JP5772183B2 - Control apparatus for gas chromatograph apparatus and control program used for the control apparatus - Google Patents

Description

  The present invention relates to a control device for a gas chromatograph (GC) analyzer and a control program used therefor. In addition, GC said here also includes the gas chromatograph mass spectrometry which uses a mass spectrometer as a detector.

  The GC device separates sample components temporally by flowing the sample gas vaporized in the sample vaporization chamber to the column, and sequentially detects the sample components separated by a detector provided downstream of the column. is there.

  Such a GC apparatus is generally provided with an apparatus for controlling the analysis and processing data obtained by the analysis. Such control / data processing is executed by a program built in the apparatus, but by executing a similar control / data processing program on a personal computer (PC) connected to the GC apparatus, control of the apparatus and data processing are performed. Is also performed.

  For example, in the control / data processing program of Non-Patent Document 1, the length / inner diameter, film thickness, pressure of each part of the device, carrier gas type, split ratio, etc. are used as parameters in the control / data processing program. Is input to a personal computer (PC) in which is installed, a function of calculating in advance the flow rate and average linear velocity of the sample gas flowing through the column is provided. The user (analyzer) can start the actual analysis after judging whether the calculated flow rate and average linear velocity are suitable for the analysis of the sample to be measured.

“GCsolution”, [online] Shimadzu Corporation, [Search April 22, 2011], Internet <URL: http://www.an.shimadzu.co.jp/data-net/gcsolv2.htm>

  Conventionally, in order to efficiently analyze a plurality of components, a plurality of flow paths are provided in parallel, and a column is provided in each flow path. In this case, the flow rate and the average linear velocity are calculated for each flow path, and the flow rate control is performed.

On the other hand, in order to perform detailed analysis of sample components, a plurality of columns are connected in series to one flow path, and each column is controlled (this is called multi-dimensional GC = MD GC ). ). In MDGC, as shown in FIG. 6, a branch part is provided between the columns, and control is individually performed for each column between the flow path inlet and the branch part, between the branch parts, and between the branch part and the flow path outlet. By doing so, each flow rate was controlled. However, in such MDGC, the apparatus becomes complicated, and in order to make the target analysis the optimum condition, the parameters for each column are changed little by little, and the effect of the change on other columns is confirmed. However, trial and error of changing parameters further had to be repeated.

  The problem to be solved by the present invention is to provide a control device that can reduce labor and time required for trial and error until the GC device obtains an optimal analysis condition, and a control program used for the control device. .

The control device for a gas chromatograph apparatus according to the present invention, which has been made to solve the above problems,
In one channel, a plurality of columns are connected in series without a branching section ,
A control device for a gas chromatograph apparatus in which the plurality of columns are controlled by a single control system ,
A plurality of column selecting means for allowing the user to select the plurality of columns;
Parameter input means for allowing a user to input parameters necessary for calculating a flow rate and an average linear velocity in each of the plurality of columns;
A calculation means for calculating a flow rate and / or an average linear velocity in each of the plurality of columns based on a parameter input by a user;
It is characterized by having.

  In the control apparatus for a GC apparatus according to the present invention, a plurality of columns connected to one flow path are controlled by a single control system rather than being controlled for each column as in the conventional MDGC. . Therefore, the control system of the GC apparatus can be prevented from becoming complicated, and the number of parameters required for the control can be reduced. Therefore, labor and time required for trial and error until obtaining the optimum analysis conditions can be reduced. be able to.

Further, a gas chromatograph control program according to the present invention, which has been made to solve the above problems,
In one channel, a plurality of columns are connected in series without a branching section ,
A control program used in a control device for a gas chromatograph apparatus in which the plurality of columns are controlled by a single control system , the computer comprising:
A plurality of column selecting means for allowing the user to select the plurality of columns;
Parameter input means for allowing a user to input parameters necessary for calculation of flow rate and average linear velocity in each of the plurality of columns,
A calculation means for calculating a flow rate and / or an average linear velocity in each of the plurality of columns based on a parameter input by a user;
It is made to function as.

The present invention can calculate the flow rate and / or the average linear velocity for each of a plurality of columns connected in series in a single flow path controlled by a single control system. Conventionally, flow control of a plurality of serial columns has been performed in an apparatus having a plurality of control systems in the middle of a flow path such as MDGC. However, in the present invention, the number of control systems can be reduced as compared with that. Since the number of parameters to be set is also reduced, it is possible to reduce the labor and time required for trial and error until obtaining the optimal analysis conditions.

The schematic block diagram of the control apparatus to which one Example of the control program for GC analysis which concerns on this invention is applied. The figure which shows the environment setting screen of the control program for GC analysis of a present Example. The figure which shows the parameter input screen of the control program for GC analysis of a present Example. The figure which shows an example of a structure of GC apparatus used with the control apparatus for GC analysis of a present Example. The table | surface which shows the analysis conditions in the GC apparatus of FIG. 4, and its result. The schematic block diagram of a MDGC apparatus.

  A schematic configuration of a control apparatus 10 to which an embodiment of a control program for GC analysis according to the present invention is applied will be described with reference to FIG. The actual state of the control device 10 of the present embodiment is a computer, a central processing unit (CPU) 11 that is a central processing unit, a memory 12, a monitor (display unit) 13 including an LCD (Liquid Crystal Display), a keyboard and a mouse. Are connected to each other, and a storage unit 15 including a large-capacity storage device such as a hard disk. The storage unit 15 is provided with a GC analysis control program 16 (hereinafter abbreviated as “program 16”). The storage unit 15 also stores an OS (Operating System) 17.

  The control device 10 includes an interface (I / F) 18 for direct connection with the GC device 20 and connection via a network such as a LAN (Local Area Network), and the communication line 19 is connected to the I / F 18. It is connected to the GC device 20 via The control device 10 is not necessarily limited to the form connected to the GC device 20 via the I / F 18, and may be integrated with the GC device 20.

  Further, in the control device 10 of the present embodiment, the program 16 and the OS 17 are separated from each other, but it is needless to say that the program 16 may be incorporated in a part of the OS 17.

  Next, operation | movement of the control apparatus 10 of a present Example is demonstrated. The operation described below is realized by software by the CPU 11 executing the program 16.

  When the user starts the program 16 and performs a predetermined operation, the program 16 displays a setting screen 30 for setting the device environment of the GC device 20 on the monitor 13. On the setting screen 30, the user selects an analysis unit such as an autosampler, a sample vaporizing chamber, a column, or a detector used for the GC device 20.

A selection operation on the setting screen 30 will be described. The user selects an analysis unit to be used for the GC apparatus 20 by clicking or the like in the “effective unit” column on the left column of the screen. In FIG. 2A, “column” is selected. Next, click the right arrow at the center of the screen to add the selected analysis unit to the analysis line ("Analysis line 1" in the figure) that is being expanded in the "Unit to be used for analysis" column on the right side of the screen. Is done. The “analysis line” refers to a single flow path whose internal flow rate is controlled by a single control system. A plurality of analysis lines can be provided in parallel.
In FIG. 2B, “column 2” is newly added to “analysis line 1” by the above operation. If the same operation is repeated, numbers are added in order such as “Column 3, Column 4,...” And “Column” is added to “Analysis Line 1” of “Unit Used for Analysis”. Go.

  In the conventional GC analysis control program, only one column can be selected for one analysis line (only one column can be controlled). As described above, two or more columns can be selected on the setting screen 30 for one analysis line.

Next, the user performs a predetermined operation on the program 16 to display the parameter input screen 31 shown in FIG. 3 on the monitor 13. In the parameter input screen 31, parameters necessary for GC analysis can be input for each analysis unit selected for “analysis line 1” on the setting screen 30 in FIG.

When the “Column 1” tab is selected from the tabs arranged in the upper part of the parameter input screen 31, an input screen for “Column 1” selected on the setting screen 30 is displayed. Here, input column information in the registered column field or select a pre-registered column, etc., and click the select button on it, then the parameters of the registered column selected in the selected column field Is displayed. The parameter displayed in the selected column column is column information for “column 1”.

ここで、r₁, r₂はそれぞれ「カラム１」と「カラム２」の半径（内径）、L₁, L₂はそれぞれ「カラム１」と「カラム２」の長さ、T₁, T₂はそれぞれ「カラム１」と「カラム２」のカラムオーブン温度、η₁, η₂はそれぞれ温度T₁, T₂におけるキャリアガスの粘性係数、P_iは「分析ライン１」の入口圧、P_zは「カラム１」と「カラム２」の接続部分の圧力、P_oは「分析ライン１」の出口圧、P_refは標準圧力（大気圧）、T_refは標準温度（25℃=298K）である。なお、「分析ライン１」の出口に設けられた質量分析計では真空雰囲気に保たれているため、P_o=0である。また、図４の構成において「分析ライン１」の流路内のガス流量の制御（具体的には入口圧P_iの設定）は、試料気化室４１に送給するキャリアガスの流量を調整するマスフローコントローラ４２と、試料気化室４１からキャリアガスの一部を排出するスプリット流路に設けられたスプリット弁４３と、を有する単一の流量制御系４０によって行われる。 Similarly, parameters are input on the parameter input screen 31 for “column 2” and other analysis units. When the input of the parameters is completed and the user instructs the control program 10 to start computation by a predetermined operation, the program 16 calculates the flow rate and average linear velocity in each column. For example, as shown in FIG. 4, “column 1” and “column 2” placed in different “column ovens” in a single flow path of “analysis line 1” are connected in series, and “analysis line 1” In the case of an apparatus configuration in which a “mass spectrometer” is arranged as a detector at the outlet, the flow rates F ₁ and F ₂ and average linear velocities u ₁ and u ₂ of “column 1” and “column 2” are respectively Hagen. -Based on Poiseuille's law, it can be calculated by the following formula.

Here, r ₁ and r ₂ are the radii (inner diameters) of “column 1” and “column 2”, respectively, L ₁ and L ₂ are the lengths of “column 1” and “column 2”, respectively, T ₁ and T ₂ column oven temperature "column 2" and each "column 1", eta _1, coefficient of viscosity of the carrier gas in each eta ₂ temperature T _1, T _2, P _i is the inlet pressure of the "analysis line 1", P _z Is the pressure at the connection between “Column 1” and “Column 2”, P _o is the outlet pressure of “Analysis Line 1”, P _ref is the standard pressure (atmospheric pressure), and T _ref is the standard temperature (25 ° C. = 298 K) is there. Incidentally, a mass spectrometer which is provided at the outlet of the "Analysis Line 1" because it is kept in a vacuum atmosphere, a P _o = 0. Further, (set of inlet pressure P _i in particular) controlling the gas flow rate in the flow path of the "Analysis Line 1" in the configuration of Figure 4, to adjust the flow rate of feed Kyusuru carrier gas into the sample vaporizing chamber 41 This is performed by a single flow rate control system 40 having a mass flow controller 42 and a split valve 43 provided in a split flow path for discharging a part of the carrier gas from the sample vaporizing chamber 41.

The table of FIG. 5 shows the results of actually calculating the flow rate and the average linear velocity by the above formula. In this table, the thick frame column is a parameter input by the user. The inlet pressure is input as a gauge pressure. Other pressure values are absolute pressures. In addition, the outlet pressure of “column 1” and the inlet pressure of “column 2” correspond to _Pz in the above equation, and therefore have the same value.

  When the user determines that the flow rate and average linear velocity calculated by the program 16 are appropriate, the user performs a predetermined operation on the program 16 and reflects the input parameters on the GC device 20 before actually Perform an analysis.

  Although one embodiment of the GC analysis control device according to the present invention has been described above, it is obvious that the above is only an example, and changes, modifications, or additions are made as appropriate within the scope of the present invention. It doesn't matter.

  For example, in the above embodiment, an example in which the flow rate and the average linear velocity are calculated for two columns is shown, but even when there are three or more columns, the number of simultaneous equations is increased and the same. It will be apparent to those skilled in the art that the flow rate and average linear velocity of each column can be calculated by the equation. Moreover, it does not matter whether one column oven is provided for each column as in the above embodiment or one column oven is provided so as to contain a plurality of columns.

10 ... Control device 11 ... CPU
12 ... Memory 13 ... Monitor 14 ... Input unit 15 ... Storage unit 16 ... GC analysis control program 17 ... OS
18 ... I / F
DESCRIPTION OF SYMBOLS 19 ... Communication line 20 ... GC apparatus 30 ... Setting screen 31 ... Parameter input screen 40 ... Flow rate control system 41 ... Sample vaporization chamber 42 ... Mass flow controller 43 ... Split valve

Claims (2)

In one channel, a plurality of columns are connected in series without a branching section ,
A control device for a gas chromatograph apparatus in which the plurality of columns are controlled by a single control system ,
A plurality of column selecting means for allowing the user to select the plurality of columns;
Parameter input means for allowing a user to input parameters necessary for calculating a flow rate and an average linear velocity in each of the plurality of columns;
A calculation means for calculating a flow rate and / or an average linear velocity in each of the plurality of columns based on a parameter input by a user;
A control device for a gas chromatograph apparatus, comprising: In one channel, a plurality of columns are connected in series without a branching section ,
A control program used in a control device for a gas chromatograph apparatus in which the plurality of columns are controlled by a single control system , the computer comprising:
A plurality of column selecting means for allowing the user to select the plurality of columns;
Parameter input means for allowing a user to input parameters necessary for calculation of flow rate and average linear velocity in each of the plurality of columns,
A calculation means for calculating a flow rate and / or an average linear velocity in each of the plurality of columns based on a parameter input by a user;
A control program characterized by functioning as

Images