JP3764575B2 - Liquid vaporization reference gas generator - Google Patents

Liquid vaporization reference gas generator Download PDF

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Publication number
JP3764575B2
JP3764575B2 JP34230697A JP34230697A JP3764575B2 JP 3764575 B2 JP3764575 B2 JP 3764575B2 JP 34230697 A JP34230697 A JP 34230697A JP 34230697 A JP34230697 A JP 34230697A JP 3764575 B2 JP3764575 B2 JP 3764575B2
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Prior art keywords
gas
valve
container
liquid
gas container
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JPH11160207A (en
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司 佐竹
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Horiba Ltd
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Horiba Ltd
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Description

【０００１】
【発明の属する技術分野】
本発明は常温で液体の物質を気化させて基準濃度のガスを作成するための液体気化基準ガス発生装置に関する。
【０００２】
【従来の技術】
液体を気化させて既知濃度のガスを作成する方法としては、従来、例えば図４に示すようなバブリングによる方法がある。これは、気化すべき液体ａを入れたバブル管ｂを恒温槽ｃ内に貯留した水の中に浸漬させ、その気体導入管ｄからバランスガスを導入してこれを液体ａ中でバブリングさせることにより、バランスガスと共に気化した液体ａを吐出管ｅから取り出すようにしたものであり、液体ａの飽和蒸気圧分を含んだ基準ガスを作成する一般的な方法として知られている。
【０００３】
【発明が解決しようとする課題】
上述したような従来のバブリングによる方法では、バブル管ｂの温度が恒温水槽ｃによって安定化されるものの、気化すべき液体ａによっては、その気化潜熱により液体温度が変化するため、発生気体の濃度が安定しないことがある。発生気体の濃度を安定化するためには、バブル管ｂを多段に組み込んだ構成が採られることがあるが、例えばメタノール等においては、このような構成によっても濃度の不安定性を解消することはできなかった。
【０００４】
本発明はこのような実情に鑑みてなされ、常温で液体の物質を気化させて基準濃度のガスを高精度に作成することのできる液体気化基準ガス発生装置を提供することを目的としている。
【０００５】
【課題を解決するための手段】
本発明は上述の課題を解決するための手段を以下のように構成している。
すなわち、気化すべき液体を封入する液体容器内の空間部と第１開閉弁を介して接続されるガス容器と、このガス容器と第２開閉弁を介して接続される排気手段と、前記ガス容器に接続されるバランスガス導入ラインとを具備してなり、前記ガス容器内に前記液体容器において発生した蒸気を導入した後、前記ガス容器内における圧力に基づいて前記ガス容器内にバランスガスを導入し、所望の濃度を有するガスを発生させることを特徴としている。
【０００６】
排気手段を作動させた状態下で、まず、第１開閉弁と第２開閉弁を開いて液体容器内の空間部とガス容器内とを連通させ、液体蒸気でガス容器内の気体をパージする。次いで、その第１開閉弁を閉じて第２開閉弁を開き、ガス容器内を真空引きする。その後、第２開閉弁を閉じて第１開閉弁を開きガス容器内を液体の飽和蒸気で充満させる。そして、バランスガスを必要に応じてガス容器内に導入すれば所望の濃度のガスを作成できる。
【０００７】
なお、第１開閉弁を閉じて第２開閉弁を開いて所定の（減）圧力になるまでガス容器内を排気した後、第２開閉弁を閉じ、その後、第１開閉弁を開いて液体蒸気をガス容器内に導入するとともに、バランスガスを必要に応じてガス容器内に導入することによっても、所望の濃度のガスを作成することができる。また、第１開閉弁を開いて、所定の圧力に達するまでガス容器内に液体蒸気を導入した後、第１開閉弁を閉じ、バランスガスを必要に応じてガス容器内に導入してもよい。
【０００８】
【発明の実施の形態】
以下に本発明の液体気化基準ガス発生装置の実施形態を図面に基づいて詳細に説明する。
図１は装置の全体構成を示し、符号１は気化すべき液体（例えばメタノール），２はその液体１を封入した液体容器，３は圧力計，４はガス容器，５は圧力計，６はガス容器４と液体容器２内の空間部７とを連通する連通管、８はバランスガスをガス容器４に導入するための導入管，９は排気管，１０は吸引ポンプ（排気手段），１１〜１３は電磁開閉弁，１４はニードルバルブであり、各電磁開閉弁１１〜１３および吸引ポンプ１０はコントローラ（図示省略）と接続され、予め設定・記憶された制御プログラムに従って制御駆動される。なお、上述の電磁開閉弁１１が本発明でいう第１開閉弁，電磁開閉弁１３が第２開閉弁である。
【０００９】
上述のような構成にて、例えば、図２および図３に示すようなフローで所望濃度の基準ガス（校正ガス）を得ることができる。以下、順を追って説明すると、まず、吸引ポンプ１０を起動させ（ステップＳ１）、次いで、第１開閉弁１１と第２開閉弁１３をオン操作し（ステップＳ２）、液体容器２の空間部７とガス容器４とを連通させ、圧力計５の指示値が圧力計３の指示値と等しくなるまで（ステップＳ３）、液体１の蒸気でガス容器４内の気体をパージする。
【００１０】
圧力計５の指示値が圧力計３の指示値と等しくなると、第１開閉弁１１をオフし（ステップＳ４）、ガス容器４内を真空引きする。圧力計５の指示値が０（真空）になると（ステップＳ５）第２開閉弁１３をオフし（ステップＳ６）、次いで、第１開閉弁１１をオンし（ステップＳ７）、圧力計５の指示値が圧力計３の指示値（＝ＰL ）と等しくなるまで（ステップＳ８）液体容器２内の空間部７とガス容器４とを連通させて、ガス容器４内を液体１の飽和蒸気で充満させ、その圧力計３の指示値ＰL をコントローラに一時記憶させておく。
【００１１】
圧力計５の指示値が圧力計３の指示値と等しくなると、第１開閉弁１１をオフし（ステップＳ９）、また、電磁開閉弁１２をオンすることにより（ステップＳ１０）、バランスガス（例えばＮ2 ）をガス容器４内に導入する。その間、圧力計５で計測されるガス容器４内の圧力ＰT は、ＰT ＝ＰL ＋ＰB （バランスガスの圧力）の関係式を満たし、その濃度ＤT ＝ＰL ／ＰT となる。従って、所望の濃度値（＝ＤTD）を得るためには、圧力計５の指示値ＰT ＝ＰL ／ＤTDの関係式が満たされるまで電磁開閉弁１２を開いておけばよい（Ｓ１１）。所望の濃度値が得られた後は電磁開閉弁１２を閉じ（ステップＳ１２）、かつ、吸引ポンプ１０を停止させる（ステップＳ１３）。
【００１２】
上述の所望の濃度値（＝ＤTD）は予めコントローラに設定しておくことにより、ステップＳ１〜Ｓ１３が順次自動的に行われ、ガス容器４内に所望濃度のガスを温度変化等の影響を受けることなく安定な状態で得ることができ、特に、濃度の不安定なメタノール等であっても基準ガスの作成が容易となる。なお、圧力計３を設けない場合には、ステップＳ３およびステップＳ８にて、圧力計５の指示値が予め設定した適切な値になった時点にて第１開閉弁１１をオフにすればよい。
【００１３】
また、上述のフローとは別に、第１開閉弁１１を閉じて第２開閉弁１３を開き、所定の（減）圧力になるまでガス容器４内を排気した後、第２開閉弁１３を閉じ、その後、第１開閉弁１１を開いて蒸気をガス容器４内に導入するとともに、バランスガスを必要に応じてガス容器４内に導入するようにしてもよく、あるいは、第１開閉弁１１を開き、所定の圧力に達するまでガス容器４内に蒸気を導入した後、第１開閉弁１１を閉じ、バランスガスを必要に応じてガス容器４内に導入するようにしてもよい。
【００１４】
【発明の効果】
以上説明したように、本発明の液体気化基準ガス発生装置は、気化すべき液体を封入する液体容器内の空間部と第１開閉弁を介して接続されるガス容器と、このガス容器と第２開閉弁を介して接続される排気手段と、前記ガス容器に接続されるバランスガス導入ラインとを具備してなり、前記ガス容器内に前記液体容器において発生した蒸気を導入した後、前記ガス容器内における圧力に基づいて前記ガス容器内にバランスガスを導入し、所望の濃度を有するガスを発生させるようにした点に特徴があり、液体の飽和蒸気をガス容器内に封じ込め、その後、バランスガスとの分圧により濃度を決定するようにしたので、温度変化に依存することなく、濃度安定性が良好となり、所望濃度のガスを容易かつ確実に得ることができる。
【図面の簡単な説明】
【図１】 本発明の液体気化基準ガス発生装置の一実施形態を示す構成図である。
【図２】 前記装置の制御作動を説明するためのフローチャートの前半部である。
【図３】 前記フローチャートの後半部である。
【図４】 従来の液体気化装置の一例を示す構成図である。
【符号の説明】
１…液体、２…液体容器、４…ガス容器、７…空間部、８…バランスガス導入ライン，１０…排気手段，１１…第２開閉弁，１３…第２開閉弁。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a liquid vaporization reference gas generator for producing a gas having a reference concentration by vaporizing a liquid substance at room temperature.
[0002]
[Prior art]
As a method of creating a gas having a known concentration by vaporizing a liquid, there is a conventional method by bubbling as shown in FIG. This involves immersing the bubble tube b containing the liquid a to be vaporized in the water stored in the thermostatic chamber c, introducing a balance gas from the gas introduction tube d, and bubbling it in the liquid a. Thus, the liquid a vaporized together with the balance gas is taken out from the discharge pipe e, and is known as a general method for creating a reference gas containing the saturated vapor pressure of the liquid a.
[0003]
[Problems to be solved by the invention]
In the conventional bubbling method as described above, the temperature of the bubble tube b is stabilized by the constant temperature water tank c. However, depending on the liquid a to be vaporized, the liquid temperature changes due to the latent heat of vaporization. May not be stable. In order to stabilize the concentration of the generated gas, a configuration in which bubble tubes b are incorporated in multiple stages may be employed. For example, in methanol or the like, concentration instability can be eliminated even with such a configuration. could not.
[0004]
The present invention has been made in view of such circumstances, and an object of the present invention is to provide a liquid vaporization reference gas generation apparatus capable of vaporizing a liquid substance at room temperature to create a reference concentration gas with high accuracy.
[0005]
[Means for Solving the Problems]
In the present invention, means for solving the above-described problems are configured as follows.
That is, the gas container being connected via a space part and the first on-off valve in the liquid material container you enclosing the liquid to be vaporized, and evacuation means are connected through the gas container and the second on-off valve, wherein Ri Na and and a balance gas introduction line connected to a gas container, after introducing the steam generated in the liquid container to the gas container, the gas container based on the pressure in the gas container introducing a balance gas, it is characterized in Rukoto to generate a gas having a desired concentration.
[0006]
In a state where the exhaust means is operated, first, the first on-off valve and the second on-off valve are opened to connect the space in the liquid container and the gas container, and the gas in the gas container is purged with liquid vapor. . Next, the first on-off valve is closed, the second on-off valve is opened, and the gas container is evacuated. Thereafter, the second on-off valve is closed, the first on-off valve is opened, and the gas container is filled with liquid saturated vapor. If a balance gas is introduced into the gas container as necessary, a gas having a desired concentration can be created.
[0007]
After closing the first on-off valve and opening the second on-off valve to evacuate the gas container until a predetermined (reduced) pressure is reached, the second on-off valve is closed, and then the first on-off valve is opened and the liquid is opened. By introducing the vapor into the gas container and introducing the balance gas into the gas container as required, a gas having a desired concentration can be produced. Further, after opening the first on-off valve and introducing the liquid vapor into the gas container until a predetermined pressure is reached, the first on-off valve may be closed and the balance gas may be introduced into the gas container as necessary. .
[0008]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of a liquid vaporization reference gas generator according to the present invention will be described below in detail with reference to the drawings.
FIG. 1 shows the overall configuration of the apparatus. Reference numeral 1 is a liquid to be vaporized (for example, methanol), 2 is a liquid container containing the liquid 1, 3 is a pressure gauge, 4 is a gas container, 5 is a pressure gauge, and 6 is A communication pipe for communicating the gas container 4 and the space 7 in the liquid container 2, 8 is an introduction pipe for introducing balance gas into the gas container 4, 9 is an exhaust pipe, 10 is a suction pump (exhaust means), 11 -13 are electromagnetic on-off valves and 14 is a needle valve. The electromagnetic on-off valves 11-13 and the suction pump 10 are connected to a controller (not shown), and are controlled and driven according to a control program set and stored in advance. The electromagnetic on-off valve 11 is a first on-off valve and the electromagnetic on-off valve 13 is a second on-off valve in the present invention.
[0009]
With the configuration as described above, for example, a reference gas (calibration gas) having a desired concentration can be obtained by the flow shown in FIGS. Hereinafter, the description will be made in order. First, the suction pump 10 is started ( step S1), then the first on- off valve 11 and the second on-off valve 13 are turned on ( step S2), and the space portion 7 of the liquid container 2 is turned on. And the gas container 4 are communicated, and the gas in the gas container 4 is purged with the vapor of the liquid 1 until the indicated value of the pressure gauge 5 becomes equal to the indicated value of the pressure gauge 3 ( step S3).
[0010]
When the indicated value of the pressure gauge 5 becomes equal to the indicated value of the pressure gauge 3, the first on- off valve 11 is turned off ( step S4), and the gas container 4 is evacuated. When the indicated value of the pressure gauge 5 becomes 0 (vacuum) ( step S5), the second on- off valve 13 is turned off ( step S6), and then the first on- off valve 11 is turned on ( step S7). Until the value becomes equal to the indicated value (= P L ) of the pressure gauge 3 ( step S8), the space 7 in the liquid container 2 and the gas container 4 are communicated, and the gas container 4 is filled with saturated vapor of the liquid 1 It is filled and allowed temporarily stored in the controller and the pressure gauge 3 indicated value P L.
[0011]
When the indicated value of the pressure gauge 5 becomes equal to the indicated value of the pressure gauge 3, the first on- off valve 11 is turned off ( step S9), and the electromagnetic on-off valve 12 is turned on ( step S10), whereby a balance gas (for example, N 2 ) is introduced into the gas container 4. Meanwhile, the pressure P T in the gas container 4 measured by the pressure gauge 5 satisfies the relational expression P T = P L + P B (balance gas pressure), and the concentration is D T = P L / P T. . Therefore, in order to obtain a desired concentration value (= D TD ), the electromagnetic on-off valve 12 should be opened until the relational expression P T = P L / D TD of the pressure gauge 5 is satisfied (S11). ). After the desired concentration value is obtained, the electromagnetic on-off valve 12 is closed ( step S12), and the suction pump 10 is stopped ( step S13).
[0012]
By setting the desired concentration value (= D TD ) in the controller in advance, steps S1 to S13 are automatically performed sequentially, and the gas having the desired concentration in the gas container 4 is influenced by temperature change or the like. In particular, it is easy to create a reference gas even for methanol or the like having an unstable concentration. Incidentally, in the case without the pressure gauge 3, at steps S3 and S8, it is sufficient to turn off the first on-off valve 11 at the time when the instruction value of the pressure gauge 5 is in the proper preset value .
[0013]
In addition to the above-described flow, the first on- off valve 11 is closed and the second on- off valve 13 is opened. After the gas container 4 is exhausted to a predetermined (reduced) pressure, the second on- off valve 13 is closed. Thereafter, the first on-off valve 11 may be opened to introduce steam into the gas container 4, and the balance gas may be introduced into the gas container 4 as necessary. Alternatively, the first on- off valve 11 may be open, after introducing the steam into the gas container 4 to reach a predetermined pressure, closing the first on-off valve 11 may be a balanced gas, if necessary, be introduced into the gas container 4.
[0014]
【The invention's effect】
As described above, the liquid vaporized reference gas generator of the present invention, a gas container connected via the space portion and the first on-off valve of the liquid body in the container you enclosing the liquid to be vaporized, the gas container When an exhaust means connected via a second on-off valve, wherein Ri Na and and a balance gas introduction line connected to a gas container, after introducing the steam generated in the liquid container to the gas container , Characterized in that a balance gas is introduced into the gas container based on the pressure in the gas container to generate a gas having a desired concentration, and a liquid saturated vapor is contained in the gas container, then, since so as to determine the concentration by partial pressures of the balance gas, without depending on the temperature change, density stability is improved, can be obtained easily and ensure the desired concentration of the gas.
[Brief description of the drawings]
FIG. 1 is a configuration diagram showing an embodiment of a liquid vaporization reference gas generation device of the present invention.
2 is a first half of a flowchart for explaining the control operation of the device.
3 is a second half of the flowchart.
FIG. 4 is a configuration diagram showing an example of a conventional liquid vaporizer.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Liquid, 2 ... Liquid container, 4 ... Gas container, 7 ... Space part, 8 ... Balance gas introduction line, 10 ... Exhaust means, 11 ... 2nd on-off valve, 13 ... 2nd on-off valve.

Claims (2)

気化すべき液体を封入する液体容器内の空間部と第１開閉弁を介して接続されるガス容器と、このガス容器と第２開閉弁を介して接続される排気手段と、前記ガス容器に接続されるバランスガス導入ラインとを具備してなり、前記ガス容器内に前記液体容器において発生した蒸気を導入した後、前記ガス容器内における圧力に基づいて前記ガス容器内にバランスガスを導入し、所望の濃度を有するガスを発生させることを特徴とする液体気化基準ガス発生装置。A gas container which is connected via the space portion and the first on-off valve of the liquid body in the container you enclosing the liquid to be vaporized, and evacuation means are connected through the gas container and the second on-off valve, the gas Ri Na and and a balance gas introduction line connected to a container, after introducing the steam generated in the liquid container to the gas container, the balance gas into the gas container based on the pressure in the gas container introducing a liquid vaporized reference gas generating device according to claim Rukoto to generate a gas having a desired concentration. 前記バランスガス導入ラインに開閉弁を具備してなり、前記第１開閉弁を閉じる一方、前記第２開閉弁を開き、バランスガス導入ラインに設けられた開閉弁を閉じて、前記排気手段によって前記ガス容器内を排気した後、第２開閉弁を閉じ、第１開閉弁を開いて、前記ガス容器内に前記液体容器において発生した蒸気を導入し、しかる後に、第１開閉弁を閉じ、バランスガス導入ラインに設けられた開閉弁を開いて、前記ガス容器内における圧力に基づいて前記ガス容器内にバランスガスを導入することにより、所望の濃度を有するガスを発生させる請求項１に記載の液体気化基準ガス発生装置。The balance gas introduction line is provided with an on-off valve, the first on-off valve is closed, the second on-off valve is opened, the on-off valve provided in the balance gas introduction line is closed, and the exhaust means After evacuating the gas container, the second on-off valve is closed, the first on-off valve is opened, the steam generated in the liquid container is introduced into the gas container, and then the first on-off valve is closed to balance. The gas according to claim 1, wherein a gas having a desired concentration is generated by opening an on-off valve provided in a gas introduction line and introducing a balance gas into the gas container based on a pressure in the gas container. Liquid vaporization reference gas generator.
JP34230697A 1997-11-26 1997-11-26 Liquid vaporization reference gas generator Expired - Fee Related JP3764575B2 (en)

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JP3764575B2 true JP3764575B2 (en) 2006-04-12

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