JP6927346B1 - Water quality analysis method - Google Patents

Water quality analysis method Download PDF

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JP6927346B1
JP6927346B1 JP2020028487A JP2020028487A JP6927346B1 JP 6927346 B1 JP6927346 B1 JP 6927346B1 JP 2020028487 A JP2020028487 A JP 2020028487A JP 2020028487 A JP2020028487 A JP 2020028487A JP 6927346 B1 JP6927346 B1 JP 6927346B1
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和彦 角田
和彦 角田
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Kurita Water Industries Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract

【課題】セル内面のファウリングによる測定誤差発生を防ぐことができると共に、メンテナンスの頻度を低減することができる水質分析方法を提供する。【解決手段】測定セル１内のサンプル水による吸光又は散乱を発光体６及び受光体７によって測定する水質分析装置を用いる水質分析方法において、測定セル１内のサンプル水を測定後に排出すると共に、測定セル１内の残留サンプル水量が所定量以下になった後に測定セル１内に洗浄水を供給して測定セルを洗浄する。【選択図】図１PROBLEM TO BE SOLVED: To provide a water quality analysis method capable of preventing the occurrence of measurement error due to fouling on the inner surface of a cell and reducing the frequency of maintenance. SOLUTION: In a water quality analysis method using a water quality analyzer that measures absorption or scattering of sample water in a measurement cell 1 by a light emitter 6 and a light receiver 7, the sample water in the measurement cell 1 is discharged after measurement and is discharged. After the amount of residual sample water in the measurement cell 1 becomes equal to or less than a predetermined amount, wash water is supplied into the measurement cell 1 to wash the measurement cell. [Selection diagram] Fig. 1

Description

本発明は、水質分析方法に係り、特に、比色法または比濁法を測定原理とする水質分析装置を用いた水質分析方法に関する。 The present invention relates to a water quality analysis method, and more particularly to a water quality analysis method using a water quality analyzer based on a colorimetric method or a turbidity method as a measurement principle.

オンライン型の水質分析計においては、測定セルにサンプル水を注入し、測定項目に応じた測定試薬を添加し発色または白濁させ、測定試薬添加前後の吸光度の変化を測定する事によりサンプル水中の薬剤濃度を算出している（特許文献１，２）。 In an online water quality analyzer, sample water is injected into a measurement cell, a measurement reagent is added according to the measurement item to develop color or cloudiness, and the change in absorbance before and after the addition of the measurement reagent is measured to measure the drug in the sample water. The concentration is calculated (Patent Documents 1 and 2).

この水質分析計にあっては、サンプル水中のＳＳまたは微生物が測定セル内で堆積または繁殖し、測定セル内壁が汚染（ファウリング）され、吸光度を測定するセンサーが正常な値を検出できなくなることがある。 In this water quality analyzer, SS or microorganisms in the sample water accumulate or propagate in the measurement cell, the inner wall of the measurement cell is contaminated (fouling), and the sensor that measures the absorbance cannot detect the normal value. There is.

すなわち、従来では、測定セル内部に通水速度は２〜５ｃｍ／ｓｅｃで通水している。この通水速度では測定セル内部に一度付着したＳＳは剥離しないため測定セル内部に滞留してしまう。また、微生物由来のファウリングも流速が低いため、剥離せず、測定セル壁面上で繁殖してしまう。 That is, conventionally, water is passed through the inside of the measurement cell at a water flow rate of 2 to 5 cm / sec. At this water flow rate, the SS once adhered to the inside of the measurement cell does not peel off, so that it stays inside the measurement cell. In addition, since the flow velocity of fouling derived from microorganisms is low, it does not peel off and propagates on the wall surface of the measurement cell.

特許文献３には、かかる問題点を解決する水質分析方法として、測定セル内のサンプル水による吸光又は散乱を発光体及び受光体によって測定する水質分析装置を用いる水質分析方法において、測定セル内のサンプル水を測定サイクル毎に排出する水質分析方法が記載されている。なお、特許文献３には、測定セルからのサンプルの排出方法として、サンプル供給用ポンプを逆回転させる方法が記載されている。 Patent Document 3 describes, as a water quality analysis method for solving such a problem, in a water quality analysis method using a water quality analyzer that measures absorption or scattering of sample water in a measurement cell by a light emitter and a light receiver, in the measurement cell. A water quality analysis method for discharging sample water at each measurement cycle is described. In addition, Patent Document 3 describes a method of rotating the sample supply pump in the reverse direction as a method of discharging the sample from the measurement cell.

この特許文献３の水質分析方法によると、通水セル内部のメンテナンス頻度を少なくすることができる。しかし、完全に通水セル内の汚れを除去することはできないため、定期的なメンテナンスが必要であった。例えば、測定セルを洗浄するために、洗浄剤を測定セルに注入すると、洗浄剤がアルカリ性の場合、サンプル水中の硬度成分が析出してセル内面に付着するため、定期的なメンテナンスが必要であった。 According to the water quality analysis method of Patent Document 3, the frequency of maintenance inside the water flow cell can be reduced. However, since it is not possible to completely remove the dirt in the water flow cell, regular maintenance is required. For example, when a cleaning agent is injected into the measuring cell to clean the measuring cell, if the cleaning agent is alkaline, the hardness component in the sample water precipitates and adheres to the inner surface of the cell, so that regular maintenance is required. rice field.

特開２０１０−１８１１５０号公報Japanese Unexamined Patent Publication No. 2010-181150 特開２０１４−１８６０２７号公報Japanese Unexamined Patent Publication No. 2014-186027 特開２０１９−１７４１７３号公報Japanese Unexamined Patent Publication No. 2019-174173

本発明は、セル内面のファウリングによる測定誤差発生を防ぐことができると共に、メンテナンスの頻度を低減することができる水質分析方法を提供することを目的とする。 An object of the present invention is to provide a water quality analysis method capable of preventing the occurrence of measurement error due to fouling on the inner surface of a cell and reducing the frequency of maintenance.

本発明の水質分析方法は、測定セル内のサンプル水による吸光又は散乱を発光体及び受光体によって測定する水質分析装置を用いる水質分析方法において、測定セル内のサンプル水を測定後に排出すると共に、測定セル内の残留サンプル水量が所定量以下になった後に測定セル内に洗浄水を供給して測定セルを洗浄することを特徴とする。 The water quality analysis method of the present invention is a water quality analysis method using a water quality analyzer that measures absorption or scattering of sample water in a measurement cell by a light emitter and a light receiver, and discharges the sample water in the measurement cell after measurement. After the amount of residual sample water in the measuring cell becomes equal to or less than a predetermined amount, washing water is supplied into the measuring cell to wash the measuring cell.

本発明の一態様では、前記測定セル内の残留サンプル水の量が測定セルの容積の１０％以下になった後に洗浄水を測定セル内に供給する。 In one aspect of the present invention, wash water is supplied into the measurement cell after the amount of residual sample water in the measurement cell becomes 10% or less of the volume of the measurement cell.

本発明の一態様では、前記測定セル内にサンプル水を供給する供給管が接続されており、測定セル内のサンプル水の水位が該供給管の接続部分以下になった後に洗浄水を測定セル内に供給する。 In one aspect of the present invention, a supply pipe for supplying sample water is connected to the measurement cell, and the washing water is measured after the water level of the sample water in the measurement cell becomes equal to or lower than the connection portion of the supply pipe. Supply inside.

本発明の一態様では、サンプル水の供給管に測定試薬の添加部が設けられている。 In one aspect of the present invention, the sample water supply pipe is provided with an addition portion for the measurement reagent.

本発明では、測定後に測定セル内を洗浄水で洗浄することにより測定セル内部のファウリングを防止し、精度の高い水質測定を行うことができる。 In the present invention, fouling inside the measurement cell can be prevented by washing the inside of the measurement cell with washing water after the measurement, and highly accurate water quality measurement can be performed.

本発明では、測定セル内の残留サンプル水が規定量以下（全量排出を含む。）となった後に洗浄水を測定セル内に供給するので、洗浄水中の洗浄薬成分とサンプル水とが反応して析出物が析出することが防止され、析出物による測定セル内部のファウリングが防止される。 In the present invention, since the washing water is supplied into the measuring cell after the residual sample water in the measuring cell becomes less than the specified amount (including the discharge of the entire amount), the cleaning agent component in the washing water reacts with the sample water. This prevents the precipitates from precipitating and prevents fouling inside the measurement cell due to the precipitates.

また、測定セル内部のサンプル水の残留量が少なくなってから洗浄水を供給することにより、洗浄水へのサンプル水の混入が抑制され、測定セル内部の洗浄効率が高くなる。 Further, by supplying the cleaning water after the residual amount of the sample water inside the measurement cell is reduced, the mixing of the sample water into the cleaning water is suppressed, and the cleaning efficiency inside the measuring cell is improved.

実施の形態に係る水質分析装置の概略的な断面図である。It is the schematic sectional drawing of the water quality analyzer which concerns on embodiment. 本発明方法の一例を示すシーケンス図である。It is a sequence diagram which shows an example of the method of this invention.

図１を参照して実施の形態について説明する。測定セル１は、下部にサンプル水の流入口２を有し、上部にサンプル水の流出口３を有する。測定セル１の一方の側面は透明部４となっており、該透明部４の反対側のセル内面は白色の反射面５となっている。透明部４の外部を覆うようにカバー８が設けられ、該カバー８内に、発光ダイオード等よりなる発光体６と、フォトダイオード等よりなる受光体７とが設けられている。発光体６からの光がセル１内のサンプル水を透過し、反射面５で反射され、サンプル水を透過して受光体７で受光され、吸光度が測定される。セル１の容積は０．３〜３．０ｍＬ特に０．５〜１．０ｍＬ程度が好適であるが、これに限定されない。 An embodiment will be described with reference to FIG. The measurement cell 1 has a sample water inlet 2 at the bottom and a sample water outlet 3 at the top. One side surface of the measurement cell 1 is a transparent portion 4, and the inner surface of the cell on the opposite side of the transparent portion 4 is a white reflecting surface 5. A cover 8 is provided so as to cover the outside of the transparent portion 4, and a light emitting body 6 made of a light emitting diode or the like and a light receiving body 7 made of a photodiode or the like are provided in the cover 8. The light from the light emitting body 6 passes through the sample water in the cell 1, is reflected by the reflecting surface 5, passes through the sample water, is received by the light receiving body 7, and the absorbance is measured. The volume of the cell 1 is preferably about 0.3 to 3.0 mL, particularly about 0.5 to 1.0 mL, but is not limited thereto.

サンプル水の流入口２にサンプル水の供給管９が接続されている。該供給管９に第１試薬の注入管１１と第２試薬の注入管１２とが接続されている。 A sample water supply pipe 9 is connected to the sample water inlet 2. The injection pipe 11 of the first reagent and the injection pipe 12 of the second reagent are connected to the supply pipe 9.

測定セル１の上部に、洗浄水の供給口１６が設けられている。該供給口１６に、バルブ１４を有した洗浄水供給配管１５が接続されている。 A washing water supply port 16 is provided above the measurement cell 1. A washing water supply pipe 15 having a valve 14 is connected to the supply port 16.

サンプル水は、ポンプ例えばチューブポンプ１０から供給管９を介して測定セル１に供給される。供給管９を流れる間に第１及び第２試薬をそれぞれ定量的に添加し、吸光度を測定する。 The sample water is supplied to the measurement cell 1 from a pump, for example, a tube pump 10 via a supply pipe 9. The first and second reagents are quantitatively added while flowing through the supply pipe 9, and the absorbance is measured.

測定サイクル毎にチューブポンプ１０を逆回転させて測定セル１内の水を一旦排出する。この際、測定セル１内の残留サンプル水量が規定量以下となった後に測定セル１内に洗浄水を供給して測定セル１を洗浄する。 The tube pump 10 is rotated in the reverse direction every measurement cycle to temporarily discharge the water in the measurement cell 1. At this time, after the amount of residual sample water in the measurement cell 1 becomes equal to or less than the specified amount, wash water is supplied into the measurement cell 1 to wash the measurement cell 1.

このように測定セル１内の残留サンプル水量が規定量以下となった後に測定セル１内に洗浄水を供給して測定セル１を洗浄することにより、サンプル水中の硬度成分と洗浄剤成分との反応による、洗浄剤注入点での析出（詰まり）を防止することができる。すなわち、洗浄水注入時のサンプル水と洗浄水とが混合することによるサンプル水中の硬度成分の析出がなくなるため、高濃度の洗浄剤含有洗浄水を測定セル１に注入した場合であっても、洗浄水供給口１６付近が詰まりにくくなる。これにより、効率の良い測定セル１の洗浄と長期安定稼働が可能となる。さらに、洗浄剤含有洗浄水が残留サンプル水で薄まることなく、高濃度のまま測定セル１内に供給されるので、洗浄効果を高くすることが可能となる。 After the amount of residual sample water in the measurement cell 1 becomes equal to or less than the specified amount in this way, the cleaning water is supplied into the measurement cell 1 to wash the measurement cell 1, so that the hardness component and the detergent component in the sample water are combined. Precipitation (clogging) at the cleaning agent injection point due to the reaction can be prevented. That is, since the hardness component does not precipitate in the sample water due to the mixing of the sample water and the washing water at the time of injecting the washing water, even when the high-concentration cleaning agent-containing washing water is injected into the measurement cell 1, the measurement cell 1 is injected. The vicinity of the wash water supply port 16 is less likely to be clogged. This enables efficient cleaning of the measurement cell 1 and long-term stable operation. Further, since the cleaning agent-containing cleaning water is supplied into the measurement cell 1 in a high concentration without being diluted with the residual sample water, the cleaning effect can be enhanced.

この実施の形態では、サンプル水は測定セル１内に下部から導入し、測定セル１上部から流出するようにしているところから、測定セル１内の下部に汚れ等が溜まる。しかし、チューブポンプ１０の通水方向を反転させることにより、測定セル１内の下部に溜まった汚れや試薬を含むサンプル水を排出することができる。また、測定セル１内の水位が減少することに伴い、測定セル１内に負圧が発生し、試薬の供給流路内に残った試薬も一緒に排水することができる。これにより、洗浄水を注入した際に試薬成分が析出する問題を解消することができる。 In this embodiment, since the sample water is introduced into the measurement cell 1 from the lower part and flows out from the upper part of the measurement cell 1, dirt and the like are accumulated in the lower part in the measurement cell 1. However, by reversing the water flow direction of the tube pump 10, the sample water containing dirt and reagents accumulated in the lower part of the measurement cell 1 can be discharged. Further, as the water level in the measurement cell 1 decreases, a negative pressure is generated in the measurement cell 1, and the reagent remaining in the reagent supply flow path can be drained together. As a result, it is possible to solve the problem that the reagent component is precipitated when the washing water is injected.

本手法での測定シーケンスの一例を図２に示す。 FIG. 2 shows an example of the measurement sequence in this method.

本発明でも、特許文献３と同様に、セル１内のサンプル水の線速度が６ｃｍ／ｓｅｃ以上、例えば６〜２０ｃｍ／ｓｅｃ好ましくは６〜１０ｃｍ／ｓｅｃとなるようにサンプル水量を制御するのが好ましい。このようにサンプル水の線速度を６ｃｍ／ｓｅｃ以上とすることにより、測定セル１のファウリングが防止される。即ち、６ｃｍ／ｓｅｃ以上の通水速度にすることで、水流の剪断力により測定セル内壁に付着したファウリング物質はセル内壁から剥離し測定セル外に放出される。また測定セル内の通水速度を上げることにより発生する乱流もファウリング物質の剥離に寄与している。 In the present invention as well, as in Patent Document 3, the amount of sample water is controlled so that the linear velocity of the sample water in the cell 1 is 6 cm / sec or more, for example, 6 to 20 cm / sec, preferably 6 to 10 cm / sec. preferable. By setting the linear velocity of the sample water to 6 cm / sec or more in this way, fouling of the measurement cell 1 is prevented. That is, by setting the water flow rate to 6 cm / sec or more, the fouling substance adhering to the inner wall of the measurement cell due to the shearing force of the water flow is separated from the inner wall of the measurement cell and released to the outside of the measurement cell. In addition, the turbulent flow generated by increasing the water flow rate in the measurement cell also contributes to the exfoliation of the fouling substance.

なお、測定を行っている間、継続してサンプル水線速度を６ｃｍ／ｓｅｃ以上としてもよく、測定に先だってサンプル水線速度を６ｃｍ／ｓｅｃ以上とし、測定時にはサンプル水線速度をそれよりも低い値（停止も含む。）として測定を行ってよい。 The sample water line velocity may be continuously set to 6 cm / sec or more during the measurement, the sample water line velocity may be set to 6 cm / sec or more prior to the measurement, and the sample water line velocity may be lower than that at the time of measurement. The measurement may be performed as a value (including stop).

上記測定セル１は反射面５を有しているが、セル１の両側面を透明部とし、一方の透明部の外側に発光体を配置し、他方の透明部の外側に受光体を配置してもよい。 The measurement cell 1 has a reflecting surface 5, but both side surfaces of the cell 1 are transparent portions, a light emitting body is arranged outside one transparent portion, and a light receiving body is arranged outside the other transparent portion. You may.

１ 測定セル
５ 反射面
６ 発光体
７ 受光体
９ サンプル水の供給管
１０ チューブポンプ
１６ 洗浄水供給口 1 Measurement cell 5 Reflective surface 6 Light emitter 7 Receiver 9 Sample water supply tube 10 Tube pump 16 Washing water supply port

Claims (4)

測定セル内のサンプル水による吸光又は散乱を発光体及び受光体によって測定する水質分析装置を用いる水質分析方法において、
測定セル内のサンプル水を測定後に排出すると共に、
測定セル内の残留サンプル水量が所定量以下になった後に測定セル内に洗浄水を供給して測定セルを洗浄する水質分析方法であって、
該サンプル水が硬度成分を含み、
該洗浄水がアルカリ性の洗浄剤を含み、
該測定セルは、下部に該サンプル水の流入口を有すると共に、上部に該洗浄水の供給口を有し、
該測定セル内の測定後のサンプル水を、該サンプル水の流入口から該測定セルより排出することを特徴とする水質分析方法。 In a water quality analysis method using a water quality analyzer that measures absorption or scattering of sample water in a measurement cell with a light emitter and a light receiver.
The sample water in the measurement cell is discharged after measurement, and at the same time, it is discharged.
This is a water quality analysis method for cleaning the measurement cell by supplying washing water into the measurement cell after the amount of residual sample water in the measurement cell becomes less than a predetermined amount.
The sample water contains a hardness component and contains
The cleaning water contains an alkaline cleaning agent and contains
The measurement cell has an inlet for the sample water at the bottom and a supply port for the wash water at the top.
A water quality analysis method, characterized in that the sample water after measurement in the measurement cell is discharged from the measurement cell from the inlet of the sample water. 前記測定セル内の残留サンプル水の量が測定セルの容積の１０％以下になった後に洗浄水を測定セル内に供給することを特徴とする請求項１の水質分析方法。 The water quality analysis method according to claim 1, wherein the washing water is supplied into the measurement cell after the amount of residual sample water in the measurement cell becomes 10% or less of the volume of the measurement cell. 前記測定セル内にサンプル水を供給する供給管が接続されており、
測定セル内のサンプル水の水位が該供給管の接続部分以下になった後に洗浄水を測定セル内に供給することを特徴とする請求項１又は２の水質分析方法。 A supply pipe for supplying sample water is connected to the measurement cell.
The water quality analysis method according to claim 1 or 2, wherein the washing water is supplied into the measurement cell after the water level of the sample water in the measurement cell becomes equal to or lower than the connection portion of the supply pipe. サンプル水の供給管に測定試薬の添加部が設けられていることを特徴とする請求項３の水質分析方法。 The water quality analysis method according to claim 3, wherein an addition portion of a measurement reagent is provided in a sample water supply pipe.
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