CN220626160U - Water quality sulfide detection system - Google Patents
Water quality sulfide detection system Download PDFInfo
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- CN220626160U CN220626160U CN202220655936.8U CN202220655936U CN220626160U CN 220626160 U CN220626160 U CN 220626160U CN 202220655936 U CN202220655936 U CN 202220655936U CN 220626160 U CN220626160 U CN 220626160U
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 100
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000001514 detection method Methods 0.000 title claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 79
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 58
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 32
- 238000010521 absorption reaction Methods 0.000 claims abstract description 30
- 238000002835 absorbance Methods 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims description 19
- 238000011161 development Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 9
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 3
- 239000000523 sample Substances 0.000 description 28
- 238000000034 method Methods 0.000 description 18
- 150000004763 sulfides Chemical class 0.000 description 10
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 238000012544 monitoring process Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000007664 blowing Methods 0.000 description 7
- 230000020477 pH reduction Effects 0.000 description 7
- -1 sulfide ions Chemical class 0.000 description 7
- 239000007924 injection Substances 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000002798 spectrophotometry method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910001447 ferric ion Inorganic materials 0.000 description 2
- 238000004401 flow injection analysis Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 229910052945 inorganic sulfide Inorganic materials 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- HJXIRCMNJLIHQR-UHFFFAOYSA-N 2-n,2-n-dimethylbenzene-1,2-diamine Chemical compound CN(C)C1=CC=CC=C1N HJXIRCMNJLIHQR-UHFFFAOYSA-N 0.000 description 1
- 102000018832 Cytochromes Human genes 0.000 description 1
- 108010052832 Cytochromes Proteins 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
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- 230000007954 hypoxia Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model provides a water quality sulfide detection system, which comprises an eviction tank and a reaction tank, wherein a water sample is injected into the eviction tank, a certain amount of rings are communicated with the inlet end of the eviction tank, quantitative phosphoric acid is placed on the quantitative rings, a nitrogen inlet pipe and a nitrogen valve are arranged on a pipeline of the phosphoric acid feeding eviction tank, the nitrogen valve feeds nitrogen to push the phosphoric acid to enter the eviction tank for a small amount for many times, after the water sample is acidified by the phosphoric acid in a dropwise adding mode, sulfide is converted into hydrogen sulfide and is blown out from the upper end of the eviction tank after being blown out by the nitrogen, and the hydrogen sulfide enters from the lower end of the reaction tank after passing through the pipeline; the position of the reaction tank is lower than the lowest part of the driving-out tank, quantitative absorption liquid is arranged in the reaction tank, quantitative color developing liquid is added into the reaction tank which absorbs hydrogen sulfide for reaction, the absorbance of the reacted liquid is tested, the reaction tank is a special cross pipe, and a transverse pipe of the special cross pipe is a light passing area. The utility model improves the expelling rate and the expelling stability, is suitable for small-volume detection, and reduces the detection cost.
Description
Technical Field
The utility model relates to the technical field of water quality sulfide detection, in particular to a water quality sulfide detection system.
Background
Sulfide is an important index for evaluating the current situation of water environment pollution, sulfide existing in water refers to water-soluble inorganic sulfide and acid-soluble metal sulfide, and the sulfide comprises soluble sulfide, HS-, S2-, soluble sulfide and acid-soluble metal sulfide existing in suspended matters, and unionized organic and inorganic sulfide, and has the characteristics of strong toxicity, high corrosiveness, easy volatilization and the like. The sulfides in water are easily converted into hydrogen sulfide, and the hazard is generally expressed as follows: consuming oxygen in water, resulting in death of aquatic organisms; corroding the metal pipeline; can be oxidized into sulfuric acid by microorganisms, thereby exacerbating pollution; can act with human cytochrome, oxidase and disulfide bond (-S-S-) in the substances to influence oxidation process of cells and cause hypoxia of cells and tissues. When people inhale low-concentration hydrogen sulfide, the eyes, the respiratory system and the central nervous system are affected, and when people inhale high-concentration hydrogen sulfide, the people can be fatal in a short time. Sulfide is one of important parameters representing water quality, the content of sulfide is an important index of water pollution, the sulfide is listed as a main monitoring item in environmental water quality monitoring and wastewater monitoring, and the content of sulfide is strictly limited by GB 3838-2002 surface Water environmental quality Standard and GB 8978-1996 comprehensive wastewater discharge Standard. Therefore, the development of sulfide monitors has great significance for environmental monitoring. Aiming at water quality sulfides, china has a set of water quality detection method and standard, wherein the limit value of sulfide in drinking water is 0.02mg/L.
In the prior art, the sulfide automatic analyzer is mainly a foreign instrument, and the performance of domestic equipment is a certain gap compared with that of foreign instruments, but the foreign instruments generally have the defects of high price, high maintenance and operation cost and the like. Therefore, under the background that water resources are increasingly deficient and water pollution is increasingly serious, the online monitor of the water quality sulfide is developed, so that the online monitor of the water quality sulfide has great significance, not only can early warn the sulfide pollution of the water source area in advance, but also can effectively compete with foreign countries, reduce the monitoring cost of the water quality sulfide, and improve the monitoring reliability.
The analysis methods for sulfides in water are dozens of, but most of the methods are not popularized and used. At present, the methods adopted by various standards in China mainly comprise: iodimetry, methylene blue spectrophotometry, and gas phase molecular absorption spectrometry. Among them, methylene blue spectrophotometry is one of the most commonly used methods for measuring sulfides at present. The method comprises the following principle: after the water sample is acidified, sulfide is converted into hydrogen sulfide, the hydrogen sulfide is blown out by nitrogen, and in an acidic solution containing ferric ions, sulfide ions act on amino dimethylaniline to generate methylene blue, and the color depth is in direct proportion to the concentration of the sulfide ions in the water. Determination of Water quality sulfide methylene blue spectrophotometry (GB/T16489-1996) the limit of detection of this method was determined to be 0.005mg/L (100 ml sample).
The main defects of the methylene blue spectrophotometry, acidification by adding acid, nitrogen stripping and absorption color development device for measuring the water quality sulfide are as follows: (1) the non-automation is not applicable to the on-line device. (2) The acid adding acidification, nitrogen stripping and absorption color development device has large system volume, large energy consumption and more waste liquid. (3) The acid adding acidification, nitrogen stripping and absorption color development device is not simple and convenient to operate, and the joints are more, so that the gas tightness is required to be checked again.
The utility model patent CN 210269805U of China, disclose a kind of full-automatic water quality sulfide acidizing and blowing detection system, the device can be applied to the relevant detecting instrument of the flow injection method of sulfide and used, the said water quality preconditioning device makes the solid particulate matter in the water sample to be measured deposit, and send the pretreated water sample to be measured into the sulfide acidizing and blowing device; the sulfide acidification blowing device acidizes sulfide in the water sample to be detected, and blows the acidized hydrogen sulfide into the sulfide fixing device by adopting nitrogen; the sulfide-removed waste liquid enters the waste liquid collecting device. However, this solution has the following problems: (1) the device is only suitable for being matched with instruments related to flow injection, and is not suitable for being used by sequential injection instruments. (2) The acidification, nitrogen stripping and absorption color development device is basically a pipeline type, is easy to block a pipe, difficult to maintain and easy to cross-pollute, has poor analysis accuracy, has large pipeline residue and is easy to generate memory effect. (3) The acidification, nitrogen stripping and absorption color development device has high requirements on a matched peristaltic pump, and needs precise matching of rotating speed and time, so that the device is complex, high in failure rate and high in cost.
At present, the methylene blue spectrophotometry has the problems that a small-volume water sample is ejected and sucked back in the application process, the photoelectric detection is influenced by ejected air flow, the ejection efficiency is low due to incomplete absorption of hydrogen sulfide gas, and the water samples with different concentrations are unstable in ejection rate.
As a detection instrument for sulfides in water with stronger hazard, how to solve the problem of unstable extraction rate of water samples with different concentrations, the online monitoring analyzer for the sulfides in water can stably operate and accurately test on a measuring site is a technical problem to be solved by the technicians in the field.
Disclosure of Invention
In order to solve the problems, the utility model aims to provide a water quality sulfide detection system with stable gas-expelling efficiency.
For this purpose, the above object of the present utility model is achieved by the following technical solutions:
a water quality sulfide detection system is characterized in that: the device comprises an expulsion pond and a reaction pond, wherein a water sample is injected into the expulsion pond, the inlet end of the expulsion pond is communicated with a certain amount of rings, a certain amount of phosphoric acid is placed on the quantitative rings, a first peristaltic pump is arranged on the quantitative rings to push the phosphoric acid to be pushed into the expulsion pond for a small amount of times, a nitrogen gas inlet pipe and a nitrogen gas valve are arranged on a pipeline of the phosphoric acid feeding expulsion pond, the nitrogen gas valve feeds nitrogen to push the phosphoric acid to be pushed into the expulsion pond for a small amount of times, after the water sample is acidified in a dropwise adding manner, sulfide is converted into hydrogen sulfide and is blown out by the nitrogen gas and then is led out from the upper end of the expulsion pond, and the hydrogen sulfide enters from the lower end of the reaction pond after passing through the pipeline; the position of the reaction tank is lower than the driving-out tank and lower than the lowest part of the driving-out tank, quantitative absorption liquid is arranged in the reaction tank, quantitative color development liquid is added in the reaction tank absorbing hydrogen sulfide for reaction, the absorbance of the liquid after the reaction is tested, the reaction tank is a special cross pipe, and a transverse pipe of the special cross pipe is a light passing area.
The utility model can also adopt or combine the following technical proposal when adopting the technical proposal:
as a preferable technical scheme of the utility model: the driving-out pool is a circular tube, and the inner wall of the upper end is arc-shaped.
As a preferable technical scheme of the utility model: the device is provided with a ten-way valve, the ten-way valve is communicated with a plurality of pipelines to respectively convey the standard liquid, the water sample and the pure water to the driving-out tank, and the ten-way valve is communicated with a plurality of pipelines to respectively convey the acid liquid, the color development liquid and the absorption liquid to the reaction tank.
As a preferable technical scheme of the utility model: the third valve is arranged on a pipeline for exhausting gas from the driving-out tank, the fifth valve is arranged on a pipeline for communicating the driving-out tank with the reaction tank, the reaction tank is communicated with waste gas and waste liquid at the top end through the pipeline, and the fourth valve is arranged on the pipeline.
As a preferable technical scheme of the utility model: the ten-way valve is communicated with the waste liquid pool, and the expelling pool and the reaction pool are emptied to the waste liquid pool through the ten-way valve and are respectively cleaned by pure water.
The utility model provides a water quality sulfide detection system, which has the following beneficial effects: the method is characterized in that a small-volume expelling system is utilized for automatic sample injection, acid is added in a simulated dripping manner to acidify a water sample, sulfide is converted into hydrogen sulfide, nitrogen is used for blowing out the hydrogen sulfide, in an acid solution containing ferric ions, the sulfide ions and para-aminodimethylaniline act to generate methylene blue, the color depth is in direct proportion to the concentration of the sulfide ions in water, and a first peristaltic pump is utilized for pushing phosphoric acid to enter an expelling pool for a plurality of times, so that dripping expelling is simulated, the problems of insufficient absorption of the hydrogen sulfide caused by excessive single sample injection of phosphoric acid are effectively avoided, the expelling efficiency is improved, the problem of unstable expelling of water samples with different concentrations is solved, and the effect of stable expelling rate of water samples with different concentrations is realized; and phosphoric acid is spaced apart through nitrogen gas, and when other gases are not introduced to influence the expelling efficiency, the nitrogen gas is effectively utilized to disturb the water sample to be detected and the phosphoric acid for many times, so that the expelling efficiency is improved, the mode that the phosphoric acid is introduced into the expelling pool also realizes the purpose of small-volume sequential injection of water quality sulfides, and the miniaturization of the whole detection system is realized. Especially, the design of the special-shaped cross-shaped tube of the reaction tank realizes small-volume large-optical-path, and improves the transverse optical path and the detection precision under the requirement of the same small-volume absorption liquid.
Drawings
FIG. 1 is a schematic flow chart of a water quality sulfide detection system provided by the utility model;
FIG. 2 is a schematic illustration of a partial structure of the present utility model;
in the figure: an expulsion pool 1 and a reaction pool 2; a dosing ring 3; a nitrogen inlet pipe 4; a nitrogen valve 5; a first peristaltic pump 6; a ten-way valve 7; a third valve 8; a fifth valve 9; a fourth valve 10; a waste liquid pool 11; a check valve 12.
Detailed Description
The utility model will be described in further detail with reference to the drawings and specific embodiments.
The utility model relates to a water quality sulfide detection system, which comprises an eviction tank 1 and a reaction tank 2, wherein a water sample is injected into the eviction tank 1, a certain amount of ring 3 is communicated with the inlet end of the eviction tank 1, a certain amount of phosphoric acid is placed on the quantitative ring 3, the quantitative ring 3 is provided with a first peristaltic pump 6 to push the phosphoric acid to be pushed into the eviction tank 1 a small amount of times, a pipeline of the phosphoric acid, through which the phosphoric acid is led into the eviction tank 1, is provided with a nitrogen inlet pipe 4 and a nitrogen valve 5, the pipeline of the nitrogen valve 5 is provided with a check valve 12, nitrogen is fed into the nitrogen valve 5 to push the phosphoric acid to be pushed into the eviction tank 1 a small amount of times, after the water sample is acidified by the phosphoric acid in a dropwise adding mode, sulfide is converted into hydrogen sulfide, blown out by the nitrogen gas, and then is led out from the upper end of the eviction tank 1, and the hydrogen sulfide enters from the lower end of the reaction tank 2 after passing through the pipeline; the position of the reaction tank 2 is lower than the driving-out tank 1 and lower than the lowest part of the driving-out tank 1, quantitative absorption liquid is arranged in the reaction tank 2, quantitative color development liquid is added into the reaction tank 2 absorbing hydrogen sulfide for reaction, the absorbance of the reacted liquid is tested, the reaction tank 2 is a special-shaped cross pipe, and a transverse pipe of the special-shaped cross pipe is a light passing area.
In the water quality sulfide detection system, during the process of expelling and absorbing, a certain volume of absorption liquid firstly enters a reaction tank 2, then a certain volume of water sample to be detected enters an expelling tank 1, phosphoric acid stored in a quantitative ring 3 is intermittently pushed into the expelling tank, the middle is separated by nitrogen, and finally, nitrogen is introduced at a flow rate of 30mL/min for 300 seconds. The nitrogen drives the expelled hydrogen sulfide gas to enter the reaction tank 2 to be absorbed by the absorption liquid. The nitrogen valve 5 is opened only in the gradual flow process, and other processes are closed.
The water quality sulfide detection system comprises an expulsion pond 1 and a reaction pond 2, wherein the expulsion pond 1 is filled with a water sample to be detected and phosphoric acid to convert sulfide into hydrogen sulfide and is filled with nitrogen for blowing out, the blown hydrogen sulfide is filled into the reaction pond through a guide pipe, absorption liquid is filled into the reaction pond to absorb the hydrogen sulfide, a color reagent is filled into the reaction pond 2 for reaction after the hydrogen sulfide is blown out, the content of the sulfide is judged through detection of absorbance after the reaction is finished, wherein the phosphoric acid is quantified through a quantitative loop, and is pushed by a first peristaltic pump 6 to enter the expulsion pond 1 for a plurality of times in a small amount, dropwise adding and expulsion are simulated, the problem of insufficient absorption of the hydrogen sulfide caused by excessive instantaneous generation of excessive hydrogen sulfide due to excessive adding of the phosphoric acid at one time is effectively avoided, the expulsion efficiency is improved, the problem of unstable expulsion of water samples with different concentrations is solved by adopting a mode of dropwise adding and the effect of stable water sample rates with different concentrations is realized; and phosphoric acid is separated by nitrogen, so that nitrogen is effectively utilized to disturb the water sample to be tested and phosphoric acid for many times while other gases are not introduced to influence the expelling efficiency, and the expelling efficiency is improved.
The driving-out pond 1 is admitted air from the lower part of the reaction pond 2, the lowest part of the driving-out pond 1 is not lower than the highest part of the reaction pond 2, the reaction pond 2 is in a special cross shape, and the absorbance is detected through a cross-shaped transverse tube body.
In the utility model, the driving-out pool 1, the pipeline and the reaction pool 2 are designed in series, the position of the driving-out pool 1 is higher than that of the reaction pool 2, the driving-out gas of the driving-out pool 1 is led out from the upper end of the driving-out pool, and enters from the lower end of the reaction pool 2, so that the liquid absorbing the hydrogen sulfide in the reaction pool 2 is prevented from flowing back to the driving-out pool 1, and the driving-out of the driving-out pool 1 is not influenced.
According to the water quality sulfide detection system, the reaction tank 2 is the special-shaped cross pipe, the transverse pipe of the special-shaped cross pipe is the light passing area, the light path is only extended in the horizontal direction, the volume of the whole reaction tank is not increased, the water quality sulfide detection system is suitable for small-volume sequential injection, the reaction with small volume and large light path is realized, the light absorption result is more accurate, the requirements of absorption liquid and hydrogen sulfide are reduced, and the running cost of the whole detection equipment is reduced.
The driving-out pool 1 is a circular tube, the inner wall of the upper end is free from being circular arc, enough space is provided for gas-liquid separation, and cleaning is convenient.
The device is provided with a ten-way valve 7, the ten-way valve 7 is communicated with a plurality of pipelines to respectively convey standard liquid, water sample and pure water to the driving-out tank 1, and the ten-way valve 7 is communicated with a plurality of pipelines to respectively convey acid liquid, color development liquid and absorption liquid to the reaction tank 2.
The third valve 8 is arranged on a pipeline for exhausting gas from the driving-out tank 1, the fifth valve 9 is arranged on a pipeline for exhausting gas from the driving-out tank 1 and communicating the reaction tank 2, the reaction tank 2 is communicated with waste gas and waste liquid from the top end through the pipeline, and the fourth valve 10 is arranged on the pipeline.
The ten-way valve 7 is communicated with the waste liquid pool 11, and the driving-out pool 1 and the reaction pool 2 are emptied to the waste liquid pool 11 through the ten-way valve 7 and are respectively cleaned by pure water.
The utility model provides an expulsion reaction system for detecting water quality sulfides, which is applied to the water quality sulfide detection system and comprises an expulsion pond 1 and a reaction pond 2 which are connected through a pipeline, wherein the lowest position of the expulsion pond 1 is higher than the highest position of the reaction pond 2, the reaction pond 2 is a special-shaped cross-shaped pipe, the expulsion reaction system can also be applied to the expulsion reaction system for detecting the water quality sulfides with other structures, the liquid in the reaction pond 2 is prevented from flowing back to the expulsion pond, the light path can be prolonged in the horizontal detection direction under the condition that the volume of the whole reaction pond is not increased, the detection system is suitable for the detection of small volume and large light path, and the accuracy of the detection result is improved.
The driving-out pool 1 is a circular tube, and the inner wall of the top of the circular tube is arc-shaped.
Example 1
As shown in figures 1-2, the water quality sulfide detection system disclosed by the utility model utilizes a small-volume expelling system to automatically sample, adds acid in a dropwise manner to acidify a water sample, converts sulfide into hydrogen sulfide, blows out the hydrogen sulfide by using nitrogen, and enables sulfide ions to react with para-amino dimethylaniline in an acidic solution containing high-iron ions to generate methylene blue, wherein the color depth is in direct proportion to the concentration of the sulfide ions in water.
In this example, an ultraviolet-visible spectrophotometer (available from Shanghai precision analysis instruments Co., ltd.); electronic balance (selected from beijing Sidoris balance Co., ltd.); solenoid valve (selected from japanese SMC corporation); ten-way valve (own); optoelectronic systems (present company); touch screens (present company); homemade online small-volume eviction system (own).
The reagents used in the experiment are all analytically pure, and the experiment water is self-made distilled water.
100mg/L sulfide stock solution: standard (outsourcing) and zinc sulphide as the main ingredient.
Phosphoric acid solution=25% (V/V).
Absorption solution: and 40g/L of sodium hydroxide.
2g/L para-amino dimethylaniline (solvent 25% sulfuric acid V/V and 10% ferric chloride V/V).
Ferric chloride solution: 5g of ferric chloride was dissolved in 100mL of distilled water, and the mixture was used after filtration.
The whole detection flow comprises the following steps: an eviction absorption process, a color reaction process and a cleaning process.
Eviction and absorption process: firstly, quantitatively feeding a certain volume of absorption liquid into a reaction tank, then quantitatively feeding a certain volume of water sample to be measured into an expulsion tank, storing phosphoric acid in a quantitative ring, intermittently pushing the expulsion tank, separating the middle by nitrogen, and finally, introducing nitrogen at a flow rate of 30mL/min for 300s. The nitrogen drives the expelled hydrogen sulfide gas to enter the reaction tank to be absorbed by the absorption liquid. The nitrogen valve is opened only in the gradual flow process, and other flow processes are closed.
Color reaction flow: and adding quantitative color developing solution into the reaction tank absorbing hydrogen sulfide, reacting for 600s, and testing the absorbance at 660 nm.
The cleaning process comprises the following steps: evacuating the reaction tank and the driving-out tank; pure water is pumped into the driving-out pool and the reaction pool cleaning system; the reaction tank and the driving-out tank are rinsed by pure water.
The small-volume eviction system adopted by the water quality sulfide detection system of the embodiment is required to reach the measurement lower limit of 0.005mg/L, and the small-volume eviction system with the volume of waste liquid of which the single test is smaller than 55mL (360 samples of 20L waste liquid and each sample is smaller than 55mL waste liquid) is required to be satisfied, and the system mainly solves the problems that: (1) the total volume of the waste liquid is less than 55ml, and the total volume of the washing waste liquid of the driving-out pool and the reaction pool is not more than 15ml. In the scheme I, the driving-out pool is 18 ml-7 ml of the reaction pool, 10ml of water sample and +1ml of phosphoric acid are driven out during driving-out, the guide pipe is led out to below the liquid level of the absorption liquid of the reaction pool, 2ml of absorption liquid of the reaction pool, and after driving-out, 1ml of color developing liquid is added. After 10 minutes of reaction, absorbance at 660nm was measured, and the optical path was 30mm.
The driving-out pool is a circular pipe with 18ml, the reaction pool is 30mm in the widest, 10mm in the narrowest and 60mm in the height.
As shown in FIG. 2, through feasibility test, water samples with concentration within 0.001-0.1 mg/L are used, absorption liquid supports at most 8 repeated expulsion, optical path detection is performed by 30mm, and at most 5 repeated expulsion is supported to reach the upper measurement limit. And finally determining that the low range is repeatedly ejected for 3 times, and stably measuring a water sample with the minimum water sample concentration of 0.005mg/L, wherein the lower measurement limit is 0.005mg/L. The detection limit is <0.001mg/L. The amount of waste liquid from a single test was 54mL for 3 exclusions.
The utility model discloses a water quality sulfide detection system and a blowing absorption system thereof, which realize a sulfide online instrument based on a small-volume sequential injection type water quality sulfide acidification blowing absorption color development online system, can realize the automatic detection of water quality sulfides with different ranges, and is characterized in that the detection is performed by expelling and concentrating in the range of 0.001-0.5 mg/L and the detection is performed by diluting in the range of 0.1-5 mg/L, so that the small-volume expelling is completed, and the lower measurement limit reaches 0.005mg/L. Based on the related technology, an automatic online analysis prototype of the water quality sulfide is developed, and the automatic online analysis prototype is debugged, tested and evaluated. The results show that the absorbance and the concentration of the sulfide solution are in good linear relation in three concentration ranges of 0.0-0.1 mg/L, 0.0-0.5 mg/L and 0.0-5.0 mg/L, and the correlation coefficient R2 is 0.9991, 0.9993 and 0.9995 respectively, and the detection limit is 0.002mg/L, 0.01mg/L and 0.1mg/L respectively; RSD (0.005 mg/L, n=7) of the sulfide water sample solution is 7.28% at the measurement range of 0.0-0.1 mg/L; the RSD (0.02 mg/L, n=7) of the sulfide water sample solution was 4.19% at the measurement range of 0.0 to 0.5 mg/L. The RSD (0.2 mg/L, n=7) of the sulfide water sample solution was 4.12% at the range of 0.0 to 5.0 mg/L. The standard recovery rate is between 97.5 and 106.4 percent. Wherein, the measuring range of 0.0-5.0 mg/L is the dilution measuring range, which can be used for measuring industrial wastewater and sulfide pollution wastewater of pollution sources. Therefore, the device is suitable for measuring samples of industrial wastewater, pollution source wastewater, surface water, underground water and drinking water, improves and optimizes a sample machine on the basis, selects a storage and transportation mode of a reagent, and lays a foundation for the sulfide on-line monitoring analyzer to work stably and accurately on a measuring site.
The above detailed description is intended to illustrate the present utility model by way of example only and not to limit the utility model to the particular embodiments disclosed, but to limit the utility model to the precise embodiments disclosed, and any modifications, equivalents, improvements, etc. that fall within the spirit and scope of the utility model as defined by the appended claims.
Claims (5)
1. A water quality sulfide detection system is characterized in that: the device comprises an expulsion pond and a reaction pond, wherein a water sample is injected into the expulsion pond, the inlet end of the expulsion pond is communicated with a certain amount of rings, a certain amount of phosphoric acid is placed on the quantitative rings, a first peristaltic pump is arranged on the quantitative rings to push the phosphoric acid to be pushed into the expulsion pond for a small amount of times, a nitrogen gas inlet pipe and a nitrogen gas valve are arranged on a pipeline of the phosphoric acid feeding expulsion pond, the nitrogen gas valve feeds nitrogen to push the phosphoric acid to be pushed into the expulsion pond for a small amount of times, after the water sample is acidified in a dropwise adding manner, sulfide is converted into hydrogen sulfide and is blown out by the nitrogen gas and then is led out from the upper end of the expulsion pond, and the hydrogen sulfide enters from the lower end of the reaction pond after passing through the pipeline; the position of the reaction tank is lower than the driving-out tank and lower than the lowest part of the driving-out tank, quantitative absorption liquid is arranged in the reaction tank, quantitative color development liquid is added in the reaction tank absorbing hydrogen sulfide for reaction, the absorbance of the liquid after the reaction is tested, the reaction tank is a special cross pipe, and a transverse pipe of the special cross pipe is a light passing area.
2. The water quality sulfide detection system according to claim 1, wherein: the driving-out pool is a circular tube, and the inner wall of the upper end is arc-shaped.
3. The water quality sulfide detection system according to claim 1, wherein: the device is provided with a ten-way valve, the ten-way valve is communicated with a plurality of pipelines to respectively convey the standard liquid, the water sample and the pure water to the driving-out tank, and the ten-way valve is communicated with a plurality of pipelines to respectively convey the acid liquid, the color development liquid and the absorption liquid to the reaction tank.
4. A water quality sulfide detection system according to claim 3, wherein: the third valve is arranged on a pipeline for exhausting gas from the driving-out tank, the fifth valve is arranged on a pipeline for communicating the driving-out tank with the reaction tank, the reaction tank is communicated with waste gas and waste liquid at the top end through the pipeline, and the fourth valve is arranged on the pipeline.
5. The water quality sulfide detection system according to claim 4, wherein: the ten-way valve is communicated with the waste liquid pool, and the driving-out pool and the reaction pool are emptied to the waste liquid pool through the ten-way valve and are respectively filled with pure water for cleaning.
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