embodiment] The present embodiment will be described in detail with reference to the drawings. Note that the same or corresponding parts in the drawings are given the same reference numerals, and in principle, their description will not be repeated.
[0013] 1 is a diagram showing a schematic configuration of a gas chromatograph analysis system 1000 according to this embodiment. The gas chromatograph analysis system 1000 includes a control device 100, a gas chromatograph device 200, an input device 300, and a display device 400.
[0014] The gas chromatograph 200 includes a gas supply B1, a conditioning device 210, a sample vaporization chamber 220, a column oven Ov1, a separation column CL1, a detection device 230, and heaters Ht1 and Ht2. The heater Ht1 may correspond to the "first heating device" in this disclosure, and the heater Ht2 may correspond to the "second heating device" in this disclosure.
[0015] The gas supply source B1 supplies a carrier gas to the sample vaporization chamber 220. The gas supply source B1 is, for example, a gas tank that stores the carrier gas. The carrier gas is, for example, helium (He). The adjusting device 210 adjusts the flow rate of the carrier gas by adjusting the supply pressure applied to the carrier gas supplied from the gas supply source B1 based on a control signal received from the control device 100. As shown in FIG. 1 , the adjusting device 210 is disposed between the gas supply source B1 and the sample vaporization chamber 220.
[0016] The sample vaporization chamber 220 is provided with a septum 221 for inserting the adsorption unit SP1. The adsorption unit SP1 is a device used in solid-phase microextraction and includes a fiber that adsorbs the sample. Solid-phase microextraction is a method of extracting and concentrating volatile components generated from a liquid or solid sample using the adsorption unit SP1. The fiber is housed inside a needle. In the adsorption unit SP1 of this embodiment, the fused silica fiber is coated with a liquid phase (adsorption phase). The liquid phase can be, for example, polydimethylsiloxane (PDMS), divinylbenzene (DVB), or the like.
[0017] In this embodiment, the surface area of the coated liquid phase is 44.0 mm 2 More specifically, the surface area of the liquid phase is, for example, 44.0 mm 2 or 62.8 mm 2 In this embodiment, the liquid phase volume of the adsorption part SP1 is 3.8 μL or more. More specifically, the liquid phase volume of the adsorption part SP1 is, for example, 3.8 μL or 11.8 μL. The surface area of the liquid phase of the adsorption part used in a general solid-phase microextraction method is 9.4 mm 2 and the liquid phase volume is 0.6 μL.
[0018] In other words, the surface area and volume of the liquid phase of the adsorption unit SP1 in this embodiment are larger than those of adsorption units used in such general solid-phase microextraction methods. The larger the surface area and volume of the liquid phase, the greater the amount of sample gas that can be adsorbed by the adsorption unit SP1. The adsorption unit SP1 in this embodiment may be for either a manual or autosampler use.
[0019] As shown in FIG. 1 , after the sample is adsorbed onto the adsorption unit SP1, the adsorption unit SP1 is inserted into the sample vaporization chamber 220 via the septum 221. The heater Ht1 heats the sample vaporization chamber 220 based on a control signal received from the control device 100. The sample adsorbed onto the adsorption unit SP1 is desorbed from the adsorption unit SP1 by heating from the heater Ht1. Hereinafter, the process of desorbing the sample adsorbed onto the adsorption unit SP1 by heating from the heater Ht1 is referred to as "thermal desorption."
[0020] The sample desorbed by thermal desorption is introduced into a separation column CL1 in a column oven Ov1 together with a carrier gas supplied from a gas supply source B1. Various compounds contained in the sample gas are separated while passing through the separation column CL1 and are sequentially introduced into the detection device 230. In this way, the gas chromatograph device 200 separates and detects the components contained in the sample gas.
[0021] The control device 100 includes a processor 110 and a storage device 120. The processor 110 is a computing entity (computer) that executes various processes by executing various programs. The processor 110 includes, for example, a central processing unit (CPU) and a micro-processing unit (MPU). The processor 110 has the function of executing various processes by executing programs, but some or all of these functions may be implemented by application-specific integrated circuits such as field programmable gate arrays (FPGAs) and application-specific integrated circuits (ASICs).
[0022] That is, the term "processor" is not limited to a processor in the narrow sense that executes processing using a stored program, such as a CPU or MPU, but may also include hardwired circuits such as an ASIC or FPGA. Therefore, processor 110 can also be interpreted as processing circuitry in which processing is predefined by computer-readable code and / or hardwired circuits. Processor 110 may be configured on a single chip or multiple chips.
[0023] Furthermore, the processor 110 and related processing circuits may be configured as multiple computers interconnected by wire or wirelessly, such as via a local area network or a wireless network. The processor 110 and related processing circuits may also be configured as a cloud computer that performs remote calculations based on input data and outputs the results of the calculations to other devices at remote locations.
[0024] The storage device 120 may include volatile memory such as dynamic random access memory (DRAM) or static random access memory (SRAM), and non-volatile memory such as read-only memory (ROM) or flash memory. The storage device 120 may be one or more non-transitory computer-readable media or one or more computer-readable storage media. For example, the storage device 120 may be an optical medium such as an SD card, a hard disk drive (HD), a solid-state drive (SSD), a CD, or a DVD. As shown in FIG. 1 , the storage device 120 stores a control program P1.
[0025] The input device 300 is a device that receives commands from a user. The input device 300 may be, for example, a keyboard, a mouse, or buttons. The display device 400 is a device that displays information such as detection results to the user. The display device 400 is realized by, for example, a liquid crystal or organic EL (Electro Luminescence) monitor. The input device 300 and the display device 400 may be provided integrally as a touch screen.
[0026] 2A and 2B are diagrams illustrating the adsorption and desorption of a sample to the adsorption part SP1. Fig. 2A is a diagram illustrating an example of adsorption of a volatile component of a liquid sample S. Fig. 2B is a diagram illustrating an example of adsorption of a volatile component of a solid sample S. As shown in Figs. 2A and 2B, whether the sample S is a liquid or a solid, the volatile component of the sample S vaporized by heating is adsorbed to the adsorption part SP1.
[0027] 2C shows an example of desorbing the sample S adsorbed on the adsorption unit SP1. As shown in FIG. 2C, when the sample vaporization chamber 220 is heated by the heater Ht1, the sample S is desorbed from the adsorption unit SP1 and introduced into the separation column CL1.
[0028] As described above, the surface area of the liquid phase in the adsorption part SP1 of this embodiment is 44.0 mm 2 The adsorption part SP1 having such a large volume of liquid phase has a surface area of the liquid phase of 9.4 mm2 as described above. 2 This allows a larger amount of sample gas to be adsorbed than an adsorption section with a liquid phase volume of 0.6 μL. However, if a large amount of sample gas is adsorbed, a large amount of sample gas needs to be desorbed from the adsorption section SP1, which may reduce the desorption efficiency.
[0029] If the gas chromatograph 200 employs the split injection method, increasing the split ratio improves the desorption efficiency, but reduces the amount of sample gas introduced into the separation column CL1, resulting in a decrease in the sensitivity of the chromatogram. Therefore, in the gas chromatograph analysis system 1000 of this embodiment, the supply pressure of the carrier gas is increased during the period when thermal desorption is performed. The split injection method is an injection method in which only a portion of the heated and vaporized sample is introduced into the separation column CL1 and the majority of the heated and vaporized sample is discharged.
[0030] 3 is a flowchart showing a process for increasing the supply pressure of the carrier gas during the thermal desorption period. The control device 100 executes a control program P1 stored in the storage device 120 to realize the process of the flowchart in FIG. 3.
[0031] The control device 100 determines whether the thermal desorption period has started (step S100). When analysis is performed using an autosampler, the control device 100 determines whether the thermal desorption period has started in accordance with a program that controls the autosampler. When analysis is performed using an autosampler, the process automatically transitions to the thermal desorption step after the adsorption unit SP1 is inserted into the sample vaporization chamber 220. On the other hand, when analysis is performed manually, the control device 100 determines that the thermal desorption period has started, for example, when it receives a command from a user to start thermal desorption.
[0032] If the thermal desorption period has not started (NO in step S100), the control device 100 ends the process. If the thermal desorption has started (YES in step S100), the control device 100 sets the supply pressure of the carrier gas to 250 kPa (step S110). The supply pressure of 250 kPa is a predetermined value that maximizes the desorption efficiency of the sample. The supply pressure of 250 kPa is determined based on experiments and simulations. In other words, the control device 100 controls the adjustment device 210 so that the supply pressure of the carrier gas is 250 kPa. Note that 250 kPa in step S110 may correspond to the "first pressure" in this disclosure.
[0033] The control device 100 heats the sample vaporization chamber 220 (step S120). That is, the control device 100 drives the heater Ht1. Then, the control device 100 determines whether the thermal desorption period has ended (step S130). The thermal desorption period is a predetermined period, for example, one minute from the start of thermal desorption. The one-minute thermal desorption period is a period predetermined to maximize the desorption efficiency of the sample. The thermal desorption period is determined based on experiments and simulations. Note that, in some aspects, the thermal desorption period may be another period, such as two minutes or three minutes. If the thermal desorption period has not ended (NO in step S130), the control device 100 repeats the process of step S130. That is, the control device 100 waits until the thermal desorption period has elapsed.
[0034] If the thermal desorption period has elapsed (YES in step S130), the control device 100 sets the supply pressure of the carrier gas to 100 kPa (step S140). In other words, the control device 100 controls the adjustment device 210 so that the supply pressure of the carrier gas is 100 kPa. In step S130, the control device 100 stops driving the heater Ht1.
[0035] The 100 kPa in step S140 may correspond to the "second pressure" in the present disclosure. The supply pressure of the carrier gas in step S140 is lower than the supply pressure of the carrier gas in step S110. The 100 kPa in step S140 is a supply pressure that is predetermined depending on the type of carrier gas so that the sample gas can be appropriately separated in the separation column CL1.
[0036] Next, the control device 100 determines whether a predetermined period of time has elapsed (step S150). The predetermined period of time is a predetermined period of time, such as 5 seconds or 10 seconds after the end of thermal desorption. If the predetermined period of time has not elapsed (NO in step S150), the control device 100 repeats the process of step S150. That is, the control device 100 waits until the predetermined period of time has elapsed. The predetermined period of time in step S150 is a period for stabilizing the supply pressure at 100 kPa.
[0037] If the predetermined period has elapsed (YES in step S150), the control device 100 heats the separation column CL1 (step S160). That is, the control device 100 drives the heater Ht2. The sample desorbed in the sample vaporization chamber 220 passes through the separation column CL1 in a gaseous state as a result of the heating of the separation column CL1, and is introduced into the detection device 230 together with the carrier gas.
[0038] In this embodiment, during the thermal desorption period, the supply pressure of the carrier gas is increased above the supply pressure used when separating the sample gas in the separation column CL1. As a result, in the gas chromatograph analysis system 1000 of this embodiment, during the thermal desorption step, the supply of high-pressure carrier gas into the sample vaporization chamber 220 promotes desorption of the sample gas from the adsorption section SP1, thereby preventing a decrease in sample desorption efficiency. As a result, in the gas chromatograph analysis system 1000, even for components that are weakly retained by the separation column CL1, broad peak shapes are prevented from appearing in the chromatogram detected by the detection device 230.
[0039] Furthermore, in the gas chromatographic analysis system 1000 of this embodiment, the amount of sample gas introduced into the separation column CL1 is not reduced because the adsorbed sample gas is not discharged, as compared with the case where the split ratio is increased. Furthermore, in the gas chromatographic analysis system 1000 of this embodiment, a predetermined waiting period is provided in step S150, so that separation of the sample gas in the separation column CL1 can be started after the supply pressure has stabilized at 100 kPa.
[0040] 4A and 4B are timing charts showing the supply pressure and column oven temperature in this embodiment. In Fig. 4A, the vertical axis represents the supply pressure of the carrier gas, and the horizontal axis represents the elapsed time. In Fig. 4B, the vertical axis represents the column oven temperature, and the horizontal axis represents the elapsed time. At timing Tm1, thermal desorption begins.
[0041] With the start of thermal desorption, the supply pressure of the carrier gas is controlled to 250 kPa. At timing Tm2 when the thermal desorption period ends, the supply pressure of the carrier gas is controlled to 100 kPa. Thereafter, at timing Tm3 when a predetermined period has elapsed, the heater Ht2 is driven, and the temperature of the column oven Ov1 begins to rise.
[0042] In this way, in this embodiment, during the thermal desorption period, the supply pressure of the carrier gas is increased above the supply pressure when the sample gas is separated in the separation column CL1, thereby promoting desorption of the sample gas and suppressing a decrease in the desorption efficiency of the sample.
[0043] [Modification] In the above example, the control device 100, the gas chromatograph device 200, the input device 300, and the display device 400 are provided separately. However, the control device 100, the gas chromatograph device 200, the input device 300, and the display device 400 may be provided integrally. In other words, the gas chromatograph device 200 may include the control device 100, the input device 300, and the display device 400.
[0044] In the above example, the surface area of the suction part SP1 is 44.0 mm 2 In the above example, the liquid phase amount is 3.8 μL or more. However, in one aspect, the surface area of the adsorption part SP1 is 44.0 mm 2 The liquid phase volume may be less than 3.8 μL. The liquid phase volume may also be less than 3.8 μL. Even if the amount of sample gas that can be adsorbed by the adsorption unit SP1 is small, if the adsorption unit SP1 adsorbs a sample gas that has a strong interaction with the adsorption unit SP1, the desorption efficiency of the sample in the sample vaporization chamber 220 will decrease. Even in such a case, as described above, by increasing the supply pressure of the carrier gas during the thermal desorption period above the supply pressure when the sample gas is separated in the separation column CL1, the desorption of the sample gas can be promoted and a decrease in the desorption efficiency of the sample can be suppressed.
[0045] In the above example, a predetermined period is set in step S150 to stabilize the supply pressure, but in some aspects, heating of separation column CL1 may be started when the supply pressure drops to 100 kPa. That is, the predetermined period does not have to be set in step S150.
[0046] In the above example, the carrier gas supply pressure during the thermal desorption period is 250 kPa, and the carrier gas supply pressure after the thermal desorption is 100 kPa. However, in some aspects, the carrier gas supply pressure may be other values. For example, the carrier gas supply pressure during the thermal desorption period may be in the range of 230 kPa to 270 kPa, and the carrier gas supply pressure after the thermal desorption may be in the range of 80 kPa to 120 kPa.
[0047] Aspects It will be understood by those skilled in the art that the exemplary embodiments described above are examples of the following aspects.
[0048] (Item 1) One embodiment of a gas chromatograph analysis system is a gas chromatograph analysis system that separates components in a sample gas introduced by solid-phase microextraction. The gas chromatograph analysis system includes a gas chromatograph device that separates components in a sample gas introduced by solid-phase microextraction, and a control device that controls the gas chromatograph device. The gas chromatograph device includes a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted, a gas supply source that supplies a carrier gas to the sample vaporization chamber, a regulator that regulates the amount of carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas, a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber, and a detection device that detects components in the sample gas that has passed through the separation column. The control device controls the regulator so that the supply pressure is a first pressure during a desorption period in which the sample gas is desorbed from the adsorption unit, and controls the regulator so that the supply pressure is a second pressure lower than the first pressure after the desorption period ends.
[0049] According to the gas chromatographic analysis system described in paragraph 1, in a gas chromatographic analysis system in which a sample gas is introduced by solid-phase microextraction, it is possible to suppress a decrease in desorption efficiency when the sample is desorbed from the adsorption section.
[0050] (Item 2) In the gas chromatograph analysis system described in item 1, the gas chromatograph further includes a first heating device that heats the sample vaporization chamber. The control device drives the first heating device to desorb the sample gas adsorbed by the adsorption section.
[0051] According to the gas chromatographic analysis system described in paragraph 2, the sample can be desorbed by heating.
[0052] (Item 3) In the gas chromatograph analysis system described in Items 1 or 2, the gas chromatograph further includes a second heating device that heats the separation column. The control device drives the second heating device based on the elapse of a predetermined period of time after the end of the desorption period.
[0053] According to the gas chromatographic analysis system described in the third aspect, the supply pressure can be stabilized at the second pressure, and then the sample can be controlled to pass through the separation column CL1.
[0054] (Item 4) In the gas chromatographic analysis system according to any one of Items 1 to 3, the surface area of the adsorption phase of the adsorption section is 44.0 mm 2 That's all.
[0055] According to the gas chromatographic analysis system described in the fourth aspect, an adsorption section with a large surface area of the adsorption phase can be applied.
[0056] (Item 5) In the gas chromatographic analysis system according to any one of items 1 to 3, the amount of liquid phase in the adsorption section is 3.8 μL or more.
[0057] According to the gas chromatographic analysis system described in the fifth aspect, an adsorption section with a large liquid phase volume can be applied.
[0058] (Item 6) One embodiment of a gas chromatograph analyzer separates components in a sample gas introduced therein by solid-phase microextraction. The gas chromatograph analyzer includes a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted, a gas supply source that supplies a carrier gas to the sample vaporization chamber, an adjusting device that adjusts the amount of carrier gas supplied to the sample vaporization chamber by adjusting the supply pressure applied to the carrier gas, a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber, and a detection device that detects components in the sample gas that has passed through the separation column. The adjusting device applies a first supply pressure to the carrier gas during a desorption period in which the sample gas is desorbed from the adsorption unit, and applies a second supply pressure lower than the first pressure to the carrier gas after the desorption period ends.
[0059] According to the gas chromatograph analyzer described in paragraph 6, in a gas chromatograph analyzer into which a sample gas is introduced by solid-phase microextraction, it is possible to suppress a decrease in desorption efficiency when the sample is desorbed from the adsorption section.
[0060] (Item 7) A method for controlling a gas chromatograph analyzer according to one aspect is a method for separating components in a sample gas introduced by solid-phase microextraction. The gas chromatograph includes a sample vaporization chamber into which an adsorption unit that adsorbs the sample gas is inserted, a gas supply source that supplies a carrier gas to the sample vaporization chamber, a regulator that regulates the amount of carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas, a separation column into which sample gas desorbed from the adsorption unit is introduced from the sample vaporization chamber, and a detector that detects components in the sample gas that has passed through the separation column. The control method includes, as processing executed by a computer that controls the gas chromatograph, controlling the regulator so that the supply pressure is a first pressure during a desorption period in which the sample gas is desorbed from the adsorption unit, and controlling the regulator so that the supply pressure is a second pressure lower than the first pressure after the desorption period ends.
[0061] According to the control method for a gas chromatograph analyzer described in paragraph 7, in a gas chromatograph analyzer into which a sample gas is introduced by solid-phase microextraction, a decrease in desorption efficiency when a sample is desorbed from an adsorption section can be suppressed.
[0062] The embodiments disclosed herein should be considered to be illustrative in all respects and not restrictive. The scope of the present invention is defined by the claims, not by the description of the above embodiments, and is intended to include all modifications within the meaning and scope of the claims.
[0063] 100 control device, 110 processor, 120 storage device, 200, 200A gas chromatograph device, 210 adjustment device, 220 sample vaporization chamber, 221 septum, 230 detection device, 300 input device, 400 display device, 1000 gas chromatograph analysis system, B1 gas supply source, CL1 separation column, Ht1, Ht2 heater, Ov1 column oven, P1 control program, S sample, SP1 adsorption section, Tm1 to Tm3 timing.
Claims
1. A gas chromatographic analysis system for separating components in a sample gas introduced by solid-phase microextraction, comprising: a gas chromatograph device for separating components in the sample gas introduced by the solid-phase microextraction; and a control device for controlling the gas chromatograph device, wherein the gas chromatograph device includes: a sample vaporization chamber into which an adsorption section that adsorbs the sample gas is inserted; a gas supply source for supplying a carrier gas to the sample vaporization chamber; an adjustment device for adjusting the amount of the carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas; a separation column into which the sample gas desorbed from the adsorption section is introduced from the sample vaporization chamber; and a detection device for detecting components in the sample gas that has passed through the separation column, wherein the control device controls the adjustment device so that the supply pressure is a first pressure during a desorption period in which the sample gas is desorbed from the adsorption section, and controls the adjustment device so that the supply pressure is a second pressure lower than the first pressure after the desorption period ends.
2. The gas chromatograph analysis system of claim 1, wherein the gas chromatograph apparatus further comprises a first heating device for heating the sample vaporization chamber, and the control device drives the first heating device to desorb the sample gas adsorbed in the adsorption section.
3. A gas chromatograph analysis system as described in claim 1 or claim 2, wherein the gas chromatograph apparatus further comprises a second heating device for heating the separation column, and the control device drives the second heating device based on the passage of a predetermined period of time after the end of the desorption period.
4. The surface area of the adsorption phase of the adsorption section is 44.0 mm 2 The gas chromatographic analysis system according to claim 1 .
5. The gas chromatographic analysis system according to claim 1, wherein the liquid phase volume of the adsorption section is 3.8 μL or more.
6. A gas chromatograph apparatus for separating components in a sample gas introduced by solid-phase microextraction, comprising: a sample vaporization chamber into which an adsorption section that adsorbs the sample gas is inserted; a gas supply source that supplies a carrier gas to the sample vaporization chamber; an adjustment device that adjusts the amount of the carrier gas supplied to the sample vaporization chamber by a supply pressure applied to the carrier gas; a separation column into which the sample gas desorbed from the adsorption section is introduced from the sample vaporization chamber; and a detection device that detects components in the sample gas that has passed through the separation column, wherein the adjustment device applies a supply pressure of a first pressure to the carrier gas during a desorption period in which the sample gas is desorbed from the adsorption section, and applies a supply pressure of a second pressure lower than the first pressure to the carrier gas after the desorption period has ended.
7. A control method for a gas chromatograph apparatus which separates components in a sample gas introduced by solid-phase microextraction, the gas chromatograph apparatus comprising: a sample vaporization chamber into which an adsorption section which adsorbs the sample gas is inserted; a gas supply source which supplies a carrier gas to the sample vaporization chamber; an adjustment device which adjusts the amount of the carrier gas supplied to the sample vaporization chamber by a supply pressure given to the carrier gas; a separation column into which the sample gas desorbed from the adsorption section is introduced from the sample vaporization chamber; and a detection device which detects components in the sample gas which has passed through the separation column, the control method comprising, as processing executed by a computer which controls the gas chromatograph apparatus, a step of controlling the adjustment device so that the supply pressure is a first pressure during a desorption period in which the sample gas is desorbed from the adsorption section; and a step of controlling the adjustment device so that the supply pressure is a second pressure lower than the first pressure after the desorption period ends.
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