JP3133927U - Liquid level position variable gas-liquid separation container - Google Patents

Abstract

【Task】
In measurement using a hydride generator that uses an atomic absorption spectrophotometer, ICP emission analyzer, ICP mass spectrometer, or atomic fluorescence analyzer as detection means, the reaction solution and the measurement sample are mixed, and the hydride gas and hydrogen generated are mixed. It is necessary to separate the gas from the reaction solution.
[Solution]
The gas-liquid separation container is provided with an adjustment valve and the like, and the cross-sectional area of the tube through which the gas passes is adjusted. As a result, the pressure in the gas-liquid separation container changes and the liquid surface position of the liquid mixture is moved so as to return to a constant pressure. Thereby, since the distance to the discharge port can be optimized, it is possible to adjust to the liquid surface position where the liquid droplets do not reach and to perform efficient gas-liquid separation. Moreover, since only the adjustment valve is operated, the same gas-liquid separation container can be used even if the reaction intensity changes, and the volume in the container is adjusted at the position of the liquid mixture level. Therefore, an optimum capacity can be easily ensured even in a gas-liquid separation container having a small capacity.
[Selection] Figure 4

Description

  In the present invention, a plurality of solutions are mixed in a hydride generator using an atomic absorption spectrophotometer, an ICP emission spectrometer, an ICP mass spectrometer, and an atomic fluorescence analyzer as detection means. The present invention relates to a gas-liquid separation container that efficiently separates a gas) and a liquid (such as a reaction liquid) or an analysis system including the same.

  An example of a hydride generator will be described. Arsenic, selenium, etc. are mentioned as a component which generates hydride gas with a hydride generator. A reaction liquid that generates hydrogen gas (an example of the reaction liquid is a mixed solution of a sodium borohydride solution and a hydrochloric acid solution) and a measurement sample containing the target component are mixed to generate hydride gas. In the measurement, it is necessary to efficiently introduce the hydride gas generated in the atomic absorption spectrophotometer, the ICP emission analyzer, the ICP mass spectrometer, and the atomic fluorescence analyzer. In order to achieve this, the mixed solution is introduced into the gas-liquid separation container, the generated gas and liquid are separated, and only the gas is introduced into the analyzer. FIG. 1 shows an example of a hydride generator using a gas-liquid separation container. Reaction solution A2 and reaction solution B3 necessary for generating measurement sample 1 and hydride gas are passed through pumps 4, 5, 6, introduced into mixer 7, and mixed into gas-liquid separation container 8. Introduce. The reaction time depends on the inner diameter and length of the tube connecting the mixer 7 and the gas-liquid separation container 8. The mixed liquid introduced into the gas-liquid separation container 8 is separated into liquid and gas, and the liquid is discharged as waste liquid. The gas contains a measurement component (hydride gas) and is introduced into a detection device 9 such as an atomic absorption photometer, an ICP emission analyzer, an ICP mass spectrometer, or an atomic fluorescence analyzer for measurement. FIG. 2 shows the structure of a general gas-liquid separation container. A liquid mixture obtained by mixing the sample solution and the reaction liquid is introduced from the liquid mixture inlet 10, and the liquid mixture fills up to the waste liquid outlet 11. At this time, the liquid surface position 12 is at the same height as the waste liquid discharge port 11 because the internal pressure is applied. The generated gas (hydride gas and hydrogen gas) is discharged from the gas discharge port 13, the gas and the liquid are separated, and the generated gas is connected to a device such as an atomic absorption photometer. In order to efficiently introduce the generated gas into a detection device such as an atomic absorption photometer, an ICP emission spectrometer, an ICP mass spectrometer, or an atomic fluorescence analyzer, argon gas or the like is introduced from the carrier gas inlet 14. However, when the reaction in which the gas is generated is intense, the liquid droplets scatter to the gas outlet 13 and block the gas passage, so that the liquid and the gas cannot be separated efficiently. The use of a gas-liquid separation container with a long distance to the gas discharge port can suppress the effects of liquid scattering, but the volume in the container increases, resulting in gas diffusion and efficient guidance to the detection device. Therefore, the sensitivity of the target component cannot be obtained sufficiently. In addition, there exists patent document 1 as a related thing.

JP-A-10-274657

  In measurement using a hydride generator that uses an atomic absorption photometer, ICP emission analyzer, ICP mass spectrometer, or atomic fluorescence analyzer as a detection means, the reaction solution and the measurement sample are mixed, and the generated hydride gas and It is necessary to separate the hydrogen gas from the mixed liquid, and the gas-liquid separation container plays a role. Normally, a gas-liquid separation container allows a certain amount of a mixture of a reaction solution and a measurement sample to stay in the container for a certain period of time, and then separates the hydride gas and hydrogen gas generated from the mixture into an atomic absorption photometer or ICP. It has a function of guiding to a detection device such as an emission analyzer, an ICP mass spectrometer, or an atomic fluorescence analyzer. The reaction for generating a gas from a liquid may splash liquid droplets during the reaction, depending on the amount of gas generated. When the liquid droplets fly to the gas discharge port, the gas passage is blocked, so that stable gas induction to the detection device becomes difficult, and the liquid and the gas cannot be efficiently separated. In order to suppress the influence of splashes, it is conceivable to use another gas-liquid separation container in which the liquid surface of the liquid mixture, which is the source of liquid splashes, is separated from the gas outlet, but the capacity of the gas-liquid separation container increases. The generated gas diffuses, and a stable gas flow cannot be maintained, or the sensitivity is lowered due to the gas diffusion. Moreover, it is necessary to replace the gas-liquid separation container according to the intensity of the reaction.

  In the present invention, for example, a gas discharge port of the gas-liquid separation container is provided with a mechanism that can control the flow rate of gas such as a regulating valve, and by adjusting this, gas generated is separated using the generated gas. The object is to change the pressure in the container and adjust the position of the liquid surface of the liquid mixture, which is the source of the liquid splash, so that the liquid splash does not reach the gas outlet.

  According to one aspect of the present invention, there is provided a gas-liquid separation container used in an analysis system in which a detection means and a hydride generator are combined, and the gas generated by the hydride generator is separated from the liquid. And an adjusting means for adjusting the position of the liquid surface of the mixed liquid, which is the boundary between the liquid and the liquid.

  For example, in a method in which an atomic absorption spectrophotometer, an ICP emission analyzer, an ICP mass spectrometer, or an atomic fluorescence analyzer is used as a detection means and combined with a hydride generator, a mixture of a reaction solution and a measurement sample is used. A gas-liquid separation vessel is used for the purpose of separating the hydride gas and hydrogen produced. In order to improve the reliability of measurement results, it is important to efficiently separate liquid and gas. The present invention aims to efficiently separate the generated gas from the mixed solution of the sample solution and the reaction solution, and controls the gas flow rate by providing an adjustment valve or the like at the gas discharge port of the gas-liquid separation container. In the gas-liquid separation container, hydride gas, hydrogen gas, and carrier gas generated by the reaction flow continuously, and are guided from the gas outlet to the detection device. When the reaction is intense, the flying distance of the liquid splash from the liquid surface of the mixed liquid extends, reaches the gas discharge port, and blocks the gas passage. In such a case, the regulating valve is throttled to reduce the cross-sectional area of the tube through which the gas passes and to increase the pressure in the gas-liquid separation container. Since the pressure in the container increases, the liquid level of the mixed liquid is pushed down. As a result, the distance to the gas discharge port can be increased, and the liquid surface position of the liquid mixture can be lowered so that the liquid droplets do not reach. Therefore, gas-liquid separation can be performed efficiently. Since only the regulating valve is operated, the same gas-liquid separation container can be used even if the reaction intensity changes. Moreover, since the volume in the container is adjusted at the position of the liquid mixture, the optimum capacity can be easily ensured even in a gas-liquid separation container having a small capacity.

  According to the present invention, in a gas-liquid separation container, a liquid in which a sample solution and a reaction liquid are mixed and a generated gas can be efficiently separated.

  For example, a hydride generator that uses an atomic absorption spectrophotometer, ICP emission analyzer, ICP mass spectrometer, or atomic fluorescence analyzer as a detection means generates hydride gas and hydrogen gas from a liquid and measures the target component. . The gas-liquid separation container performs the role of separating the mixed liquid (sample solution + reaction liquid) and the generated gas and guiding the gas to the detection device. In the reaction of generating gas from a liquid, the intensity of the reaction varies depending on the target component concentration and the reaction solution concentration. During the reaction, the liquid droplets are often blown off with the generation of the gas, and the liquid droplets reach the gas discharge port of the gas-liquid separation container and may prevent introduction of the gas into the detection device. In such a case, since the gas containing the target component does not reach the detection device, a good measurement result cannot be obtained. The present invention has a mechanism that can control the amount of gas generated that passes through the gas outlet per unit time, such as a cock that can adjust the cross-sectional area of the gas outlet of the gas-liquid separation container, The position can be adjusted freely. As a result, in the case of a violent reaction, the liquid level of the liquid mixture is lowered and the distance from the gas discharge port is increased to prevent the arrival of liquid droplets. Reduce the volume in the liquid separation container to suppress the dispersion of the generated gas. In the present invention, in any reaction state, gas and liquid can be efficiently separated in one gas-liquid separation container, and measurement can be performed in an optimum state.

〔Example〕
In practicing the present invention, a schematic diagram of a gas-liquid separation container for separating a mixed solution of a sample solution and a reaction solution and generated gas (hydride gas and hydrogen gas) is shown in FIG. A mixed solution of the sample solution and the reaction solution sent by a pump or the like is introduced into the inner tube from the mixed solution introduction port 15. The liquid mixture that has continued to be introduced and reaches the waste liquid discharge port 16 is discharged from the gas-liquid separation container. At this time, the mixed liquid level position 17 becomes equal to the height of the waste liquid discharge port 16. The generated gas is separated from the liquid from the liquid mixture liquid level position 17, and passes through the cock 20 that determines the cross-sectional area of the tube that passes the gas by the carrier gas such as argon gas introduced from the carrier gas inlet 19. It is carried to the outlet 18 and guided to the analyzer. Since it is a reaction that generates gas from the liquid, it is most likely to react by blowing off the liquid droplets, and when the droplets adhere to the cock 20 or the gas discharge port 18, the generated gas passage is obstructed. There is no efficient separation. In such a case, it is necessary to lower the position of the liquid mixture and separate the cock 20 and the gas outlet 18.

  FIG. 4 shows a liquid level adjustment method in the present invention. As in FIG. 3, the mixed solution of the sample solution and the reaction solution is introduced into the gas-liquid separation container through the mixed solution introduction port 21. When the reaction starts, the cock 26 is squeezed to reduce the cross-sectional area of the gas outlet 24. Since the gas discharge port 24 that is a discharge port for the generated gas and carrier gas is narrowed, the pressure in the gas-liquid separation container is increased. As the pressure increases, the liquid level position 23 is pushed down. As a result, the liquid mixture surface position 23 can be separated from the cock 26 and the gas outlet 24, and the liquid mixture liquid surface position can be optimized by adjusting the cock 26. When the reaction is intense, the cock can be squeezed, the liquid level of the mixed liquid can be lowered as much as possible, and when the reaction is gentle, the cock can be opened and the liquid level of the mixed liquid can be raised to the waste liquid discharge port. In consideration of diffusion of the generated gas in the gas-liquid separation container, it is desirable that the volume of the container above the liquid-liquid surface position is as small as possible. Since the intensity of the reaction changes depending on the concentration of the sample and the concentration of the reaction solution, it is necessary to prepare multiple gas-liquid separation containers with different volumes of the upper liquid mixture from the liquid surface position according to the degree of reaction. Although this is an extremely difficult method from the viewpoint of replacement, etc., in the present invention, the liquid level position of the mixed liquid can be freely changed by simply adjusting the cock. Can be adjusted. Thereby, gas and liquid can be efficiently separated in every reaction in one gas-liquid separation container.

  FIG. 5 shows an example of measurement using the present invention. This is a hydride gas generated by separating five arsenic compounds (trivalent arsenic, pentavalent arsenic, monomethylarsonic acid, dimethylarsinic acid, trimethylarsine oxide) using a separation column and using the gas-liquid separation container of the present invention. Is a chromatogram obtained when was introduced into an atomic absorption photometer. Since the sample introduction amount is as small as 100 μl, a small gas-liquid separation container is used. For this reason, the distance from the liquid surface position to the cock and the gas outlet is very short. However, the liquid level position of the liquid mixture was optimized by squeezing the cock and adjusted so that the liquid splash did not reach the cock and the outlet. If the present invention is not used, the liquid droplets obstruct the gas passage, so that the hydride gas, which is the target component, does not reach the detection device and cannot be measured.

  As described above, the present invention considers the following problems. For example, in measurement using a hydride generator that uses an atomic absorption spectrophotometer, ICP emission analyzer, ICP mass spectrometer, or atomic fluorescence analyzer as a detection means, a hydride gas is generated by mixing a reaction solution and a measurement sample. And hydrogen gas must be separated from the reaction solution. When the liquid droplets during the reaction flow to the gas discharge port of the gas-liquid separation container, it becomes difficult to introduce a stable gas, and the liquid and the gas cannot be separated efficiently. It is conceivable to use another gas-liquid separation container that is separated from the liquid surface position so that the liquid droplets do not reach the gas discharge port. However, the capacity of the gas-liquid separation container increases or the reaction becomes intense. Since it is necessary to replace the gas-liquid separation container according to the quality, it is disadvantageous in both the work surface and the measurement surface.

  In order to solve the above problem, for example, the present invention aims to efficiently separate the reaction liquid and the generated gas, and by providing an adjustment valve or the like in the gas discharge port of the gas-liquid separation container, Control the flow rate. The gas-liquid separation container is provided with an adjustment valve and the like, and the cross-sectional area of the tube through which the gas passes is adjusted. As a result, the pressure in the gas-liquid separation container changes and the liquid surface position of the liquid mixture is moved so as to return to a constant pressure. Thereby, since the distance to the discharge port can be optimized, it is possible to adjust to the liquid surface position where the liquid droplets do not reach and to perform efficient gas-liquid separation. Moreover, since only the adjustment valve is operated, the same gas-liquid separation container can be used even if the reaction intensity changes, and the volume in the container is adjusted at the position of the liquid mixture level. Therefore, an optimum capacity can be easily ensured even in a gas-liquid separation container having a small capacity. Further, the present invention is a gas-liquid separation container of a hydride generator using an atomic absorption spectrophotometer, an ICP emission analyzer, an ICP mass spectrometer, or an atomic fluorescence analyzer as a detection means. By adjusting the flow rate of the gas discharge port per unit time, by adjusting this, the pressure in the gas-liquid separation container is adjusted, and the liquid level position of the liquid mixture is optimized be able to. Moreover, stable gas can be induced to the detection device, and a highly accurate measurement result can be obtained.

It is a schematic diagram of a hydride generator using a general gas-liquid separation container. It is a figure of an example of the gas-liquid separation container used for the general hydride generator. It is a figure of the gas-liquid separation container (at the time of cock full open) provided with the cock for adjusting the liquid level position of a liquid mixture in order to implement this invention. It is a figure of the gas-liquid separation container (at the time of a cock half open) provided with the cock for adjusting the liquid level position of a liquid mixture in order to implement this invention. It is a figure of an example of the measurement result (chromatogram) obtained when this invention is applied.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Measurement sample 2,3 Reaction liquid 4,5,6 Pump 7 Mixer 8 Gas-liquid separation container 9 Detector 10,15,21 Mixture inlet 11,16,22 Waste liquid outlet 12,17,23 Mixed liquid Surface position 13, 18, 24 Gas exhaust port 14, 19, 25 Carrier gas inlet port 20, 26 Cock

Claims (7)

  A gas-liquid separation container used in an analysis system that combines a detection means and a hydride generator, and is a mixed liquid that is a boundary between a gas and a liquid when separating the gas and liquid generated by the hydride generator A gas-liquid separation container comprising adjusting means for adjusting the surface position.   2. The gas-liquid separation container according to claim 1, wherein the detection means is any one of an atomic absorption photometer, an ICP emission analyzer, an ICP mass spectrometer, and an atomic fluorescence analyzer.   2. The gas-liquid separation container according to claim 1, wherein the pressure in the container is changed by adjusting the cross-sectional area of the gas passage by the adjusting means, and the liquid level position of the mixed liquid is adjusted by the pressure level. .   2. The gas-liquid separation container according to claim 1, wherein the adjusting means is a cock provided in a flow path of the container.   2. The gas-liquid separation container according to claim 1, wherein the pressure in the container is changed by the adjusting means, and the liquid level position of the liquid mixture is adjusted by the pressure level.   2. The gas-liquid separation container according to claim 1, wherein the adjusting means is a regulator provided in a flow path of the container.   An analysis system combining the gas-liquid separation container according to claim 1, a detection means, and a hydride generator.

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