JPS58154656A - Gas chromatographic device - Google Patents

Abstract

PURPOSE:To obtain a series of continuous chromatogram in a short time, by changeably connecting a series of a first columm, a second column, and a gas sensor, and a series of the first column, a third column, and the gas sensor through a changeover cock. CONSTITUTION:A series of continuous chromatogram of 6 components A-F gas mixture is obtained by setting a 3-way cock as shown by full lines in the figure, separating the 3 components A, B, and C, detecting them, and then, changing the cock over as shown in the figure to separate the components D, E, and F and detect them. Since the 6 components can be separated and detected, the 2 detectors are not necessary, but only one will do. Also, only one interface for connecting output of the sensor 6c with a data processing device for calculating gas concns., etc. will do. Thus, a series of continuous chromatogram can be obtained in a short time without dividing the components of the gases.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a gas chromatograph apparatus, and particularly to a gas chromatograph apparatus having a gas calibration tube, a column, a gas sensor, and the like.

Conventionally, when it is necessary to detect various mixed gas components in a single detection operation, for example, the gas components that have permeated through a polymer membrane are stored in a gas calibration tube, and the H,
, CO, CH4, C, H,.

For example, to measure the gas concentration of six components such as C, H, C, H6, etc.9. If you try to chromatographically separate and quantify various gases with one column, you will need an extremely long column.
Because the detection time was long, a heating gas chromatograph was required, which was a problem. However, in cases where a heating gas chromatograph apparatus cannot be used for measurements, it is often necessary to use a gas chromatograph apparatus such as that shown in FIG. 1, for example.

That is, a gas mixture of six components A, B, C, D, E, and F stored in a gas measuring tube 1 via a valve 2,
A carrier cast from the carrier gas generator 14 is supplied via the switching valve 3, for example, the six-way switching valve 3a, and
Insert into 5b. The respective gases separated by the columns 5a and 5b are introduced into the gas sensors 6a and 6b to detect the components, which are amplified by the amplifiers 7a and 7b, respectively, and then sent to the recorder 8.
m.

8b to record each. In the same section, 91° 9b is a gas separation packing material filled in columns 5a and 5b, respectively, and a flow rate regulator for a 1oFi carrier gas. In this way, 92 columns 5 m, suitable for the separation of each gas,
If you install a gas sensor 5m and 5b every 5b and measure it, A
It is possible to separate and detect six components of ~F, and gas sensor/server 61
,6bjC detected and recorded friend1rtsa,s
A so-called chromatogram recorded on the recording paper b as shown in the figure is shown in FIG. In other words, the chromatogram is shown with the outputs of the gas sensors 5a and 5b on the vertical axis and the time on the horizontal axis.
The results of separate detection using a system consisting of 1 gas sensor 6, an amplifier 7m, and a recorder 8a clearly show that among the 6 components, components A, B, and C are as shown by the solid line in the figure. However, the separate detection of components D, E, and F is unclear. On the other hand, the results of separation and detection in the system formed by the column 5b, gas sensor 6b, sensor 7b, and recorder 8b indicate that A of the six components is , B, and C could not be detected separately, but components D, E, and F were clearly detected separately. Incidentally, the time until the peak appears on a chromatogram is referred to as the retention time of each component and is used for qualitative determination of the component, and the area or height of the peak is used for quantitative determination.

In this way, we were able to separate and detect the six components A to F, but the chromatogram shows that each column 5a and gas sensor 6a
Since the chromatograms are obtained for each column 5b and gas sensor 6b, it is not a series of nine consecutive chromatograms. For this reason, attempting to connect these chromatograms to a data processing device that determines the degree of dispersion of each Haji gas will result in double effort and complicated operations. In addition, in this example, the gas sensor 6a
.

6b and two interfaces to the data processing device, which is uneconomical. Furthermore, since the gas in the gas calibration tube 1 is divided into two parts and sent to the columns 5a and 5b, there are many drawbacks such as a decrease in the output of the chromatogram.

The present invention has been made in view of the above points, and its object is to provide a gas chromatograph apparatus that can obtain a series of continuous chromatograms in a short period of time.

That is, the present invention provides a first column having one end connected to a switching valve, and a column connected between the other end of the first column and a gas sensor and connected in parallel via the column switching valve. A column switching valve is used to connect the first column, the second column, and the gas sensor, and between the first column, the third column, and the gas sensor. It is characterized by being switched and connected to each other.

The present invention will now be described based on the illustrated embodiments. FIG. 3 shows an embodiment of the invention. Note that parts that are the same as those in the conventional model are given the same reference numerals, and therefore their explanations will be omitted. In this embodiment, the columns include a first column 5c whose one end is connected to the switching valve 3, and a column with 11 column switching valves connected between the other end of the first column 5C and the gas sensor 6C. It is formed from a second column 5d and a third column 5C that are connected in parallel through a gas sensor 60.
The first column 5c1, the third column 5e, and the gas sensor 6c were switched and connected, respectively. The column switching valve 11 uses, for example, a three-way switching valve tta,
This was placed in a 5C9 ml column of Ml. By doing so, a gas chromatograph apparatus that can obtain a series of continuous chromatograms in a short period of time can be obtained. That is, a mixed gas of six components A to F is introduced from the pulp 2 into the gas measuring tube 1. Next, when the six-way switching valve 31 is switched to the R path shown by the dotted line in the figure, the carrier gas from the carrier gas generator 4 is transferred to the tenth column 5C and the second The gas is sent to the gas sensor 6C via the column 5d. In addition, the six-way switching valve 3a
, and the three-way switching valve 11m are normally arranged in a flow path as indicated by the solid line in the figure, and the carrier gas from the four carrier gas generators λ is distributed between the first column 5C and the second column 5d.
The gas sensor 6C is made to come into contact with the gas sensor 6C via. In this way, the output of the gas sensor 6C is taken on the vertical axis in Fig. 4 using the recorder 8C via the amplifier 7C, and the time is plotted on the horizontal axis in the chromatogram. CO gas components were well separated and detected, D, E,
Separation and detection of F is unclear and a chromatogram is obtained. This is done in the first place so that a romatogram like this is obtained.
Types of gas separation packing materials gc and gd to be filled in the column 5C and the second column 5d, and these double force rams 5c
, 5d, etc. are determined.

Next, the three-way switching valve 11 is switched to the flow path indicated by the dotted line in the figure, and the mixed gas is sent to the gas sensor 6C via the first column 5C and the 30th column 5e. If you do this, you will now record via amplifier 7C! At 't8C, the gas components A, B, and C, as shown by the dotted line in FIG. 4, cannot be separated and detected, but the gas components D, E, and F are well separated and detected, and a nine chromatogram is obtained. This is also done in advance in order to obtain a chromatogram like this in the third column 5.
This is because the type of gas separation packing material 9C to be filled in the column 5e and the length of the column 5e are determined.

That is, the first column 5C is common, and in this first column 5C, among the six components of the mixed gas of HA-F, human, B,
The CO gas component is hardly separated, and the purpose is to separate the D, E, and F gas components, and the A, B, and CO gas components are set to be separated in the second column 5d. . And in the third column 5C, the first column 5C, E, F
Used as an auxiliary column when gas components cannot be separated well. If the first column 5C is sufficient to separate the gas components E and F, use these.

The second column 5d, which is not related to the adsorption separation of gas components E and F, may be filled with a packing material having the same particle size as the gas separation packing material 9d.

By the way, in order to obtain a series of continuous chromatograms of a mixed gas of six components A-F, first, the three-way switching valve 111m? The settings are made as shown by the solid line in the figure, and after the gas components A, B, and C are separated and detected, the three-way switching valve 111 is switched as shown by the dotted line in the figure.

It is sufficient to separately detect each gas component of E and F. In this way, as shown in FIG. 5, as time passes, A, B, C and points S
A series of consecutive chromatograms is obtained in which there are peaks for each gas component.

In this way, six component gases can be detected separately, so there is no need for two gas sensors 6C as in the past, but only one gas sensor.The output value from this gas sensor 6C is used to determine the gas #. Only one interface is required to connect to a data processing device that performs quantitative calculations. Also, without separating the gas components, the first column 5c and the second column 5d
The output of the chromatogram is improved since the first column 5C and the third column 5e are selectively fed.

A three-way solenoid valve 11b may be used as the naori ram switching valve 11, and may be linked to the operation of the six-way switching valve 3a. That is, when the A, B, and CO gas components are detected, the three-way solenoid valve 11b is linked to perform a switching operation. In this way, manual operation becomes easier.

Furthermore, if the lengths of the second column 5d and the third column 5e are different, the flow rate of the carrier gas will change when the three-way switching valve 11m is switched, and the so-called baseline, which is the horizontal axis of the chromatogram, will change. Since this results in a lack of quantitative accuracy, the lengths of these two columns 5a and 5e and the types of gas separation packing materials gd and 9e to be filled are made the same. In this way, the flow velocity becomes four-dimensional, so there is no need to adjust the flow velocity.

Furthermore, if the time difference between gas component C and gas component d as shown in FIG. , three-way switching valve 11a and third column 5
The detection time between e and gI4! Install a pipe to
It is also possible to provide a detection time difference.

Furthermore, various gas separation fillers 9c, 9d, and 9e are available, and the most suitable filler can be used as required.

and respective columns 5c, 5d.

In 5e, a plurality of types of gas separation packing materials may be used to optimize gas separation, and it is not necessarily limited to using 1 m of gas separation packing materials for one column.

Another embodiment of the invention is shown in FIG.

In this embodiment, the three-way switching valve 11m is installed on the gas sensor 6C side. In this case as well, the same effects as in the above case can be achieved.

As described above, the present invention switches and connects the first column, the second column, and the gas sensor, and the first column, the third column, and the gas sensor via the column switching valve. By switching the power switch valve, it is possible to continuously separate and detect various gases, and a series of continuous chromatograms can be obtained in a short time. A gas chromatograph device can be obtained.

[Brief explanation of the drawing]

Figure 1 is a system diagram of gas separation and detection in a conventional gas chromatograph, Figure 2 is a chromatogram of each gas in the conventional gas chromatograph, and Figure 3 is a gas chromatogram of an embodiment of the gas chromatograph of the present invention. Separation detection system diagram, Part 4
The figure shows a chromatogram of various gases in one embodiment of the gas chromatograph apparatus of the present invention, FIG. 5 shows a series of chromatograms of various gases in the same embodiment, and FIG. 6 shows another embodiment of the gas chromatograph apparatus of the present invention. FIG. 3 is a system diagram of an example gas separation detection. 1... Gas detection mW, 3... Switching valve, 3m... Hexagonal switching valve, 5C... First column, 5d... Second column, 5e... Third column, 6C...Gas sensor, 9C99dt 9e...Gas separation filler, 11
...Column cut 2nd figure → E78 Mukai 3rd area C 4th mouth □ Gin'' Sheep 6 prisoners

Claims (1)

[Claims] 1. A gas measuring tube, a column connected to the gas measuring tube via a switching valve that switches the flow path of the carrier gas, and a column that separates the types of gases, connected to the column and connected to the column for separation. In a gas chromatograph apparatus having a gas sensor for detecting nine gases, the column is connected to a first column having one end connected to the switching valve, and the other end of the first column is connected to the gas sensor. A second column, a third column connected in between and connected in parallel via a column switching valve.
and the column switching valve switches and connects the first column, the second column, and the gas sensor, and the first column, the third column, and the gas sensor, respectively. A gas chromatograph device whose sexual characteristics are: Z @iJ The second and third columns are the length,
The gas chromatograph apparatus according to claim 1, wherein the inner diameter is IWJ-, and the particle size of the gas separation packing material is also (''-. λ The column switching valve is a three-way solenoid valve. A gas chromatograph apparatus according to claim 1.