JP3179281U - Valve converter for improving heart-cutting technology functions of gas chromatographs - Google Patents

Abstract

A valve conversion device for improving the heart-cutting technical function of a gas chromatograph is provided.
A valve conversion device includes a heart cut device 3 connected to a sample inlet 1 and a mass spectrometry detector 8 connected to the heart cut device 3. The heart cut device 3 is separated into a first connection column 4 and a second column. The apparatus further includes a valve control device 6, which is connected to the heart cut device 3 and the mass spectrometry detector 8 via a connection column. The first column 2 and the second column separated through the heart cut device 3 are respectively connected to a plurality of valve conversion connection ports in the valve control device, and the plurality of valve conversion connection ports communicate with the mass spectrometry detector 8. And a valve conversion connection port connected to the hollow column.
[Selection] Figure 2

Description

  The present invention relates to the field of mass spectrometry of gas chromatographs, and relates to a valve converter for improving the heart cut technology function of gas chromatographs.

  The gas chromatograph heart-cutting technique uses the difference in polarity between two columns to increase the separation ability for a complex sample and the measurement sensitivity of its trace components. In general, first, separation is performed based on the boiling point in the first column with low polarity, the component part where the target compound is present is selected through the heart-cut technology, and further separation is performed in the second column with polarity, and a favorable separation effect is obtained. obtain.

A gas chromatograph-mass spectrometry detector that has been commercialized with a heart-cut device is shown in FIG. 1, and the apparatus includes a first column 2 of a heart-cut device 3 connected to a sample inlet 1 and a heart-cut device. The first connected column 4 and the second column 15 separated by the vessel 3 are a mass spectrometry detector (MS) 16 and a flame ion detector (FID) 17, or a nitrogen / phosphorus detector (respectively). NPD) or other traditional detectors (this type of detector provides rapid qualification for compounds and cannot obtain mass spectra of unknown compounds).
The heart-cut technology for commercialized gas chromatograph-mass spectrometry detectors has the following drawbacks. In the two columns 4 and 15 separated after the heart cut, only one chemical component in one column can be put into the mass spectrometry detector 16, but the chemical component in the other one column is connected to the connected column 4. It passes through a flame ion detector (FID) 17 or a nitrogen / phosphorus detector (NPD) and other conventional detectors, and analysis with one mass spectrometric detector is impossible at the same time. By adding one mass spectrometry detector, the purpose of analyzing two columns separated by two mass spectrometry detectors each after the heart cut is achieved, but one mass spectrometry detector, Expenses are required for developing new software that controls this function.

  In view of the problems existing in the known art, an object of the present invention is to provide a valve converter for improving the heart-cutting technology function of a gas chromatograph. The apparatus realizes low cost, miniaturization, and functional improvement, and can separate and analyze all components by chemical injection of a chemical component that has been heart-cut a plurality of times.

  In order to realize the above-described object, means employed by the present invention are as follows.

  In the valve conversion device for improving the heart cut technology function of the gas chromatograph, the device includes a heart cut device connected to the sample inlet and a mass spectrometry detector connected to the heart cut device. The heart cut device is separated into a first connection column and a second column. The apparatus further includes a valve control device. The valve control device is connected to the heart cut device and the mass spectrometry detector through a connection column.

  The first connection column and the second column separated through the heart-cut device are respectively connected to a plurality of valve conversion connection ports in the valve control device, and the plurality of valve conversion connection ports are valves communicating with the mass spectrometry detector. A conversion connection port and a valve conversion connection port connected to the hollow column are included.

The effects of the present invention described above are as follows.
In the device of the present invention, by adding a valve control device, some complicated components in the sample are converted into the second column using the valve conversion device, and further separated. In addition, the purpose of separating all the samples is achieved by analyzing the components of the two columns separated after the heart cut by two sample injections as required. The valve conversion technology adopted by the device of the present invention enhances the use and scope of gas chromatograph heart-cut technology, and separates and analyzes chemical components that have been heart-cut multiple times based on experimental requirements, by two sample injections. can do. Therefore, the apparatus has advantages such as low cost, downsizing, and significant improvement in function.

It is a structural diagram of a gas chromatograph-mass spectrometry detector commercialized by attaching a heart cut device in a known technique. 1 is a structural diagram of a gas chromatograph-mass spectrometry detector of the present invention equipped with a valve control device and a heart cut device. FIG. 2 is a diagram showing a gas flow path system I of the apparatus. 2 is a diagram showing a gas flow path system II of the apparatus. It is a graph of the sample of the gas chromatograph-mass spectrometry detector which does not attach the valve | bulb control apparatus in a well-known technique. It is a graph of the sample of the gas chromatograph-mass spectrometry detector separated through the heart cut device, the valve control device, and the second column. It is a graph of the sample of the gas chromatograph-mass spectrometry detector of a heart-cut device and a valve | bulb control apparatus.

  The invention will now be described by way of example with reference to the drawings.

In the valve conversion device for improving the heart cut technology function of the gas chromatograph shown in FIG. 2, the device is a first column 2 of the heart cut device 3 connected to the sample inlet 1, and the first column 2 separated by the heart cut device 3. The one connected column 4 and the second column 5 are connected to the valve control device 6, and the valve control device 6 is connected to the second connected column and the mass spectrometry detector 8 through the connected column 7.
The novelty of the present invention is that the valve control device 6 is added, and the valve control device 6 includes three connection columns (first connection column 4, second column 5, and second connection column 7). To the heart-cut device 3 and the mass spectrometric detector 8.

  The first connection column 4 and the second column 5 separated by the above-described technical means and separated through the heart cut device 3 are respectively connected to the two valve conversion connection ports 61 to 66 in the valve control device 6. Connect to the connection port. The valve conversion connection ports 61 to 66 include a valve conversion connection port connected to the mass spectrometry detector 8 and a valve conversion connection port connecting the hollow column 9.

The aforementioned apparatus realizes separation and analysis of sample components through the following steps.
(1) First, the two columns 2 and 5 after the heart cut of the gas chromatograph are mounted on the valve controller 6.
(2) Thereafter, the valve control device 6 is connected to the mass spectrometry detector 8 on the same table using the connection column 7.
(3) The valve controller 6 connects one of the two columns 4 and 5 after the heart cut to the same mass spectrometer 8 by switching the valve conversion connection ports 61 to 66, and at the same time, already One column may be empty.

  The device of the present invention switches the valve conversion connection port by the valve control device, and analyzes the components of the second column 5 separated after the heart cut. Or the analysis of the 1st connection column 4 isolate | separated after the heart cut is implemented. Alternatively, the components of the two columns separated after the heart cut through two sample injections may be analyzed, respectively, to obtain all the information of the entire sample.

  As shown in FIG. 3, the valve conversion connection ports 62, 63, 64, 65 connected to the mass spectrometry detector 8 are switched by switching the valve control device 6 to the first connection column 4 and the second connection column 7 to be connected. When the second column 5 is connected to the valve conversion connection ports 61 and 66 that connect the hollow column 9 at the same time, the first connection column 4 and the second column can be realized by the components after the heart cut from the first column 2. The connected column 7 directly enters the mass spectrometric detector for analysis, and qualitative quantitative data can be obtained. At the same time, the components separated from the second column 5 are emptied and are not analyzed.

  As shown in FIG. 4, the valve control connection ports 61, 62, 63, 66 connected to the mass spectrometric detector 8 are switched by switching the valve control device 6 to the communication position of the second column 5 and the second connection column 7 to be connected. To do. At the same time, the valve conversion connection ports 64 and 65 communicating with the hollow column 9 are rotated and connected to the communication position of the first connection column 4. Thereby, the component separated from the second column 5 enters the mass spectrometry detector 8 and is analyzed, and qualitative quantitative data can be obtained. At the same time, other components are emptied from the first connection column 4 and are not analyzed.

  Based on the two types of connection methods described above, the object (component) for performing further separation analysis is realized by freely switching to mass spectrometry.

  Analysis of sample parts or all components.

  First, the experimental method is edited based on the requirements of the gas chromatograph-mass spectrometry detector, and all components are analyzed on the sample (see FIG. 5). It is separated into five objects (objects 1, 2, 3, 4, 5 in FIG. 5). The peak retention times of objects 1, 2, 3, 4, 5 are respectively 7.90-8.30, 9.72-9.90, 9.98-10.10, 11.24-11.60, 12.30-12.60 minutes.

In the experiment, it is required that the objects 2 and 5 are passed through the second column after heart cutting and further separation analysis is performed. Objects 1, 3 and 4 that have a good separation effect are directly subjected to mass spectrometry after heart-cutting (Note: Which specific part of the component enters the second column after heart-cutting and is required for separation analysis) This experiment is simply a demonstration of how to use the valve switching device).

  The experimental purpose is realized by the following experimental methods 1 and 2.

  Determine the ingredients that require heart-cutting as required by the experiment. For example, in the experiment, the objects 2 and 5 are designed to be further separated and analyzed through the second column after the heart cut, and the objects 1, 3 and 4 are emptied after the cut and are not analyzed.

  The peak start and end holding times of the objects 2 and 5 in FIG. 5 are calculated, and the valve conversion connection port control process is input, and the valve conversion connection port is at the position shown in FIG. 4 at 9.5 minutes. Switch, introduce the second peak into the second column, switch to the position shown in FIG. 3 at 10.5 minutes, and introduce the second peak into the second column. After 12 minutes, the position is further switched to the position shown in FIG. 4, the fifth peak is introduced into the second column, and the position is switched to the position shown in FIG. 3 at 13 minutes. In this way, the second and fifth peaks can be introduced into the second column. Then, it enters into a mass spectrometry detector through the valve | bulb conversion connection port connected with the mass spectrometry detector 8, and the 2nd connection column 7, and is analyzed (refer FIG. 6). The other three peaks 1, 3, 4 are released into the atmosphere through the first connection column 4, the valve conversion connection port connected to the hollow column 9, and the hollow column 9.

  Determine the ingredients that require heart-cutting as required by the experiment. For example, in the experiment, the objects 1, 3, and 4 having a preferable separation effect are directly subjected to mass analysis after heart cutting, and the objects 2 and 5 are emptied after the cutting and are not analyzed.

  The peak start and end holding times of the objects 1, 3, and 4 in FIG. 5 are calculated, and the valve conversion connection port control process is respectively input. When the valve conversion connection port is 7.5 minutes, it is shown in FIG. Switch to the position, switch to the position shown in FIG. 4 at 8.5 minutes, and introduce the first peak into the first connected column 4. The valve conversion connection port is switched to the position shown in FIG. 3 at 9.95 minutes, and further switched to the position shown in FIG. 4 at 12 minutes to introduce the third and fourth peaks. In this way, the first, third, and fourth peaks can be introduced into the first connection column 4. After that, it enters into the mass spectrometry detector 8 through the valve conversion connection port connected to the mass spectrometry detector 8 and the second connection column 7, and is analyzed (see FIG. 7). The other two peaks 2 and 5 are released into the atmosphere through the second column, the valve conversion connection port connected to the hollow column 9, and the hollow column 9.

  As can be understood from Comparative Figures 5, 6, and 7, the impurity peaks, tailing peaks, shoulder peaks, etc. present in Figure 5 are improved after the analysis of Experimental Methods 1 and 2 (see Figures 6 and 7). The peak type became more preferable, and more accuracy was added to the qualitative quantification.

  When it is desired to obtain the analysis result of the entire sample, the analysis results obtained by the experimental method 1 (see FIG. 6) and the experimental method 2 (see FIG. 7) may be combined.

In order to give a clear explanation of the advantages of the valve control device, the samples used in Experimental Method 1 and Experimental Method 2 were relatively simple. The superiority of this technique can be demonstrated well when the sample is complex and contains hundreds of components. Depending on demand, it is possible to freely cut components that are difficult to separate in the first column and introduce them into the second column 5 for further separation (see FIG. 4).
At the same time, it is also possible to perform mass spectrometry directly on the components which remain after the heart cut and are not so complicated (see FIG. 3).

  The above are only two specific embodiments of the present invention, and the design concept of the present invention is not limited to this. Therefore, all non-substantial changes made to this embodiment using this concept are regarded as acts that infringe the scope of the utility model registration request.

1 Sample inlet 2 First column 3 Heart cut device 5 Second column 15 Second column 16 Mass spectrometry detector
17 Flame ion detector (FID)
4 First connection column 6 Valve control device 7 Second connection column 8 Mass spectrometry detector
9 Hollow column 61-66 Valve conversion connection port

Claims (2)

In the valve converter for improving the heart cut technology function of gas chromatograph,
The apparatus includes a heart cut device connected to the sample inlet, and a mass spectrometry detector connected to the heart cut device, separating the first connection column and the second column from the heart cut device,
Further, the valve conversion device for improving the heart cut technology function of the gas chromatograph, further comprising a valve control device, wherein the valve control device is connected to the heart cut device and the mass spectrometry detector through the connection column.   In the apparatus, the first connection column and the second column separated through the heart cut device are respectively connected to a plurality of valve conversion connection ports in the valve control device, and the plurality of valve conversion connection ports are mass spectrometry detectors. The valve conversion device for improving the heart cut technology function of a gas chromatograph according to claim 1, further comprising a valve conversion connection port communicating with the valve and a valve conversion connection port connected to the hollow column.

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