JP2007263815A - Toc (total organic carbon) meter - Google Patents

Toc (total organic carbon) meter Download PDF

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JP2007263815A
JP2007263815A JP2006090511A JP2006090511A JP2007263815A JP 2007263815 A JP2007263815 A JP 2007263815A JP 2006090511 A JP2006090511 A JP 2006090511A JP 2006090511 A JP2006090511 A JP 2006090511A JP 2007263815 A JP2007263815 A JP 2007263815A
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sample water
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JP4818773B2 (en
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Yoko Hayashi
陽子 林
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DKK TOA Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a TOC meter which keeps a dilution part of sample water integrated with an IC (Inorganic Carbon) body removal treatment part, capable of easily coping with dilution even the magnification of the dilution is high, has a high efficiency of the elimination of the IC and a simple constitution, and is capable of reducing cost. <P>SOLUTION: In the TOC meter which includes the dilution/IC removal tank 10 of bottomed cylindrical shape for mixing the sample water, dilution water and IC removal liquid, to the bottom of the dilution/IC removal tank 10, sample water lead-in line 14, dilution water lead-in line 16, IC removal liquid lead-in line 18 and agitation gas lead-in line 20 are connected. The mixture liquid 12 of the sample water, dilution water and IC removal liquid led in the dilution/IC removal tank, the ratio of the internal diameter a (mm) to the height b (mm) (a:b) is made 1:10 to 20. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、試料水中のＴＯＣ（全有機体炭素）を測定するＴＯＣ計に関する。   The present invention relates to a TOC meter that measures TOC (total organic carbon) in sample water.

ＴＯＣ計は、排水や河川水などの汚濁度を調べるために、試料水中に含まれる有機物量を測定する装置として用いられる。有機物の種類は数多く存在するため、個々の有機物の濃度を全て測定することは現実的に不可能である。そのため、ＴＯＣ計においては、試料水中の全ての有機物を燃焼酸化させ、このときに発生する二酸化炭素の濃度を測定し、炭素量を演算することにより、有機物の総量を得ている。   The TOC meter is used as a device for measuring the amount of organic matter contained in the sample water in order to investigate the degree of pollution of drainage or river water. Since there are many kinds of organic substances, it is practically impossible to measure all the concentrations of individual organic substances. Therefore, in the TOC meter, all organic substances in the sample water are burned and oxidized, the concentration of carbon dioxide generated at this time is measured, and the total amount of organic substances is obtained by calculating the carbon amount.

しかし、試料水中には、溶存している二酸化炭素、炭酸水素イオン、炭酸イオン、懸濁体炭酸塩類等の無機体炭素（ＩＣ）が含まれているため、有機物由来の二酸化炭素濃度を精度良く測定するには、予め試料水中のＩＣを除去したり、試料水中のＴＣ（全炭素）とＩＣを別々に測定し、ＴＣからＩＣを差し引いたりする必要がある。   However, the sample water contains dissolved carbon dioxide, bicarbonate ions, carbonate ions, suspended carbonic acid salts and other inorganic carbon (IC). In order to measure, it is necessary to remove IC in the sample water in advance, or separately measure TC (total carbon) and IC in the sample water, and subtract IC from TC.

予め試料水中のＩＣを除去する方法としては、試料水にＩＣ除去液として酸を添加し、ｐＨを１〜３にして通気を行うことにより、ＩＣを二酸化炭素に変換して除去する方法が用いられている（ＪＩＳ−Ｋ−０８０５）。   As a method for removing IC in the sample water in advance, a method is used in which the acid is added to the sample water as an IC removal solution, and the pH is adjusted to 1 to 3 so that the IC is converted to carbon dioxide and removed. (JIS-K-0805).

また、一般に試料水はＴＯＣ計の希釈部において希釈水と混合され、一定の割合に希釈された後に燃焼酸化されるが、上記希釈部とＩＣ除去処理部とを一体化させ、装置構成を簡素化させることが行われている（例えば、特許文献１参照）。   In general, sample water is mixed with dilution water in the dilution section of the TOC meter, and after being diluted to a certain ratio, it is burnt and oxidized. However, the dilution section and the IC removal processing section are integrated to simplify the device configuration. (For example, refer to Patent Document 1).

特開平７−９８３１０号公報JP 7-98310 A

上述した特許文献１の装置では、試料水、希釈水およびＩＣ除去液（酸）の計量にシリンジ型計量ポンプを用いている。しかし、試料水の希釈倍率を高くする必要が想定される場合、例えば二酸化炭素の検出器の仕様を変えずにＴＯＣ濃度の測定レンジを広くとろうとするような場合には、シリンジ型計量ポンプとしてシリンジ本体の容量が大きいものを用いるか、あるいは２段階で希釈を行わなければならず、対応が難しいという問題がある。また、シリンジ型計量ポンプは高価であり、かつ、駆動部が必要である。   In the apparatus of Patent Document 1 described above, a syringe-type metering pump is used for metering sample water, dilution water, and IC removal liquid (acid). However, when it is necessary to increase the dilution rate of the sample water, for example, when trying to widen the measurement range of the TOC concentration without changing the specification of the carbon dioxide detector, as a syringe type metering pump There is a problem that it is difficult to cope with the use of a syringe body having a large capacity or dilution in two stages. Moreover, the syringe-type metering pump is expensive and requires a drive unit.

本発明は、前述した事情に鑑みてなされたもので、試料水の希釈部とＩＣ除去処理部とを一体化したＴＯＣ計であって、試料水の希釈倍率が高い場合でも容易に対応することができ、かつＩＣの除去効率が高いとともに、構造が簡単で、コストの削減を図ることが可能なＴＯＣ計を提供することを目的とする。   The present invention has been made in view of the above-described circumstances, and is a TOC meter in which a sample water dilution unit and an IC removal processing unit are integrated, and can easily cope with a case where the dilution rate of the sample water is high. An object of the present invention is to provide a TOC meter that can reduce the cost while having a high IC removal efficiency and a simple structure.

本発明は、前記目的を達成するため、内部で試料水、希釈水およびＩＣ除去液を混合する有底筒状の希釈・ＩＣ除去槽を備えたＴＯＣ計において、前記希釈・ＩＣ除去槽は、試料水導入ライン、希釈水導入ラインおよびＩＣ除去液導入ラインが接続され、かつ、底部に攪拌ガス導入ラインが接続されているとともに、希釈・ＩＣ除去槽内における試料水、希釈水およびＩＣ除去液の混合液の内径（ｍｍ）と高さ（ｍｍ）との比を１：１０〜２０とすることができることを特徴するＴＯＣ計を提供する。   In order to achieve the above object, the present invention provides a TOC meter including a bottomed cylindrical dilution / IC removal tank in which sample water, dilution water, and an IC removal liquid are mixed. The sample water introduction line, dilution water introduction line, and IC removal liquid introduction line are connected, and the stirring gas introduction line is connected to the bottom, and the sample water, dilution water, and IC removal liquid in the dilution / IC removal tank A TOC meter is provided in which the ratio of the inner diameter (mm) to the height (mm) of the mixed liquid can be 1: 10-20.

本発明のＴＯＣ計は、希釈・ＩＣ除去槽として、内部に導入した試料水、希釈水およびＩＣ除去液の混合液の内径（ｍｍ）と高さ（ｍｍ）との比を１：１０〜２０とすることができるものを用い、希釈・ＩＣ除去槽の高さを高くしたので、希釈・ＩＣ除去槽の容積を大きくすることができ、そのため試料水の希釈倍率が高い場合でも容易に対応することができる。また、本発明のＴＯＣ計は、希釈・ＩＣ除去槽の内径を小さくしたので、試料水と攪拌ガスとの接触効率が良く、そのためＩＣの除去効率が高い。さらに、希釈部およびＩＣ除去処理部において駆動部（マルチポートバルブ、プランジャ、モータ等）が少ないため、構造が簡単で、製作が容易である。   The TOC meter of the present invention has a ratio of the inner diameter (mm) to the height (mm) of the mixture of sample water, dilution water and IC removal liquid introduced into the dilution / IC removal tank as 1: 10-20. Since the height of the dilution / IC removal tank is increased, the volume of the dilution / IC removal tank can be increased. Therefore, even when the dilution rate of the sample water is high, it can be easily handled. be able to. Moreover, since the TOC meter of the present invention has a reduced inner diameter of the dilution / IC removal tank, the contact efficiency between the sample water and the stirring gas is good, and therefore the IC removal efficiency is high. Furthermore, since there are few driving parts (multiport valve, plunger, motor, etc.) in the dilution part and the IC removal processing part, the structure is simple and the manufacture is easy.

本発明では、試料水導入ラインを希釈・ＩＣ除去槽の底部に接続することが好ましい。このようにすると、希釈・ＩＣ除去槽への試料水の導入と攪拌ガスの導入が同方向から行われ、ＩＣが除去されていない新しい試料水に新しい攪拌ガスが接触するため、この点でもＩＣの除去効率が高くなる。   In the present invention, it is preferable to connect the sample water introduction line to the bottom of the dilution / IC removal tank. In this way, the sample water and the stirring gas are introduced into the dilution / IC removal tank from the same direction, and the new stirring gas contacts the new sample water from which the IC has not been removed. The removal efficiency becomes higher.

本発明においては、希釈・ＩＣ除去槽として、内部における試料水、希釈水およびＩＣ除去液の混合液の内径（ｍｍ）と高さ（ｍｍ）との比を１：１０〜２０、より好ましくは１：１５程度とすることができるものを用い、試料水の希釈および試料水中のＩＣ除去を行う際には、希釈・ＩＣ除去槽内における上記混合液の内径（ｍｍ）と高さ（ｍｍ）との比を１：１０〜２０、より好ましくは１：１５程度とする。   In the present invention, as the dilution / IC removal tank, the ratio of the inner diameter (mm) to the height (mm) of the mixed solution of the sample water, the dilution water and the IC removal liquid is 1:10 to 20, more preferably When diluting the sample water and removing the IC in the sample water using a material that can be about 1:15, the inner diameter (mm) and the height (mm) of the mixed solution in the dilution / IC removal tank The ratio is about 1:10 to 20, more preferably about 1:15.

また、希釈・ＩＣ除去槽の高さは、希釈・ＩＣ除去槽内の混合液の高さの１．５倍程度とすることが適当である。希釈・ＩＣ除去槽の高さが低すぎると希釈・ＩＣ除去槽内の上部のスペースが小さくなって攪拌ガスによるバブリングを行うことが難しくなり、希釈・ＩＣ除去槽の高さが高すぎると希釈・ＩＣ除去槽内の上部に無駄なスペースが生じる。   The height of the dilution / IC removal tank is suitably about 1.5 times the height of the mixed solution in the dilution / IC removal tank. If the height of the dilution / IC removal tank is too low, the space in the upper part of the dilution / IC removal tank becomes small and it becomes difficult to perform bubbling with stirring gas, and if the height of the dilution / IC removal tank is too high, dilution is performed. -Useless space is created in the upper part of the IC removal tank.

本発明において、希釈・ＩＣ除去槽の内径および高さの具体的な値は、特に限定されないが、内径は１０〜２０ｍｍとし、高さはその１０〜２０倍、特に１５倍程度とすることが適当である。   In the present invention, specific values of the inner diameter and height of the dilution / IC removal tank are not particularly limited, but the inner diameter is 10 to 20 mm, and the height is 10 to 20 times, particularly about 15 times. Is appropriate.

本発明のＴＯＣ計は、試料水の希釈倍率が高い場合でも容易に対応することができ、かつＩＣの除去効率が高いとともに、構造が簡単で、コストの削減を図ることが可能である。   The TOC meter of the present invention can easily cope with the case where the dilution rate of the sample water is high, has high IC removal efficiency, has a simple structure, and can reduce costs.

以下、図面を参照して本発明を実施するための最良の形態の一例を示す。図１は本発明に係るＴＯＣ計の試料水前処理部（試料水の希釈および試料水中のＩＣ除去を行う部分）を示す概略図である。   Hereinafter, an example of the best mode for carrying out the present invention will be described with reference to the drawings. FIG. 1 is a schematic view showing a sample water pretreatment part (part for diluting sample water and removing IC in the sample water) of the TOC meter according to the present invention.

図１において、１０は内部で試料水、希釈水およびＩＣ除去液を混合する有底円筒状の希釈・ＩＣ除去槽を示す。希釈・ＩＣ除去槽１０の材質に限定はなく、例えばプラスチック類、ガラス類あるいは金属類等とすることができる。上記希釈・ＩＣ除去槽１０は、内部に導入された試料水、希釈水およびＩＣ除去液の混合液１２の内径ａ（ｍｍ）と高さｂ（ｍｍ）との比（ａ：ｂ）を１：１０〜２０とすることができるようになっている。また、希釈・ＩＣ除去槽１０の底部には、試料水導入ライン１４、希釈水導入ライン１６、ＩＣ除去液導入ライン１８、攪拌ガス導入ライン２０およびドレインライン２２が接続されている。上記各ラインには、それぞれ開閉バルブ２４、２６、２８、３０、３２が介装されている。なお、上記各ラインは希釈・ＩＣ除去槽１０の底部の手前で合流している。   In FIG. 1, reference numeral 10 denotes a bottomed cylindrical dilution / IC removal tank in which sample water, dilution water and IC removal liquid are mixed. The material of the dilution / IC removal tank 10 is not limited, and may be plastics, glasses, metals, or the like. The dilution / IC removal tank 10 has a ratio (a: b) of the inner diameter a (mm) to the height b (mm) of the mixed solution 12 of sample water, dilution water, and IC removal solution introduced therein. : 10 to 20 can be set. A sample water introduction line 14, a dilution water introduction line 16, an IC removal liquid introduction line 18, a stirring gas introduction line 20 and a drain line 22 are connected to the bottom of the dilution / IC removal tank 10. Open / close valves 24, 26, 28, 30, and 32 are interposed in the respective lines. Note that the above lines merge before the bottom of the dilution / IC removal tank 10.

本例の試料水前処理部は、バルブの操作により試料水導入ライン１４、希釈水導入ライン１６、ＩＣ除去液導入ライン１８より希釈・ＩＣ除去槽１０内に試料水、希釈水（純水等）およびＩＣ除去液（塩酸等）を導入するとともに、バルブの操作により攪拌ガス導入ライン２０より希釈・ＩＣ除去槽１０内に攪拌ガス（エア等）を導入することにより、試料水、希釈水およびＩＣ除去液の混合液のバブリングを行い、試料水の希釈および試料水中のＩＣ除去を行うものである。なお、希釈・ＩＣ除去槽１０からの処理液の取り出しは適宜手段で行うことができる。例えば、希釈・ＩＣ除去槽１０の上部から処理液流出管を用いて試料液の取り出しを行うことができる。また、処理液の前処理後はドレインライン２２により処理液を排出した後、次の前処理を行う。   The sample water pretreatment unit of the present example is operated by operating the valve from the sample water introduction line 14, the dilution water introduction line 16, and the IC removal liquid introduction line 18 into the dilution / IC removal tank 10. ) And IC removal liquid (hydrochloric acid, etc.), and by introducing stirring gas (air etc.) into the dilution / IC removal tank 10 from the stirring gas introduction line 20 by operating the valve, The liquid mixture of the IC removing liquid is bubbled to dilute the sample water and remove the IC in the sample water. Note that the processing liquid can be taken out from the dilution / IC removal tank 10 by any appropriate means. For example, the sample liquid can be taken out from the upper part of the dilution / IC removal tank 10 using the treatment liquid outflow pipe. Further, after the pretreatment of the treatment liquid, the treatment liquid is discharged through the drain line 22 and then the next pretreatment is performed.

上述した実施形態の試料水前処理部は、例えば図２に示すような構成のＴＯＣ計に使用することができる。図２において、１００は試料水前処理部、１０２は試料水導入部、１０４は燃焼部、１０６はキャリヤガス供給手段、１０８は除湿器、１１０は検出器である非分散型赤外分析計（ＮＤＩＲ）を示す。   The sample water pretreatment part of embodiment mentioned above can be used for the TOC meter of a structure as shown, for example in FIG. In FIG. 2, 100 is a sample water pretreatment section, 102 is a sample water introduction section, 104 is a combustion section, 106 is a carrier gas supply means, 108 is a dehumidifier, and 110 is a non-dispersive infrared analyzer (110). NDIR).

本例のＴＯＣ計は、試料水前処理部１００において試料水の希釈および試料水中のＩＣ除去を行った後、キャリヤガス供給手段１０６により燃焼部１０４内にキャリヤガスを流した状態で、試料水を試料水導入部１０２から燃焼部１０４内に導入する。燃焼部１０４内では、気化した試料水のガス中の有機物が触媒の作用により酸化され、ＣＯ２に変換される。その後、ガスを除湿器１０８を通して検出器１１０に導入し、ガス中のＣＯ２濃度を測定することにより、試料水中のＴＯＣ濃度を求めるものである。前述した実施形態の試料水前処理部は、本例のＴＯＣ計の試料水前処理部１００に使用することができる。 In the TOC meter of this example, after the sample water is diluted in the sample water pretreatment unit 100 and the IC is removed from the sample water, the carrier water is supplied into the combustion unit 104 by the carrier gas supply means 106, Is introduced into the combustion section 104 from the sample water introduction section 102. In the combustion unit 104, organic substances in the vaporized sample water gas are oxidized by the action of the catalyst and converted to CO 2 . Thereafter, the gas is introduced into the detector 110 through the dehumidifier 108, and the TOC concentration in the sample water is obtained by measuring the CO 2 concentration in the gas. The sample water pretreatment part of embodiment mentioned above can be used for the sample water pretreatment part 100 of the TOC meter of this example.

次に、実施例を示す。有底円筒状の容器内にＩＣ濃度が１０ｍｇ／Ｌの標準液（無機体炭素残留率試験液）およびＩＣ除去液（塩酸）を導入し、バブリング流量２００ｍｌ／分、バブリング時間６０秒でエアによるバブリングを行った。この場合、実施例および比較例１、２において、容器の内径および高さ、容器内の混合液の内径および高さ、容器内の混合液の内径と高さとの比をそれぞれ表１に示す値とした。   Next, an example is shown. A standard solution (inorganic carbon residual rate test solution) with an IC concentration of 10 mg / L and an IC removal solution (hydrochloric acid) are introduced into a bottomed cylindrical container, and the bubbling flow rate is 200 ml / min and the bubbling time is 60 seconds. Bubbling was performed. In this case, in Examples and Comparative Examples 1 and 2, the ratios of the inner diameter and height of the container, the inner diameter and height of the mixed liquid in the container, and the inner diameter and height of the mixed liquid in the container are shown in Table 1, respectively. It was.

Figure 2007263815
実施例、比較例で前処理を行った処理液中のＩＣ濃度をＴＯＣ計により前述のようにして測定した。この場合、処理液をＴＯＣ計の燃焼部に導入し、燃焼ガス中のＣＯ２濃度を検出器で測定した。また、各容器に付き前処理およびＩＣ濃度測定を１０回ずつ行った。結果を図３のグラフに示す。ＩＣ除去率は、フルスケールの３％以内であれば、ＪＩＳの規格に準じていることになる。本実験では、０〜１０ｍｇ／Ｌのレンジの測定において、ＩＣ濃度が１０ｍｇ／Ｌの標準液を測定しているため、測定値が１０ｍｇ／Ｌの３％以内、すなわち０．３ｍｇ／Ｌ以下であれば、ＪＩＳの規格に準じていることになる。図１より、本発明のように容器内の混合液の内径と高さとの比を１：１０〜２０とした場合、ＩＣの除去効率が高くなり、試料水中のＩＣ除去を短時間で行うことができることがわかる。
Figure 2007263815
 The IC concentration in the treatment liquid pretreated in the examples and comparative examples was measured with a TOC meter as described above. In this case, the treatment liquid was introduced into the combustion section of the TOC meter, and the CO 2 concentration in the combustion gas was measured with a detector. Further, pretreatment and IC concentration measurement were performed 10 times for each container. The results are shown in the graph of FIG. If the IC removal rate is within 3% of the full scale, it conforms to the JIS standard. In this experiment, since the standard solution with an IC concentration of 10 mg / L is measured in the range of 0 to 10 mg / L, the measured value is within 3% of 10 mg / L, that is, 0.3 mg / L or less. If there is, it conforms to the JIS standard. As shown in FIG. 1, when the ratio of the inner diameter to the height of the mixed liquid in the container is set to 1:10 to 20 as in the present invention, the IC removal efficiency is increased and the IC removal from the sample water is performed in a short time. You can see that

本発明に係るＴＯＣ計の試料水前処理部を示す概略図である。It is the schematic which shows the sample water pre-processing part of the TOC meter which concerns on this invention. ＴＯＣ計の一例を示す概念図である。It is a conceptual diagram which shows an example of a TOC meter. 実施例における処理液中のＩＣ濃度の測定結果を示すグラフである。It is a graph which shows the measurement result of IC density | concentration in the process liquid in an Example.

符号の説明Explanation of symbols

１０ 希釈・ＩＣ除去槽
１２ 混合液
１４ 試料水導入ライン
１６ 希釈水導入ライン
１８ ＩＣ除去液導入ライン
２０ 攪拌ガス導入ライン
２２ ドレインライン
10 Dilution / IC removal tank 12 Mixture 14 Sample water introduction line 16 Dilution water introduction line 18 IC removal liquid introduction line 20 Stirring gas introduction line 22 Drain line

Claims (2)

内部で試料水、希釈水およびＩＣ除去液を混合する有底筒状の希釈・ＩＣ除去槽を備えたＴＯＣ計において、前記希釈・ＩＣ除去槽は、試料水導入ライン、希釈水導入ラインおよびＩＣ除去液導入ラインが接続され、かつ、底部に攪拌ガス導入ラインが接続されているとともに、希釈・ＩＣ除去槽内における試料水、希釈水およびＩＣ除去液の混合液の内径（ｍｍ）と高さ（ｍｍ）との比を１：１０〜２０とすることができることを特徴するＴＯＣ計。   In a TOC meter equipped with a bottomed cylindrical dilution / IC removal tank that mixes sample water, dilution water and IC removal liquid inside, the dilution / IC removal tank comprises a sample water introduction line, a dilution water introduction line, and an IC. The removal liquid introduction line is connected and the stirring gas introduction line is connected to the bottom, and the inner diameter (mm) and height of the mixture of sample water, dilution water and IC removal liquid in the dilution / IC removal tank A TOC meter characterized in that the ratio to (mm) can be 1: 10-20. 試料水導入ラインが希釈・ＩＣ除去槽の底部に接続されていることを特徴する請求項１に記載のＴＯＣ計。
The TOC meter according to claim 1, wherein the sample water introduction line is connected to the bottom of the dilution / IC removal tank.
JP2006090511A 2006-03-29 2006-03-29 TOC meter Expired - Fee Related JP4818773B2 (en)

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Publication number Priority date Publication date Assignee Title
JPWO2021100229A1 (en) * 2019-11-18 2021-05-27
KR102359468B1 (en) * 2020-09-17 2022-02-07 서울과학기술대학교 산학협력단 Improve Total Organic Carbon Analysis Method with pretreatment and homogeneity evaluation of Sample

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JPS5771685A (en) * 1980-10-22 1982-05-04 Toshiba Corp Device for removing inorganic carbon
JPS60127460A (en) * 1983-12-14 1985-07-08 Nishihara Environ Sanit Res Corp Continuous analysis type total organic carbon meter
JPH0798310A (en) * 1993-09-29 1995-04-11 Shimadzu Corp Toc meter with multifunctional sample weighing and filling part

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JPS51105886A (en) * 1975-03-14 1976-09-20 Sumitomo Chemical Co ZENJUKI TANSORYOSOKUTE ISOCHI
JPS5771685A (en) * 1980-10-22 1982-05-04 Toshiba Corp Device for removing inorganic carbon
JPS60127460A (en) * 1983-12-14 1985-07-08 Nishihara Environ Sanit Res Corp Continuous analysis type total organic carbon meter
JPH0798310A (en) * 1993-09-29 1995-04-11 Shimadzu Corp Toc meter with multifunctional sample weighing and filling part

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2021100229A1 (en) * 2019-11-18 2021-05-27
WO2021100229A1 (en) * 2019-11-18 2021-05-27 株式会社島津製作所 Total organic carbon measurement method and total organic carbon measurement device
JP7310917B2 (en) 2019-11-18 2023-07-19 株式会社島津製作所 Total organic carbon measuring method and total organic carbon measuring device
KR102359468B1 (en) * 2020-09-17 2022-02-07 서울과학기술대학교 산학협력단 Improve Total Organic Carbon Analysis Method with pretreatment and homogeneity evaluation of Sample

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