JPH11218530A - Data processor for chromatograph - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a data processor for chromatograph, by which a peak parameter and an identification table can be generated automatically without the intervention of a user. SOLUTION: A standard sample which contains a known component only in a known amount is analyzed chromatographically, and a signal from a detector is converted sequentially into digital data so as to be stored in a memory in a time-series manner (S1). The data, which are stored in the memory are read out, a chromatogram is constituted, and a waveform processing parameter such as a slope value, a minimum peak area (or a height) or the like is decided on the basis of its baseline part (S2). Then, the peak of the chromatogram is detected by using the parameter (S3), and the identification table of the known component is created (S4). It is stored in the memory. An unknown sample is analyzed, its chromatogram is analyzed on the basis of the date, and its component is quantitatively determined.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a data processing device for a chromatograph such as a gas chromatograph and a liquid chromatograph.

[0002]

2. Description of the Related Art Computers such as personal computers and workstations can be connected to chromatographs that are commercially available in recent years, and control of chromatographs and processing of data collected by detectors are performed by these computers and the like. It can be done with. Conventionally, regarding the processing of collected data, signals conventionally transmitted from the detector every moment are converted into digital data, chromatograms are created, peaks are detected from the created chromatograms, and their positions are detected. Data processing of calculating (holding time) and height or area (strength) has been automatically performed.

[0003]

For example, when a peak is detected from a chromatogram, a value of a rising / falling slope (slope value) for defining a starting point and an ending point of the peak or a peak is considered. The minimum size (minimum peak height or area) must be determined in advance. In a conventional chromatographic data processing device, these parameters have to be manually determined in advance by a user and given to the device (specifically, a computer operated by a data analysis program).

In order to determine what component the peak is, the retention time of the known component and the relative height or area of the peak must be stored in advance in the form of a reference table. In the past, such a table (identification table) had to be created in advance by the user.

The present invention has been made to solve such a problem, and an object of the present invention is to provide a chromatographic data processing apparatus capable of automatically generating a peak parameter and an identification table. To provide.

[0006]

The chromatographic data processing apparatus according to the present invention, which has been made to solve the above-mentioned problems, comprises: a) sequentially converting signals from a chromatographic detector into digital data; Analysis data storage means for sequentially storing; b) reference data creation means for creating a waveform processing parameter and an identification table based on data stored in the analysis data storage means for the standard sample. .

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS Before analyzing an unknown sample, a standard sample containing a known amount of a component to be analyzed is prepared and analyzed by chromatography. The signal output from the detector of the chromatograph is sent to analysis data storage means, where it is sequentially converted into digital data and stored in a time series. The reference data creation unit creates a waveform processing parameter and an identification table based on the data of the standard sample stored in the analysis data storage unit. Normally, a chromatogram is created from data stored in chronological order in the analysis data storage means, and a waveform processing parameter and an identification table are created based on the chromatogram. For example, the slope value, minimum peak height / area, and the like are determined from the baseline portion of the chromatogram of the standard sample. Also, using the waveform processing parameters determined in this way, peak detection is performed in the sample elution portion, based on the detected peak,
Create an identification table for the components contained in the standard sample. Further, a calibration curve is created based on the height / area of the detected peak and the known concentration of the component in the standard sample, and the parameters are also entered in the identification table.

[0008] In addition to the above elements, c) sampling means for controlling an autosampler to automatically set a standard sample and an unknown sample in a chromatograph; and d) a waveform created as described above by reference data creating means. Component identification means for identifying each component of the unknown sample based on the processing parameters and the identification table and the data stored in the analysis data storage means for the unknown sample, and identifying the unknown sample from the analysis of the standard sample It is also possible to automate all the series of analysis up to.

[0009]

In the chromatographic data processing apparatus according to the present invention, the apparatus automatically creates the waveform processing parameters and the identification table without manual operation by the user. Therefore, by combining with an autosampler, the standard sample and the sample to be analyzed are set in the autosampler in advance, and the analysis schedule is specified. Will be able to do it. In particular, when the number of samples and the number of analysis target components are large, the effect of labor saving in analysis is very large.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A gas chromatograph according to an embodiment of the present invention will be described with reference to FIGS. The gas chromatograph of this embodiment is provided with an autosampler 20 in addition to the main body 10 including the injector 11, the column 12, the detector 13, and the main body control device 14. The operation of the autosampler 20 is controlled by a sampler controller 21. The sampler controller 21 operates in synchronization with the main body 10 by exchanging data and commands with the main body controller 14. CPU 15, memory 16, input device (keyboard, mouse, etc.) 17 and output device (CRT, printer, etc.) 18 are provided in main body control device 14.
Reference numeral 15 denotes an injector 11 in addition to the sampler controller 21 described above.
It is connected to the column oven 19 and the like (via respective interfaces not shown) and controls their operations. The CPU 15 is also connected to the detector 13 of the column 12 and performs various data processing described later by receiving a signal therefrom. Therefore, the main body control device 14 also operates as the data processing device.

The procedure of analysis by the present gas chromatograph will be described below. First, for an unknown sample to be analyzed,
Determine the analysis target components that are considered to be contained in the components. This may be determined in advance by qualitative analysis. Then, a standard sample containing a predetermined amount of the target component is prepared. The standard sample and the unknown sample (single or plural) to be analyzed are supplied to the turntable 22 of the autosampler 20.
Set to. Then, the input device 1 of the main body control device 14
7, the turntable 22 for the standard sample and the unknown sample
Is input (FIG. 3) to instruct the start of automatic analysis.

The CP receiving these data and commands
U15 performs an automatic analysis according to the procedure shown in FIG.
First, a standard sample is subjected to chromatographic analysis as a first schedule (schedule # 1) (step S1). Specifically, the input standard sample turntable position is given to the sampler control device 21 to sample the standard sample, and the sample is injected into the injector 11. And
The detection signal transmitted from the detector 13 is converted into digital data by an A / D converter (not shown), and is sequentially stored in the memory 16 so as not to lose the time series.

After the retention time of the target component has sufficiently passed, data sampling is completed, and waveform processing parameters are created based on the data stored in the memory 16 (S
2). That is, first, the data stored in the memory 16 is sequentially taken out in time series, and a chromatogram (FIG. 4) is created. Then, the baseline portion (section A in FIG. 4)
Then, the slope value is calculated. The section A is set in advance to, for example, t1 to t2 minutes after the injection so as to be before the elution time of the sample. The calculation of the slope value itself can use a conventionally used method. next,
The maximum value of the height or the area of the peak obtained by partially detecting the peak in the section A is defined as “minimum peak height” or “minimum peak area”. Note that a standard (default) value may be determined in advance for each of these waveform processing parameters, and the parameter may be corrected (optimized) based on the chromatogram of the standard sample.

Next, the peak of the chromatogram of the standard sample is detected using the waveform processing parameters generated in step S2 (S3). Then, for each detected peak, the time of the peak top (retention time) is detected, and the area (or height) is calculated (FIG. 5). From these values, a target component identification table is created (S4,
(Fig. 6). In the identification table, in addition to the detected peak top time, the permissible width of each component is also entered. Also,
A calibration curve [concentration] = F1 × [area] + F2 is calculated based on the content (known) of the target component introduced into the standard sample, and its coefficients F1 and F2 are also entered in this identification table.

Here, the component name, the percentage value of the allowable range of the retention time of the component, and the data of the concentration in the standard sample (template; FIG. 7) are given to the main body controller 14 in advance. As shown in FIG. 8, a more specific identification table can be created.

The waveform processing parameters and the identification table created in this way are stored in the memory 16, and then the analysis of unknown samples after schedule # 2 is performed (S
5). In analyzing the data of the unknown sample, the content of the component is calculated using the waveform processing parameters and the identification table stored in the memory 16 and output to the output device 18.

A blank analysis (analysis using only a carrier without injecting a sample) is performed in schedule # 1, and the waveform processing parameters are determined.
In step 2, the analysis of the standard sample may be performed to automatically create an identification table.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of a gas chromatograph according to one embodiment of the present invention.

FIG. 2 is a flowchart showing a procedure of automatic analysis by a gas chromatograph as an example.

FIG. 3 is an example of an analysis schedule table.

FIG. 4 shows an example of a chromatogram.

FIG. 5 is a table showing peak times and peak areas of the chromatogram in FIG. 4;

FIG. 6 is an example of an identification table.

FIG. 7 shows an example of a template.

FIG. 8 is an example of an identification table described more specifically.

[Explanation of symbols]

 10: Main body 14: Main body control device 19: Column oven 20: Autosampler

Claims (1)

[Claims] 1. An analysis data storage means for sequentially converting a signal from a detector of a chromatograph into digital data and storing the data in a time series; and b) a data for a standard sample stored in the analysis data storage means. And a reference data generating means for generating a waveform processing parameter and an identification table based on the data.