CN113155758A - Automatic high-precision online heavy metal detector for boiler and manufacturing method thereof - Google Patents
Automatic high-precision online heavy metal detector for boiler and manufacturing method thereof Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 230000005540 biological transmission Effects 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 17
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 82
- 239000000243 solution Substances 0.000 claims description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 61
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 60
- 238000002156 mixing Methods 0.000 claims description 48
- 229910052793 cadmium Inorganic materials 0.000 claims description 35
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 238000004448 titration Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 18
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 239000011133 lead Substances 0.000 claims description 11
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 238000012360 testing method Methods 0.000 claims description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 229940074391 gallic acid Drugs 0.000 claims description 4
- 235000004515 gallic acid Nutrition 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000001393 triammonium citrate Substances 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- JGUQDUKBUKFFRO-CIIODKQPSA-N dimethylglyoxime Chemical compound O/N=C(/C)\C(\C)=N\O JGUQDUKBUKFFRO-CIIODKQPSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000036647 reaction Effects 0.000 claims description 3
- 238000010079 rubber tapping Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 3
- 239000001433 sodium tartrate Substances 0.000 claims description 3
- 229960002167 sodium tartrate Drugs 0.000 claims description 3
- 235000011004 sodium tartrates Nutrition 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- 235000011046 triammonium citrate Nutrition 0.000 claims description 3
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 abstract description 5
- 230000010354 integration Effects 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 6
- -1 dimethylglyoxime-sodium tartrate Chemical compound 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 3
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 description 1
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- 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
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- 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
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Abstract
The invention discloses an automatic high-precision online heavy metal detector for a boiler and a manufacturing method thereof, wherein the online heavy metal detector specifically comprises four parts, namely a chemical color development reaction tank, a liquid transmission processing system, a spectrophotometry detection device and a digital control display system; the digital control display system consists of a control center, and an alarm device, a display device and an operation device which are respectively connected with the control center; the operation device controls the action of the liquid transmission processing system through the control center to complete the liquid reaction action in the chemical color reaction tank, then the control center collects information in the chemical color reaction tank through sequentially connecting the A/D signal converter and the chemical signal collector to carry out automatic comparison analysis, and then the control center carries out digital display on the comparison analysis result through the alarm device and the display device. The invention has strong pertinence to a boiler system, sensitive response, online monitoring and good integration degree.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to an automatic high-precision online heavy metal detector for a boiler and a manufacturing method thereof.
Background
At present, heavy metals are widely applied to industrial production, particularly, about 70% of electric power in China is from thermal power generation at present, and can be applied to a boiler device which adopts austenitic stainless steel as a pipeline material in large quantity, although waste water discharged from a boiler is treated by waste water, if various harmful metal elements contained in the austenitic stainless steel and the water are discharged out of a standard due to undetected accuracy, sudden water pollution events are easily caused, harm is caused to the environment and human bodies, and therefore, the heavy metals in the boiler water are necessary to be quickly distinguished and quickly detected.
Unfortunately, no instrument specially used for detecting the element structure of the adopted materials of the boiler and the harmful metal elements in the boiler water exists in the market, and no corresponding instrument capable of monitoring on line and having sensitive reaction exists.
Therefore, an automatic high-precision online heavy metal detector for a boiler and a manufacturing method thereof, which have the advantages of strong pertinence to a boiler system, sensitive response, online monitoring and good integration degree, are urgently needed in the market.
Disclosure of Invention
The invention aims to provide a manufacturing method of an automatic high-precision online heavy metal detector for a boiler, which has strong pertinence to a boiler system, sensitive response, online monitoring and good integration degree.
In order to achieve the purpose, the invention adopts the following technical scheme: an automatic high-precision online heavy metal detector for a boiler specifically comprises four parts, namely a chemical color development reaction tank, a liquid transmission treatment system, a spectrophotometry detection device and a digital control display system; the spectrophotometry detection device is composed of a chemical signal collector and an A/D signal converter; the digital control display system consists of a control center, and an alarm device, a display device and an operation device which are respectively connected with the control center; the operation device controls the action of the liquid transmission processing system through the control center to complete the liquid reaction action in the chemical color reaction tank, then the control center collects information in the chemical color reaction tank through sequentially connecting the A/D signal converter and the chemical signal collector to carry out automatic comparison analysis, and then the control center carries out digital display on the comparison analysis result through the alarm device and the display device;
wherein the chemical color reaction tank is divided into reaction sub-tanks of six different elements of copper, nickel, lead, cadmium, iron and chromium;
the manufacturing method of the reaction sub-tanks of the six different elements comprises the following steps:
s1: manufacturing method of copper sub-tank
The copper sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent A and a reagent B, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system;
secondly, mixing ammonium chloride, strong ammonia water and triammonium citrate according to a mass ratio of 1: 7: 40, adding deionized water with the mixing mass being 3.5 times of that of the mixture, and stirring uniformly to obtain a reagent A;
dissolving bicyclohexanoneoxalyl dihydrazone in 45-50 times of the mass of bicyclohexanoneoxalyl dihydrazone in the volume ratio of 1: 1, heating the mixed solution to 62-65 ℃ and stirring the mixed solution until the mixed solution is dissolved to obtain a reagent B;
fourthly, the reagent A obtained in the second step and the reagent B obtained in the third step are mixed according to the ratio of 5: 4 to obtain a mixed preparation agent, and when the mixed preparation agent is used for titrating the water body to be detected, the mixed preparation agent is prepared by the following steps: the volume ratio of the water body to be detected is 9: 40, carrying out titration;
s2: method for manufacturing chromium sub-cell
The chromium sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent C and a reagent D, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system;
adopting a 1+7 sulfuric acid solution reagent as the reagent C; and (3) reagent D: the method comprises the following steps of (1): 20, grinding the mixture in a mortar and uniformly mixing to obtain mixed powder, namely the reagent D;
thirdly, mixing the reagent C and the reagent D with the water body to be detected according to the mass ratio of 1.5: 0.4: titration is carried out according to the proportion of 100;
s3: nickel sub-tank manufacturing method
The nickel sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent E and a reagent F, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system;
② reagent E is ammonium persulfate; the reagent F is prepared by mixing dimethylglyoxime, sodium tartrate, sodium hydroxide and deionized water according to the mass ratio of 1: 10: 20: 100, and ultrasonically stirring until the mixture is dissolved to obtain a reagent F;
thirdly, mixing the reagent E, the reagent F and the water body to be detected according to the mass ratio of 1: 6: 14, carrying out titration;
s4: method for manufacturing lead separation tank
Firstly, preparing raw materials into 2.5mol/L sodium chloride aqueous solution, 0.1mol/L magnesium chloride aqueous solution, 0.1mol/L tris (hydroxymethyl) aminomethane aqueous solution and 0.1mol/L hydrochloric acid aqueous solution;
secondly, mixing the trihydroxymethyl aminomethane solution prepared in the step I and the hydrochloric acid aqueous solution according to the volume ratio of 25: 21, mixing, adding water to a constant volume of 100ml, and obtaining a mixed salt solution;
thirdly, mixing the mixed salt solution obtained in the second step with the sodium chloride solution and the magnesium chloride solution obtained in the first step according to the volume ratio of 5: 4: 1, mixing to obtain a lead tapping titration reagent G; when the water body to be detected is titrated by the reagent G, according to the reagent G: the volume ratio of the water body to be detected is 3: 7, proportioning and titrating;
s5: cadmium separation tank manufacturing method
Dissolving purchased cadmium test in 780-795 times of absolute ethanol by mass, and performing ultrasonic treatment for 2 hours to obtain a cadmium test ethanol solution;
② mixing hexadecyl trimethyl ammonium chloride and triethanolamine according to the mass ratio of 100: (4-5), dissolving the mixture in deionized water with the mass 20 times that of the mixture to obtain a prefabricated mixed solution, heating the prefabricated mixed solution to 65-70 ℃, stirring for 3-4 h, dropwise adding tetraethyl orthosilicate with the mass 6-8% of the prefabricated mixed solution into the prefabricated mixed solution, stirring for 3.5-4 h, finally centrifugally separating out solid content, washing the obtained solid content with ethanol for 2-3 times, soaking and stirring the washed solid content in NaCI/methanol solution with the mass fraction of 1.5-2% of the solute with sodium chloride as the solute and methanol as the solvent for 1.5-2 h, centrifuging the soaked and stirred mixed solution to obtain a second solid content, filtering the second solid content, and naturally drying to obtain a carrier;
thirdly, mixing the carrier obtained in the second step with the ethanol solution of cadmium testing solution obtained in the first step according to the mass ratio of 1: (27-29), adding deionized water accounting for 3.3-3.5 times of the volume of the ethanol solution of cadmium tested and absolute ethyl alcohol accounting for 2.3-2.5 times of the volume of the ethanol solution of cadmium tested into the mixed product, fully infiltrating and uniformly stirring under the condition of keeping out of the sun, obtaining a final solid content through centrifugation, repeatedly cleaning the final solid content with deionized water until the final solid content is clean, and redissolving the solid content in deionized water accounting for 6.8-7 times of the volume of the ethanol solution of cadmium tested to form a cadmium color developing agent solution; when the cadmium color developing agent solution is used for titrating a water body to be detected, the volume mixing ratio of the cadmium color developing agent solution, 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
s6: iron sub-tank manufacturing method
Firstly, mixing gallic acid, copper nitrate and deionized water according to a mass ratio of 2: 1: mixing and stirring the solution according to the proportion of 1000 until the solute is completely dissolved, heating the solution to 65-70 ℃, stirring the solution for 15-20 min, and storing the obtained solution in a dark place to obtain an iron cell reaction solution; when the reaction solution is used for titrating a water body to be detected, the volume mixing ratio of the iron sub-tank reaction solution, the 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
compared with the prior art, the invention has the following advantages because of adopting the scheme: (1) for the detection of copper in water, the invention manufactures the accurate detection kit for copper ions, uses the bicyclohexanoneoxalyl dihydrazone as a reagent A, uses a mixed solution of ammonium chloride-ammonia water-triammonium citrate as a reagent B, has the relative errors of the measured value and the ICP-AES method which are both less than 2 percent compared with the current national standard method, and can be stably stored for 2 weeks. (2) The quick detection of hexavalent chromium in water is realized by taking the diphenylcarbazide as a color developing agent, the (1+7) sulfuric acid as a reagent A and the DPC-NaCI mixed powder as a reagent B, the test of one water sample can be completed within 10min, and the used reagent can be stored for at least two months. (3) The invention takes persulfuric acid as a reagent A and dimethylglyoxime-sodium tartrate mixed solution as a reagent B to manufacture the nickel ion accurate detection kit, the actual water sample is tested by adopting the kit, the relative error is less than 2 percent compared with the ICP-AES method, and the reagent can be stably stored for 2 weeks under the condition of keeping out of the sun. (4) Firstly, synthesizing a silicon carrier, utilizing silicon spheres to load a color developing agent to form a composite color developing agent, preparing a color developing agent of cadmium ions, and respectively optimizing the loading condition and the color developing condition of the composite color developing agent. Experiments show that through optimization and fixation of parameters in multiple aspects, the composite color developing agent disclosed by the invention is finally determined to have better recognition on cadmium ions, and can be used for online rapid and accurate detection of the cadmium ions. (5) According to the invention, a novel complex is generated by using the reaction of copper nitrate and gallic acid, and the synthesized complex is characterized by a spectrophotometer, so that the complex is found to have specific identification on iron ions in the presence of a certain amount of sodium hydroxide, and the concentration of the iron ions and the fluorescence value of the material are in a linear positive correlation in a certain range, so that the complex can be applied to the online rapid and accurate detection of the iron ions. (6) The lowest detection limits of the six main metal elements detected by the method can respectively reach 0.01mg/L of copper, 0.03mg/L of nickel, 0.003mg/L of hexavalent chromium, 0.05mg/L of lead, 0.1 mu g/L of cadmium and 0.01mg/L of iron, which are slightly superior to the existing level of the industry, and the deviation of the detection result and the ICP-AES (inductively coupled plasma-atomic emission spectrometry) measurement result is not more than 2%, so that the method has higher accuracy. Therefore, the invention has the characteristics of strong pertinence to a boiler system, sensitive response, online monitoring and good integration degree.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention
In the figure: the device comprises a chemical signal collector 1, a chemical color reaction tank 2, a liquid transmission processing system 3, an A/D signal converter 4, a control center 5, an alarm device 6, a display device 7 and an operation device 8.
Detailed Description
Example 1:
an automatic high-precision online heavy metal detector for a boiler specifically comprises four parts, namely a chemical color reaction tank 2, a liquid transmission processing system 3, a spectrophotometry detection device and a digital control display system; the spectrophotometry detection device is composed of a chemical signal collector 1 and an A/D signal converter 4; the digital control display system consists of a control center 5, and an alarm device 6, a display device 7 and an operation device 8 which are respectively connected with the control center 5; the operation device 8 controls the action of the liquid transmission processing system 3 through the control center 5 to complete the liquid reaction action in the chemical chromogenic reaction tank 2, then the control center 5 collects information in the chemical chromogenic reaction tank 2 through sequentially connecting the A/D signal converter 4 and the chemical signal collector 1 to carry out automatic comparison analysis, and then the control center 5 carries out digital display on the comparison analysis result through the alarm device 6 and the display device 7;
wherein the chemical color reaction tank 2 is divided into reaction sub-tanks of six different elements of copper, nickel, lead, cadmium, iron and chromium;
the manufacturing method of the reaction sub-tanks of the six different elements comprises the following steps:
s1: manufacturing method of copper sub-tank
The copper sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent A and a reagent B, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system 3;
secondly, mixing ammonium chloride, strong ammonia water and triammonium citrate according to a mass ratio of 1: 7: 40, adding deionized water with the mixing mass being 3.5 times of that of the mixture, and stirring uniformly to obtain a reagent A;
dissolving bicyclohexanoneoxalyl dihydrazone in 45-50 times of the mass of bicyclohexanoneoxalyl dihydrazone in the volume ratio of 1: 1, heating the mixed solution to 62-65 ℃ and stirring the mixed solution until the mixed solution is dissolved to obtain a reagent B;
fourthly, the reagent A obtained in the second step and the reagent B obtained in the third step are mixed according to the ratio of 5: 4 to obtain a mixed preparation agent, and when the mixed preparation agent is used for titrating the water body to be detected, the mixed preparation agent is prepared by the following steps: the volume ratio of the water body to be detected is 9: 40, carrying out titration;
s2: method for manufacturing chromium sub-cell
The chromium sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent C and a reagent D, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system 3;
adopting a 1+7 sulfuric acid solution reagent as the reagent C; and (3) reagent D: the method comprises the following steps of (1): 20, grinding the mixture in a mortar and uniformly mixing to obtain mixed powder, namely the reagent D;
thirdly, mixing the reagent C and the reagent D with the water body to be detected according to the mass ratio of 1.5: 0.4: titration is carried out according to the proportion of 100;
s3: nickel sub-tank manufacturing method
The nickel sub-pool comprises a reaction device and a reagent kit, wherein the reagent kit comprises a reagent E and a reagent F, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system 3;
② reagent E is ammonium persulfate; the reagent F is prepared by mixing dimethylglyoxime, sodium tartrate, sodium hydroxide and deionized water according to the mass ratio of 1: 10: 20: 100, and ultrasonically stirring until the mixture is dissolved to obtain a reagent F;
thirdly, mixing the reagent E, the reagent F and the water body to be detected according to the mass ratio of 1: 6: 14, carrying out titration;
s4: method for manufacturing lead separation tank
Firstly, preparing raw materials into 2.5mol/L sodium chloride aqueous solution, 0.1mol/L magnesium chloride aqueous solution, 0.1mol/L tris (hydroxymethyl) aminomethane aqueous solution and 0.1mol/L hydrochloric acid aqueous solution;
secondly, mixing the trihydroxymethyl aminomethane solution prepared in the step I and the hydrochloric acid aqueous solution according to the volume ratio of 25: 21, mixing, adding water to a constant volume of 100ml, and obtaining a mixed salt solution;
thirdly, mixing the mixed salt solution obtained in the second step with the sodium chloride solution and the magnesium chloride solution obtained in the first step according to the volume ratio of 5: 4: 1, mixing to obtain a lead tapping titration reagent G; when the water body to be detected is titrated by the reagent G, according to the reagent G: the volume ratio of the water body to be detected is 3: 7, proportioning and titrating;
s5: cadmium separation tank manufacturing method
Dissolving purchased cadmium test in 780-795 times of absolute ethanol by mass, and performing ultrasonic treatment for 2 hours to obtain a cadmium test ethanol solution;
② mixing hexadecyl trimethyl ammonium chloride and triethanolamine according to the mass ratio of 100: (4-5), dissolving the mixture in deionized water with the mass 20 times that of the mixture to obtain a prefabricated mixed solution, heating the prefabricated mixed solution to 65-70 ℃, stirring for 3-4 h, dropwise adding tetraethyl orthosilicate with the mass 6-8% of the prefabricated mixed solution into the prefabricated mixed solution, stirring for 3.5-4 h, finally centrifugally separating out solid content, washing the obtained solid content with ethanol for 2-3 times, soaking and stirring the washed solid content in NaCI/methanol solution with the mass fraction of 1.5-2% of the solute with sodium chloride as the solute and methanol as the solvent for 1.5-2 h, centrifuging the soaked and stirred mixed solution to obtain a second solid content, filtering the second solid content, and naturally drying to obtain a carrier;
thirdly, mixing the carrier obtained in the second step with the ethanol solution of cadmium testing solution obtained in the first step according to the mass ratio of 1: (27-29), adding deionized water accounting for 3.3-3.5 times of the volume of the ethanol solution of cadmium tested and absolute ethyl alcohol accounting for 2.3-2.5 times of the volume of the ethanol solution of cadmium tested into the mixed product, fully infiltrating and uniformly stirring under the condition of keeping out of the sun, obtaining a final solid content through centrifugation, repeatedly cleaning the final solid content with deionized water until the final solid content is clean, and redissolving the solid content in deionized water accounting for 6.8-7 times of the volume of the ethanol solution of cadmium tested to form a cadmium color developing agent solution; when the cadmium color developing agent solution is used for titrating a water body to be detected, the volume mixing ratio of the cadmium color developing agent solution, 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
s6: iron sub-tank manufacturing method
Firstly, mixing gallic acid, copper nitrate and deionized water according to a mass ratio of 2: 1: mixing and stirring the solution according to the proportion of 1000 until the solute is completely dissolved, heating the solution to 65-70 ℃, stirring the solution for 15-20 min, and storing the obtained solution in a dark place to obtain an iron cell reaction solution; when the reaction solution is used for titrating a water body to be detected, the volume mixing ratio of the iron sub-tank reaction solution, the 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
according to the online heavy metal detector manufactured by the embodiment, the lowest detection limits of six main metal elements to be detected can respectively reach 0.01mg/L of copper, 0.03mg/L of nickel, 0.003mg/L of hexavalent chromium, 0.05mg/L of lead, 0.1 mu g/L of cadmium and 0.01mg/L of iron which are slightly superior to the existing level of the industry, the deviation between the detection result and the ICP-AES (inductively coupled plasma-atomic emission spectrometry) measurement result is not more than 2%, and the kit can be stored for at least 2 weeks at low cost and is convenient to use.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (1)
1. The utility model provides an online heavy metal detector of automatic high accuracy for boiler which characterized in that: the online heavy metal detector specifically comprises four parts, namely a chemical color reaction tank (2), a liquid transmission processing system (3), a spectrophotometry detection device and a digital control display system; the spectrophotometry detection device is specifically composed of a chemical signal collector (1) and an A/D signal converter (4); the digital control display system consists of a control center (5), and an alarm device (6), a display device (7) and an operation device (8) which are respectively connected with the control center (5); the operation device (8) controls the action of the liquid transmission processing system (3) through the control center (5) to complete the liquid reaction action in the chemical chromogenic reaction tank (2), then the control center (5) collects information in the chemical chromogenic reaction tank (2) through sequentially connecting the A/D signal converter (4) and the chemical signal collector (1) to perform automatic comparison analysis, and then the control center (5) digitally displays the comparison analysis result through the alarm device (6) and the display device (7);
wherein the chemical color reaction tank (2) is divided into reaction sub-tanks of six different elements of copper, nickel, lead, cadmium, iron and chromium;
the manufacturing method of the reaction sub-tanks of the six different elements comprises the following steps:
s1: manufacturing method of copper sub-tank
The copper sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent A and a reagent B, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system (3);
secondly, mixing ammonium chloride, strong ammonia water and triammonium citrate according to a mass ratio of 1: 7: 40, adding deionized water with the mixing mass being 3.5 times of that of the mixture, and stirring uniformly to obtain a reagent A;
dissolving bicyclohexanoneoxalyl dihydrazone in 45-50 times of the mass of bicyclohexanoneoxalyl dihydrazone in the volume ratio of 1: 1, heating the mixed solution to 62-65 ℃ and stirring the mixed solution until the mixed solution is dissolved to obtain a reagent B;
fourthly, the reagent A obtained in the second step and the reagent B obtained in the third step are mixed according to the ratio of 5: 4 to obtain a mixed preparation agent, and when the mixed preparation agent is used for titrating the water body to be detected, the mixed preparation agent is prepared by the following steps: the volume ratio of the water body to be detected is 9: 40, carrying out titration;
s2: method for manufacturing chromium sub-cell
The chromium sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent C and a reagent D, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system (3);
adopting a 1+7 sulfuric acid solution reagent as the reagent C; and (3) reagent D: the method comprises the following steps of (1): 20, grinding the mixture in a mortar and uniformly mixing to obtain mixed powder, namely the reagent D;
thirdly, mixing the reagent C and the reagent D with the water body to be detected according to the mass ratio of 1.5: 0.4: titration is carried out according to the proportion of 100;
s3: nickel sub-tank manufacturing method
The nickel sub-pool consists of a reaction device and a kit, wherein the kit comprises a reagent E and a reagent F, and the reaction device comprises a reaction container and a titration device controlled by a liquid transmission processing system (3);
② reagent E is ammonium persulfate; the reagent F is prepared by mixing dimethylglyoxime, sodium tartrate, sodium hydroxide and deionized water according to the mass ratio of 1: 10: 20: 100, and ultrasonically stirring until the mixture is dissolved to obtain a reagent F;
thirdly, mixing the reagent E, the reagent F and the water body to be detected according to the mass ratio of 1: 6: 14, carrying out titration;
s4: method for manufacturing lead separation tank
Firstly, preparing raw materials into 2.5mol/L sodium chloride aqueous solution, 0.1mol/L magnesium chloride aqueous solution, 0.1mol/L tris (hydroxymethyl) aminomethane aqueous solution and 0.1mol/L hydrochloric acid aqueous solution;
secondly, mixing the trihydroxymethyl aminomethane solution prepared in the step I and the hydrochloric acid aqueous solution according to the volume ratio of 25: 21, mixing, adding water to a constant volume of 100ml, and obtaining a mixed salt solution;
thirdly, mixing the mixed salt solution obtained in the second step with the sodium chloride solution and the magnesium chloride solution obtained in the first step according to the volume ratio of 5: 4: 1, mixing to obtain a lead tapping titration reagent G; when the water body to be detected is titrated by the reagent G, according to the reagent G: the volume ratio of the water body to be detected is 3: 7, proportioning and titrating;
s5: cadmium separation tank manufacturing method
Dissolving purchased cadmium test in 780-795 times of absolute ethanol by mass, and performing ultrasonic treatment for 2 hours to obtain a cadmium test ethanol solution;
② mixing hexadecyl trimethyl ammonium chloride and triethanolamine according to the mass ratio of 100: (4-5), dissolving the mixture in deionized water with the mass 20 times that of the mixture to obtain a prefabricated mixed solution, heating the prefabricated mixed solution to 65-70 ℃, stirring for 3-4 h, dropwise adding tetraethyl orthosilicate with the mass 6-8% of the prefabricated mixed solution into the prefabricated mixed solution, stirring for 3.5-4 h, finally centrifugally separating out solid content, washing the obtained solid content with ethanol for 2-3 times, soaking and stirring the washed solid content in NaCI/methanol solution with the mass fraction of 1.5-2% of the solute with sodium chloride as the solute and methanol as the solvent for 1.5-2 h, centrifuging the soaked and stirred mixed solution to obtain a second solid content, filtering the second solid content, and naturally drying to obtain a carrier;
thirdly, mixing the carrier obtained in the second step with the ethanol solution of cadmium testing solution obtained in the first step according to the mass ratio of 1: (27-29), adding deionized water accounting for 3.3-3.5 times of the volume of the ethanol solution of cadmium tested and absolute ethyl alcohol accounting for 2.3-2.5 times of the volume of the ethanol solution of cadmium tested into the mixed product, fully infiltrating and uniformly stirring under the condition of keeping out of the sun, obtaining a final solid content through centrifugation, repeatedly cleaning the final solid content with deionized water until the final solid content is clean, and redissolving the solid content in deionized water accounting for 6.8-7 times of the volume of the ethanol solution of cadmium tested to form a cadmium color developing agent solution; when the cadmium color developing agent solution is used for titrating a water body to be detected, the volume mixing ratio of the cadmium color developing agent solution, 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
s6: iron sub-tank manufacturing method
Firstly, mixing gallic acid, copper nitrate and deionized water according to a mass ratio of 2: 1: mixing and stirring the solution according to the proportion of 1000 until the solute is completely dissolved, heating the solution to 65-70 ℃, stirring the solution for 15-20 min, and storing the obtained solution in a dark place to obtain an iron cell reaction solution; when the reaction solution is used for titrating a water body to be detected, the volume mixing ratio of the iron sub-tank reaction solution, the 0.01mol/L sodium hydroxide solution and the water body to be detected is 1: 1: 8.
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Application publication date: 20210723 |