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JP7119491B2 - Water quality analysis method - Google Patents
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JP7119491B2 - Water quality analysis method - Google Patents

Water quality analysis method Download PDF

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JP7119491B2
JP7119491B2 JP2018060065A JP2018060065A JP7119491B2 JP 7119491 B2 JP7119491 B2 JP 7119491B2 JP 2018060065 A JP2018060065 A JP 2018060065A JP 2018060065 A JP2018060065 A JP 2018060065A JP 7119491 B2 JP7119491 B2 JP 7119491B2
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measurement
sample water
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water
reagent
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和彦 角田
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Kurita Water Industries Ltd
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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。 TECHNICAL FIELD 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 measurement principle of colorimetry or nephelometry.

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 on-line water quality analyzer, sample water is injected into the measurement cell, a measurement reagent is added according to the measurement item to cause color development or cloudiness, and the change in absorbance before and after addition of the measurement reagent is measured to determine the amount of chemicals in the sample water. Concentration is calculated (Patent Documents 1 and 2).

従来の水質分析方法にあっては、測定セル内に試薬を添加し混合させる場合、後述の図2(比較例2)の通り、測定セル1の上流部に設けられた定流量弁12に流すサンプル水を電磁弁11の開閉を行うことによって発生する脈動によって行っていた。しかし、この方法では、定流量弁12および電磁弁11の流路が狭いため、サンプル水中のSS(懸濁物質)や微生物由来のファウリングにより定流量弁12や電磁弁11が閉塞し、測定試薬の撹拌が不十分になり、正常な測定ができなくなるという問題があった。 In the conventional water quality analysis method, when a reagent is added and mixed in the measurement cell, the reagent is flown through the constant flow valve 12 provided upstream of the measurement cell 1 as shown in FIG. 2 (Comparative Example 2) described later. Sample water was sampled by pulsation generated by opening and closing the electromagnetic valve 11 . However, in this method, since the flow paths of the constant flow valve 12 and the solenoid valve 11 are narrow, the constant flow valve 12 and the solenoid valve 11 are clogged due to SS (suspended solids) in the sample water and fouling derived from microorganisms. There was a problem that the stirring of the reagent became insufficient, making normal measurement impossible.

即ち、定流量弁12や電磁弁11が閉塞し、透過水量が減少すると、測定試薬の撹拌が不十分となり、測定結果が安定しない。なお、定流量弁12は、電磁弁11が開状態の時にサンプル水の圧力が変動しても、測定セル1内部へサンプル水が一定量流れるようにするために設置されている。測定セル1内にサンプル水が流入しすぎると、添加した試薬が測定セル1外へ流出してしまうため、測定ができない。 That is, when the constant flow valve 12 or the solenoid valve 11 is blocked and the amount of permeated water is reduced, the measurement reagent is not stirred sufficiently, and the measurement result is unstable. The constant flow rate valve 12 is installed to allow a constant amount of sample water to flow into the measuring cell 1 even if the pressure of the sample water fluctuates when the solenoid valve 11 is open. If too much sample water flows into the measuring cell 1, the added reagent will flow out of the measuring cell 1, making measurement impossible.

特開2010-181150号公報Japanese Unexamined Patent Application Publication No. 2010-181150 特開2014-186027号公報JP 2014-186027 A

上記の通り、従来の技術では、測定セル内でのサンプル水と測定試薬との撹拌を、測定セル上流部に設けられた電磁弁を開閉させ、発生する脈動によって行っていたが、定流量弁および電磁弁の流路が狭いため、サンプル水中のSSや微生物由来のファウリングにより閉塞し、測定試薬の撹拌が不十分になり、正常な測定ができなくなることがあった。 As described above, in the conventional technology, the sample water and the measurement reagent are stirred in the measurement cell by opening and closing the electromagnetic valve provided upstream of the measurement cell, and by the pulsation generated. In addition, since the flow path of the solenoid valve is narrow, it may be clogged by fouling derived from SS or microorganisms in the sample water, and the agitation of the measurement reagent may become insufficient, making normal measurement impossible.

本発明は、測定セル内でのサンプル水と測定試薬との撹拌が十分に行われ、測定精度が高くなると共に、流路の閉塞も防止される水質分析方法を提供することを目的とする。 SUMMARY OF THE INVENTION An object of the present invention is to provide a water quality analysis method in which sample water and a measurement reagent are sufficiently agitated in a measurement cell, measurement accuracy is improved, and clogging of the flow path is prevented.

本発明の水質分析方法は、測定セル内に測定試薬を供給した後、該測定セル内にサンプル水を供給し、測定試薬とサンプル水とを撹拌した後、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、測定セル内に測定試薬を供給した後、サンプル水供給用チューブポンプを短時間作動させて測定セル内にサンプル水を供給することにより、測定試薬とサンプル水とを撹拌することを特徴とする。 In the water quality analysis method of the present invention, a measurement reagent is supplied into a measurement cell, a sample water is supplied into the measurement cell, the measurement reagent and the sample water are stirred, and then the sample water in the measurement cell absorbs light or In a water quality analysis method using a water quality analyzer that measures scattering using a light-emitting body and a light-receiving body, after supplying a measurement reagent into the measurement cell, the tube pump for supplying sample water is operated for a short time to supply sample water into the measurement cell. It is characterized by stirring the measuring reagent and the sample water by supplying.

本発明では、好ましくは、前記サンプル水の供給時に前記チューブポンプを0.1~0.2sec作動させ、測定セルの容積の20~40%のサンプル水を測定セル内に供給する。 In the present invention, preferably, the tube pump is operated for 0.1 to 0.2 sec when supplying the sample water, and 20 to 40% of the volume of the measuring cell is supplied to the measuring cell.

本発明では、サンプル水をチューブポンプによって測定セルに供給する。チューブポンプは、吐出水が脈動する。本発明では、この脈動によって測定セル内でサンプル水と測定試薬とを撹拌する。この方法によると、サンプル水と測定試薬とが十分に撹拌され、精度の高い水質分析を行うことができる。また、電磁弁及び定流量弁を用いないことにより、流路の閉塞も防止される。 In the present invention, sample water is supplied to the measuring cell by a tube pump. The tube pump pulsates the discharged water. In the present invention, this pulsation agitates the sample water and the measurement reagent in the measurement cell. According to this method, the sample water and the measurement reagent are sufficiently stirred, and highly accurate water quality analysis can be performed. In addition, by not using a solenoid valve and a constant flow valve, clogging of the flow path is also prevented.

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。1 is a schematic cross-sectional view of a water quality analyzer according to an embodiment; FIG. 従来例に係る水質分析装置の概略的な断面図である。FIG. 2 is a schematic cross-sectional view of a water quality analyzer according to a conventional example; 実験結果を示すグラフである。It is a graph which shows an experimental result. 実験結果を示すグラフである。It is a graph which shows an experimental result.

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はサンプル水の流入口2と流出口3とを有する。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 measuring cell 1 has an inlet 2 and an outlet 3 for sample water. One side surface of the measurement cell 1 is a transparent portion 4 , and the cell inner surface on the opposite side of the transparent portion 4 is a white reflective surface 5 . A cover 8 is provided so as to cover the outside of the transparent portion 4. Inside the cover 8, a light emitter 6 such as a light emitting diode and a light receiver 7 such as a photodiode are provided. Light from the light emitter 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 photoreceptor 7, and 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 to this.

サンプル水は、チューブポンプ10によって測定セル1に供給される。本発明では、好ましくは測定セル1内に測定試薬を供給した後、測定セル1の容積の20~40%のサンプル水を測定セル1に供給する。チューブポンプ10は、吐出水が脈動するので、この脈動によって測定セル1内においてサンプル水と測定試薬とが十分に撹拌される。 Sample water is supplied to the measuring cell 1 by a tube pump 10 . In the present invention, preferably after supplying the measuring reagent into the measuring cell 1 , sample water of 20 to 40% of the volume of the measuring cell 1 is supplied to the measuring cell 1 . The tube pump 10 pulsates the discharged water, and the pulsation sufficiently agitates the sample water and the measurement reagent in the measurement cell 1 .

また、チューブポンプ10はSSやバイオファウリングによる閉塞が生じにくい。そのため、本発明によると、長期にわたって高精度の水質測定を行うことができる。 Further, the tube pump 10 is less prone to clogging due to SS or biofouling. Therefore, according to the present invention, highly accurate water quality measurement can be performed over a long period of time.

以下の比較例1及び実施例1では、測定試薬として塩化ベンゼトニウム、およびpH緩衝水溶液を用い、サンプル水として実稼働中の開放循環式冷却水を用いた。 In Comparative Example 1 and Example 1 below, benzethonium chloride and a pH buffer aqueous solution were used as measurement reagents, and open circulation cooling water in actual operation was used as sample water.

[比較例1]
図2の通り、測定セル(容積0.7mL)に測定試薬を0.06mL添加後、電磁弁を0.2~0.4sec開状態にし、測定セルの容積に対して15~30%のサンプル水をパルス的に測定セル内に供給し、測定試薬と撹拌した(この際、流量計によってサンプル水供給速度を測定した。)。次いで、センサー値を読み取り、検量線に基づいてポリマー濃度を求めた。サンプル水の供給速度及びポリマー濃度の経時変化を図2,3に示す。
[Comparative Example 1]
As shown in FIG. 2, after adding 0.06 mL of the measurement reagent to the measurement cell (volume 0.7 mL), the solenoid valve is opened for 0.2 to 0.4 sec, and 15 to 30% of the volume of the measurement cell is sampled. Water was supplied in pulses into the measurement cell and stirred with the measurement reagent (at this time, the sample water supply rate was measured by a flow meter). The sensor values were then read and the polymer concentration determined based on the calibration curve. 2 and 3 show changes over time in sample water supply rate and polymer concentration.

[実施例1]
測定試薬を測定セル内部に添加後、図1の通り、チューブポンプを0.1~0.2sec稼働させ、測定セルの容積に対して20~40%のサンプル水を脈動状に測定セル1内に供給した。それ以外は比較例1と同一条件にて試験を行った。サンプル水の供給速度及びポリマー濃度の経時変化を図2,3に示す。
[Example 1]
After adding the measurement reagent to the inside of the measurement cell, as shown in FIG. supplied to Other than that, the test was conducted under the same conditions as in Comparative Example 1. 2 and 3 show changes over time in sample water supply rate and polymer concentration.

[参考例1]
サンプル水を採取し、サンプル水中のポリマー濃度を比濁法によって分析した。結果を図3にラボ分析値として示す。
[Reference example 1]
Sample water was taken and the polymer concentration in the sample water was analyzed by nephelometric method. The results are shown in FIG. 3 as laboratory analysis values.

図3の通り、実施例1の値はほぼ参考例1と一致している。これに対し、比較例1では参考例1の値との乖離が大きい。この実験結果より、本発明によると高精度の測定が可能となることが認められた。 As shown in FIG. 3, the values of Example 1 substantially match those of Reference Example 1. On the other hand, in Comparative Example 1, the divergence from the value in Reference Example 1 is large. From this experimental result, it was confirmed that the present invention enables highly accurate measurement.

また、図2の通り、本発明によると、測定セルへの通水速度は長期にわたって一定に保たれることが認められた。 Also, as shown in FIG. 2, according to the present invention, it was found that the water flow rate to the measuring cell was kept constant over a long period of time.

1 測定セル
5 反射面
6 発光体
7 受光体
10 チューブポンプ
11 電磁弁
12 定流量弁
REFERENCE SIGNS LIST 1 measurement cell 5 reflective surface 6 light emitter 7 light receiver 10 tube pump 11 solenoid valve 12 constant flow valve

Claims (1)

測定セル内に測定試薬を供給した後、該測定セル内にサンプル水を供給し、測定試薬とサンプル水とを撹拌した後、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、測定セル内に測定試薬を供給した後、サンプル水供給用チューブポンプを0.1~0.2sec作動させて測定セル内に測定セルの容積の20~40%のサンプル水を供給することにより、測定試薬とサンプル水とを撹拌することを特徴とする水質分析方法。
After supplying the measuring reagent into the measuring cell, supplying the sample water into the measuring cell, and stirring the measuring reagent and the sample water, the light absorption or scattering by the sample water in the measuring cell is detected by the light-emitting body and the light-receiving body. In the water quality analysis method using the water quality analyzer to be measured, after supplying the measurement reagent into the measurement cell, the sample water supply tube pump is operated for 0.1 to 0.2 sec to fill the measurement cell with 20% of the volume of the measurement cell. A water quality analysis method characterized by supplying ~40% sample water and stirring the measurement reagent and the sample water.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010181150A (en) 2009-02-03 2010-08-19 Kurita Water Ind Ltd Method and instrument for measuring concentration of dissolved substance, and method and device for detecting color tone
JP2017127815A (en) 2016-01-20 2017-07-27 栗田工業株式会社 Polymer liquid dissolving-diluting apparatus
JP2019174174A (en) 2018-03-27 2019-10-10 栗田工業株式会社 Water quality analysis method
JP2019174173A (en) 2018-03-27 2019-10-10 栗田工業株式会社 Water quality analysis method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11197477A (en) * 1998-01-16 1999-07-27 Isis:Kk Liquid mixing machine

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010181150A (en) 2009-02-03 2010-08-19 Kurita Water Ind Ltd Method and instrument for measuring concentration of dissolved substance, and method and device for detecting color tone
JP2017127815A (en) 2016-01-20 2017-07-27 栗田工業株式会社 Polymer liquid dissolving-diluting apparatus
JP2019174174A (en) 2018-03-27 2019-10-10 栗田工業株式会社 Water quality analysis method
JP2019174173A (en) 2018-03-27 2019-10-10 栗田工業株式会社 Water quality analysis method

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