CN104101722B - Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection - Google Patents
Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection Download PDFInfo
- Publication number
- CN104101722B CN104101722B CN201410336615.1A CN201410336615A CN104101722B CN 104101722 B CN104101722 B CN 104101722B CN 201410336615 A CN201410336615 A CN 201410336615A CN 104101722 B CN104101722 B CN 104101722B
- Authority
- CN
- China
- Prior art keywords
- electrode
- liquid feeding
- feeding unit
- titration
- titer
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000004458 analytical method Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 title claims abstract description 24
- 238000013459 approach Methods 0.000 title claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 77
- 238000004448 titration Methods 0.000 claims abstract description 70
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Inorganic materials [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 47
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 45
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002253 acid Substances 0.000 claims abstract description 25
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 23
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 claims abstract description 21
- 239000004332 silver Substances 0.000 claims abstract description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011575 calcium Substances 0.000 claims abstract description 19
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 19
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 18
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 29
- 238000003918 potentiometric titration Methods 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 239000012086 standard solution Substances 0.000 claims description 24
- 241000370738 Chlorion Species 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 description 21
- 238000012360 testing method Methods 0.000 description 18
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 14
- 239000007787 solid Substances 0.000 description 14
- 238000005259 measurement Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 238000000954 titration curve Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- -1 Nitrite anions Chemical class 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- SXYCCJAPZKHOLS-UHFFFAOYSA-N chembl2008674 Chemical compound [O-][N+](=O)C1=CC=C2C(N=NC3=C4C=CC=CC4=CC=C3O)=C(O)C=C(S(O)(=O)=O)C2=C1 SXYCCJAPZKHOLS-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- HIEFXWXCLCHBPG-UHFFFAOYSA-L dipotassium;diiodide Chemical compound [K+].[K+].[I-].[I-] HIEFXWXCLCHBPG-UHFFFAOYSA-L 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000004313 potentiometry Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses entry automatic continuous analysis device and analytical approach thereof in a kind of Industrial Boiler water quality detection, this device it comprise container, potentiometric titrimeter main frame, five electrodes and four liquid feeding unit; These five electrodes are respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, and these four liquid feeding unit are respectively standard acid solution liquid feeding unit, silver nitrate titer liquid feeding unit, standard Potassiumiodate-potassium iodide liquid feeding unit and EDTA titer liquid feeding unit; These five electrodes are placed in this container, the liquid outlet of these four liquid feeding unit is all placed in this container, this potentiometric titrimeter main frame is with five electrode interfaces, these five electrode interfaces are connected respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, the control system that the built-in titration parameters of this potentiometric titrimeter main frame controls and data export.
Description
Technical field
The present invention relates to a kind of water technology, particularly relate to entry automatic continuous analysis device and analytical approach thereof in a kind of Industrial Boiler water quality detection.
Background technology
Industrial Boiler water need keep the basicity of certain numerical value, and object is corrosion in order to slow down metallic conduit and fouling.According to national technical standard, basicity is divided into again phenolphthalein alkalinity and full basicity.PH value, basicity are less than normal, and the metal contacted with water may be caused to produce sour corrosion; Otherwise pH value, basicity are bigger than normal, the metal contacted with water may be caused to produce alkaline corrosion.Industrial Boiler water also needs to control impurity concentration and is no more than limit value, and impurity concentration exceedes limit value, also may accelerate metal erosion, cause fouling.Chlorion is that in all impurity, performance is the most stable, and chlorine ion concentration is convenient to detect, and therefore industrially generally controls impurity concentration to control chlorine ion concentration.Owing to can cause Industrial Boiler oxygen corrosion containing oxygen, sulphite is the most frequently used deoxygenation medicament, and therefore Industrial Boiler water also needs to control inferior sulfate radical concentration.Hardness (calcium, magnesium ion) too high meeting causes the easy fouling of Industrial Boiler, and therefore Industrial Boiler water also needs to control hardness.Dissolved solid represents dissolved matter impurity content in water, usually after measuring conductivity, calculates dissolved solid content admittedly to lead than method.Dissolved solid is larger, and illustrate that the impurity content in water is large, otherwise impurity content is little, therefore Industrial Boiler water detects dissolved solid.
Therefore, in order to slow down corrosion of metal and reduce fouling, GB/T1576 " Industrial Boiler water quality " lists routine monitoring project in the project such as dissolved solid, pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, hardness, inferior sulfate radical concentration.
Mostly existing Industrial Boiler water quality inspection technique is to be analyzed by manual inspection or the potentiometric titration of individual event object.Seven projects have detected needs more than one hour consuming time.
Potentiometric titration is that compare with direct potentiometric method, potentiometric titration does not need potential electrode potential value accurately by measuring potential change to determine the method for titration end-point in titration process, and potentiometric titration leans on the hop of electrode potential to indicate titration end-point.
Existing dissolved solid, pH value, phenolphthalein alkalinity, full basicity, chlorion, hardness, inferior sulfate radical testing process are separately carried out separately, and testing process is as follows:
1, dissolved solid measures (admittedly leading than method)
After gathering the testing sample of certain volume, conductance electrode is put into sample, and conductivity can transmit electric potential signal to main frame, and main frame, after electric potential signal conversion, demonstrates the conductivity value of sample.According to admittedly leading ratio, calculate the content of dissolved solid.
2, pH value measures
After gathering the testing sample of certain volume, pH electrode is put into sample, and sample pH can transmit electric potential signal to main frame, and main frame, after electric potential signal conversion, demonstrates the pH value of sample.
3, phenolphthalein alkalinity and full Basicity Determination
After gathering the testing sample of certain volume, pH electrode is put into sample, in sample, drips sulfuric acid standard solution, until pH drops to a threshold value, calculate basicity value with testing sample volume, standard acid consumption volume and concentration.Limit value is set as that the result of pH value 8.0-8.3 is phenolphthalein alkalinity, and limit is set as that the result of pH value 4.0-4.3 is full basicity.
4, determination of chloride ion
After gathering the testing sample of certain volume, regulate sample pH to neutral or acid, drip the potentiometric titration that silver nitrate standard solution carries out chlorion in solution, until hop point occurs, titration stops.Chlorine ion concentration value is calculated with testing sample volume, silver nitrate standard solution consumption volume and concentration thereof.
5, Determination of Hardness
After gathering the testing sample of certain volume, regulate sample pH to 10.0 ± 0.1, using eriochrome black T as indicator, in solution, drip disodium ethylene diamine tetraacetate (EDTA) standard solution until solution is terminal in blueness.Hardness number is calculated with testing sample volume, EDTA standard solution consumption volume and concentration thereof.
6, sulfite determination
After gathering the testing sample of certain volume, add 1mL starch indicator and 1mL hydrochloric acid solution (1+1), shake up.Be titrated to micro-blueness with Potassiumiodate-potassium iodide standard solution, be titration end-point.Inferior sulfate radical concentration value is calculated with testing sample volume, Potassiumiodate-potassium iodide standard solution consumption volume and concentration thereof.
Mostly existing Industrial Boiler water quality inspection technique is according to national standard method, seven projects are respectively according to GB/T6904-2008 the mensuration of pH value " in industrial circulating cooling water and the boiler feed water ", the mensuration of GB/T1576-2008 " Industrial Boiler water quality " annex H basicity, the indirect determination of GB/T1576-2008 " Industrial Boiler water quality " annex E pot water dissolved solid, the mensuration (iodimetric titration) of GB/T1576-2008 " Industrial Boiler water quality " annex I sulphite, GB/T6909-2009 " mensuration of boiler feed water and chilled water analytical approach hardness ", GB/T15453-2008 " industrial circulating cooling water and boiler feed water in chloride ion conductor " independent detection.Skilled testing staff is single completes seven projects, needs more than 1 hour consuming time, and not only detection efficiency is low and there is many limitations.As by indicator and color change acuity, by precipitation adsorption, disturb by strict pH titration environment and various anions and canons, by the impact etc. of the manual titration human factor of analyst.
Summary of the invention
One of technical matters that patent of the present invention will solve is, above-mentioned when detecting the dissolved solid of Industrial Boiler water, pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, hardness, inferior sulfate radical concentration for prior art, the defect that prior art efficiency is lower, there is provided entry automatic continuous analysis device and analytical approach thereof in a kind of Industrial Boiler water quality detection, its test item comprises dissolved solid, pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, hardness and inferior sulfate radical concentration.
The present invention solves this technical problem adopted technical scheme: entry automatic continuous analysis device in a kind of Industrial Boiler water quality detection, and it comprises container, potentiometric titrimeter main frame, five electrodes and four liquid feeding unit; These five electrodes are respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, and these four liquid feeding unit are respectively standard acid solution liquid feeding unit, silver nitrate titer liquid feeding unit, standard Potassiumiodate-potassium iodide liquid feeding unit and EDTA titer liquid feeding unit; These five electrodes are placed in this container, the liquid outlet of these four liquid feeding unit is all placed in this container, this potentiometric titrimeter main frame is with five electrode interfaces, these five electrode interfaces are connected respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, the control system that the built-in titration parameters of this potentiometric titrimeter main frame controls and data export.
Further, this potentiometric titrimeter main frame also comprises a communication interface be connected with computing machine, and this control system is connected with computing machine by this communication interface.
Further, also comprise for accommodating and fix the electrode protection unit of these five electrodes.
Further, also comprise the titration platform being provided with stirrer, this container is placed on this titration platform.
Particularly, this container is measuring cup.
As another object of the present invention, additionally provide a kind of entry automatic continuous analysis method in Industrial Boiler water quality detection, its step is as follows successively:
A, gather the conductivity of sample by conductance electrode;
B, closedown conductance electrode, open pH electrode and standard acid solution liquid feeding unit, carries out phenolphthalein alkalinity titration and full basicity titration to this sample, and image data;
C, closedown pH electrode, open silver electrode and silver nitrate titer liquid feeding unit, carry out chlorion potentiometric titration in the sample of completing steps b, and image data;
D, closedown silver electrode, open platinum electrode, standard acid solution liquid feeding unit and standard Potassiumiodate-potassium iodide liquid feeding unit, after the sample acidifying of completing steps c, carry out inferior sulfate radical potentiometric titration, and image data; E, closedown platinum electrode, open calcium electrode and EDTA titer liquid feeding unit, carry out hardness potentiometric titration after the pH of the sample of completing steps d is adjusted to 10, and image data.
Preferably, the standard acid solution in this standard acid solution liquid feeding unit is sulfuric acid standard solution, and the concentration of sulfuric acid standard solution is C
1/2H2SO4=0.1000mol/L; The titer of the silver nitrate titer in this silver nitrate titer liquid feeding unit is T=3.34mg/mL; The titer of the Potassiumiodate-potassium iodide titer in this standard Potassiumiodate-potassium iodide liquid feeding unit is T=1.0mg/mL; The titer of the EDTA titer in this EDTA titer liquid feeding unit is T=0.1mol/L.
Compared with prior art, good effect of the present invention be the present invention seven independently testing process comprehensively become a testing process, after realizing primary sample, complete the detection of conductivity (dissolved solid), pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, inferior sulfate radical concentration, hardness successively.Whole test process is consuming time foreshorten to ten minutes within.This characteristic feature of an invention improves detection efficiency, reduces person works's amount, save sample consumption and standard items consumption simultaneously.
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is entry automatic continuous analysis device schematic diagram in Industrial Boiler water quality detection of the present invention.
Fig. 2 is the analytical approach process flow diagram that the present invention analyzes dissolved solid, pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, inferior sulfate radical concentration, hardness continuously.
Fig. 3 is the phenolphthalein alkalinity titration curve of embodiment.
Fig. 4 is the full basicity titration curve of embodiment.
Fig. 5 is the chlorion titration curve of embodiment.
Fig. 6 is the Hardness Titration curve of embodiment.
Wherein, 1-standard acid solution liquid feeding unit; 2-silver nitrate titer liquid feeding unit; 3-standard Potassiumiodate-potassium iodide liquid feeding unit; 4-EDTA titer liquid feeding unit; 5-conductance electrode; 6-pH electrode; 7-silver electrode; 8-calcium electrode; 9-platinum electrode.
Embodiment
Embodiment
As shown in Figure 1, entry automatic continuous analysis device in the Industrial Boiler water quality detection of the present embodiment, it comprises container, potentiometric titrimeter main frame, five electrodes, four liquid feeding unit and titration platforms; These five electrodes are respectively conductance electrode 5, pH electrode 6, silver electrode 7, platinum electrode 9 and calcium electrode 8, and these four liquid feeding unit are respectively standard acid solution liquid feeding unit 1, silver nitrate titer liquid feeding unit 2, standard Potassiumiodate-potassium iodide liquid feeding unit 3 and EDTA titer liquid feeding unit 4.
This container is placed on titration platform, and titration platform is provided with stirrer.These five electrodes are placed in container, for the data of sample in collection container.The liquid outlet of these four liquid feeding unit is all placed in container, to container liquid feeding.This potentiometric titrimeter main frame is with five electrode interfaces and a communication interface be connected with computing machine, these five electrode interfaces are connected respectively conductance electrode 5, pH electrode 6, silver electrode 7, platinum electrode 9 and calcium electrode 8, it gathering real-time pH value in conductivity data, collection sample initial pH value and phenolphthalein alkalinity and full basicity titration process to being applied to respectively, gathering silver electrode 7 potential value of chlorion potentiometric titration process, gathering platinum electrode 9 current potential of inferior sulfate radical potentiometric titration process, and gathers calcium electrode 8 current potential in hardness potentiometric titration process.The control system that the built-in titration parameters of this potentiometric titrimeter main frame controls and data export.Preferably, the potentiometric titrimeter main frame model of described this control system built-in is Metrohm 905 Titrando.Control system is connected with computing machine by communication interface, even if obtained phenolphthalein alkalinity titration, full basicity titration, chlorion potentiometric titration, inferior sulfate radical potentiometric titration, hardness Potentiometric Data are shown and make data processing on computing machine, even if comprise the display of the titration curve figure of Fig. 3, Fig. 4, Fig. 5 and Fig. 6.
Preferably, this container is the measuring cup of the sample of accommodating setting volume to the present embodiment.
This device also comprises accommodating respectively after analysis and the electrode protection unit of fixed electorde.After analysis, with accommodating respectively after each electrode of distilled water flushing and be fixed in this electrode protection unit.
As shown in Figure 2, entry automatic continuous analysis method in the Industrial Boiler water quality detection of the present embodiment, its analytic target is Industrial Boiler water, analyze its dissolved solid, pH value, phenolphthalein alkalinity, full basicity, chlorine ion concentration, inferior sulfate radical concentration, hardness, specific analytical method comprises the following steps:
A, be fixed on the titration platform of potentiometric titrimeter by the container that setting volume sample is housed, conductance electrode 5 gathers the conductivity of sample.
B, closedown conductance electrode 5, open pH electrode 6 and standard acid solution liquid feeding unit 1.PH electrode 6 gathers the initial pH value of sample and the real-time pH value of basicity titration process, and basicity titration is carried out successively: phenolphthalein alkalinity titration, and its titration end-point pH is 8.0-8.3; And full basicity titration, its titration end-point pH is 4.0-4.3, when arriving titration end-point, read the standard acid solution phenolphthalein alkalinity volumetric solution volume in standard acid solution liquid feeding unit 1 and full basicity volumetric solution volume respectively, calculate phenolphthalein alkalinity and full basicity, the initial pH value that pH electrode 6 gathers is the pH value of sample; Standard acid solution refers to the acid solution of concentration known, and preferably, standard acid solution is sulfuric acid standard solution to the present embodiment, and the concentration of sulfuric acid standard solution is C
1/2H2SO4=0.1000mol/L.Standard acid solution also can be nitric acid standard solution.
C, closedown pH electrode 6 open silver electrode 7, in the sample that above-mentioned full basicity titration is complete, chlorion potentiometric titration is carried out with silver nitrate titer liquid feeding unit 2, silver electrode 7 gathers silver electrode 7 electrode potential value in chlorion potentiometric titration process, chlorion potentiometric titration is dynamic titration, titration end-point is the hop point of silver electrode 7 current potential, when reading titration end-point, the consumption volume of silver nitrate titer in silver nitrate titer liquid feeding unit 2, calculates chlorine ion concentration.Silver nitrate titer refers to the liquor argenti nitratis ophthalmicus of concentration known or titer, and in the present embodiment, the titer of silver nitrate titer is T=3.34mg/mL.
D, closedown silver electrode 7, open platinum electrode 9, standard acid solution liquid feeding unit and standard Potassiumiodate-potassium iodide liquid feeding unit 3.Detect in complete sample to above-mentioned chlorine ion concentration and add 20mL standard acid solution, acidifying is carried out to sample.Inferior sulfate radical potentiometric titration is carried out with in the standard Potassiumiodate-sample of potassium iodide liquid feeding unit 3 after acidifying, platinum electrode 9 gathers platinum electrode 9 potential value in sulphurous acid potentiometric titration process, inferior sulfate radical potentiometric titration is dynamic titration, titration end-point is the hop point of platinum electrode 9 current potential, when reading titration end-point, the consumption volume of Potassiumiodate-potassium iodide titer in standard iodine acid potassium-potassium iodide liquid feeding unit 3, calculates inferior sulfate radical concentration.Potassiumiodate-potassium iodide titer refers to the Potassiumiodate-liquor kalii iodide of concentration known or titer, and in the present embodiment, the titer of Potassiumiodate-potassium iodide titer is T=1.0mg/mL.
E, closedown platinum electrode 9, open calcium electrode 8 and EDTA titer liquid feeding unit 4.In the sample that above-mentioned inferior sulfate radical Concentration Testing is complete, add proper volume ammoniacal liquor buffer solution, make the pH of sample reach 10.In the sample of pH=10, hardness potentiometric titration is carried out with EDTA titer liquid feeding unit 4, calcium electrode 8 gathers calcium electrode 8 potential value in EDTA potentiometric titration process, hardness potentiometric titration is static titration, titration end-point is the hop point of calcium electrode 8 current potential, when reading titration end-point, the consumption volume of EDTA titer in EDTA titer liquid feeding unit 4, calculates hardness.EDTA titer refers to the EDTA solution of concentration known or titer, and in the present embodiment, the titer of EDTA titer is T=0.1mol/L.
Carry out setting parameter before analysis, be specially:
Conductance measurement optimum configurations:
PH value, basicity titration parameters are arranged: setting endpoint titration pattern (SET pH) (1) starts condition: the initial pH value gathering sample; Signal drift: close; Stand-by period: 10s; Suspend 20s.(2) phenolphthalein alkalinity titration: setting titration end-point is pH=8.3; Dynamic titration, range of control is 2pH; Maximum liquid feeding speed 10mL/min; Minimum liquid feeding speed 25 μ L/min; Stopping criterion: drift about 50 μ L/min.(3) full basicity titration: setting titration end-point is pH=4.2; Dynamic titration, range of control is 1.5pH; Maximum liquid feeding speed 5mL/min; Minimum liquid feeding speed 25; Stopping criterion: drift about 50 μ L/min; The measurement point time interval: 2.0s.Temperature 25 DEG C.
Chlorion titration parameters is arranged: dynamically titration mode (DET U): (1) starts condition: initial measurement signal drift closes, minimum latency 5s, maximum latency 10s, liquid feeding speed 5mL/min; (2) titration parameters: accept measured value signal drift 30mV/min, minimum latency 2s, maximum latency 20s; Measurement point density 4; Smallest incremental 10 μ L, maximal increment closes, maximal value liquid feeding speed; (3) titration end-point: first hop point of silver electrode current potential.
Nitrite anions titration parameters is arranged: dynamically titration mode (DET U): (1) starts condition: initial measurement signal drift closes, minimum latency 5s, maximum latency 10s, liquid feeding speed 5mL/min; (2) titration parameters: accept measured value signal drift 30mV/min, minimum latency 2s, maximum latency 20s; Measurement point density 4; Smallest incremental 10 μ L, maximal increment closes, maximal value liquid feeding speed; (3) titration end-point: first hop point of platinum electrode current potential.
Hardness Titration optimum configurations: static titration mode (MET U): (1) starts condition: initial measurement signal drift closes, minimum latency 5s, maximum latency 10s, liquid feeding speed 5mL/min; (2) titration parameters: accept measured value signal drift 30mV/min, minimum latency 2s, maximum latency 20s; Measurement point density 4; Smallest incremental 10 μ L, maximal increment closes, maximal value liquid feeding speed; (3) titration end-point: first hop point of calcium electrode current potential.
The computing formula of the present embodiment is:
PH value (25 DEG C)=pH electrode gathers the initial pH value of sample.(1-1)
Phenolphthalein alkalinity, mmol/L:
Wherein, V
1---the volumetric solution volume (mL) of sulfuric acid standard solution in phenolphthalein alkalinity titration,
V
s---the setting volume of sample is also sample volume (mL),
---the concentration (mol/L) of sulfuric acid standard solution.
Full basicity, mmol/L:
Wherein, V
2---the volumetric solution volume (mL) of sulfuric acid standard solution in full basicity titration,
V
s---the setting volume of sample is also sample volume (mL),
---the concentration (mol/L) of sulfuric acid standard solution.
Chlorine ion concentration [Cl
-], mg/L:
Wherein: V
01---reagent blank (mL),
V
3---the consumption volume (mL) of silver nitrate titer,
T
1---the titer (mg/mL) of silver nitrate titer,
V
s---the setting volume of sample is also sample volume (mL).
Inferior sulfate radical concentration [SO
3 2-], mg/L:
Wherein: V
02---reagent blank (mL),
V
4---the consumption volume (mL) of Potassiumiodate-potassium iodide titer,
T
2---the titer (mg/mL) of Potassiumiodate-potassium iodide titer,
V
s---the setting volume of sample is also sample volume (mL).
Hardness, mmol/L:
Wherein: V
03---reagent blank (mL),
V
5---the consumption volume (mL) of Potassiumiodate-potassium iodide titer,
T
3---the titer (mg/mL) of Potassiumiodate-potassium iodide titer,
V
s---the setting volume of sample is also sample volume (mL).
Further, detecting analytic process is: measure sample that 80mL mixes in measuring cup, sulfuric acid concentration of standard solution is
silver nitrate standard solution titer is the reagent blank V of T=3.34mg/mL, silver nitrate
0=0.010mL, sulfuric acid standard solution, silver nitrate standard solution, Potassiumiodate-potassium iodide standard solution, EDTA standard solution are added different liquid feeding unit respectively, conductance electrode, pH electrode, silver electrode, platinum electrode, calcium electrode are arranged on titration platform, titration platform there is stirrer, starts titration.Adopt 2 replicate determinations in the present embodiment, the data of 2 parallel titration are in table 1:
Table 1 potentiometric titration detects data
According to the determination data of table 1, according to the computing formula of above-mentioned (1-1), (1-2), (1-3), (1-4), (1-5) and (1-6), calculate.The result of calculation of twice replicate determination is in table 2:
Table 2 measurement result
The present invention is not limited to above-mentioned embodiment, if do not depart from the spirit and scope of the present invention to various change of the present invention or modification, if these are changed and modification belongs within claim of the present invention and equivalent technologies scope, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. an entry automatic continuous analysis device in Industrial Boiler water quality detection, is characterized in that: it comprises container, potentiometric titrimeter main frame, five electrodes and four liquid feeding unit; These five electrodes are respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, and these four liquid feeding unit are respectively standard acid solution liquid feeding unit, silver nitrate titer liquid feeding unit, standard Potassiumiodate-potassium iodide liquid feeding unit and EDTA titer liquid feeding unit;
These five electrodes are placed in this container, the liquid outlet of these four liquid feeding unit is all placed in this container, this potentiometric titrimeter main frame is with five electrode interfaces, these five electrode interfaces are connected respectively conductance electrode, pH electrode, silver electrode, platinum electrode and calcium electrode, the control system that the built-in titration parameters of this potentiometric titrimeter main frame controls and data export.
2. entry automatic continuous analysis device in Industrial Boiler water quality detection as claimed in claim 1, it is characterized in that: this potentiometric titrimeter main frame also comprises a communication interface be connected with computing machine, this control system is connected with computing machine by this communication interface.
3. entry automatic continuous analysis device in Industrial Boiler water quality detection as claimed in claim 1, is characterized in that: also comprise for accommodating and fix the electrode protection unit of these five electrodes.
4. entry automatic continuous analysis device in Industrial Boiler water quality detection as claimed in claim 1, it is characterized in that: also comprise the titration platform being provided with stirrer, this container is placed on this titration platform.
5. entry automatic continuous analysis device in Industrial Boiler water quality detection as claimed in claim 1, is characterized in that: this container is measuring cup.
6. utilize an analytical approach for entry automatic continuous analysis device in Industrial Boiler water quality detection described in claim 1, it is characterized in that, its step is as follows successively:
A, gather the conductivity of sample by conductance electrode;
B, closedown conductance electrode, open pH electrode and standard acid solution liquid feeding unit, carries out phenolphthalein alkalinity titration and full basicity titration to this sample, and image data;
C, closedown pH electrode, open silver electrode and silver nitrate titer liquid feeding unit, carry out chlorion potentiometric titration in the sample of completing steps b, and image data;
D, closedown silver electrode, open platinum electrode, standard acid liquid feeding unit and standard Potassiumiodate-potassium iodide liquid feeding unit, after the sample acidifying of completing steps c, carry out inferior sulfate radical potentiometric titration, and image data;
E, closedown platinum electrode, open calcium electrode and EDTA titer liquid feeding unit, carry out hardness potentiometric titration after the pH of the sample of completing steps d is adjusted to 10, and image data.
7. utilize the analytical approach of entry automatic continuous analysis device in described Industrial Boiler water quality detection as claimed in claim 6, it is characterized in that: the standard acid solution in this standard acid solution liquid feeding unit is sulfuric acid standard solution, and the concentration of sulfuric acid standard solution is
8. utilize the analytical approach of entry automatic continuous analysis device in described Industrial Boiler water quality detection as claimed in claim 6, it is characterized in that: the titer of the silver nitrate titer in this silver nitrate titer liquid feeding unit is T=3.34mg/mL.
9. utilize the analytical approach of entry automatic continuous analysis device in described Industrial Boiler water quality detection as claimed in claim 6, it is characterized in that: the titer of the Potassiumiodate-potassium iodide titer in this standard Potassiumiodate-potassium iodide liquid feeding unit is T=1.0mg/mL.
10. utilize the analytical approach of entry automatic continuous analysis device in described Industrial Boiler water quality detection as claimed in claim 6, it is characterized in that: the titer of the EDTA titer in this EDTA titer liquid feeding unit is T=0.1mol/L.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410336615.1A CN104101722B (en) | 2014-07-15 | 2014-07-15 | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection |
| PCT/CN2015/083420 WO2016008369A1 (en) | 2014-07-15 | 2015-07-07 | Multiple item continuous automatic analysis apparatus for industrial boiler water quality testing and analysis method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410336615.1A CN104101722B (en) | 2014-07-15 | 2014-07-15 | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104101722A CN104101722A (en) | 2014-10-15 |
| CN104101722B true CN104101722B (en) | 2015-09-30 |
Family
ID=51670042
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410336615.1A Active CN104101722B (en) | 2014-07-15 | 2014-07-15 | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN104101722B (en) |
| WO (1) | WO2016008369A1 (en) |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104101722B (en) * | 2014-07-15 | 2015-09-30 | 广州特种承压设备检测研究院 | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection |
| CN105181889B (en) * | 2015-09-30 | 2017-08-01 | 王竞 | A kind of liquid analysis method and device of use potentiometric titration |
| CN105353080A (en) * | 2015-10-24 | 2016-02-24 | 常州大学 | Beaker translation serial equipment used for removing chloride ions in soft coal calcination object |
| CN105954343A (en) * | 2016-04-26 | 2016-09-21 | 重庆鹏凯精细化工有限公司 | Device for rapid determination of content of sodium chloride in hydroxyethyl/hydroxypropyl methyl cellulose |
| CN106770923A (en) * | 2017-03-07 | 2017-05-31 | 李刚 | A kind of oil field wet steam generator water quality automatic detection device and method |
| CN109187848B (en) * | 2018-09-17 | 2021-06-18 | 沈阳工业大学 | Automatic titration method for alumina, caustic alkali and carbon alkali in sodium aluminate solution |
| CN112485316A (en) * | 2020-11-17 | 2021-03-12 | 安徽神剑新材料股份有限公司 | Electrochemical titration method for testing total chlorine in industrial monobutyl tin oxide |
| CN112630374A (en) * | 2020-12-30 | 2021-04-09 | 山西华兴铝业有限公司 | Automatic potentiometric titration detection method for analyzing content of effective calcium oxide in lime |
| CN112782252B (en) * | 2021-01-07 | 2022-03-25 | 安徽大学 | Method for quantitatively detecting potassium permanganate |
| CN112782251B (en) * | 2021-01-07 | 2022-03-25 | 安徽大学 | Method for quantitatively detecting potassium dichromate |
| CN112782253B (en) * | 2021-01-07 | 2022-03-25 | 安徽大学 | Method for quantitatively detecting potassium ferrate |
| CN114965861B (en) * | 2021-02-20 | 2023-10-17 | 宝山钢铁股份有限公司 | Method and device for jointly measuring concentration of sulfuric acid and zinc ions in electrogalvanizing solution |
| CN113702473A (en) * | 2021-08-26 | 2021-11-26 | 中国科学院青岛生物能源与过程研究所 | Method for measuring alkalinity of surfactant based on potentiometric titration method |
| CN113702241B (en) * | 2021-08-26 | 2023-10-20 | 泰安市特种设备检验研究院 | Method for rapidly determining content of dissolved solids in boiler water |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201716289U (en) * | 2010-04-21 | 2011-01-19 | 中科天融(北京)科技有限公司 | Sewage water quality automatic monitoring equipment |
| CN103018417A (en) * | 2012-12-12 | 2013-04-03 | 江苏省特种设备安全监督检验研究院 | Boiler water quality detection device based on flow injection analysis and soft-measuring technology |
| CN203376309U (en) * | 2013-07-31 | 2014-01-01 | 厦门百谷生物工程有限公司 | Multi-parameter water quality detector |
| CN103575789A (en) * | 2012-08-07 | 2014-02-12 | 陕西福天宝环保科技有限公司 | Water hardness detection mechanism |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4851104A (en) * | 1987-02-27 | 1989-07-25 | General Signal Corporation | Instrument for potentiometric electrochemical measurements |
| JPH09236576A (en) * | 1996-02-29 | 1997-09-09 | Horiba Ltd | Water quality analyser |
| US6936156B2 (en) * | 2001-08-30 | 2005-08-30 | The United States Of America As Represented By The Secretary Of The Department Of The Interior | Automated self-calibrating water quality monitoring sensor housing assembly |
| CN201152870Y (en) * | 2007-06-08 | 2008-11-19 | 郑州格林分析仪表科技有限公司 | Intelligent water quality analysis meter |
| CN201255732Y (en) * | 2007-11-02 | 2009-06-10 | 宫卓立 | Water hardness degree on-line detecting device |
| CN102565144B (en) * | 2011-01-04 | 2014-11-19 | 上海仪迈仪器科技有限公司 | Achievement device and method for concurrently measuring conductivity and pH value in the same solution |
| CN102183520B (en) * | 2011-04-26 | 2014-07-16 | 东北电力大学 | Water hardness on-line measurement device based on solution image technology and measurement method thereof |
| CN202453323U (en) * | 2012-02-24 | 2012-09-26 | 深圳市特种设备安全检验研究院 | Device for continuously analyzing pH (potential of hydrogen) value, phenolphthalein alkalinity, total alkalinity and chlorine ion concentration |
| CN102590318B (en) * | 2012-02-24 | 2014-06-11 | 深圳市特种设备安全检验研究院 | Method and device for continuously analyzing pH value, phenolphthalein end-point alkalinity, total alkalinity and chloridion concentration |
| CN103344690A (en) * | 2013-06-16 | 2013-10-09 | 苏州博讯仪器有限公司 | Water quality analyzer |
| CN104101722B (en) * | 2014-07-15 | 2015-09-30 | 广州特种承压设备检测研究院 | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection |
-
2014
- 2014-07-15 CN CN201410336615.1A patent/CN104101722B/en active Active
-
2015
- 2015-07-07 WO PCT/CN2015/083420 patent/WO2016008369A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201716289U (en) * | 2010-04-21 | 2011-01-19 | 中科天融(北京)科技有限公司 | Sewage water quality automatic monitoring equipment |
| CN103575789A (en) * | 2012-08-07 | 2014-02-12 | 陕西福天宝环保科技有限公司 | Water hardness detection mechanism |
| CN103018417A (en) * | 2012-12-12 | 2013-04-03 | 江苏省特种设备安全监督检验研究院 | Boiler water quality detection device based on flow injection analysis and soft-measuring technology |
| CN203376309U (en) * | 2013-07-31 | 2014-01-01 | 厦门百谷生物工程有限公司 | Multi-parameter water quality detector |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104101722A (en) | 2014-10-15 |
| WO2016008369A1 (en) | 2016-01-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104101722B (en) | Entry automatic continuous analysis device and analytical approach thereof in Industrial Boiler water quality detection | |
| CN102590318B (en) | Method and device for continuously analyzing pH value, phenolphthalein end-point alkalinity, total alkalinity and chloridion concentration | |
| CN202453323U (en) | Device for continuously analyzing pH (potential of hydrogen) value, phenolphthalein alkalinity, total alkalinity and chlorine ion concentration | |
| CN203405441U (en) | Instrument for detecting COD (chemical oxygen demand) of high-chlorine wastewater on line by basic potassium permanganate method | |
| CN107703202A (en) | A kind of permanganate index on-line monitoring automatic Titration decision method and its device | |
| US20130203171A1 (en) | Analytical method and titration device | |
| CN104267083A (en) | Method for measuring content of fluorine ions in hydrochloric acid by using ion meter | |
| CN115655383A (en) | Method and system for detecting valence state imbalance state of electrolyte of all-vanadium redox flow battery | |
| CN104977393B (en) | A kind of ship ballast water treatment system online effective chlorine detector and detection method | |
| CN109406588A (en) | Soil nitrate-N multi-parameter detecting method and instrument based on ion selective electrode | |
| CN112881587B (en) | Combined determination method and device for concentration of free acid and stannous in electrotinning solution | |
| CN101571530A (en) | Compound for ultraviolet-detecting anions containing sulfur by ion chromatography post-column derivatization | |
| CN110487850A (en) | A kind of degassing conductivity measurement system and method | |
| CN202492579U (en) | Regenerative control device for acidic cupric chloride etchant | |
| WO2023010804A1 (en) | Water sample characteristic detection method and apparatus | |
| CN104569105A (en) | Copper ion-selective electrode and method for measuring copper ion concentration by using copper ion-selective electrode | |
| CN102590317B (en) | PH composite electrode method for measuring content of nitrite ions in solution | |
| CN209745868U (en) | Online measuring device for concentration of silver ions in mixed acid solution | |
| CN211292685U (en) | Multi-parameter water quality measuring system | |
| CN103852509A (en) | Potentiometric titration analysis method for cyanide | |
| CN113237994A (en) | Method for rapidly analyzing and detecting impurity sodium sulfide in barium sulfide solution | |
| CN111896676A (en) | Device and method for automatically measuring ions in water by adopting anti-pollution pH electrode | |
| EP3472597B1 (en) | A method for measuring the concentration of a chemical species using a reagent baseline | |
| CN114660159B (en) | Method for slowing down corrosion of rectification system of vinyl acetate device | |
| CN205333567U (en) | System for adopt electrolysis automatic monitoring liquid multi -parameter |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240724 Address after: 510663 No.9, Keke Road, Huangpu District, Guangzhou City, Guangdong Province Patentee after: Guangzhou Special Equipment Testing and Research Institute (Guangzhou Special Equipment Accident Investigation Technology Center Guangzhou Elevator Safety Operation Monitoring Center) Country or region after: China Address before: Room 322, No. 9 Science Research Road, Luogang District, Guangzhou City, Guangdong Province, 510633 Patentee before: GUANGZHOU SPECIAL PRESSURE EQUIPMENT INSPECTION AND Research Institute Country or region before: China |
|
| TR01 | Transfer of patent right |