JP5168248B2 - Control system for multi-dimensional gas chromatograph apparatus and multi-dimensional gas chromatograph apparatus using the system - Google Patents

Description

  The present invention relates to a control system for safely using a multi-dimensional gas chromatograph apparatus using a plurality of columns having different separation characteristics, and a multi-dimensional gas chromatograph apparatus using the control system.

  In fields such as environmental analysis, petrochemical analysis, fragrance analysis, and food analysis, it is necessary to separate each component in a sample with a complex composition containing many kinds of trace components and perform quantitative analysis with high sensitivity. In a typical gas chromatograph (GC) apparatus, peaks of a plurality of components cannot be completely separated, and in many cases, sufficient analysis cannot be performed. In such a case, a multi-dimensional gas chromatograph apparatus (hereinafter referred to as MDGC) in which a plurality of columns having different separation characteristics are combined is very useful.

  In MDGC, roughly divided, two system configurations can be considered. One of them is the first column, the first detector for detecting each component in the sample gas separated by the first column, the second column and the second column having different separation characteristics from the first column. A second detector for detecting each component in the separated sample gas, and a flow path for selectively sending the sample gas that has passed through the first column to either the second column or the first detector. This is a system configuration in which the switching channel switching unit is accommodated in one column oven (see, for example, Patent Document 1). The other is a system in which the first column, the first detector, and the flow path switching unit are accommodated in one column oven, and the second column and the second detector are accommodated in another column oven. It is a configuration. In the latter case, it is common to construct a system by combining two independent GCs (see Non-Patent Document 1, for example).

JP 2009-103666 A

“High-resolution multi-dimensional GC / GCMS system for separating target components from complex matrices” [online], Shimadzu Corporation, [Search July 21, 2009], Internet <URL: http: // www. an.shimadzu.co.jp/gc/mdgc/mdgc.htm>

  In the MDGC configured as described in Patent Document 1, a plurality of columns are heated at the same temperature. However, the columns used in MDGC have different separation characteristics, and their heat resistant temperatures are also different. Therefore, even if the temperature in the column oven (column oven temperature) is a temperature that can withstand a certain column, it may exceed the heat resistance temperature of other columns.

  If the column oven temperature exceeds the heat resistant temperature of the column, the column may be deformed or damaged, which may adversely affect the analysis. However, in the conventional MDGC, there is no system and apparatus that considers the heat-resistant temperature of each column.

  The problem to be solved by the present invention is to provide an MDGC control system for preventing the column from being deformed or broken, and an MDGC using the control system.

A control system for a multidimensional gas chromatograph apparatus according to the present invention, which has been made to solve the above problems,
In a control system for a multidimensional gas chromatograph apparatus comprising a plurality of columns and a common temperature control means for heating the plurality of columns to the same column temperature,
A heat-resistant temperature input section for the user to enter the heat-resistant temperature of each column;
An upper limit setting unit for setting the lowest temperature among the input heat-resistant temperatures as an upper limit value of the column temperature;
An upper limit control unit for controlling the temperature control means so that the column temperature does not exceed the upper limit;
It is characterized by having.

Furthermore, the control system for the multidimensional gas chromatograph apparatus according to the present invention is:
An analysis parameter input unit for a user to input parameters used for component analysis, including the column temperature;
A warning unit that issues a warning when the input column temperature exceeds the upper limit;
It is characterized by having.

  Note that the heat-resistant temperature may be automatically input to the heat-resistant temperature input unit by the user inputting the column type, name, or the like instead of them. Thus, even if the user does not know the heat resistant temperature of the column, the information can be easily given to the system. Here, the column name refers to information for specifying each column, and indicates an ID number or a management number given in advance.

  According to the MDGC control system of the present invention, the user inputs the heat-resistant temperature of each column before performing analysis, so that the upper limit value of the column temperature is set, for example, in the MDGC control unit comprising a computer, Based on this upper limit value, temperature control means such as a column oven is controlled. Thereby, deformation and breakage of the column due to excessive heating can be prevented, and precise component analysis becomes possible.

  The column temperature may be maintained at a constant temperature, or may be controlled so as to change with time. Even when the column temperature is changed in this way, the control system of the present invention controls the temperature adjusting means so that the column temperature does not exceed the set upper limit temperature, and therefore MDGC can be used safely and suitably.

The apparatus block diagram which shows one Example of MDGC which concerns on a present Example. The flowchart which shows the procedure of the control program of MDGC which concerns on a present Example. The figure which shows an example of the input screen of heat-resistant temperature in MDGC of a present Example. The figure which shows an example of the input screen of an analysis parameter in MDGC of a present Example. The figure which shows the structure for performing the automatic input of heat-resistant temperature in MDGC of a present Example.

  An embodiment of the MDGC according to the present invention will be described with reference to FIG. FIG. 1 is an MDGC device configuration diagram according to the present embodiment.

  The MDGC of this embodiment includes a sample vaporizing chamber 1 to which a carrier gas (for example, helium He) is supplied from a carrier gas flow path 2, an injector 3 for injecting a liquid sample into the sample vaporizing chamber 1, and an inlet to the sample vaporizing chamber 1. A first column 5 having an end connected thereto, a flow path switching unit 6 connected to an outlet end of the first column 5, and a first detection connected to one of two outlet ends of the flow path switching unit 6 , A second column 8 having an inlet end connected to the other outlet end of the flow path switching unit 6, a second detector 9 connected to the outlet end of the second column 8, a first column 5, And a column oven 4 having a heater (not shown) that accommodates the second column 8 and the flow path switching unit 6 therein. The first column 5 and the second column 8 are heated to a constant or time-varying column temperature set by the user by a column oven 4 commonly used for these.

  The channel switching unit 6 is, for example, a Deans-type channel switching device, and switches the flow of the switching gas having the same component as the carrier gas supplied from the switching gas supply unit 10 according to the command of the analysis control unit 27, thereby The gas that has passed through the first column 5 is made to flow alternatively to one of the first detector 7 side and the second column 8 side. At this time, the switching gas is supplied to the other of the first detector 7 side and the second column 8 side.

  Both detection signals from the first detector 7 and the second detector 9 are sent to the data processing unit 26. The data processing unit 26 creates a chromatogram based on the obtained detection signal and performs quantitative analysis and qualitative analysis of various components by performing waveform analysis of the chromatogram. The operations of the injector 3, the flow path switching unit 6, the heater (not shown) attached to the column oven 4, the switching gas supply unit 10, and the like are controlled by the analysis control unit 27 under the general instruction of the central control unit 20. . The upper limit temperature of the column oven 4 is also controlled by the upper limit control unit 22 incorporated in the central control unit 20. Further, the central control unit 20 controls the analysis control unit 27 and the data processing unit 26, and receives processing results such as chromatograms from the data processing unit 26 and displays them on the display unit 25. The central control unit 20 is connected to an input unit 24 including a heat-resistant temperature input unit 241 that inputs heat-resistant temperatures of the columns 5 and 8 and an analysis parameter input unit 242 that inputs various parameters used for analysis. The entities of the central control unit 20 and the data processing unit 26 are general-purpose personal computers, and control and processing of each part of the MDGC are achieved by operating predetermined control / processing programs installed in the personal computer. The The input unit 24 can be configured with a normal keyboard, touch panel, or the like, and similarly operates as the heat resistant temperature input unit 241 and the analysis parameter input unit 242 by a predetermined program installed in the personal computer.

  As a characteristic configuration of the MDGC of the present embodiment, the central control unit 20 includes an upper limit setting unit 21, an upper limit control unit 22, and a warning unit 23 as functional blocks. These are also processing functions realized by operating the control / processing program on the CPU of the personal computer.

An example of a typical analysis operation in the MDGC of the present embodiment will be schematically described with reference to FIGS. 2 is a flowchart showing a processing procedure of a program for executing the control system of the present invention, FIGS. 3 and 4 are diagrams showing an example of an input screen for heat-resistant temperature and analysis parameters,
FIG. 5 is a schematic diagram showing a configuration for automatically inputting the heat-resistant temperature.
Prior to the analysis, the user sets the heat-resistant temperatures for the first column 5 and the second column 8. First, by performing a predetermined operation with the input unit 24, a setting screen as shown in FIG. 3 is displayed on the screen of the display unit 25. The setting screen of FIG. 3 is provided with a heat-resistant temperature input unit 241 for inputting the heat-resistant temperatures of the first column 5 and the second column 8, and the heat-resistant temperature of each column is input to the heat-resistant temperature input unit 241. (Step S1), the upper limit value of the heating temperature (column temperature) of the column oven 4 is set in the upper limit setting unit 21 of the central control unit 20 (Step S2).

Next, the user sets various conditions for executing the analysis in the analysis parameter input unit 242 of the setting screen as shown in FIG. 4 (step S3). Here, the analysis parameters are the sizes of the first and second columns such as the inner diameter and length, the column temperature, the supply pressure of the carrier gas, the supply pressure of the switching gas (or the linear velocity of the gas), and the carrier gas (switching gas). The kind of. These analysis parameters may be input individually or by inputting a value (method name or the like) that specifies a group value that is predetermined and held (stored) in a lump. You may make it input a parameter collectively.
Here, if the input column temperature exceeds the upper limit value determined by the upper limit setting unit 21, the warning unit 23 displays a warning message on the screen of the display unit 25 or makes a sound warning. To do. In the case of analysis in which the column temperature changes with time, a warning is issued when the maximum value exceeds the upper limit value. If there is no problem with the input parameters, the analysis is started according to these parameters (step S5). As a result, it is possible to prevent the column from being deformed or damaged due to the user making a mistake in inputting the column temperature.

  In the MDGC control system according to the present invention, the analysis can be performed in accordance with the operation of a predetermined program installed in the personal computer in advance without inputting the above analysis parameters. In this case, the functions of the analysis parameter input unit 242 and the warning unit 23 may be omitted from the above configuration. Similarly, program steps corresponding to these functions can also be omitted from the flowchart of FIG.

  Further, what is input to the heat resistant temperature input unit 241 in FIG. 3 is the value of the heat resistant temperature of each column, but a general user may not know the heat resistant temperature of the column. In this case, the heat-resistant temperature can be automatically input by inputting the column type and name to the name input unit 241A provided in the heat-resistant temperature input unit 241. This configuration will be described with reference to FIG. As shown in FIG. 5, the central control unit 20 further includes a storage unit 241 </ b> B, and stores heat-resistant temperature data associated with column types and names. When the user inputs the column type or name to the name input unit 241A provided in the heat-resistant temperature input unit 241 in FIG. 3, the corresponding heat-resistant temperature data is read from the storage unit 241B, and the heat-resistant temperature output is performed. The heat-resistant temperature data is output to the part 241C (heat-resistant temperature input field in FIG. 3). By providing the heat resistant temperature input unit 241 with such a function, it is possible for a general user to use the MDGC more easily.

  In addition, the function to control the column oven by inputting information on the heat-resistant temperature of each column and setting the upper limit value of the column temperature as described above is a state in which control / processing software is already installed in the central control unit. And can be added by newly installing an update program.

  Furthermore, in the present embodiment, an example is shown in which the branching unit branches to two detectors, but the number of detectors can be further increased by applying the same idea.

DESCRIPTION OF SYMBOLS 1 ... Sample vaporization chamber 2 ... Carrier gas flow path 3 ... Injector 4 ... Column oven 5 ... 1st column 6 ... Flow path switching part 7 ... 1st detector 8 ... 2nd column 9 ... 2nd detector 10 ... Switching gas Supply unit 20 ... central control unit 21 ... upper limit setting unit 22 ... upper limit control unit 23 ... warning unit 24 ... input unit 241 ... heat resistant temperature input unit 241A ... name input unit 241B ... storage unit 241C ... heat resistant temperature output unit 242 ... analysis parameter Input unit 25 ... display unit 26 ... data processing unit 27 ... analysis control unit

Claims (5)

In a control system for a multidimensional gas chromatograph apparatus comprising a plurality of columns and a common temperature control means for heating the plurality of columns to the same column temperature,
A heat-resistant temperature input section for the user to enter the heat-resistant temperature of each column;
An upper limit setting unit for setting the lowest temperature among the input heat-resistant temperatures as an upper limit value of the column temperature;
An upper limit control unit for controlling the temperature control means so that the column temperature does not exceed the upper limit;
A control system for a multi-dimensional gas chromatograph apparatus, comprising: Furthermore, an analysis parameter input unit for a user to input parameters used for component analysis, including the column temperature,
A warning unit that issues a warning when the input column temperature exceeds the upper limit;
The control system for a multidimensional gas chromatograph apparatus according to claim 1, comprising: The heat-resistant temperature input unit is a name input unit for inputting the type or name of the column,
A storage unit that stores heat-resistant temperature data associated with the type or name of the column;
The multi-dimensional gauge according to claim 1, wherein a heat-resistant temperature of each column is read from the storage unit based on a type or name of the column input to the name input unit. Control system for a chromatographic device.   In the multidimensional gas chromatograph apparatus provided with a plurality of columns and a common temperature control means for heating the plurality of columns to the same column temperature, the control system according to any one of claims 1 to 3. A multi-dimensional gas chromatograph that is installed. A control program for a multi-dimensional gas chromatograph apparatus comprising a plurality of columns and a common temperature control means for heating the plurality of columns to the same column temperature, the computer comprising:
Heat resistant temperature input section that allows the user to input the heat resistant temperature of each column,
An upper limit setting unit for setting the lowest temperature among the input heat-resistant temperatures as an upper limit value of the column temperature;
An upper limit control unit for controlling the temperature adjusting means so that the column temperature does not exceed the upper limit;
A control program for a multi-dimensional gas chromatograph apparatus, characterized in that

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