JP4760734B2 - Control device for analytical instruments - Google Patents

Description

  The present invention relates to a control device that controls the operation and operation of an analytical instrument such as a liquid chromatograph and a gas chromatograph. More specifically, the present invention relates to an automatic analytical instrument that performs sequential analysis while automatically exchanging and selecting a large number of samples. The present invention relates to a control device.

  For example, in a liquid chromatograph, a large number of sample containers containing liquid samples are set in advance in an autosampler rack, and an operator inputs and sets an analysis schedule table that defines the analysis order and analysis conditions of these samples. When the analysis start is instructed, the sample containers are sequentially selected according to the analysis schedule table, and the analysis is automatically executed under the designated analysis conditions (see, for example, Patent Document 1).

  In such liquid chromatographs and gas chromatographs, a separation unit that separates components using a column or the like and a detection unit that detects various separated components are often configured as separate units. A system is often constructed by combining a separation unit and a detection unit. For example, in the example shown in FIG. 6, a liquid chromatograph (LC) unit 30 and a mass spectrometer (MS) unit 31 are combined, and a sample separated by the LC unit 30 is introduced into the MS unit 31 for detection. The structure of a chromatograph mass spectrometer (LC / MS) is shown.

  In the LC / MS, when the LC unit 30 and the MS unit 31 are products of the same manufacturer, the synchronous operation of both the units 30 and 31 is often considered. It may be possible to operate the MS unit 31 according to the analysis schedule table set on the 30a. On the other hand, when the LC unit 30 and the MS unit 31 are from different manufacturers, the operations of the units 30 and 31 are independently controlled by the control devices 30a and 31a. Must be set separately for each of the control devices 30a and 31a.

  In this case, the number of repeated analyzes set in the analysis schedule of the LC unit 30 and the number of repeated analyzes set in the analysis schedule of the MS unit 31 need to match. There is a risk that the sample separated in 30 and sent to the MS unit 31 may not be detected by the MS unit 31 at all. For this reason, it is important for the user (especially the operator who is responsible for the analysis work) to know the number of repeated analyzes in one continuous analysis when performing the continuous analysis.

  When one row corresponds to one analysis in the analysis schedule table displayed on the display screen, it is easy to know the number of analyzes from the number of rows. However, if the specification of input / setting of the analysis schedule table is such that a plurality of analyzes can be set for one line, the operator cannot know the number of analyzes intuitively. Furthermore, when the analysis schedule table for a series of continuous analyzes is described separately in a plurality of analysis schedule tables (for example, an analysis schedule table for unknown samples and an analysis schedule table for standard samples), the operator performs analysis. It is almost impossible to know the number of times.

JP 2005-127814 A

  The present invention has been made in view of such a problem, and the object of the present invention is that the analysis procedure and the specification of the contents when executing a series of continuous analyzes are over a plurality of analysis schedule tables. Even if it is a case, it is providing the control apparatus of the analytical instrument which a user can confirm the total frequency | count of analysis in the continuous analysis easily.

In order to solve the above-mentioned problems, the present invention controls the operation of an analytical instrument that sequentially performs analysis by changing and selecting samples sequentially and setting analysis conditions according to an analysis schedule table set in advance. The analysis schedule table can set, as the analysis schedule table, identification information of one or more containers in which a sample is stored and the number of repeated analyzes per same container can be set in one line, and the first A continuous analysis is performed in accordance with the first and second analysis schedule tables so as to execute an analysis of all the rows set in another second analysis schedule table for each specified number of rows in the analysis schedule table. In a control device capable of
a) The number of analyzes for each row is obtained from the container identification information set in each row of the first analysis schedule table and the number of repeated analyzes, and the number of analyzes corresponding to all the rows in the first analysis schedule table is calculated. First computing means;
b) Obtain the number of analyzes for each row from the container identification information set in each row of the second analysis schedule table and the number of repeated analyzes, and calculate the number of analyzes corresponding to all the rows in the second analysis schedule table. A second computing means;
c) The number of insertions of the analysis set in the second analysis schedule table is obtained from the total number of rows in the first analysis schedule table and the specified number of rows for insertion, and the number of insertions and the first and second A third computing means for calculating the total number of continuous analyzes from the number of analyzes obtained by the computing means;
d) display means for displaying the total number of analyzes on a display screen;
It is characterized by having.

  As one aspect of the control device for an analytical instrument according to the present invention, the first analysis schedule table is for setting information related to the order and contents of the analysis for the sample that is the purpose of analysis, and the second analysis schedule table is It can be set as the structure for setting the information regarding the order and content of the analysis with respect to the standard sample whose component is known.

  In the analytical instrument control device according to the present invention, when the operator inputs and sets the first and second analysis schedule tables, respectively, and further specifies the number of inserted rows, the first and second calculation means Calculates the number of analyzes for each row based on the numerical value set for each row in each analysis schedule table, and further calculates the sum of the number of analyzes for each row to calculate the number of analyzes for all rows set in each analysis schedule table N1 and N2 are obtained respectively. The third computing means obtains the number of insertions during continuous analysis from the number of rows in the first analysis schedule table and the interval between the number of inserted rows, and multiplies the number of insertions by the number of analyzes N2 in the entire second analysis schedule table. The total number of analyzes is calculated by adding the number of analyzes N1 of the entire first analysis schedule table to this. The display means displays the total number of analyzes at a predetermined position or column on the screen.

  If the setting contents of the first and second analysis schedule tables and the insertion line number interval are changed by editing work or the like, the total number of analyzes may change. Therefore, when such information is changed, the calculation of the total number of analyzes by the first, second and third calculation means may be retried. As a result, the total number of analyzes that always reflects the latest analysis schedule table can be displayed.

  According to the control device for an analytical instrument according to the present invention, even if the operator cannot immediately grasp the total number of analyzes from the contents of the analysis schedule table displayed on the screen, the total number of analyzes is displayed as a numerical value. Therefore, for example, when it is necessary to match the total number of analyzes of this analytical instrument with other analytical instruments, data processing devices, etc., the coincidence / mismatch can be determined immediately. As a result, an operation error such as an input / setting error in the analysis schedule table can be easily found, and the execution of the analysis in an inappropriate state can be avoided.

  Hereinafter, a liquid chromatograph as an embodiment of an analytical instrument to which a control device according to the present invention is applied will be described with reference to the drawings.

  FIG. 1 is a block diagram of the main part of a liquid chromatograph according to this embodiment. The liquid chromatograph includes a mobile phase container 1, a liquid feed pump 2, an autosampler 3, a column 6 built in a column oven 5, a detector 7, and a system controller 8 and a system controller 8 that send control signals to these parts, respectively. A personal computer 9 is provided for managing analysis work and for analyzing and processing data obtained by the detector 7. An operation unit 10 such as a keyboard and a display 11 are connected to the personal computer 9.

  The analysis operation by the liquid chromatograph will be schematically explained. Under the system controller 8 that receives an instruction from the personal computer 9, the liquid feed pump 2 supplies the mobile phase sucked from the mobile phase container 1 at a substantially constant flow rate. Flow to column 6 via autosampler 3. The autosampler 3 has a rack 4 on which a number of sample containers are mounted. A predetermined container is selected under the control of the system controller 8 and a sample in the container is injected into the mobile phase at a predetermined timing. To do. This sample rides on the mobile phase and is introduced into the column 6. Since the time for each component in the sample to pass through the column 6 varies depending on the component, each component in the sample is temporally separated while passing through the column 6. The detector 7 sequentially detects the components separated and eluted by the column 6 in this way, and sends detection data to the personal computer 9 via the system controller 8. The personal computer 9 performs predetermined data processing on the received data to create a chromatogram, and further performs qualitative analysis and quantitative analysis based on the chromatogram data.

  Operation control and data processing of each part through the system controller 8 are achieved by executing a dedicated control / processing program installed in the personal computer 9. Creation and editing of an analysis schedule table, which will be described later, or calculation processing of the total number of analyzes is one of the functions realized by executing the control / processing program. Therefore, the control apparatus according to the present invention is an apparatus that is embodied by using a personal computer as a hardware resource and executing a specific program using the hardware resource.

Next, characteristic control operations in the liquid chromatograph of the present embodiment will be described with reference to FIGS.
In order to continuously analyze a large number of samples mounted on the rack 4, the operator needs to set an analysis schedule table by operating the operation unit 10 prior to analysis. In this apparatus, two analysis schedule tables are provided: a first analysis schedule table (sequence analysis table) mainly relating to analysis of unknown samples and a second analysis schedule table relating to analysis of standard samples. FIGS. 3 and 4 are examples of analysis schedule tables displayed on the screen of the display 11. The two analysis schedule tables include tabs 21 with text labels “Sequence analysis” and “Standard sample injection”, 23 can be switched. 3, when the “sequence analysis” tab 21 is clicked to display the first analysis schedule table 20, FIG. 4 is to click the “standard sample injection” tab 23 to display the second analysis schedule table 22. This is the case. As will be described later, FIG. 5 is also an example when the first analysis schedule table 20 is displayed.

  The input / selection items in each row in each analysis schedule table 20, 22 are a rack number, a sample number, the number of injections, an injection amount, and an analysis method. For the sample number, a start point and an end point are indicated. For example, as shown in the third row of the table 20 shown in FIG. 3, the start point is “6” and the end point is “10”. In some cases, 5 samples with sample numbers from “6” to “10”, ie, “6”, “7”, “8”, “9”, “10” are analyzed. Means to be targeted. The number of injections means the number of repeated injections (analysis) per sample, and the injection amount is the injection amount per injection. The analysis method is an analysis condition including, for example, a set temperature of the column oven 5, an analysis time per analysis, and the like. This is selected by designating a file name registered in advance as one file. It is like that.

  In general, in a liquid chromatograph, since a continuous analysis time is long, a calibration curve may change or the state of the apparatus may fluctuate during the analysis. Therefore, in order to re-create a calibration curve or re-calibrate the apparatus, the analysis of the standard sample can be appropriately inserted during the repeated analysis of the unknown sample. Here, a text box 24 is provided in the “standard sample injection” tab 23 to indicate the interval between the number of inserted lines. By inputting a numerical value in this text box 24, the second analysis schedule table 22 is displayed. It is possible to specify the number of rows in the first analysis schedule table 20 in which analysis of all set standard samples (in the example of FIG. 4, analysis of two rows of numbers “1” and “2”) is executed. I am doing so. In FIGS. 3 and 4, since the numerical value in the text box 24 is “0”, this means that the analysis of the standard sample is not inserted at all during the repeated analysis of the unknown sample. On the other hand, in FIG. 5, since the numerical value in the text box 24 is “3”, this means that the analysis of the standard sample is inserted every three rows of the first analysis schedule table 20.

  For example, when the operator inputs / sets the analysis schedule tables 20 and 22 shown in FIGS. 3 and 4 and inputs an appropriate numerical value other than “0” in the text box 24, FIG. 5 corresponds to the operation. As shown in FIG. 6, a white triangle arrow mark 25 indicating the timing of executing the standard sample analysis is displayed outside the leftmost frame of the first analysis schedule table 20. When the execution of the standard sample is instructed, first, the analysis of the standard sample is executed before the analysis of the unknown sample, so that the first sample is positioned above the number “1”. A white triangular arrow mark 25 is added, and a second white triangular arrow mark 25 is added every third line, that is, between the numbers “3” and “4”. If the operator changes the numerical value in the text box 24, the position of the white triangle arrow mark 25 is changed accordingly.

In the personal computer 9, when a numerical value is input to the text box 24 as described above, the process shown in FIG. 2 is performed in parallel with the process of displaying the white triangle arrow mark 25. Execute the process. That is, first, a calculation process of the total number of analyzes is executed (step S1). As a specific procedure, as shown in FIG. 2B, the number of analyzes N1 in the analysis sequence set in the first analysis schedule table 20 is calculated (step S10). Starting point m _i of the sample numbers in the i-th row in the first analysis schedule table _20, the end point n _i, when the number of injections and L _i, can be calculated N1 by the following equation (1).
N1 = Σ {(n _i −m _i +1) × L _i } (1)
Here, Σ is the sum from i = 1 to L (the total number of rows in the first analysis schedule table, “6” in the example of FIG. 3).

For example, in the second row (i = 2) of the first analysis schedule table 20, (n ₁ −m ₁ +1) × L ₁ = (5-2 + 1) × 2 = 8, and eight analyzes are performed in this one row. Number of times. Then, N1 is calculated to be “28”. When the numerical value in the text box 24 is 0, this N1 is displayed as it is in the analysis number display column 26 at the bottom of the analysis schedule table 20.

  Next, the number of analyzes N2 in the standard sample injection sequence set in the second analysis schedule table 22 is calculated (step S11). The calculation method is the same as that in step S10, and N2 may be obtained by calculating the right side of equation (1) with the second analysis schedule table 22 as a target. In the example of FIG. 4, N2 is calculated to be “5”.

Then, the total number of analyzes T is calculated by the following equation (2) (step S12).
T = N1 + Integer {(L−1) / N) +1} × N2 (2)
Here, N is the insertion line interval for executing the standard sample analysis, that is, a numerical value in the text box 24, and Integer {(L-1) / N) +1} is the second analysis schedule table in this series of continuous analysis. 22 is the number of times of analysis insertion. In the example of FIG. 5, Integer {(L-1) / N) +1} = (6-1) / 3) + 1 = 2, and the total number of analyzes T = 28 + 2 × 5 = 38. The total number of analyzes T thus obtained is displayed in the number-of-analysis display column 26 at the bottom of the analysis schedule table 20 as shown in FIG. 5 (step S2).

  For example, when the start point, the end point, and the number of injections of the sample number in the first analysis schedule table 20 are changed, or when a new line is added or deleted, the first analysis schedule table 20 Since the value of the number of analyzes N1 corresponding to is likely to change, the calculation / display processing of the total number of analyzes as described above is executed, and the numerical value in the analysis number display column 26 is updated. The same applies when the start point, end point, and number of injections of the sample number in the second analysis schedule table 22 are changed, or when a new line is added or deleted. The same applies when the numerical value in the text box 24 is changed. In this way, the total number of analyzes reflecting the settings of the analysis schedule tables 20 and 22 can always be displayed.

  It should be noted that the above-described embodiment is merely an embodiment of the present invention, and it is obvious that modifications, additions, and additions within the scope of the present invention are included in the scope of the claims of the present application. For example, the above embodiment is an example in which the present invention is applied to a liquid chromatograph, but it can also be applied to a control device of another analytical instrument such as a gas chromatograph.

The block block diagram of the liquid chromatograph which is one Example of this invention. The flowchart which shows the characteristic process in the liquid chromatograph of a present Example. The figure which shows an example of the analysis schedule table displayed on the screen of a display in the liquid chromatograph of a present Example. The figure which shows an example of the analysis schedule table displayed on the screen of a display in the liquid chromatograph of a present Example. The figure which shows an example of the analysis schedule table displayed on the screen of a display in the liquid chromatograph of a present Example. The figure which shows the structural example of a liquid chromatograph mass spectrometer.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Mobile phase container 2 ... Liquid feed pump 3 ... Autosampler 4 ... Rack 5 ... Column oven 6 ... Column 7 ... Detector 8 ... System controller 9 ... Personal computer 10 ... Operation part 11 ... Display 20 ... 1st analysis schedule Table 21 ... "Sequence analysis" tab 22 ... Second analysis schedule table 23 ... "Standard sample injection" tab 24 ... Text box 25 ... White triangle arrow mark 26 ... Analysis frequency display field

Claims (3)

A control device that controls the operation of an analytical instrument that sequentially performs analysis by sequentially changing and selecting samples according to an analysis schedule table that is set in advance and setting analysis conditions. The identification information of one or a plurality of containers in which the container is stored and the number of repeated analyzes per container can be set in one line, and a different number is specified for each number of lines specified in the first analysis schedule table. In a control device capable of executing continuous analysis in accordance with the first and second analysis schedule tables so as to execute analysis of all rows set in the second analysis schedule table,
a) The number of analyzes for each row is obtained from the container identification information set in each row of the first analysis schedule table and the number of repeated analyzes, and the number of analyzes corresponding to all the rows in the first analysis schedule table is calculated. First computing means;
b) Obtain the number of analyzes for each row from the container identification information set in each row of the second analysis schedule table and the number of repeated analyzes, and calculate the number of analyzes corresponding to all the rows in the second analysis schedule table. A second computing means;
c) The number of insertions of the analysis set in the second analysis schedule table is obtained from the total number of rows in the first analysis schedule table and the specified number of rows for insertion, and the number of insertions and the first and second A third computing means for calculating the total number of continuous analyzes from the number of analyzes obtained by the computing means;
d) display means for displaying the total number of analyzes on a display screen;
An analytical instrument control device comprising:   The first analysis schedule table is for setting information related to the analysis order and contents of the sample that is the object of analysis, and the second analysis schedule table is information related to the analysis order and contents for the standard sample whose components are known. 2. The control device for an analytical instrument according to claim 1, wherein   When any one of the setting contents of the first analysis schedule table, the setting contents of the second analysis schedule table, or the specified number of rows to be inserted is changed, the first, second and third calculation means 2. The analytical instrument control device according to claim 1, wherein the calculation of the total number of analyzes is retried.

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