KR20060000407A - Tube oven of gas chromatography and apparatus for analysing of gas using the same - Google Patents

Abstract

The present invention relates to a tube oven and a gas analyzer for gas chromatography, wherein the tube oven is provided in a vessel containing a medium having a higher heat capacity and a higher thermal conductivity than an air, and is provided in the vessel to provide heat for heating the medium. It includes a heater. In addition, it comprises a coiled column surrounding the heater in a spaced apart state, and phase separation of the analysis gas provided. The tube oven having the above-described configuration satisfies the conditions of miniaturization and weight reduction, and the gas analysis device including the tube oven can be used directly in the work site as well as in the laboratory.

Description

Tube Oven of Gas Chromatography and apparatus for analysing of gas using the same

BRIEF DESCRIPTION OF THE DRAWINGS It is a block diagram which shows the tube oven applied to the conventional gas chromatography analyzer.

Figure 2 is a block diagram showing a tube oven applied to the gas chromatography analysis apparatus according to an embodiment of the present invention.

3 is a block diagram showing a gas chromatography analysis apparatus including a tube oven according to another embodiment of the present invention.

Explanation of symbols on main parts of drawing

100 container 110 medium

120: heater 130: coiled column

140: heat insulating member 150: tube oven

160: multiport valve 170: detection unit

180: control unit

The present invention relates to a tube oven and a gas analysis device. More particularly, the present invention relates to a tubular oven of gas chromatography modularized so that various detectors can be used in combination, and a gas analyzing apparatus including the same.

In general, chromatography refers to a variety of solids or liquids as a stationary phase, a gas or liquid as a moving phase, and a sample is introduced into the mobile phase while allowing the mobile phase to pass through the stationary phase. Refers to an analysis method for separating a sample by component by using a difference in adsorption or partition coefficient between the mobile phase and the fixed phase.

The chromatographic method has been developed in various kinds, and is used for a wide range of analysis, including separation of natural products, purification of medicines, purification of other chemicals, and the like.

The chromatography method has a different name depending on the type of mobile phase applied. When the mobile phase is a gas, it is called gas chromatography, and when the mobile phase is a liquid, it is called liquid chromatography. In addition, when the pressure applied to the mobile phase in liquid chromatography is high, it is referred to as High Pressure Liquid Chromatography (HPLC) or High Performance Liquid Chromatography (HPLC).

In addition, thin layer chromatography coated with silica gel powder on glass plates or synthetic resin plates is widely used for simple analysis, and ion exchange chromatography that separates and analyzes ions using ionic bonds instead of using a difference in partition coefficient. Ion Exchange Chromatography is also being developed and used.

Although chromatographic apparatuses have been developed and commercially supplied with various chromatographic methods, fundamentally, the chromatographic apparatus has a physical property of the sample to be analyzed, that is, partition coefficient, molecular weight and ion between the fixed and mobile phases. As it is based on separation using sex, the optimal separation and analysis conditions of the desired sample cannot be defined or determined uniformly.

In addition, it is determined by the interaction of various analysis elements, such as the selection of the stationary and mobile phases, the flow rate of the mobile phase, the temperature of the oven in which the distribution takes place, and the selection of a detector to detect the sample eluting separately. The determination of the analytical elements in the method is a very important factor that can influence the analysis results. Therefore, the analysts have always had to select the optimal analysis method by chromatography.

In particular, the gas chromatography apparatus has a very simple structure including an analytical sample providing unit, a column oven including a column, a detector, and the like as an essential component thereof, and has a higher accuracy and accuracy than a liquid chromatography apparatus such as high pressure liquid chromatography. It is widely used because of its high sensitivity, easy maintenance and repair, and simple facilities, which is particularly advantageous for basic analysis and routine analysis performed commercially.

However, the gas chromatography apparatus includes the tube oven shown in FIG. 1.                         

1 is a block diagram showing a tube oven applied to a conventional gas chromatography apparatus.

Referring to FIG. 1, the tube oven 50 includes a column 40, a heater 36, a fan 32, an air inlet 30, an air outlet 34, and a container 40 having a space for receiving air. ). The air inlet 30 is formed on the first side of the container 40, and the air outlet 34 is formed on the second side opposite to the first side of the container. The heater 36 provides heat for heating the air present in the container and serves to circulate the heat provided from the fan 32 and the heater 36. In addition, the air inlet 30 and the air outlet 34 serve to control the temperature inside the container.

The tube oven 50 having the above-described configuration is very large in size because of the structure of heating the column 38 by circulating heated air, and its weight is also heavy. For this reason, the analysis of a sample is not performed in the field, but the situation is performed in the laboratory in which the said gas chromatography apparatus is installed. This causes a problem that the analysis time of the sample is long.

It is therefore a first object of the present invention to provide a lightweight tube oven suitable for forming a gas analysis device.

A second object of the present invention is to provide a lightweight and modular gas analysis device including the tube oven described above.

According to an embodiment of the present invention for achieving the object of the present invention, the tube oven is provided in the container and the container containing a medium having a heat capacity and thermal conductivity superior to the air (air), the heat for heating the medium It includes a heater to provide. In addition, it comprises a coiled column surrounding the heater in a spaced apart state, and phase separation of the analysis gas provided.

In addition, according to an embodiment of the present invention for achieving another object of the present invention, the gas analysis device is connected to the coil-like column and gas lines for phase separation of the supplied analysis gas, and is provided in the gas line And a multiport valve for selectively supplying analyte gas into the column. The tube oven receives a medium having a better heat capacity and thermal conductivity than air to heat the analytical gas supplied to the coiled column, and provides a heat to the medium for heating the analytical gas, and an impregnated in the medium. Accommodate coiled columns. The control unit is connected to the column, and measures the phase separated analysis gas to analyze and monitor the detection unit and the data detected by the detection unit and transmits the result to the display unit.

The tube oven according to the invention can be applied to a chromatographic apparatus having various detections, and particularly preferably to a gas chromatography apparatus.

Hereinafter, a tube oven applied to a gas chromatography apparatus according to a preferred embodiment of the present invention will be described with reference to the accompanying drawings.

Figure 2 is a block diagram showing a tube oven applied to the gas chromatography apparatus according to an embodiment of the present invention.                     

The tube oven 150 of the gas chromatography apparatus shown in FIG. 2 is a heater providing heat for heating the medium 110 contained in the container 100 containing the medium 110 having excellent heat capacity and thermal conductivity. 120 and a coiled column 130 for separating the analysis sample provided and the heat insulating member 140 surrounding the container.

The vessel 100 is a cylindrical housing having a space for receiving the medium 110, the heater 120, and the coiled column 130. The container 100 preferably has a Teflon material having more stable properties even at high temperatures.

The medium 110 is a material that replaces air. The medium 110 has a larger heat capacity than air and has a stable physical property even at a high temperature of 300 ° C or higher. The above-described medium may maintain a stable temperature even after heating, and may heat the analytical sample provided into the column more quickly and stably by maximizing the contact area of the column.

The heater 120 provides heat for heating the medium contained in the container, is provided in the direction of the central axis of the container 100, and is impregnated in the medium contained in the container. The heater 120 preferably uses a hot wire. It is preferred that the hot wire is a Teflon-coated hot wire so that it does not react with the medium to corrode.

The coiled column 130 is a tube or capillary filled with a filler for filtering an analyte to be analyzed and has a coil shape surrounding the heater to form a longer length. The coiled column 130 may be selected according to the physical and chemical properties of the analytical sample, and may be used by purchasing a commercially available product.

The length of the coiled column 130 can vary widely from less than 2m to more than 50m in general. In addition, the coil column 130 is preferably formed of a material such as stainless steel, glass, fused silica or Teflon.

An injection part I and an discharge part O are formed in the coil column 130. The injection unit I is an inlet through which an analytical sample or carrier gas is injected, and the discharge unit O is an inlet through which an analyte sample is separated into a predetermined phase. The carrier gas may be any one that can be used as a mobile phase of gas chromatography in addition to mainly inert gas such as helium or nitrogen.

The heat insulating member 140 surrounds the container 100 to further increase the heat insulating property and the heat retention of the container 100. The edge member 140 preferably has a structure in which glass fibers and asbestos are laminated.

Although not shown in the drawings, the inlet port I of the coiled column 130 may include a first connection unit (not shown) that may be connected to a sample providing unit (not shown) and a carrier gas providing unit (not shown). It is preferable to have a. In addition, the outlet O of the coil column 130 is preferably provided with a second connecting means (not shown) that can be connected to the detector.

The tube oven 150 having the above-described configuration can adjust the temperature of the analytical sample provided to the coiled column to 1/10 ° C., and has the characteristics of miniaturization and light weight. Because of this, it is easy to move and easy to apply desorption to the gas chromatography apparatus.

3 is a block diagram showing a gas chromatography apparatus including a tube oven according to another embodiment of the present invention.

The gas chromatography apparatus illustrated in FIG. 3, that is, the gas analyzing apparatus 200 includes a tube oven 150, a multiport valve 160, a detector 170, a controller 180, and the like.

The tube oven 150 accommodates a medium (not shown) having a better heat capacity and thermal conductivity than air to heat an analytical sample supplied to a coiled column (not shown), and heats the analytical sample. A heater (not shown) for providing heat to the medium and a container (not shown) for receiving the coiled column 130 impregnated in the medium. Here, the tube oven 150 has been described in detail in the above embodiment and will be omitted to avoid duplication.

The multiport valve 160 is connected to the gas lines 162a, 162b, and 162c to which an analytical sample (analytical gas) is provided, respectively, and is connected to an inlet of the coiled column 130 accommodated in the tube oven 150. . It is also connected to a carrier gas providing unit (not shown) that provides a carrier gas for carrying the analysis sample.

The multi-port valve 160 is controlled by a controller (not shown) to provide various types of analysis samples (analysis gas) provided in the gas lines to a predetermined amount, and selectively into the coil column. Such control enables the analysis of the plurality of samples in one gas analyzer.

The detector 170 is provided at the column of the tube oven, that is, at the distal end of the column, and detects data such as components and mass of the phase-separated sample discharged from the outlet of the column.

For example, a flame ionization detector, a thermal conductivity detector, an electron capture detector, an atomic emission detector, a thermal ion detector, and the like may be used as the detection unit. Can be mentioned. The flame ionization detector is most widely used in gas chromatography and has a mass-sensitivity characteristic that is superior to concentration-sensitivity because it is sensitive to the number of small atoms entering the detector per unit time.

The thermal conductivity of both the detector is large and present operations are simple in the device based on the thermal conductivity change in the gas stream arising from, and the linear response range of the molecules of the sample to be analyzed (to 10 ^5), organic and inorganic chemical species There is an advantage that the sample is not destroyed after detection. Electron capture detectors are most widely used for environmental sample analysis because of their high selectivity to halogen elements and the advantages of not significantly altering analyte samples over flame detectors. The atomic emission detector obtains emission spectra with a diode array emission spectrometer connected to the plasma. These spectra are obtained with a spectrometer with a flat diode array that can detect emission radiation from about 170 nm to 780 nm. Thermal ion detectors are particularly useful for detecting and quantifying phosphorus-containing pesticides because they have selectivity for organic compounds containing phosphorus and nitrogen. The controller 180 analyzes, monitors, and measures data detected by the detector 170, and transmits the result to the display unit.

Hereinafter, the detection method of the analysis gas using the gas analysis apparatus which has the above-mentioned structure is demonstrated.

First, a predetermined amount of carrier gas and analytical gas flow into the column of the tube oven by controlling the multiport valve 160. At this time, the amount of analysis gas injected into the column due to the control of the multiport valve is limited to a small amount. Subsequently, the analytical gas introduced into the coiled column is heated to a predetermined temperature by a medium heated in the tube oven. The heated analyte gas phase separates through the coiled column. The phase separated analyte gas is then provided to the detector through the outlet of the coiled column. The phase separation gas provided to the detector is passed through the detector to generate data indicating the components constituting the gas and the concentration thereof. The generated data is analyzed and monitored through the control unit and transmitted to the display unit 182. The data displayed on the display unit is confirmed by the operator.

The tube oven of the present invention having the above-described configuration can adjust the temperature of the analytical sample provided to the coiled column to 1/10 ° C, and has the characteristics of miniaturization and light weight. For this reason, it is easy to move and easy to apply a desorption to a gas chromatography apparatus. In addition, the analysis device including the tube oven is applied to analyze various types of analytical gases. It also significantly reduces the work and time required for setting and analysis time and can be used directly in the lab as well as in the laboratory. In addition, the reliability of the analysis results can be greatly improved.

While the foregoing has been described with reference to preferred embodiments of the present invention, those skilled in the art will be able to variously modify and change the present invention without departing from the spirit and scope of the invention as set forth in the claims below. It will be appreciated.

Claims (10)

A container containing a medium having a higher heat capacity and a higher thermal conductivity than air; A heater provided in the vessel and providing heat for heating the medium; And And a coiled column surrounding the heaters spaced apart from each other and phase separating the analytical gas provided therein. The gas oven of claim 1, wherein the vessel is a Teflon cylinder. The tube oven of claim 1, wherein the medium is a thermally stable material at a temperature of 300 ° C. or higher. The tube oven of claim 1, wherein the heater is a Teflon-coated hot wire. The tube oven of claim 1, further comprising a heat insulating member surrounding the container. A multiport valve for connecting the coil-type column and gas lines for phase separation of the analysis gas to be supplied and for selectively supplying the analysis gas provided in the gas line into the column; A heater for receiving a medium having a better heat capacity and thermal conductivity than air for heating the analytical gas supplied to the coiled column, and providing heat to a medium for heating the analytical gas, and a coiled column impregnated in the medium. Tube oven comprising a; A detector connected to the coiled column and measuring an analyte gas discharged from the column by phase separation; And And a controller which analyzes, monitors, and measures data detected by the detection unit, and transmits the result to the display unit. The gas analyzer of claim 6, wherein the multiport valve is connected to a carrier gas providing unit. 7. The gas analyzer of claim 6, wherein the vessel is a Teflon cylinder and the medium is a thermally stable material at a temperature of at least 300 < 0 > C. The gas analyzer of claim 6, wherein the tube oven further comprises a heat insulating member surrounding the container. The method of claim 6, wherein the detection unit Flame Ionization Detector, Thermal Conductivity Detector, Electron Capture Detector, Atomic Emission Detector and Thermal Ion Detector Gas analysis device characterized in that any one selected from the group consisting of a detector.

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