JP2003004714A - Analyzer for component in hermetically closed container - Google Patents

Abstract

PROBLEM TO BE SOLVED: To calculate a component contained in the gas or liquid in a hermetically closed container by one apparatus and to analyze a plurality of components in the same sample. SOLUTION: The analyzer for the component in the hermetically closed container is equipped with a first sampling means 2 for sampling the gas of the gas part A in the hermetically closed container 6, a second sampling means 3 for sampling the liquid part B in the hermetically closed container 6, a gas chromatograph 4 for analyzing the component contained in the gas sampled by the first sampling means and the component contained in the liquid sampled by the second sampling means 3 and a data processing means 5 for calculating the components contained in the gas part and liquid part of the hermetically closed container on the basis of the detection result of the gas chromatograph. The first sampling means is equipped with the sampling needle 23 communicating with the gas part of the hermetically closed container and a sampling pipe (sampling group 22) for taking out the gas of the gas part of the hermetically closed container through the sampling needle.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to an apparatus for analyzing components contained in a closed container such as a can or a bottle.

[0002]

2. Description of the Related Art A method called a headspace method is known as a method for analyzing components such as oxygen and carbon dioxide contained in a gas portion in a closed container such as a can or a bottle.
In this headspace method, a gas is taken out of the closed container by inserting a needle into the closed container, and the taken out gas is detected by a sensor. Further, generally, a chromatograph is known as a method for analyzing the components of a sample.

Conventionally, when analyzing the components contained in a closed container, the gas portion is measured by changing the sensor for each component by the headspace method and the liquid portion is measured by a predetermined analysis method. It is carried out.

[0004]

Conventionally, in order to carry out the component measurement for all the components contained in the gas portion and the liquid portion in the closed container, the sensor is exchanged for each component by the headspace method. By doing so, each component of the gas part in the closed container is measured, and for the liquid part, the component is measured by a predetermined analysis method, and the analysis results of both measurements are summed. Therefore, there is a problem that two analyzers are required, one for measuring the component contained in the gas portion and the other for measuring the component contained in the liquid portion.

Further, in order to measure a plurality of components, it is necessary to replace the sensor for each component, but in the component analysis by each sensor, the sample can be used only once, and the same sample can analyze a plurality of components. I can't do it. Therefore, conventionally, in order to analyze a plurality of components, there is no choice but to analyze using different samples, and there is a problem that the plurality of components in the same sample cannot be analyzed. Further, since it is necessary to replace the sensor for each component, there are problems that the operation is troublesome and the measurement requires a long time. In addition, there is also a problem that it is necessary to manually add up the analysis results of the components contained in the gas portion and the components contained in the liquid portion.

Therefore, the present invention solves the above-mentioned conventional problems, and the components contained in the gas and the liquid in the closed container can be obtained by one apparatus, and the plural components in the same sample can be obtained. An object is to provide an in-vessel component analysis device that can perform analysis.

[0007]

According to a first aspect of the present invention, there is provided a device for analyzing a component in a hermetically sealed container, wherein the gas in a gas portion of the hermetically sealed container is collected.
Collecting means, second collecting means for collecting the liquid portion of the closed container, components contained in the gas collected by the first collecting means and components contained in the liquid collected by the second collecting means are analyzed. A gas chromatograph and a data processing means for calculating the total of the components contained in the gas portion and the liquid portion in the closed container based on the detection result of the gas chromatograph, and the first sampling means is the gas portion of the closed container. And a sampling tube for venting the gas in the gas portion of the closed container through the sampling needle.

The analysis of the components contained in the closed container is first
Each detection result obtained by introducing into the gas chromatograph the gas in the gas portion of the closed container collected by the collecting means of 1 and the gas obtained by gasifying the liquid portion of the closed container collected by the second collecting means Is used to calculate the total of the components contained in the gas portion and the liquid portion in the closed container.

According to the present invention, the gas portion of the closed container collected by the first collecting means and the liquid portion of the closed container collected by the second collecting means are measured by a gas chromatograph so that the same sample can be obtained. A plurality of components contained in can be analyzed.

Further, according to the present invention, the gas portion of the closed container is sampled by the first sampling means, the liquid portion of the sealed container is sampled by the second sampling means, and these are measured by a gas chromatograph. By processing the data of (1), it is possible to analyze the combined components of the gas portion and the liquid portion in the closed container with one device.

Further, the first collecting means is provided with a collecting means for collecting the whole gas in the gas portion of the closed container by gas exchange between the collecting pipe and the switching means. By opening and closing the container, the gas in the closed container collected from the sampling tube can be collected as necessary.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described in detail below with reference to the drawings. FIG. 1 is a diagram for explaining the outline of the function of the component analysis device in a closed container according to the present invention. The component analysis device 1 in a closed container includes a first collection means 2 for collecting a gas in a gas portion A of the closed container 6, and a closed container 6.
Second sampling means 3 for sampling the liquid portion B of the gas chromatograph 4 for analyzing the components contained in the gas sampled by the first sampling means 2 and the components contained in the liquid sampled by the second sampling means 3. And a data processing means 5 for calculating the total of the components contained in the gas portion A and the liquid portion B in the closed container 6 based on the detection result of the gas chromatograph 4.

The first sampling means 2 is a collection needle 23 that penetrates the lid portion of the closed container 6 and is ventilated with the gas portion A in the closed container 6 to take out the gas in the gas portion A, and the collection needle 23. The first sampling loop 22 is provided for temporarily holding the gas collected in 1. The configuration using the first sampling loop 22 as the sampling tube will be described below.

A detachable pipe 29 is attached to the collecting needle 23.
A purge gas such as He gas is supplied by a. Between the charge gas source (not shown) and the pipe 29a, a first stop valve 21b, a pressure regulator 24, and a pressure gauge 25 are connected in order from the charge gas source side, and the air remaining in the sampling needle 23 is purged by the purge gas. Purge. The first sampling loop 22 is attached to a sampling valve 21a composed of a 6-way valve or the like.
It is performed by switching a.

To take the gas into the first sampling loop 22, the sampling valve 21a is switched to the position shown by the solid line in the figure, and the gas taken out from the sampling needle 23 is first sampled through the second stop valve 21c. The surplus gas introduced into the loop 22 and not retained in the first sampling loop 22 is discharged from the port indicated by the symbol in the figure. This surplus gas can be collected by the collector 27 via the flow meter 28 and the collecting pipe 29b. The volume of gas in the gas portion A of the closed container 6 can be obtained from the amount of gas collected by the collector 27 and the volume in the path. In addition, from the operation of the flow meter 28 and the bubbles in the collector 27, it is possible to confirm the flow state of the path passing through the collection needle 23, the second stop valve 21c, the sampling valve 21a, the first sampling loop 22, and the like. .

To take out the gas from the first sampling loop 22, the sampling valve 21a is switched to the position shown by the broken line in the figure, and the purge gas is sent from the purge gas source 20a. The gas held in the first sampling loop 22 is sent to the gas chromatograph via the trap tube 26 for analysis. The trap tube 26 removes carbon dioxide and water. The analysis result of the gas chromatograph 4 is sent to the data processing means 5.

The second sampling means 3 is a closed container 6 that has been sampled.
A reaction tube 33 for gasifying the liquid portion B of the above, and a second sampling loop 32 for collecting the gasified gas. The reaction tube 33 forms a reaction path by connecting to the second sampling loop 32 via the sampling valve 31a. The sample taken out from the liquid portion B of the closed container 6 is gasified in the reaction tube 33, and the gasified gas is passed through the second sampling loop 32 and collected. The reaction tube 33
Oxygen can be introduced therein through the valve 31c, and gas can be exhausted from the reaction path through the valve 31b.

In order to take in the gas into the second sampling loop 32, the sampling valve 31a is switched to the position shown by the solid line in the drawing, the liquid in the liquid portion B of the closed container 6 is introduced into the reaction tube 33, and then the valve is opened. Oxygen is introduced through 31c and completely burned at high temperature. By this reaction, the nitrogen component becomes nitrogen gas and nitrogen oxides, and carbon becomes carbon dioxide. This combustion product gas can be taken into the second sampling loop 32 by passing through a reaction path passing through the reaction tube 33, the sampling valve 31 a, the second sampling loop 32, and the pump 34.

To take out the gas from the second sampling loop 32, the sampling valve 31a is switched to the position shown by the broken line in the figure, and the purge gas is sent from the purge gas source 20b. The combustion reaction gas in the second sampling loop 32 is introduced into a reduction device (not shown) to convert nitrogen oxides into nitrogen gas, and then sent to the gas chromatograph 4 for analysis. The analysis result of the gas chromatograph 4 is sent to the data processing means 5. The data processing means 5 calculates the total of the gas and liquid components contained in the closed container 6 based on the component result of the gas portion and the component result of the liquid portion measured by the gas chromatograph 4.

The procedure for analyzing a gas component by the in-vessel component analyzer of the present invention will be described with reference to the flow chart shown in FIG. First, set the initial conditions for the gas chromatograph. Initial conditions include, for example, column temperature, current value, zero adjustment of baseline (step S
1). Next, the valve or the like is set to the initial position. In this initial position setting, the first stop valve 2 for purge gas is used.
1b is set to a closed position, the sampling valve 21a is set to a charge position for passing the gas collected in the first sampling loop 22, and the second sampling valve 21c to the sampling loop 22 is set to a closed position (step S2). ).

After setting the initial position, the closed container 6 is set at a predetermined position so that the sampling needle 23 penetrates the gas portion A. For example, the lid portion of the closed container 6 is attached to the sampling needle 23.
Position it so that it is located below. by this,
By lowering the sampling needle 23, the sampling needle 23 can penetrate the lid portion of the closed container 6, and the opening formed at the tip can be inside the gas portion A. At this stage, only the positioning is performed and the sampling needle 23 is not yet inserted into the gas portion A (step S3).

Pipe 2 attached to the end of pressure gauge 25
9a is connected to the sampling needle 23, the first stop valve 21b for purge gas is opened, the purge gas is released from the opening at the tip of the sampling needle 23, and the air remaining in the sampling needle 23 is discharged ( Step S4). After closing the first stop valve 21b to stop the supply of the purge gas (step S5), the pipe 29a is removed from the sampling needle 23. When measuring the gas volume of the gas portion A, the collecting pipe 29b is connected to the flow meter 28 (step S).
6).

The sampling needle 23 is inserted into the lid portion of the closed container 6, and the opening at the tip is put into the gas portion A. As a result, the gas portion A in the closed container 6 communicates with the inside of the sampling needle 23. In the step S3, by positioning the lid portion of the closed container 6 at a position below the sampling needle 23, the handle interlocking with the sampling needle 23 is lowered to seal the sampling needle 23. It can be inserted into the lid portion of the container 6 (step S7).

Next, the second stop valve 21 connected between the sampling needle 23 and the sampling valve 21a.
Open c. By opening the second stop valve 21c, the gas portion A of the closed container 6 and the sampling loop 22
And will communicate with each other. When the sampling loop 22 is communicated, the gas portion A of the closed container 6 and the sampling needle 23
Due to the internal pressure, the gas in the gas portion A flows into the sampling loop 22, and is further collected by the collector 27 through the flow meter 28 and the collecting pipe 29b. As a result, the inside of the sampling loop 22 is replaced by the gas in the gas portion A, so that the gas in the gas portion A can be collected in the sampling loop 22 (step S).
8).

The collector 27 includes a sampling needle 23, a second stop valve 21c, a sampling valve 21a, a sampling loop 22, a flow meter 28, and a collecting pipe 29b.
The gas of all gas parts A except the gas remaining therein is collected. Therefore, by obtaining the volume of the remaining portion in advance, the gas portion A
Can measure the volume of gas (step S
9).

Next, the sampling needle 23 is separated from the closed container 6. This disconnection can be performed by raising the handle that interlocks with the sampling needle 23 (step S1).
1). After separating the sampling needle 23 from the closed container 6, the sampling valve 21a is moved to the discharge position (see FIG.
The sampling valve 21a therein is switched to the position shown by the broken line), and the purge gas is supplied from the purge gas source 20a. As the purge gas, the gas held in the sampling loop 22 is sent to the gas chromatograph 4 through the trap pipe 26. The gas chromatograph 4 analyzes the gas held in the sampling loop 22 (step S11). The sampling valve 21a is returned to the charge position (step S12), and the second stop valve 2
1c is closed (step S13).

Next, the procedure for analyzing a liquid component by the in-vessel component analyzer of the present invention will be described with reference to the flow chart shown in FIG. After setting the initial conditions of the gas chromatograph as in step S1 (step S21),
Set the valve etc. to the initial position. In this initial position setting, the valve 31b is closed and the second sampling loop 32 is connected to the reaction path including the reaction tube 33 by the sampling valve 31a (step S22).

After setting the initial position, the liquid collected from the liquid portion of the closed container 6 is set in the reaction tube 33 (step S23). After setting the sample, the valve 31b,
31c is opened, and oxygen gas is purged into the reaction tube 33 (step S24). A system in which the valves 31b and 31c are closed and the reaction path including the reaction tube 33 is closed (step S2
5) Burn the sample in the reaction tube 33 (step S2)
6).

After the combustion is completed, the sampling valve 3
1a is switched (sampling valve 31a in FIG.
A position indicated by a broken line in FIG. 2), and purge gas is supplied from the purge gas source 20b. The purge gas is sent to the gas chromatograph 4 through the gas held in the sampling loop 32. At this time, the nitrogen oxides are converted into nitrogen gas by passing through the reducing device. Gas chromatograph 4
Analyzes the gas held in the sampling loop 32 (step S27).

The components of the gas portion and the liquid portion are distinguished from each other by electrically switching the polarity of the detector in the gas chromatograph, switching by the valve of each flow path, and the like in the steps S11 and S27. other,
It can be performed by data processing of the analysis result obtained by the gas chromatograph.

The data processing means calculates the total amount of components contained in the closed container by using the analysis results of the components of the gas portion and the liquid portion of the closed container sent from the gas chromatograph. Further, when the analysis result from the gas chromatograph includes both the gas part component and the liquid part component, the gas part component and the liquid part component are identified by data processing to calculate the total component amount.

According to the aspect of the present invention, the total amount of the components contained in both the gas portion and the liquid portion in the closed container can be determined. According to the aspect of the present invention, it is possible to simultaneously analyze a plurality of components contained in the same sample. Further, according to the aspect of the present invention, it is possible to collect the gas in the closed container collected from the collecting tube.

[0033]

As described above, according to the in-vessel component analysis device of the present invention, the components contained in the gas and the liquid in the closed container can be determined by one device.

[Brief description of drawings]

FIG. 1 is a schematic diagram illustrating the configuration of an in-vessel component analysis device of the present invention.

FIG. 2 is a flow chart for explaining a gas component analysis procedure by the container component analysis device of the present invention.

FIG. 3 is a flow chart for explaining a liquid component analysis procedure by the in-vessel component analysis apparatus of the present invention.

[Explanation of Codes] 1 ... In-container component analysis device, 2 ... First sampling means, 21a ...
Sampling valve, 21b ... first stop valve, 2
1c ... 2nd stop valve, 22 ... 1st sampling loop, 23 ... sampling needle, 24 ... pressure regulator, 25 ... pressure gauge,
26 ... Trap tube, 27 ... Collector, 28 ... Flowmeter, 29
a ... pipe, 29b ... collection pipe, 3 ... second sampling means, 31a ... sampling valve, 31b ... valve, 3
2 ... 2nd sampling loop, 33 ... Reaction tube, 4 ... Gas chromatograph, 5 ... Data processing means, 6 ... Can (bin), A ... Gas part, B ... Liquid part.

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Shinsuke Kurihara             1-1 Midori, Moriya-cho, Kitasoma-gun, Ibaraki             Asahi Breweries, Ltd. Ibaraki Factory (72) Inventor Manabu Hashida             21-1 Midori, Moriya-cho, Kitasoma-gun, Ibaraki Prefecture             Asahi Breweries, Ltd. General Evaluation Center (72) Inventor Mikihiko Suzuki             1 Nishinokyo Kuwabaracho, Nakagyo Ward, Kyoto City, Kyoto Prefecture             Shimadzu Corporation (72) Inventor Tomohide Masaoka             1 Nishinokyo Kuwabaracho, Nakagyo Ward, Kyoto City, Kyoto Prefecture             Shimadzu Corporation (72) Inventor Masami Matsui             1 Nishinokyo Kuwabaracho, Nakagyo Ward, Kyoto City, Kyoto Prefecture             Shimadzu Corporation F term (reference) 2G052 AA00 AC14 AD02 AD06 AD42                       AD46 BA02 BA14 CA02 CA04                       GA27 JA00

Claims (2)

[Claims] 1. A first sampling device for collecting gas in a gas portion of a hermetic container, comprising: a sampling needle for ventilating a gas portion of the hermetic container; and a sampling pipe for taking out gas in the gas portion of the hermetic container through the sampling needle. Sampling means, second sampling means for sampling the liquid portion of the closed container, gas components collected by the first sampling means, and gas chromatograph for analyzing each component of the liquid collected by the second sampling means And a data processing means for calculating the components contained in the gas part and the liquid part in the closed container based on the detection result of the gas chromatograph. 2. The first collection means comprises a collection means for collecting all the gas in the gas portion of the closed container by gas exchange, and the collection means is openable / closable between the collection tube and the gas chromatograph. The component analysis device in a closed container according to claim 1, wherein the component analysis device is provided in.