WO2016008369A1 - Appareil d'analyse automatique continue à paramètres multiples pour tester la qualité de l'eau d'une chaudière industrielle et procédé d'analyse pour celui-ci - Google Patents

Appareil d'analyse automatique continue à paramètres multiples pour tester la qualité de l'eau d'une chaudière industrielle et procédé d'analyse pour celui-ci Download PDF

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WO2016008369A1
WO2016008369A1 PCT/CN2015/083420 CN2015083420W WO2016008369A1 WO 2016008369 A1 WO2016008369 A1 WO 2016008369A1 CN 2015083420 W CN2015083420 W CN 2015083420W WO 2016008369 A1 WO2016008369 A1 WO 2016008369A1
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electrode
standard
titration
water quality
industrial boiler
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PCT/CN2015/083420
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English (en)
Chinese (zh)
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杨麟
余芬
杜玉辉
刘娟
赵军明
孙婷婷
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广州特种承压设备检测研究院
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Publication of WO2016008369A1 publication Critical patent/WO2016008369A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor

Definitions

  • the invention relates to a water treatment technology, in particular to a multi-project continuous automatic analysis device for industrial boiler water quality detection and an analysis method thereof.
  • alkalinity is further divided into phenolphthalein alkalinity and total alkalinity.
  • the pH value and alkalinity are too small, which may cause acid corrosion of the metal in contact with water.
  • the pH value and alkalinity are too large, which may cause alkaline corrosion of the metal in contact with water.
  • Industrial boiler water also needs to control the impurity concentration not to exceed the limit, and the impurity concentration exceeds the limit, which may also accelerate metal corrosion and cause scaling.
  • Chloride ion is the most stable of all impurities, and the chloride ion concentration is easy to detect.
  • the concentration of chloride ions is generally controlled in the industry to control the impurity concentration.
  • oxygenation can cause oxygen corrosion in industrial boilers
  • sulfite is the most commonly used oxygen scavenger, so industrial boiler water needs to control sulfite concentration.
  • Excessive hardness (calcium, magnesium ions) can cause industrial boilers to scale easily, so industrial boiler water needs to control hardness.
  • the dissolved solids represent the content of dissolved impurities in the water, and the dissolved solids content is usually calculated by the solid conductivity ratio after determining the electrical conductivity. The larger the dissolved solids, the larger the impurity content in the water, and the smaller the impurity content, so the industrial boiler uses water to detect dissolved solids.
  • GB/T 1576 "Industrial Boiler Water Quality" lists dissolved solids, pH, phenolic alkalinity, total alkalinity, chloride ion concentration, hardness, sulfite concentration, etc. Enter the regular monitoring project.
  • Potentiometric titration is a method of determining the end point of titration by measuring the change of potential during the titration. Compared with the direct potentiometry, potentiometric titration does not require accurate measurement of the electrode potential. Potentiometric titration is based on A sudden jump in the electrode potential to indicate the end point of the titration.
  • the existing dissolved solids, pH, phenolic alkalinity, full alkalinity, chloride ion, hardness, and sulfite detection processes are separately performed.
  • the detection process is as follows:
  • the conductivity electrode After collecting a certain volume of the sample to be tested, the conductivity electrode is placed in the sample, and the conductivity of the sample transmits a potential signal to the host. After the host converts the potential signal, the conductivity value of the sample is displayed. Based on the solid conductivity ratio, the content of dissolved solids was calculated.
  • the pH electrode After collecting a certain volume of the sample to be tested, the pH electrode is placed in the sample, and the pH value of the sample will transmit a potential signal to the host. After the host converts the potential signal, the pH value of the sample is displayed.
  • the pH electrode After collecting a certain volume of the sample to be tested, the pH electrode is placed in the sample, and the sulfuric acid standard solution is added dropwise to the sample until the pH falls to a certain limit, and the alkali is calculated by the volume of the sample to be tested, the volume of the standard acid solution, and the concentration. Degree value.
  • the result of setting the limit value to pH 8.0-8.3 is phenolphthalein alkalinity
  • the result of setting the pH to 4.0-4.3 is the full alkalinity.
  • the chloride ion concentration value is calculated by the volume of the sample to be tested, the volume of the silver nitrate standard solution, and the concentration thereof.
  • the existing industrial boiler water quality testing technology is mostly in accordance with the national standard method.
  • the seven projects are in accordance with GB/T 6904-2008 "Determination of pH in industrial circulating cooling water and boiler water", GB/T 1576-2008 “Industrial boiler Water quality” Appendix H alkalinity determination, GB/T 1576-2008 “Industrial boiler water quality” Appendix E Indirect determination of dissolved water in pot water, GB/T 1576-2008 “Industrial boiler water quality” Appendix I Determination of sulfite ( Iodometric method), GB/T 6909-2009 “Boiler water and cooling water analysis method hardness determination”, GB/T 15453-2008 "industrial circulating cooling water and determination of chloride ion in boiler water” independent testing.
  • One of the technical problems to be solved by the present invention is to detect the dissolved solids, pH value, phenolic alkalinity, total alkalinity, chloride ion concentration, hardness, and sulfite concentration of the industrial boiler water according to the prior art described above.
  • the defect of low efficiency of the prior art provides a multi-project continuous automatic analysis device for industrial boiler water quality detection and an analysis method thereof, and the detection items include dissolved solid matter, pH value, phenolphthalein alkalinity, full alkalinity, chloride ion Concentration, hardness and sulfite concentration.
  • a multi-item continuous automatic analysis device for industrial boiler water quality detection which comprises a container, a potentiometric titrator main unit, five electrodes and four dosing units; the five electrodes The electrodes are a conductivity electrode, a pH electrode, a silver electrode, a platinum electrode and a calcium electrode, and the four liquid adding units are a standard acid liquid adding unit, a silver nitrate standard liquid adding unit, a standard potassium iodate-potassium iodide adding unit, and EDTA standard liquid adding unit; the five electrodes are placed in the container, the liquid outlets of the four liquid adding units are placed in the container, the potentiometric titrator main unit has five electrode interfaces, the five electrodes The interface is respectively connected with a conductivity electrode, a pH electrode, a silver electrode, a platinum electrode and a calcium electrode, and the potentiometric titrator has a built-in control system for
  • the potentiometric titrator main unit further includes a communication interface connected to the computer, and the control system is connected to the computer through the communication interface.
  • an electrode protection unit for accommodating and fixing the five electrodes is further included.
  • a titration stand provided with a stirrer is placed, the container being placed on the titration stand.
  • the container is a measuring cup.
  • step c after acidifying the sample to be tested in step c, performing sulfite potential titration, and collecting the number
  • step d turn off the platinum electrode, turn on the calcium electrode and EDTA standard liquid dosing unit, will complete step d
  • the positive effect of the present invention is that the invention integrates seven independent detection processes into one detection process, and after completing one sampling, the conductivity (dissolved solid matter), pH value, and Determination of phenolphthalein alkalinity, total alkalinity, chloride ion concentration, sulfite concentration, hardness. The entire testing process was reduced to less than ten minutes.
  • the invention is characterized by improved detection efficiency, reduced personnel workload, and reduced sample consumption and standard consumption.
  • FIG. 1 is a schematic view showing a multi-item continuous automatic analyzing device for water quality testing of an industrial boiler according to the present invention.
  • FIG. 2 is a flow chart of an analytical method for continuously analyzing dissolved solids, pH, phenolphthalein alkalinity, total alkalinity, chloride ion concentration, sulfite concentration, and hardness according to the present invention.
  • Figure 3 is a phenolphthalein basicity titration curve of the examples.
  • Figure 4 is a full alkalinity titration curve of the examples.
  • Figure 5 is a chloride ion titration curve of the examples.
  • Figure 6 is a hardness titration curve of the example.
  • 1-standard acid liquid adding unit 2- silver nitrate standard liquid adding unit; 3-standard potassium iodate-potassium iodide adding unit; 4-EDTA standard liquid adding unit; 5-conducting electrode; 6-pH Electrode; 7-silver electrode; 8-calcium electrode; 9-platinum electrode.
  • the multi-item continuous automatic analysis device for the industrial boiler water quality detection of the present embodiment comprises a container, a potentiometric titrator main unit, five electrodes, four dosing units and a titration stand; the five electrodes are respectively Conductive electrode 5, pH electrode 6, silver electrode 7, platinum electrode 9 and calcium electrode 8, the four liquid adding units are standard acid liquid adding unit 1, silver nitrate standard liquid adding unit 2, standard potassium iodate - Potassium iodide addition unit 3 and EDTA standard solution addition unit 4.
  • the container is placed on a titration stand and a stirrer is provided on the titration stand.
  • the five electrodes are placed in a container for collecting data of the sample being tested in the container.
  • the liquid outlets of the four liquid adding units are placed in the container, and the container is filled with liquid.
  • the potentiometric titrator has five electrode interfaces and a communication interface connected to the computer. The five electrode interfaces respectively connect the conductivity electrode 5, the pH electrode 6, the silver electrode 7, the platinum electrode 9 and the calcium electrode 8, respectively.
  • the initial pH value of the sample to be measured For the application of the conductivity data, the initial pH value of the sample to be measured, the real-time pH value during the phenolphthalein alkalinity and the full alkalinity titration, the silver electrode 7 potential value during the chloride ion potentiometric titration process, and the sulfite potential titration process
  • the potentiometric titrator has a built-in titration parameter control and data output control system.
  • the potentiometric titrator host model with the control system is Metrohm 905Titrando.
  • the control system is connected to the computer through the communication interface, and the obtained phenolphthalein alkali titration, full alkalinity titration, chloride ion potentiometric titration, sulfite potential titration, hardness potential titration data are displayed on the computer and data processing is performed, including the diagram. 3. Even if the titration graphs of Figures 4, 5 and 6 are displayed.
  • the container is a measuring cup for accommodating a set volume of the sample to be tested.
  • the device further includes an electrode protection unit that respectively accommodates and fixes the electrodes after the analysis. After the analysis is completed, the electrodes are rinsed with distilled water and then housed and fixed in the electrode protection unit.
  • the continuous automatic analysis method for multi-projects in the water quality testing of industrial boilers of the present embodiment is analyzed for industrial boiler water, and the dissolved solid matter, pH value, phenolphthalein alkalinity, total alkalinity, and chloride ion concentration are analyzed.
  • sulfite concentration, hardness, specific analysis methods include the following steps:
  • the container containing the set volume of the sample to be tested is fixed on the titration stand of the potentiometric titrator, and the conductivity electrode 5 collects the conductivity of the sample to be tested.
  • the pH electrode 6 collects the initial pH value of the sample to be tested and the real-time pH value of the alkalinity titration process.
  • the alkalinity titration is carried out in sequence: phenolphthalein titration, the titration end point pH is 8.0-8.3; and the full alkalinity titration, the titration end point
  • the pH is 4.0-4.3.
  • the standard acid phenolphthalein titration solution volume and the full alkalinity titration solution volume in the standard acid liquid addition unit 1 are respectively read to calculate the phenolphthalein alkalinity and the full alkalinity.
  • the initial pH value collected by the pH electrode 6 is the pH value of the sample to be tested;
  • the standard acid solution refers to the acidic solution of a known concentration.
  • the standard acid solution can also be a standard solution of nitric acid.
  • the silver electrode 7 is turned off, the platinum electrode 9, the standard acid liquid addition unit and the standard potassium iodate-potassium iodide liquid addition unit 3 are turned on.
  • 20 mL of a standard acid solution was added to acidify the sample.
  • the sulfite potential titration is carried out in the acidified sample by using the standard potassium iodate-potassium iodide adding unit 3, and the platinum electrode 9 is used to collect the potential value of the platinum electrode 9 during the titration of sulfurous acid, and the sulfite potential titration is dynamic titration.
  • the titration end point is the jump point of the platinum electrode 9 potential, and the consumption volume of the potassium iodate-potassium iodide standard solution in the standard potassium iodate-potassium iodide liquid addition unit 3 is read at the end point of the titration, and the sulfite concentration is calculated.
  • the potassium iodate-potassium iodide standard solution refers to a potassium iodate-potassium iodide solution having a known concentration or titer.
  • the platinum electrode 9 is turned off, and the calcium electrode 8 and the EDTA standard liquid addition unit 4 are turned on.
  • the endpoint is the jump point of the potential of the calcium electrode 8, and the consumption volume of the EDTA standard solution in the EDTA standard solution dosing unit 4 at the end point of the titration is read, and the hardness is calculated.
  • the EDTA standard solution refers to an EDTA solution having a known concentration or titer.
  • Chloride ion titration parameter setting Dynamic titration mode (DET U): (1) Start condition: initial measurement value signal drift off, minimum waiting time 5s, maximum waiting time 10s, dosing speed 5mL/min; (2) titration parameters: Accepted measurement value signal drift 30mV/min, minimum waiting time 2s, maximum waiting time 20s; measuring point density 4; minimum increment 10 ⁇ L, maximum increment off, maximum filling rate; (3) titration end point: silver electrode potential The first jump point.
  • Dynamic titration mode (DET U): (1) Start condition: initial measurement value signal drift off, minimum waiting time 5s, maximum waiting time 10s, dosing speed 5mL/min; (2) titration parameters: Accepted measurement value signal drift 30mV/min, minimum waiting time 2s, maximum waiting time 20s; measuring point density 4; minimum increment 10 ⁇ L, maximum increment off, maximum filling rate; (3) titration end point: silver electrode potential The first jump point.
  • Nitrite titration parameter setting Dynamic titration mode (DET U): (1) Start condition: initial measurement value signal drift off, minimum waiting time 5s, maximum waiting time 10s, dosing speed 5mL/min; (2) titration parameters : Accept the measured value signal drift 30mV/min, minimum waiting time 2s, maximum waiting time 20s; measuring point density 4; minimum increment 10 ⁇ L, maximum increment off, maximum filling rate; (3) titration end point: platinum electrode potential The first jump point.
  • Dynamic titration mode (DET U): (1) Start condition: initial measurement value signal drift off, minimum waiting time 5s, maximum waiting time 10s, dosing speed 5mL/min; (2) titration parameters : Accept the measured value signal drift 30mV/min, minimum waiting time 2s, maximum waiting time 20s; measuring point density 4; minimum increment 10 ⁇ L, maximum increment off, maximum filling rate; (3) titration end point: platinum electrode potential The first jump point.
  • Hardness Titration Parameter Setting Static Titration Mode (MET U): (1) Start Condition: Initial Measurement Signal drift off, minimum waiting time 5s, maximum waiting time 10s, filling speed 5mL/min; (2) titration parameters: accept measurement signal drift 30mV/min, minimum waiting time 2s, maximum waiting time 20s; measuring point density 4 Minimum increment 10 ⁇ L, maximum incremental off, maximum dosing rate; (3) Titration end point: the first jump point of the calcium electrode potential.
  • pH (25 ° C) pH electrode collects the initial pH of the sample being tested. (1-1)
  • Phenolphthalein, mmol/L Phenolphthalein, mmol/L:
  • V 1 is a titration liquid volume (mL) of the sulfuric acid standard solution in the phenolphthalein basic titration
  • V S the set volume of the sample to be tested, ie the sample volume (mL),
  • V 2 is the titration liquid volume (mL) of the sulfuric acid standard solution in the full alkalinity titration
  • V S the set volume of the sample to be tested, ie the sample volume (mL),
  • V 3 the volume of consumption of silver nitrate standard solution (mL)
  • V S - the set volume of the sample to be tested, ie the sample volume (mL).
  • V S - the set volume of the sample to be tested, ie the sample volume (mL).
  • V S - the set volume of the sample to be tested, ie the sample volume (mL).
  • the detection and analysis process is: measuring 80 mL of the uniformly mixed test sample in the measuring cup, and the concentration of the sulfuric acid standard solution is
  • the sulfuric acid standard solution, silver nitrate standard solution, potassium iodate-potassium iodide standard solution and EDTA standard solution are respectively added to different
  • the liquid adding unit, the electric conducting electrode, the pH electrode, the silver electrode, the platinum electrode, and the calcium electrode are mounted on the titration stand, and a stirrer is arranged on the titration stand to start titration.
  • two parallel measurements were used, and the data of two parallel titrations are shown in Table 1:

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Abstract

La présente invention concerne un appareil d'analyse automatique continu à paramètres multiples pour tester la qualité de l'eau d'une chaudière industrielle et un procédé d'analyse pour celui-ci. L'appareil comprend un récipient, un hôte de titrage potentiométrique, cinq électrodes, et quatre unités de distribution de liquide ; les cinq électrodes sont une électrode de conductivité, une électrode de pH, une électrode d'argent, une électrode de platine, et une électrode de calcium ; les quatre unités de distribution de liquide sont une unité de distribution de liquide acide standard, une unité de distribution de liquide de nitrate d'argent standard, une unité de distribution de liquide d'iodate de potassium-iodure de potassium standard, et un distributeur de liquide standard d'EDTA ; les cinq électrodes sont disposées à l'intérieur du récipient, et les sorties de liquide des quatre unités de distribution de liquide sont toutes agencées à l'intérieur du récipient ; l'hôte de titrage potentiométrique a cinq interfaces d'électrode, et les cinq interfaces d'électrode sont connectées respectivement à l'électrode de conductivité, l'électrode de pH, l'électrode d'argent, l'électrode de platine, et l'électrode de calcium ; il est disposé à l'intérieur de l'hôte de titrage potentiométrique un système de commande pour commander les paramètres de titrage et la sortie des données.
PCT/CN2015/083420 2014-07-15 2015-07-07 Appareil d'analyse automatique continue à paramètres multiples pour tester la qualité de l'eau d'une chaudière industrielle et procédé d'analyse pour celui-ci WO2016008369A1 (fr)

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CN102183520A (zh) * 2011-04-26 2011-09-14 东北电力大学 基于溶液图像技术的水质硬度在线测量装置及其测量方法
CN102590318A (zh) * 2012-02-24 2012-07-18 深圳市特种设备安全检验研究院 连续分析pH值、酚酞碱度、总碱度和氯离子浓度的分析方法及装置
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CN203376309U (zh) * 2013-07-31 2014-01-01 厦门百谷生物工程有限公司 多参数水质检测仪
CN104101722A (zh) * 2014-07-15 2014-10-15 广州特种承压设备检测研究院 工业锅炉水质检测中多项目连续自动分析装置及其分析方法

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