JP2013170934A - Total organic carbon meter - Google Patents

Total organic carbon meter Download PDF

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JP2013170934A
JP2013170934A JP2012035102A JP2012035102A JP2013170934A JP 2013170934 A JP2013170934 A JP 2013170934A JP 2012035102 A JP2012035102 A JP 2012035102A JP 2012035102 A JP2012035102 A JP 2012035102A JP 2013170934 A JP2013170934 A JP 2013170934A
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sample introduction
sample
rod
opening
cover
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JP5811887B2 (en
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Kenji Iharada
健志 居原田
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Shimadzu Corp
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Shimadzu Corp
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Abstract

PROBLEM TO BE SOLVED: To provide a total organic carbon meter in which an opening can be closed when a sample is disposed.SOLUTION: In a total organic carbon meter, a sample tray 6 on which a sample is placed is disposed within a sample introduction mechanism 10 linked to one end portion of a combustion pipe 1 and then moved by a sample introduction rod 7 in a preset direction from the one end portion to another end portion of the combustion pipe 1 so as to be disposed within a central portion of the combustion pipe 1 to be the inside of a combustion furnace 2, and organic substances in the sample are combusted. The sample introduction mechanism 10 includes a case part 3 in which a sample introduction and rod opening 3d is formed, the sample introduction rod 7 in which the sample tray 6 is placed in the distal end portion thereof and which is inserted from the sample introduction and rod opening 3d in the preset direction, and a cover 4 which is formed on an outer circumferential surface of the sample introduction rod 7. The sample introduction rod 7 in which the sample tray 6 is placed in the distal end portion thereof is inserted from the sample introduction and rod opening 3d, such that a gap between the sample introduction and rod opening 3d and the sample introduction rod 7 is closed with the cover 4.

Description

本発明は、土壌・堆積物・農畜産物等の固体試料や、河川水・湖沼水・海水・雨水・地下水等の液体試料等の試料中の炭素分を測定する全有機炭素計に関する。   The present invention relates to a total organic carbon meter that measures the carbon content in solid samples such as soil, sediment, agricultural and livestock products, and liquid samples such as river water, lake water, seawater, rainwater, and groundwater.

近年、公害調査等のため、上下水道水、各種プラント用水、河川等の水中に含まれる有機炭素濃度の計測が重要な項目の一つとなっている。このような有機炭素濃度の計測には全有機炭素計（ＴＯＣ計）が用いられている。
さらに、ＴＯＣ測定の要求は固体試料にも広まり、固体試料測定用ＴＯＣ計は、一定量の固体試料をセラミック製試料皿に載置して、試料皿ごと石英ガラス製燃焼管の内部に挿入することにより、固体試料中の有機物を燃焼（酸化反応）させ、発生した二酸化炭素を赤外線検出器で測定している。 In recent years, measurement of organic carbon concentration in water such as water and sewage water, water for various plants, and rivers has become one of the important items for pollution investigations. A total organic carbon meter (TOC meter) is used for measuring the organic carbon concentration.
Furthermore, the demand for TOC measurement also spreads to solid samples, and a solid sample measuring TOC meter places a certain amount of solid sample on a ceramic sample pan and inserts the sample pan into the quartz glass combustion tube. Thus, the organic matter in the solid sample is burned (oxidation reaction), and the generated carbon dioxide is measured with an infrared detector.

このようなＴＯＣ計では、燃焼管１は、内部に挿入された試料皿６が加熱されるように、９００℃程度に加熱されている燃焼反応用筒型電気炉（燃焼炉）２の内部に水平方向に配置されている（図５及び図６参照）。また、燃焼管１の内部を一定方向（例えば、右から左へ）にキャリアガス（例えば、純度９９．９９重量％の酸素ガス）が流通するように、燃焼管１の一端部（右部）にキャリアガス入口１１が形成されている。そして、燃焼管１の他端部（左部）には、酸化触媒５が充填されており、固体試料から発生した炭素分等はキャリアガスとともに酸化触媒層５に達し、酸化触媒５により酸化されて二酸化炭素となる。
なお、燃焼管１の他端部（左部）には、ドレンセパレータを経由して非分散形赤外線ガス分析計（ＮＤＩＲ）に接続されており、燃焼管１からの二酸化炭素ガスとキャリアガスとはＮＤＩＲへ導かれて固体試料中の炭素分が検出されることになる（例えば、特許文献１参照）。 In such a TOC meter, the combustion tube 1 is placed in the interior of a combustion reaction cylindrical electric furnace (combustion furnace) 2 heated to about 900 ° C. so that the sample pan 6 inserted therein is heated. They are arranged in the horizontal direction (see FIGS. 5 and 6). Also, one end (right part) of the combustion pipe 1 so that a carrier gas (for example, oxygen gas having a purity of 99.99 wt%) flows through the inside of the combustion pipe 1 in a certain direction (for example, from right to left). A carrier gas inlet 11 is formed in the front. The other end portion (left portion) of the combustion tube 1 is filled with an oxidation catalyst 5, and carbon and the like generated from the solid sample reach the oxidation catalyst layer 5 together with the carrier gas and are oxidized by the oxidation catalyst 5. To carbon dioxide.
The other end (left part) of the combustion tube 1 is connected to a non-dispersive infrared gas analyzer (NDIR) via a drain separator, and carbon dioxide gas and carrier gas from the combustion tube 1 Is guided to NDIR to detect the carbon content in the solid sample (see, for example, Patent Document 1).

このようなＴＯＣ計を用いて、測定者が一の固体試料が載置された試料皿６から次の固体試料が載置された試料皿６への交換を行うためには、交換作業場所の温度を低くする必要があるため、電気炉２の外部に所定の距離で突出するよう燃焼管１の一端部（右部）を形成した上で、燃焼管１の一端部（右部）に試料導入ポート部（試料導入機構）を連結している。そして、試料導入ポート部から燃焼管１の一端部の内部に配置した試料皿６を、測定者は試料導入ロッド１７を押し込むことで設定方向（例えば、右から左へ）に移動させることにより、燃焼管１の中央部の内部に配置している。   Using such a TOC meter, in order for the measurer to exchange from the sample pan 6 on which one solid sample is placed to the sample pan 6 on which the next solid sample is placed, Since it is necessary to lower the temperature, after forming one end portion (right portion) of the combustion tube 1 so as to protrude outside the electric furnace 2 at a predetermined distance, a sample is formed on one end portion (right portion) of the combustion tube 1. The introduction port part (sample introduction mechanism) is connected. Then, the measurer moves the sample pan 6 arranged inside the one end portion of the combustion tube 1 from the sample introduction port portion in a setting direction (for example, from right to left) by pushing the sample introduction rod 17. Arranged inside the center of the combustion tube 1.

ここで、図５は、従来のＴＯＣ計の試料導入ポート部の一例の概略構成図である。
試料導入ポート部２０は、上壁部に試料導入用開口部１３ｃと右壁部に円形状（例えば直径６ｍｍ）のロッド用開口部１３ｄと、下壁部にガス導入用開口部１３ｅとが形成された円筒形状のケース部１３と、試料導入用開口部１３ｃに配置されるカバー１４と、設定方向でロッド用開口部１３ｄからＯリング１３ａを介して挿入される試料導入ロッド１７と、ガス導入用開口部１３ｅに連結されたキャリアガス入口１１とを備える。 Here, FIG. 5 is a schematic configuration diagram of an example of a sample introduction port portion of a conventional TOC meter.
The sample introduction port portion 20 is formed with a sample introduction opening 13c in the upper wall portion, a circular rod opening portion 13d (for example, 6 mm in diameter) in the right wall portion, and a gas introduction opening portion 13e in the lower wall portion. A cylindrical case portion 13 formed, a cover 14 disposed in the sample introduction opening 13c, a sample introduction rod 17 inserted from the rod opening 13d through the O-ring 13a in the setting direction, and a gas introduction And a carrier gas inlet 11 connected to the opening 13e.

試料導入ロッド１７は、ステンレス製であって直径６ｍｍの円柱形状をしており、その先端部に試料皿６が載置されるようになっているとともに、後端部に操作ツマミが形成されている。
カバー１４は、ネジの回転によって上下方向に数ｍｍ動くようになっており、下方位置に位置したときには、上壁部の試料導入用開口部１３ｃの周辺部と密着することで、ケース部１３の内部の気密を確保し、一方、上方位置に位置したときには、水平方向にスライドさせることで、ケース部１３の内部が開放されるようになっている。 The sample introduction rod 17 is made of stainless steel and has a cylindrical shape with a diameter of 6 mm. The sample pan 6 is placed on the front end portion thereof, and an operation knob is formed on the rear end portion. Yes.
The cover 14 moves several millimeters in the vertical direction by the rotation of the screw. When the cover 14 is positioned at the lower position, the cover 14 is brought into close contact with the peripheral portion of the sample introduction opening 13c on the upper wall portion. When the airtightness of the inside is ensured, on the other hand, when located at the upper position, the inside of the case portion 13 is opened by sliding in the horizontal direction.

そして、燃焼管１の中央部の内部に配置された固体試料を分析する際には、キャリアガス入口１１からケース部１３の内部に５００ｍｌ／ｍｉｎでキャリアガスが導かれ、燃焼管１の内部を設定方向（例えば、右から左へ）にキャリアガスが５００ｍｌ／ｍｉｎで流通するようになっている。   And when analyzing the solid sample arrange | positioned inside the center part of the combustion pipe 1, carrier gas is guide | induced to the inside of the case part 13 from the carrier gas inlet 11 at 500 ml / min, and the inside of the combustion pipe 1 is carried out. The carrier gas is circulated at a rate of 500 ml / min in the setting direction (for example, from right to left).

このような試料導入ポート部２０によれば、測定者はネジ上端のツマミを手で回転させることによってカバー１４を上方位置に位置させ、カバー１４を手で水平方向にスライドさせた後、試料導入用開口部１３ｃからケース部１３の内部にある試料導入ロッド１７の先端部に試料皿６を配置する。そして、測定者はカバー１４を手で水平方向にスライドさせてネジ上端のツマミを手で回転させることによって、カバー１４を下方位置に位置させる。次に、測定者は試料導入ロッド１７を設定方向に手で押し込んで移動させることにより、試料皿６を燃焼管１内部の中央部に配置する。   According to such a sample introduction port section 20, the measurer manually positions the cover 14 by rotating the knob at the upper end of the screw, slides the cover 14 in the horizontal direction, and then introduces the sample. The sample pan 6 is disposed from the opening 13c to the tip of the sample introduction rod 17 inside the case portion 13. Then, the measurer slides the cover 14 in the horizontal direction by hand and rotates the knob at the upper end of the screw by hand to position the cover 14 in the lower position. Next, the measurer pushes the sample introduction rod 17 by hand in the setting direction and moves it to place the sample dish 6 in the center of the combustion tube 1.

また、図６は、従来のＴＯＣ計の試料導入ポート部の他の一例の概略構成図である。なお、上述した試料導入ポート部２０と同様のものについては、同じ符号を付している。
試料導入ポート部３０は、右壁部に円形状（例えば直径３０ｍｍ）の試料導入兼ロッド用開口部２３ｄと、下壁部にガス導入用開口部２３ｅとが形成された円筒形状のケース部２３と、設定方向で試料導入兼ロッド用開口部２３ｄから挿入される試料導入ロッド１７と、ガス導入用開口部２３ｅに連結されたキャリアガス入口１１とを備える。 FIG. 6 is a schematic configuration diagram of another example of a sample introduction port portion of a conventional TOC meter. In addition, the same code | symbol is attached | subjected about the thing similar to the sample introduction port part 20 mentioned above.
The sample introduction port part 30 is a cylindrical case part 23 in which a circular (for example, diameter of 30 mm) sample introduction / rod opening 23d is formed on the right wall and a gas introduction opening 23e is formed on the lower wall. And a sample introduction rod 17 inserted from the sample introduction / rod opening 23d in the set direction, and a carrier gas inlet 11 connected to the gas introduction opening 23e.

燃焼管１の他端部（左部）には、５００ｍｌ／ｍｉｎで吸引する定流量ポンプ３１が接続されている。
そして、燃焼管１の中央部の内部に配置された固体試料を分析する際には、キャリアガス入口１１からケース部２３の内部に１０００ｍｌ／ｍｉｎでキャリアガスが導かれ、燃焼管１の内部を設定方向（例えば、右から左へ）にキャリアガスが５００ｍｌ／ｍｉｎで定流量ポンプ３１によって流通するとともに、定流量ポンプ３１に吸引される流量を超えた量のキャリアガスが、試料導入兼ロッド用開口部２３ｄと試料導入ロッド１７との隙間から排出されるようになっている。これにより、空気が燃焼管１の内部に侵入することを防いでいる。 A constant flow rate pump 31 that sucks at 500 ml / min is connected to the other end portion (left portion) of the combustion tube 1.
And when analyzing the solid sample arrange | positioned inside the center part of the combustion pipe 1, carrier gas is guide | induced to the inside of the case part 23 from the carrier gas inlet 11 at 1000 ml / min, and the inside of the combustion pipe 1 is carried out. The carrier gas is circulated by the constant flow pump 31 at a rate of 500 ml / min in the setting direction (for example, from right to left), and the amount of carrier gas that exceeds the flow rate sucked by the constant flow pump 31 is for the sample introduction and rod. The gas is discharged from the gap between the opening 23d and the sample introduction rod 17. This prevents air from entering the combustion pipe 1.

このような試料導入ポート部３０によれば、測定者は試料導入ロッド１７の先端部に試料皿６を配置した後、ケース部２３の内部に試料導入兼ロッド用開口部２３ｄから試料導入ロッド１７を手で挿入する。次に、測定者は試料導入ロッド１７を設定方向に手で押し込んで移動させることにより、試料皿６を燃焼管１内部の中央部に配置する。   According to such a sample introduction port portion 30, the measurer places the sample dish 6 at the tip of the sample introduction rod 17, and then the sample introduction rod 17 from the sample introduction / rod opening 23 d inside the case portion 23. Insert by hand. Next, the measurer pushes the sample introduction rod 17 by hand in the setting direction and moves it to place the sample dish 6 in the center of the combustion tube 1.

特開平５−５２８３７号公報JP-A-5-52837

しかしながら、上述したような試料導入ポート部２０では、試料皿６を配置するための試料導入用開口部１３ｃを手動で開放したり閉鎖したりするカバー構造が必要であり、さらにケース部１３の内部に試料皿６を配置するまでの操作手順が多くなるという問題点があった。
また、上述したような試料導入ポート部３０では、燃焼管１の内部を設定方向にキャリアガスが５００ｍｌ／ｍｉｎで流通するように定流量ポンプ３１が必要であり、さらにキャリアガスの無駄が多くなるという問題点があった。
そこで、本発明は、試料を配置すると開口部を閉鎖することができる全有機炭素計を提供することを目的とする。 However, in the sample introduction port portion 20 as described above, a cover structure for manually opening and closing the sample introduction opening 13c for arranging the sample dish 6 is required. There is a problem that the operation procedure until the sample pan 6 is arranged increases.
Further, in the sample introduction port portion 30 as described above, the constant flow pump 31 is necessary so that the carrier gas flows through the inside of the combustion tube 1 in the set direction at 500 ml / min, and the waste of the carrier gas is increased. There was a problem.
Then, an object of this invention is to provide the total organic carbon meter which can close an opening part, if a sample is arrange | positioned.

上記課題を解決するためになされた本発明の全有機炭素計は、試料を載置した試料皿が、燃焼管の一端部に連結された試料導入機構の内部に配置された後、前記燃焼管の一端部から他端部へ向かう設定方向に試料導入ロッドによって移動することにより、燃焼炉の内部となる前記燃焼管の中央部の内部に配置され、当該試料中の有機物が燃焼する全有機炭素計であって、前記試料導入機構は、試料導入兼ロッド用開口部が形成されたケース部と、先端部に試料皿が載置され、前記設定方向で試料導入兼ロッド用開口部から挿入される試料導入ロッドと、前記試料導入ロッドの外周面に形成されたカバーとを備え、先端部に試料皿が載置された試料導入ロッドが試料導入兼ロッド用開口部から挿入されることにより、前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぐようにしている。   The total organic carbon meter of the present invention, which has been made to solve the above-mentioned problems, is configured such that after a sample pan on which a sample is placed is placed inside a sample introduction mechanism connected to one end of the combustion tube, the combustion tube Is moved by a sample introduction rod in a setting direction from one end of the sample to the other end, so that it is arranged inside the center of the combustion tube, which is the inside of the combustion furnace, and the total organic carbon in which the organic matter in the sample burns The sample introduction mechanism includes a case portion in which a sample introduction / rod opening is formed, and a sample pan placed on the tip, and is inserted from the sample introduction / rod opening in the setting direction. A sample introduction rod, and a cover formed on the outer peripheral surface of the sample introduction rod, and a sample introduction rod having a sample tray placed on the tip is inserted from the opening for sample introduction and rod, Sample introduction and rod opening Part and a gap between the sample introduction rod and so as to close a cover.

以上のように、本発明の全有機炭素計によれば、開口部を手動で開放したり閉鎖したりするカバー構造や定流量ポンプが必要でなくなる。また、キャリアガスの無駄も少なくなる。さらに、ケース部の内部に試料皿を配置するまでの操作手順が容易となる。   As described above, according to the total organic carbon meter of the present invention, a cover structure and a constant flow pump for manually opening and closing the opening are not necessary. Further, the waste of carrier gas is reduced. Furthermore, the operation procedure until the sample dish is arranged inside the case part becomes easy.

（他の課題を解決するための手段及び効果）
また、上記の発明において、前記カバーは、前記試料導入ロッドの外周面で設定方向と逆方向に移動可能に形成され、先端部に試料皿が載置された試料導入ロッドが試料導入兼ロッド用開口部から挿入されて、前記燃焼管の一端部の内部に試料皿が配置されたときには、前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぎ、前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぎながら、前記試料導入ロッドが設定方向に挿入されていくことにより、前記試料皿が燃焼管の中央部の内部に配置されるようにしてもよい。
さらに、上記の発明において、前記試料導入ロッドに対して前記カバーが設定方向に動くように作用する弾性体が、前記試料導入ロッドに取付けられているようにしてもよい。 (Means and effects for solving other problems)
In the above invention, the cover is formed on the outer peripheral surface of the sample introduction rod so as to be movable in the direction opposite to the setting direction, and the sample introduction rod having the sample dish placed on the tip is used for the sample introduction and rod. When the sample dish is placed inside the one end of the combustion tube after being inserted from the opening, the gap between the sample introduction / rod opening and the sample introduction rod is closed with a cover, and the sample introduction / rod The sample pan is placed in the center of the combustion tube by inserting the sample introduction rod in the setting direction while closing the gap between the opening for sample and the sample introduction rod with a cover. Also good.
Furthermore, in the above invention, an elastic body that acts so that the cover moves in a setting direction with respect to the sample introduction rod may be attached to the sample introduction rod.

本発明に係るＴＯＣ計の試料導入ロッドの一例の概略構成図。The schematic block diagram of an example of the sample introduction rod of the TOC meter which concerns on this invention. 本発明に係るＴＯＣ計の試料導入ポート部の一例の概略構成図。The schematic block diagram of an example of the sample introduction port part of the TOC meter which concerns on this invention. 本発明に係るＴＯＣ計の試料導入ポート部の一例の概略構成図。The schematic block diagram of an example of the sample introduction port part of the TOC meter which concerns on this invention. 本発明に係るＴＯＣ計の試料導入ポート部の一例の概略構成図。The schematic block diagram of an example of the sample introduction port part of the TOC meter which concerns on this invention. 従来のＴＯＣ計の試料導入ポート部の一例の概略構成図。The schematic block diagram of an example of the sample introduction port part of the conventional TOC meter. 従来のＴＯＣ計の試料導入ポート部の他の一例の概略構成図。The schematic block diagram of another example of the sample introduction port part of the conventional TOC meter.

以下、本発明の実施形態について図面を用いて説明する。なお、本発明は、以下に説明するような実施形態に限定されるものではなく、本発明の趣旨を逸脱しない範囲で種々の態様が含まれることはいうまでもない。   Hereinafter, embodiments of the present invention will be described with reference to the drawings. Note that the present invention is not limited to the embodiments described below, and it goes without saying that various aspects are included without departing from the spirit of the present invention.

図１は、本発明に係るＴＯＣ計の試料導入ロッドの一例の概略構成図であり、図２〜図４は、本発明に係るＴＯＣ計の試料導入ポート部の一例の概略構成図である。なお、上述した試料導入ポート部３０と同様のものについては、同じ符号を付している。
試料導入ポート部１０は、右壁部に円形状（例えば直径２０ｍｍ）の試料導入兼ロッド用開口部３ｄと下壁部にガス導入用開口部３ｅとが形成された円筒形状のケース部３と、設定方向で試料導入兼ロッド用開口部３ｄから挿入される試料導入ロッド７と、ガス導入用開口部３ｅに連結されたキャリアガス入口１１とを備える。 FIG. 1 is a schematic configuration diagram of an example of a sample introduction rod of a TOC meter according to the present invention, and FIGS. 2 to 4 are schematic configuration diagrams of an example of a sample introduction port portion of the TOC meter according to the present invention. In addition, the same code | symbol is attached | subjected about the thing similar to the sample introduction port part 30 mentioned above.
The sample introduction port portion 10 includes a cylindrical case portion 3 having a circular (for example, 20 mm diameter) sample introduction / rod opening 3d on the right wall portion and a gas introduction opening 3e formed on the lower wall portion. The sample introduction rod 7 inserted from the sample introduction / rod opening 3d in the set direction and the carrier gas inlet 11 connected to the gas introduction opening 3e are provided.

試料導入ロッド７は、ステンレス製であって直径６ｍｍの円柱形状をしており、その先端部に試料皿６が載置されるようになっているとともに、後端部に操作ツマミが形成されている。
カバー４は、ステンレス製であって厚さ５ｍｍ、直径４０ｍｍの円環形状であり、その円環形状の開口（例えば直径６ｍｍ）にＯリング４ａを介して試料導入ロッド７が挿入されている。これにより、カバー４は、気密を保ったまま設定方向に移動可能になっている。また、試料導入ロッド７には、設定方向と垂直に突出するステンレス製のストッパ８ａと、設定方向と垂直に突出するステンレス製のストッパ８ｂとが形成されている。ストッパ８ａは先端部付近に形成され、ストッパ８ｂは中央部付近に形成されている。そして、カバー４は、ストッパ８ａとストッパ８ｂとの間に配置されている。
カバー４とストッパ８ｂとの間には、カバー４が設定方向に動くように作用するバネ（弾性体）９が取付けられている。これにより、バネ９によってカバー４が試料導入ロッド７に対して設定方向に動くことで、ストッパ８ａに押し付けられる。 The sample introduction rod 7 is made of stainless steel and has a cylindrical shape with a diameter of 6 mm. The sample pan 6 is placed on the front end of the sample introduction rod 7 and an operation knob is formed on the rear end. Yes.
The cover 4 is made of stainless steel and has an annular shape with a thickness of 5 mm and a diameter of 40 mm. The sample introduction rod 7 is inserted into the annular opening (for example, with a diameter of 6 mm) through an O-ring 4a. Thereby, the cover 4 can be moved in the setting direction while keeping airtightness. Further, the sample introduction rod 7 is formed with a stainless steel stopper 8a protruding perpendicular to the setting direction and a stainless steel stopper 8b protruding perpendicular to the setting direction. The stopper 8a is formed near the tip, and the stopper 8b is formed near the center. The cover 4 is disposed between the stopper 8a and the stopper 8b.
A spring (elastic body) 9 is attached between the cover 4 and the stopper 8b so that the cover 4 moves in the setting direction. Thereby, the cover 4 is pressed against the stopper 8a by the spring 9 moving in the setting direction with respect to the sample introduction rod 7.

そして、燃焼管１の中央部の内部に配置された固体試料を分析する際には、キャリアガス入口１１からケース部３の内部に５００ｍｌ／ｍｉｎでキャリアガスが導かれ、燃焼管１の内部を設定方向（例えば、右から左へ）にキャリアガスが５００ｍｌ／ｍｉｎで流通するようになっている。   And when analyzing the solid sample arrange | positioned inside the center part of the combustion pipe 1, carrier gas is guide | induced to the inside of the case part 3 from the carrier gas inlet 11 at 500 ml / min, and the inside of the combustion pipe 1 is carried out. The carrier gas is circulated at a rate of 500 ml / min in the setting direction (for example, from right to left).

ここで、ＴＯＣ計によって測定者が一の固体試料が載置された試料皿６から次の固体試料が載置された試料皿６への交換を行う方法の一例について説明する。
まず、測定者は、試料導入ロッド７の先端部に試料皿６を配置する（図２参照）。次に、測定者は、ケース部３の内部に試料導入兼ロッド用開口部３ｄから試料導入ロッド７を手で挿入する（図３参照）。これにより、燃焼管１の一端部の内部に試料皿６が配置されたときには、カバー４がケース部３の試料導入兼ロッド用開口部３ｄの周辺部とＯリング３ａを介して密着することで、試料導入兼ロッド用開口部３ｄと試料導入ロッド７との隙間をカバー４で塞ぐ。そして、キャリアガス入口１１からケース部３の内部に５００ｍｌ／ｍｉｎでキャリアガスを導くことで、図２の状態のときに侵入した空気を押し出すため、キャリアガスを一定時間（例えば、６０秒間）パージする。このとき、測定者は、試料導入ロッド７を手で持ったままでもよく、何かで固定してもよい。 Here, an example of a method of exchanging from the sample dish 6 on which the solid sample is placed by the measurer to the sample dish 6 on which the next solid sample is placed by the TOC meter will be described.
First, the measurer places the sample pan 6 at the tip of the sample introduction rod 7 (see FIG. 2). Next, the measurer manually inserts the sample introduction rod 7 into the case portion 3 through the sample introduction / rod opening 3d (see FIG. 3). Thereby, when the sample pan 6 is disposed inside one end portion of the combustion tube 1, the cover 4 is in close contact with the peripheral portion of the sample introduction / rod opening 3d of the case portion 3 via the O-ring 3a. The gap between the sample introduction / rod opening 3 d and the sample introduction rod 7 is closed by the cover 4. Then, by introducing the carrier gas from the carrier gas inlet 11 into the case portion 3 at 500 ml / min to push out the air that has entered in the state of FIG. 2, the carrier gas is purged for a certain time (for example, 60 seconds). To do. At this time, the measurer may hold the sample introduction rod 7 with his hand or fix it with something.

次に、測定者は、試料導入兼ロッド用開口部３ｄと試料導入ロッド７との隙間をカバー４で塞ぎながら、試料導入ロッド７を設定方向に手で押し込んでいくことで試料皿６を移動させて、燃焼管１の中央部の内部に配置する（図４参照）。このとき、キャリアガス入口１１からケース部３の内部に５００ｍｌ／ｍｉｎでキャリアガスが導かれ、燃焼管１の内部を設定方向（例えば、右から左へ）にキャリアガスが５００ｍｌ／ｍｉｎで流通する。そして、燃焼管１の他端部（左部）には、酸化触媒５が充填されており、固体試料から発生した有機物等はキャリアガスとともに酸化触媒層５に達し、酸化触媒５により酸化されて二酸化炭素となる。このとき、測定者は、試料導入ロッド７を手で持ったままでもよく、何かで固定してもよい。   Next, the measurer moves the sample pan 6 by manually pushing the sample introduction rod 7 in the setting direction while closing the gap between the sample introduction / rod opening 3d and the sample introduction rod 7 with the cover 4. And disposed inside the central portion of the combustion tube 1 (see FIG. 4). At this time, the carrier gas is introduced from the carrier gas inlet 11 into the case portion 3 at a rate of 500 ml / min, and the carrier gas flows through the inside of the combustion tube 1 in a set direction (for example, from right to left) at a rate of 500 ml / min. . The other end (left part) of the combustion tube 1 is filled with an oxidation catalyst 5, and organic matter generated from the solid sample reaches the oxidation catalyst layer 5 together with the carrier gas and is oxidized by the oxidation catalyst 5. It becomes carbon dioxide. At this time, the measurer may hold the sample introduction rod 7 with his hand or fix it with something.

そして、固体試料の分析が終了した際には、測定者は、試料導入兼ロッド用開口部３ｄから試料導入ロッド７を設定方向と逆方向に手で引っ張る（図３参照）。さらに、測定者は、試料導入ロッド７を設定方向と逆方向に手で引っ張ることで、試料導入ロッド７を試料導入兼ロッド用開口部３ｄから取り出す（図２参照）。そして、測定者は一の固体試料が載置された試料皿６から次の固体試料が載置された試料皿６への交換を行う。   When the analysis of the solid sample is completed, the measurer manually pulls the sample introduction rod 7 from the sample introduction / rod opening 3d in the direction opposite to the setting direction (see FIG. 3). Further, the measurer pulls the sample introduction rod 7 by hand in the direction opposite to the setting direction, thereby removing the sample introduction rod 7 from the sample introduction / rod opening 3d (see FIG. 2). Then, the measurer exchanges the sample dish 6 on which one solid sample is placed with the sample dish 6 on which the next solid sample is placed.

以上のように、本発明の試料導入ポート部１０によれば、試料導入用開口部を手動で開放したり閉鎖したりするカバー構造や定流量ポンプが必要ではなくなる。また、キャリアガスの無駄も少なくなる。さらに、ケース部３の内部に試料皿６を配置するまでの操作手順が容易となる。   As described above, according to the sample introduction port portion 10 of the present invention, a cover structure and a constant flow pump for manually opening and closing the sample introduction opening are not necessary. Further, the waste of carrier gas is reduced. Furthermore, the operation procedure until the sample pan 6 is arranged inside the case portion 3 is facilitated.

＜他の実施形態＞
（１）上述したＴＯＣ計では、測定者が試料導入ロッド７を手で押し込んでいく構成を示したが、モータやソレノイドによって試料導入ロッド７を押し込んでいくような構成としてもよい。
（２）上述したＴＯＣ計では、バネ９によってカバー４がケース部３の試料導入兼ロッド用開口部３ｄの周辺部と密着する構成を示したが、モータやソレノイドによってカバー４がケース部３の試料導入兼ロッド用開口部３ｄの周辺部と密着するような構成としてもよい。 <Other embodiments>
(1) In the above-described TOC meter, a configuration in which the measurer pushes the sample introduction rod 7 by hand is shown, but a configuration in which the sample introduction rod 7 is pushed by a motor or a solenoid may be used.
(2) In the TOC meter described above, the cover 4 is in close contact with the periphery of the sample introduction / rod opening 3d of the case portion 3 by the spring 9, but the cover 4 is attached to the case portion 3 by a motor or solenoid. It is good also as a structure which closely_contact | adheres to the peripheral part of 3d of sample introduction and rod openings.

本発明は、土壌・堆積物・農畜産物等の固体試料や、河川水・湖沼水・海水・雨水・地下水等の液体試料等の試料中の炭素分を測定する全有機炭素計等に利用することができる。   The present invention is used for a total organic carbon meter that measures carbon content in solid samples such as soil, sediment, agricultural and livestock products, and liquid samples such as river water, lake water, seawater, rainwater, and groundwater. can do.

１ 燃焼管
２ 電気炉（燃焼炉）
３ ケース部
４ カバー
３ｄ 試料導入兼ロッド用開口部
６ 試料皿
７ 試料導入ロッド
１０ 試料導入ポート部（試料導入機構） 1 Combustion tube 2 Electric furnace (combustion furnace)
3 Case part 4 Cover 3d Sample introduction / rod opening 6 Sample pan 7 Sample introduction rod 10 Sample introduction port part (sample introduction mechanism)

Claims (3)

試料を載置した試料皿が、燃焼管の一端部に連結された試料導入機構の内部に配置された後、前記燃焼管の一端部から他端部へ向かう設定方向に試料導入ロッドによって移動することにより、燃焼炉の内部となる前記燃焼管の中央部の内部に配置され、当該試料中の有機物が燃焼する全有機炭素計であって、
前記試料導入機構は、試料導入兼ロッド用開口部が形成されたケース部と、
先端部に試料皿が載置され、前記設定方向で試料導入兼ロッド用開口部から挿入される試料導入ロッドと、
前記試料導入ロッドの外周面に形成されたカバーとを備え、
先端部に試料皿が載置された試料導入ロッドが試料導入兼ロッド用開口部から挿入されることにより、前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぐことを特徴とする全有機炭素計。 After the sample pan on which the sample is placed is disposed inside the sample introduction mechanism connected to one end of the combustion tube, the sample pan is moved by the sample introduction rod in a setting direction from one end to the other end of the combustion tube. A total organic carbon meter disposed inside the central portion of the combustion tube, which is the interior of the combustion furnace, and the organic matter in the sample burns,
The sample introduction mechanism includes a case portion in which a sample introduction and rod opening is formed;
A sample pan placed on the tip, and a sample introduction rod inserted from the sample introduction and rod opening in the setting direction;
A cover formed on the outer peripheral surface of the sample introduction rod,
The sample introduction rod having the sample pan placed on the tip is inserted from the sample introduction / rod opening, thereby closing the gap between the sample introduction / rod opening and the sample introduction rod with a cover. Total organic carbon meter as a feature. 前記カバーは、前記試料導入ロッドの外周面で設定方向と逆方向に移動可能に形成され、
先端部に試料皿が載置された試料導入ロッドが試料導入兼ロッド用開口部から挿入されて、前記燃焼管の一端部の内部に試料皿が配置されたときには、前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぎ、
前記試料導入兼ロッド用開口部と前記試料導入ロッドとの隙間をカバーで塞ぎながら、前記試料導入ロッドが設定方向に挿入されていくことにより、前記試料皿が燃焼管の中央部の内部に配置されることを特徴とする請求項１に記載の全有機炭素計。 The cover is formed to be movable in the direction opposite to the setting direction on the outer peripheral surface of the sample introduction rod,
When the sample introduction rod having the sample dish placed on the tip is inserted from the sample introduction / rod opening and the sample dish is placed inside one end of the combustion tube, the sample introduction / rod opening Cover the gap between the part and the sample introduction rod with a cover,
The sample pan is placed in the center of the combustion tube by inserting the sample introduction rod in the setting direction while closing the gap between the sample introduction / rod opening and the sample introduction rod with a cover. The total organic carbon meter according to claim 1, wherein 前記試料導入ロッドに対して前記カバーが設定方向に動くように作用する弾性体が、前記試料導入ロッドに取付けられていることを特徴とする請求項２に記載の全有機炭素計。 The total organic carbon meter according to claim 2, wherein an elastic body that acts so that the cover moves in a setting direction with respect to the sample introduction rod is attached to the sample introduction rod.
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