WO2013140560A1 - APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH - Google Patents

APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH Download PDF

Info

Publication number
WO2013140560A1
WO2013140560A1 PCT/JP2012/057276 JP2012057276W WO2013140560A1 WO 2013140560 A1 WO2013140560 A1 WO 2013140560A1 JP 2012057276 W JP2012057276 W JP 2012057276W WO 2013140560 A1 WO2013140560 A1 WO 2013140560A1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
container
automatic
intensity
adjustment
Prior art date
Application number
PCT/JP2012/057276
Other languages
English (en)
Japanese (ja)
Inventor
彦北 朱
光一 千葉
寿晴 黒田
道雄 堀内
Original Assignee
システム・インスツルメンツ株式会社
独立行政法人産業技術総合研究所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by システム・インスツルメンツ株式会社, 独立行政法人産業技術総合研究所 filed Critical システム・インスツルメンツ株式会社
Priority to PCT/JP2012/057276 priority Critical patent/WO2013140560A1/fr
Publication of WO2013140560A1 publication Critical patent/WO2013140560A1/fr

Links

Images

Classifications

    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/80—Indicating pH value
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G05—CONTROLLING; REGULATING
    • G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D21/00—Control of chemical or physico-chemical variables, e.g. pH value
    • G05D21/02—Control of chemical or physico-chemical variables, e.g. pH value characterised by the use of electric means

Definitions

  • the present invention relates to an automatic pH adjusting device, and more particularly to an automatic pH adjusting device that can be suitably used for pH adjustment as a pretreatment for solid phase extraction.
  • trace elements including heavy metals is conducted for the study of material circulation in the ocean, water quality inspection of tap water, water quality survey of lake water and river water.
  • a chelate resin or the like for the purpose of separation from interference components and improvement of analysis sensitivity.
  • Patent Document 1 discloses an automatic pH adjusting device that automatically adjusts the pH of boiler water.
  • This automatic pH adjusting device includes a water supply device that supplies water containing ammonium ions to a boiler water system, and a pH measurement device that measures the pH of boiler water flowing through the boiler water system.
  • the amount of water supplied from the water supply device is controlled based on the pH measured by the pH measurement device, and the acidic components contained in the boiler water are neutralized and reduced.
  • Non-Patent Document 1 discloses an electrode insertion type pH measurement device in which an electrode is directly inserted into a sample.
  • Non-Patent Document 2 discloses a portable pH measurement device that enables pH measurement of a very small amount of sample.
  • Non-Patent Document 3 discloses a flow-type pH measuring device capable of measuring the pH of a sample flowing in a pipe.
  • the amount of sample required for analysis of trace elements is usually several ⁇ l to several tens of ml. Therefore, in the separation and concentration described above, it is sufficient if a sample exceeding the required sample amount can be prepared in a short time, and it is not necessary to use a large-scale apparatus such as Patent Document 1.
  • Patent Document 1 since ammonium ion-containing water is directly supplied to the boiler water system, there is a possibility that the hydrogen ion concentration distribution in the boiler water is biased and a long time is required for pH adjustment. Therefore, it is not suitable for adjusting the pH of the sample for separation and concentration.
  • the measurement device of Non-Patent Document 2 is portable and the device itself is small. Therefore, it is necessary to take a small amount from the sample during pH adjustment and perform pH measurement, and as a result, the pH adjustment may take a long time. Therefore, it is not suitable for pH measurement of a sample during separation and concentration.
  • Non-Patent Documents 1 to 3 it is necessary to directly contact the pH measurement device with the sample, and the possibility of contamination derived from the apparatus cannot be excluded. Therefore, it is not suitable for pH measurement of a sample during separation and concentration.
  • an object of the present invention is to provide an automatic pH adjusting device that can prepare a sample for separation and concentration in a short time or can minimize contamination factors during sample preparation.
  • a first invention is an automatic pH adjusting device, a container capable of containing a pH adjustment target solution; A stirring device capable of stirring the solution to be adjusted for pH contained in the container; When the pH adjustment target solution is accommodated in the container, a spraying device having an injection port arranged at a location where the pH adjusting agent atomized with respect to the liquid surface can be injected, It is characterized by providing.
  • the second invention is the first invention, wherein
  • the pH adjustment target solution is one to which an indicator that changes color according to pH is added,
  • a light irradiation device for irradiating light from outside the container into the container;
  • An intensity detection device that is disposed opposite to the light irradiation device and the container and detects the intensity of transmitted light that has passed through the container;
  • a pH calculator that calculates the pH of the pH adjustment target solution contained in the container using the intensity of transmitted light detected by the intensity detector; It is characterized by providing.
  • the third invention is the first or second invention, wherein
  • the light irradiation device includes a light irradiation unit that emits light
  • the intensity detector includes an intensity detector that detects the intensity of transmitted light
  • the intensity detection unit and the light irradiation unit are arranged perpendicular to the opposing surface of the container to which the intensity detection device and the light irradiation device respectively face, and the intensity detection unit is connected to the light irradiation unit. It is arrange
  • the spray apparatus which has the injection port arrange
  • the bias of the hydrogen ion concentration distribution can be reduced. Accordingly, the pH condition can be adjusted more stably, so that an amount of sample necessary for separation and concentration can be prepared in a short time. Further, since the spray device does not come into contact with the pH adjustment target solution, it is possible to eliminate a cross-contamination factor between samples.
  • the device for calculating the pH of the pH adjustment target solution contained in the container that is, the light irradiation device and the intensity detection device are arranged outside the container, the contamination derived from the device. Factors can be eliminated. Therefore, contamination factors during sample preparation can be minimized.
  • the intensity detection unit and the light irradiation unit are arranged perpendicularly to the opposing surfaces of the container facing the intensity detection device and the light irradiation device, respectively, and the intensity detection unit is Since it arrange
  • FIG. 2 is an enlarged schematic diagram of the nebulizer 28 of FIG. 1.
  • FIG. 2 is an example of the flowchart which shows the pH adjustment process routine performed by PC42.
  • FIG. 1 is a schematic diagram illustrating a configuration of an automatic pH adjusting device 10 according to the present embodiment.
  • the automatic pH adjusting device 10 of this embodiment is a device for automatically adjusting the pH of the sample 12 to which a pH indicator is added.
  • the pH automatic adjustment device 10 includes a container 14 including a rectangular main body portion 14 a that can store a sample 12 and an opening portion 14 b for taking in and out the sample 12.
  • the container 14 is a transparent container made of PET.
  • the material of the container 14 can be used instead of PET as long as it shows a high transmittance with respect to the specific wavelength light described later.
  • the main body 14 a is installed on the stirrer 16.
  • a stirrer 18 is installed inside the main body 14a.
  • the stirrer 16 rotates the stirrer 18 at a low speed by an electromagnetic coil, and the sample 12 can be gently stirred by rotating the stirrer 18 at a low speed.
  • the stirrer 18 is of a shape and material that does not wear due to contact with the main body 14a during rotation.
  • a light source unit 20 that generates an illumination light beam for irradiating the sample 12 and a pinhole plate 22 are installed.
  • the light source unit 20 for example, an LED light source, a halogen light source, a tungsten lamp, a single wavelength laser device, or the like is employed.
  • an optical diffraction device such as a mirror may be used in combination with the light sources according to the enumeration.
  • the light diffraction device is provided at a location where the light source unit 20 in FIG. 1 is disposed, and functions as the light source unit 20. Accordingly, such a light diffraction device can also be adopted as the light source unit 20.
  • a pinhole 22a that transmits part of the illumination light beam generated by the light source unit 20 is provided.
  • a pinhole plate 24 having a pinhole 24a formed at the center thereof and a spectroscope 26 for measuring the intensity of specific wavelength light out of the light flux that has passed through the pinhole 24a are installed on the other side surface of the main body portion 14a.
  • a spectroscope 26 for measuring the intensity of specific wavelength light out of the light flux that has passed through the pinhole 24a.
  • a photodiode, an optical sensor or the like having sufficient sensitivity to the specific wavelength light is employed.
  • the opening 14b is provided with a nebulizer 28 capable of injecting a liquid in a mist form.
  • the nebulizer 28 is attached to a height adjusting member (not shown). The height adjusting member is adjusted so that the liquid surface of the sample 12 and the injection port 28a do not come into contact with each other during the liquid injection.
  • FIG. 2 is an enlarged schematic view of the nebulizer 28 of FIG.
  • the nebulizer 28 includes a gas supply pipe 30 through which compressed air, an inert gas, and the like can be circulated, and a liquid supply pipe 32 through which a liquid can be circulated.
  • the gas supply pipe 30 includes a gas supply port 30a and a gas injection port 30b.
  • the gas supply port 30a is connected to an inert gas tank (not shown) such as nitrogen.
  • the liquid supply pipe 32 includes a liquid supply port 32a and a liquid ejection port 32b.
  • the liquid supply port 32 a is connected to a non-metallic tube 34.
  • FIG. 2 shows a coaxial nebulizer having a double-pipe structure, a coaxial type having a multi-pipe structure and a nebulizer characterized by a cross-flow type fine spray are also employed.
  • the nebulizer 28 is connected via a tube 34 to a container 38 that contains a pH adjusting liquid 36 therein.
  • a solenoid-type opening / closing valve 40 is provided in the middle of the tube 34. When the opening / closing valve 40 is opened while gas is flowing through the gas supply pipe 30, the pH adjustment liquid refined by the gas suction pressure is ejected from the liquid ejection port 32 b toward the liquid surface of the sample 12.
  • the pH automatic adjusting device 10 includes a PC 42 for controlling the entire device.
  • the spectroscope 26 is connected to the input side of the PC 42, and the transmitted light signal 44 from the spectroscope 26 is input to the PC 42.
  • an opening / closing valve 40 is connected to the output side of the PC 42 via an I / O board 46, and an opening / closing signal 48 from the PC 42 is generated from the PC 42.
  • the stirrer 16 and the height adjusting member may be connected to the output side of the PC 42.
  • a substrate integrated controller may be used instead of the PC 42 and the I / O board 46.
  • a valve opening degree conversion model for converting the valve opening degree of the opening / closing valve 40 into the opening / closing signal 48, or the difference between the target transmitted light intensity I tar corresponding to the adjustment target pH and the measured transmitted light intensity I mv A supply amount map that defines the relationship between ⁇ I and the supply amount of the pH adjusting liquid 36, a valve opening map that defines the relationship between the supply amount of the pH adjusting solution 36 and the valve opening of the opening / closing valve 40, etc. It is assumed that it is stored in
  • the amount of sample required for analysis of trace elements is usually several ⁇ l to several tens of ml, and this is necessary for pH adjustment for separation and concentration. It is sufficient if the amount exceeding the sample amount can be prepared in a short time.
  • the pH adjustment liquid 36 is added to the sample 12 in a droplet state using an auto burette or the like to adjust the pH.
  • the pH of the solution for separating and concentrating trace elements is in the vicinity of neutrality, and the injection of the adjustment liquid having a droplet size (about 0.1 to 0.3 ml) causes a drastic change in the solution pH.
  • the pH automatic adjusting device 10 of the present embodiment the pH adjusting liquid 36 can be sprayed in the form of a mist toward the liquid surface of the sample 12, so that the intensity fluctuation is reduced and the target pH is stably adjusted Can be reached. Therefore, the amount necessary for separation and concentration can be prepared in a short time.
  • the light source unit 20 and the spectroscope 26 used for pH measurement are installed outside the container 14. Further, the injection port 28 a of the nebulizer 28 does not come into contact with the liquid level of the sample 12. As described above, in the automatic pH adjusting device 10 of the present embodiment, since the device used for pH adjustment is not in contact with the sample 12, contamination factors during pH adjustment can be minimized.
  • FIG. 3 is an example of a flowchart showing a pH adjustment processing routine executed in the PC 42 in the present embodiment. Note that the routine shown in FIG. 3 is repeatedly executed at predetermined intervals.
  • a difference ⁇ I between the target transmitted light intensity I tar and the measured transmitted light intensity I mv is calculated (step 110). Specifically, first, the spectroscope 26 obtains the intensity of the specific wavelength light (measured transmitted light intensity I mv ), and the difference between the measured transmitted light intensity I mv and the target transmitted light intensity I tar is calculated as ⁇ I. It should be noted that a value that is separately set and stored in advance in the PC 42 is used as the target transmitted light intensity I tar .
  • step 120 it is determined whether or not the absolute value
  • > ⁇ I th ⁇ I is applied to the supply amount map, and the supply amount of the pH adjusting liquid 36 is calculated (step 130).
  • ⁇ ⁇ I th in this step the process proceeds to step 140.
  • the threshold value ⁇ I th used in this step can be changed as appropriate according to the pH adjustment accuracy.
  • the opening degree of the on-off valve 40 is changed (step 150). Specifically, first, the valve opening degree of the on-off valve 40 is calculated by applying the supply amount of the pH adjusting liquid 36 calculated in step 130 to the valve opening degree map. Next, the calculated valve opening is applied to the valve opening conversion model to be converted into an opening / closing signal 48 and transmitted to the opening / closing valve 40. Thereby, the supply amount of the pH adjusting liquid 36 from the nebulizer 28 is changed. Following this step, a counter value described later is reset (step 160).
  • step 140 it is determined whether or not the counter value is equal to a predetermined value.
  • the counter value used in this step is counted when
  • the automatic pH adjusting device of this embodiment will be further described with reference to experimental examples.
  • the sample for trace element analysis is basically prepared and stored under acidic conditions, and the separation and concentration of trace elements by solid phase extraction is in a weakly acidic to neutral pH range.
  • the pH of the sample is adjusted by increasing the pH of the sample by adding ammonia water as the pH adjusting liquid 36.
  • pH automatic adjustment device 10 pH automatic adjustment device 12 Sample (solution for pH adjustment) 14,38 container 16 stirrer (stirring device) 18 Stirrer (stirring device) 20 Light source part (light irradiation device, light irradiation part) 26 Spectrometer (Intensity detector, Intensity detector) 28 Nebulizer (spraying device) 28a injection port 36 pH adjusting liquid 42 PC (pH calculation device) 44 Transmitted light signal 48 Open / close signal

Landscapes

  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Automation & Control Theory (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

La présente invention se rapporte à un appareil de réglage automatique du pH et fournit automatiquement un appareil de réglage de pH qui permet la préparation de courte durée d'un échantillon de séparation et la concentration ou facteurs qui permettent de minimiser la contamination pendant la préparation de l'échantillon. Dans un appareil de réglage de pH automatique (10) selon un mode de réalisation, un fluide d'ajustement du pH (36) peut être éjecté sous la forme d'un brouillard vers la surface liquide d'un échantillon (12) pour ajuster le pH de l'échantillon (12) à un niveau cible de manière stable avec des fluctuations réduites dans l'intensité de la lumière transmise. Ainsi, un échantillon dans une quantité nécessaire pour la séparation et la concentration peut être préparé en un temps court. En outre, une unité de source de lumière (20) et un spectroscope (26), qui sont utilisés dans une mesure de pH, sont situés à l'extérieur d'un vaisseau (14) (28a), tandis qu'un orifice de jet d'un nébuliseur (28) n'entre pas en contact avec la surface liquide de l'échantillon (12). Dans l'appareil de réglage de pH automatique (10) un groupe, tel que décrit ci-dessus, les dispositifs utilisés dans un ajustement de pH n'entrent pas en contact avec l'échantillon (12), de sorte que les facteurs de contamination pendant l'ajustement du pH peut être réduite au minimum.
PCT/JP2012/057276 2012-03-22 2012-03-22 APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH WO2013140560A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/JP2012/057276 WO2013140560A1 (fr) 2012-03-22 2012-03-22 APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2012/057276 WO2013140560A1 (fr) 2012-03-22 2012-03-22 APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH

Publications (1)

Publication Number Publication Date
WO2013140560A1 true WO2013140560A1 (fr) 2013-09-26

Family

ID=49222054

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2012/057276 WO2013140560A1 (fr) 2012-03-22 2012-03-22 APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH

Country Status (1)

Country Link
WO (1) WO2013140560A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015029624A1 (fr) * 2013-08-30 2015-03-05 システム・インスツルメンツ株式会社 Dispositif d'ajustement automatique du ph
EP3719607A1 (fr) * 2019-04-02 2020-10-07 Covestro Deutschland AG Dispositif de conteneur intelligent, outil de transport, terminal utilisateur et système de gestion

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0386251A (ja) * 1989-08-28 1991-04-11 Todoroki Sangyo Kk 化学反応制御装置
JP2001249134A (ja) * 1999-12-28 2001-09-14 Matsushita Electric Ind Co Ltd タンパク質濃度計測用試薬、これを用いたタンパク質濃度計測方法および尿検査方法
JP2004085146A (ja) * 2002-08-29 2004-03-18 Miura Co Ltd ボイラ装置の腐食抑制およびスケール生成抑制方法
JP2005195412A (ja) * 2004-01-06 2005-07-21 Dkk Toa Corp Ｃｏｄ計用エアーノズル式自動滴定装置

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0386251A (ja) * 1989-08-28 1991-04-11 Todoroki Sangyo Kk 化学反応制御装置
JP2001249134A (ja) * 1999-12-28 2001-09-14 Matsushita Electric Ind Co Ltd タンパク質濃度計測用試薬、これを用いたタンパク質濃度計測方法および尿検査方法
JP2004085146A (ja) * 2002-08-29 2004-03-18 Miura Co Ltd ボイラ装置の腐食抑制およびスケール生成抑制方法
JP2005195412A (ja) * 2004-01-06 2005-07-21 Dkk Toa Corp Ｃｏｄ計用エアーノズル式自動滴定装置

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHU YANBEI ET AL.: "Bibun Genso no Bunri Noshuku-yo Koso Chushutsu Zenjido Shori System no Kaihatsu", THE OCEANOGRAPHIC SOCIETY OF JAPAN KOEN YOSHISHU, vol. 2011, 14 March 2011 (2011-03-14), pages 159 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015029624A1 (fr) * 2013-08-30 2015-03-05 システム・インスツルメンツ株式会社 Dispositif d'ajustement automatique du ph
US9952606B2 (en) 2013-08-30 2018-04-24 System Instruments Co., Ltd. Automatic pH adjustment device
EP3719607A1 (fr) * 2019-04-02 2020-10-07 Covestro Deutschland AG Dispositif de conteneur intelligent, outil de transport, terminal utilisateur et système de gestion

Similar Documents

Publication Publication Date Title
US11703494B2 (en) Measuring device
US8477295B2 (en) Automated soil measurement device
Crompton Determination of anions: a guide for the analytical chemist
US20160103089A1 (en) Opto-Electochemical Sensing System for Monitoring and Controlling Industrial Fluids
Rocha et al. An improved flow system for spectrophotometric determination of anions exploiting multicommutation and multidetection
CN105190289A (zh) 通过荧光监测水硬度
CN104614370B (zh) 一种基于纳米金的快速检测亚硝酸根的方法
WO2013140560A1 (fr) APPAREIL AUTOMATIQUE DE RÉGLAGE DU pH
CN106537119A (zh) 使用光学测量的用于泡沫浮选过程的方法和装置
CN105445389B (zh) 校准色谱系统以及分析样品的自动化方法
Chaparro et al. A multisyringe flow-based system for kinetic–catalytic determination of cobalt (II)
CN203365401U (zh) 用于测定碳酸根和碳酸氢根离子的经济型半自动滴定装置
Huseyinli et al. Spectrophotometric determination of aluminium and indium with 2, 2′, 3, 4-tetrahydroxy-3′, 5′-disulphoazobenzene
KR101897373B1 (ko) ｐＨ 자동 조정 장치
WO2008012145A1 (fr) Système et procédé de mesures de titration colorimétrique
KR100414550B1 (ko) 다성분 용액의 농도 분석 시스템 및 방법
Bodo et al. Multiwavelength fluidic sensing of water-based solutions in a channel microslide with SWIR LEDs
Carnrick et al. Spectral interferences using the Zeeman effect for furnace atomic absorption spectroscopy
Zhu et al. Rapid automatic detection of water Ca, Mg elements using laser-induced breakdown spectroscopy
Tubino et al. Flow injection visible diffuse reflectance quantitative analysis of nickel
Trojanowicz et al. Multicomponent analysis with a computerized flow injection system using LED photometric detection
Micić et al. Application of tartrazine for sensitive and selective kinetic determination of Cu (II) traces
Zhou et al. A Nonlinear Integrated Modeling Method of Extended Kalman Filter Based on Adaboost Algorithm
CN217846060U (zh) 一种水中锰离子浓度测定装置
WO2015198151A2 (fr) Dispositif de titrage colorimétrique automatique équipé d'une sonde non invasive

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12871805

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 12871805

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: JP