CN114636694A - Water environment on-line automatic detection device and detection method - Google Patents
Water environment on-line automatic detection device and detection method Download PDFInfo
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- CN114636694A CN114636694A CN202210533054.9A CN202210533054A CN114636694A CN 114636694 A CN114636694 A CN 114636694A CN 202210533054 A CN202210533054 A CN 202210533054A CN 114636694 A CN114636694 A CN 114636694A
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- 238000001514 detection method Methods 0.000 title claims abstract description 131
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000010521 absorption reaction Methods 0.000 claims abstract description 137
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 230000007246 mechanism Effects 0.000 claims abstract description 64
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 claims abstract description 48
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 23
- 239000000498 cooling water Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims description 57
- 238000010438 heat treatment Methods 0.000 claims description 24
- 229910052785 arsenic Inorganic materials 0.000 claims description 20
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 20
- 239000004065 semiconductor Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000005086 pumping Methods 0.000 claims description 13
- 239000007800 oxidant agent Substances 0.000 claims description 12
- 230000001590 oxidative effect Effects 0.000 claims description 12
- 238000005057 refrigeration Methods 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 230000002093 peripheral effect Effects 0.000 claims description 7
- 230000009977 dual effect Effects 0.000 claims description 6
- 239000007853 buffer solution Substances 0.000 claims description 5
- 238000011161 development Methods 0.000 claims description 5
- 230000017525 heat dissipation Effects 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 11
- 238000010586 diagram Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 6
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- 238000005259 measurement Methods 0.000 description 5
- 230000000630 rising effect Effects 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
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000003651 drinking water Substances 0.000 description 4
- 235000020188 drinking water Nutrition 0.000 description 4
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- 238000012546 transfer Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229910000070 arsenic hydride Inorganic materials 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- FEWJPZIEWOKRBE-LWMBPPNESA-N levotartaric acid Chemical compound OC(=O)[C@@H](O)[C@H](O)C(O)=O FEWJPZIEWOKRBE-LWMBPPNESA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 150000001495 arsenic compounds Chemical class 0.000 description 1
- HAYXDMNJJFVXCI-UHFFFAOYSA-N arsenic(5+) Chemical compound [As+5] HAYXDMNJJFVXCI-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229940093920 gynecological arsenic compound Drugs 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
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- 238000012544 monitoring process Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
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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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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The application relates to the technical field of water sample detection, in particular to an online automatic detection device and a detection method for a water environment, wherein the online automatic detection device for the water environment comprises a metering mechanism, a driving-out mechanism and a colorimetric mechanism, wherein the metering mechanism comprises a metering pipe, a peristaltic pump communicated with a first end of the metering pipe and a multi-way discharge valve communicated with a second end of the metering pipe; the ejecting mechanism comprises a reaction cup communicated with the multi-way exhaust valve, a water-gas separator communicated with the output end of the reaction cup and an absorption pipe assembly communicated with the output end of the water-gas separator, the water-gas separator comprises an external pipe body and an internal pipe body arranged inside the external pipe body, the internal pipe body is communicated with an external cooling water source, and a gas channel is reserved between the internal pipe body and the external pipe body; the water environment on-line automatic detection device can fully separate generated arsine gas from water vapor, reduce or avoid the influence of the water vapor on contrast color detection, improve the detection accuracy and improve the practicability.
Description
Technical Field
The application relates to the technical field of water sample detection, in particular to an online automatic detection device and a detection method for a water environment.
Background
As one of indispensable parts of human survival, drinking water plays an important role in daily life of people, and thus, it is necessary to ensure the health of drinking water. In some colorimetric detection methods, many reaction systems are susceptible to other interferences (ion interference, turbidity, chromaticity and the like), so that the error of test data is large, and the detection accuracy is influenced. In the process of detecting arsenic in a water sample, firstly, the arsenic is converted into gaseous arsine separated from an original system through some chemical reactions, then the gaseous arsine is absorbed by using a proper absorption liquid, and a proper color developing agent is added, so that the interference of the original reaction system can be eliminated. However, the arsenic hydride that turns into the gaseous state with arsenic ion is evicted the in-process and is very easily received vapor's influence for arsenic hydride and vapor can't effectively be separated, and absorption color comparison result error is great, and vapor still can be attached to on the inner wall of absorption pipeline moreover, because the pipe diameter of absorption pipeline is thinner, the clearance of being not convenient for, this will cause the influence to the accuracy that follow-up color comparison detected, lead to the practicality lower.
Disclosure of Invention
The water environment online automatic detection device and the detection method can fully separate generated arsine gas from water vapor, reduce or avoid the influence of the water vapor on color contrast detection, improve the detection accuracy and improve the practicability.
To this end, in a first aspect, an embodiment of the present application provides an online automatic detection device for a water environment, including: the metering mechanism comprises a metering pipe, a peristaltic pump communicated with a first end of the metering pipe and a multi-way discharge valve communicated with a second end of the metering pipe; the driving mechanism comprises a reaction cup communicated with the multi-way exhaust valve, a water-gas separator communicated with the output end of the reaction cup and an absorption tube assembly communicated with the output end of the water-gas separator, the water-gas separator comprises an external tube body and an internal tube body arranged inside the external tube body, the internal tube body is communicated with an external cooling water source, and a gas channel is reserved between the internal tube body and the external tube body; the color comparison mechanism comprises an absorption detection cup communicated with the multi-way discharge valve, and the output end of the absorption tube assembly extends into the absorption detection cup.
In a possible implementation manner, the outer tube body comprises a middle tube, a funnel structure communicated with the bottom of the middle tube, and a convergence tube communicated with the top of the middle tube, and the funnel structure extends into the reaction cup.
In a possible implementation manner, the water-gas separator further comprises a self-rotating flow guiding structure arranged inside the gas channel, and gas in the gas channel flows along the self-rotating flow guiding structure in a rotating manner.
In one possible implementation, the self-rotating flow guiding structure is a helical blade disposed on an outer circumferential side of the inner pipe body, and the outer circumferential side of the helical blade abuts against an inner surface of the intermediate pipe.
In a possible implementation manner, the intermediate pipe and the funnel structure are integrally formed, and the intermediate pipe and the converging pipe are connected through threads or a connecting flange.
In a possible implementation manner, two ends of the inner pipe body are respectively sealed, and the inner pipe body is provided with a liquid inlet pipe and a liquid return pipe in a communicated manner.
The colorimetric mechanism further comprises: the fixed pipe is arranged on the inner side wall of the absorption detection cup and is used for fixing the output end of the absorption pipe assembly; the double-light-path emitter is arranged on one side of the absorption detection cup; and the signal receiver is arranged on one side of the absorption detection cup and is opposite to the dual-light-path emitter.
In a possible implementation manner, the colorimetric mechanism further comprises an evacuation pipe communicated with the top of the absorption detection cup and an evacuation valve arranged on the evacuation pipe.
In a possible implementation manner, the absorption tube assembly comprises a solenoid valve, a first absorption tube communicated with one end of the solenoid valve, and a second absorption tube communicated with the other end of the solenoid valve, one end of the first absorption tube, which is far away from the solenoid valve, is communicated with the convergence tube of the moisture separator, and one end of the second absorption tube, which is far away from the solenoid valve, extends into the absorption detection cup and is fixed in the fixed tube.
In a possible implementation manner, the ejecting mechanism further comprises a first heating component arranged on the outer periphery side of the reaction cup; the colorimetric mechanism further comprises a second heating component arranged on the outer peripheral side of the absorption detection cup.
In a possible implementation manner, the first heating assembly is a semiconductor refrigeration sheet arranged on the outer peripheral side of the reaction cup, and the semiconductor refrigeration sheet is provided with a heat dissipation surface tightly attached to the outer surface of the reaction cup and a heat absorption surface opposite to the heat dissipation surface; the moisture separator further comprises: the water tank is provided with a cavity, a liquid return port and a liquid supply port which are communicated with the cavity, and the liquid return port is communicated with one end of the liquid return pipe, which is far away from the inner pipe body; the heat exchanger is arranged at the heat absorption surface of the semiconductor refrigeration piece and used for providing heat for the semiconductor refrigeration piece, the heat exchanger is provided with an input port and an output port, and the output port is communicated with one end, far away from the inner pipe body, of the liquid inlet pipe; and one end of the circulating pump is communicated with the liquid supply port of the water tank, and the other end of the circulating pump is communicated with the input port of the heat exchanger.
In a second aspect, an embodiment of the present application provides a water environment detection method, which adopts the above-mentioned water environment online automatic detection device, and includes the following steps: pumping a certain amount of oxidant into an absorption detection cup through a metering mechanism; pumping a quantitative water sample to be measured into the reaction cup through the metering mechanism; pumping a certain amount of buffer solution into the reaction cup through a metering mechanism; slowly adding a quantitative reducing agent into the reaction cup through the metering mechanism, completely converting arsenic in the water sample to be detected into arsine gas, separating water vapor in the reaction cup through the water-gas separator, introducing the arsine gas into the absorption detection cup through the absorption tube assembly, and standing; and (3) adding a quantitative color developing agent and a quantitative reducing agent into the absorption detection cup in sequence through a metering mechanism, performing color development detection, and analyzing to obtain the arsenic content in the water sample to be detected.
According to the online automatic detection device for the water environment, the arsine gas generated by the online automatic detection device for the water environment in the reaction cup enters the gas channel of the water-gas separator together with water vapor, the arsine gas and the water vapor flow in the gas channel in a rising mode, the inner pipe body is communicated with an external cooling water source, so that the inner pipe body has a lower temperature, the water vapor is condensed into liquid water when meeting the inner pipe body and the outer pipe body with lower temperatures when rising in the gas channel and flows back to the reaction cup along the water-gas separator, the generated arsine gas and the water vapor can be fully separated, the influence of the water vapor on color contrast detection is reduced or avoided, the detection accuracy is improved, and the practicability is improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts. In addition, in the drawings, like parts are denoted by like reference numerals, and the drawings are not drawn to actual scale.
Fig. 1 is a schematic structural diagram illustrating an online automatic detection device for water environment according to an embodiment of the present disclosure;
FIG. 2 is a schematic diagram illustrating the connection between the ejection mechanism and the colorimetric mechanism provided in the embodiments of the present application;
FIG. 3 is a schematic diagram illustrating a structure of an eviction mechanism provided by an embodiment of the present application;
FIG. 4 is a schematic structural diagram illustrating another eviction mechanism provided by embodiments of the present application;
fig. 5 is a schematic structural diagram of an absorption detection cup and a fixing tube according to an embodiment of the present disclosure.
Description of reference numerals:
1. a metering mechanism; 11. a metering tube; 12. a peristaltic pump; 13. a multi-way discharge valve;
2. a drive-out mechanism; 21. a reaction cup; 22. a water-gas separator; 221. an outer tube body; 2211. an intermediate pipe; 2212. a funnel structure; 2213. a converging tube; 222. an inner tube body; 2221. a liquid inlet pipe; 2222. a liquid return pipe; 223. a gas channel; 224. a self-spinning flow guiding structure; 225. a water tank; 226. a heat exchanger; 227. a circulation pump; 23. an absorbent tube assembly; 231. an electromagnetic valve; 232. a first absorption tube; 233. a second absorption pipe; 24. a first heating assembly; 241. a semiconductor refrigeration sheet;
3. a colorimetric mechanism; 31. an absorption detection cup; 32. a fixed tube; 33. a dual light path emitter; 34. a signal receiver; 35. emptying the pipe; 36. an evacuation valve; 37. a second heating assembly.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
As one of the elements which must be detected in the drinking water, arsenic is a key detection index, and is a harmful element capable of accumulating other toxic elements. Arsenic compounds, because of their high toxicity, are one of the heavy metal monitoring assays in domestic drinking water. The method for measuring arsenic in water mainly comprises an atomic fluorescence photometer analysis method, a colorimetric method, a simple method, an instrumental measurement method and an arsenic spot method.
In the related art, in order to separate the arsine gas from the water vapor, the arsine gas and the water vapor are treated by the drying agent, the water vapor is absorbed by the drying agent, but the drying agent can absorb a part of the arsine gas while absorbing the water vapor, so that the amount of the arsine gas entering the colorimetric mechanism is reduced, and the accuracy of colorimetric detection is influenced.
In some related arts, the inside of the used absorption tube assembly is dried by introducing dry air to dry the water vapor adhered to the inside of the absorption tube assembly, but the inside diameter of the absorption tube assembly is too small, so that the method is not easy to implement and the effect is not ideal.
Fig. 1 is a schematic structural diagram illustrating an online automatic detection device for water environment according to an embodiment of the present disclosure; FIG. 2 is a schematic diagram illustrating the connection between the ejection mechanism and the colorimetric mechanism provided in the embodiments of the present application; FIG. 3 is a schematic structural diagram illustrating an eviction mechanism provided by an embodiment of the present application; FIG. 4 is a schematic structural diagram illustrating another eviction mechanism provided by embodiments of the present application; fig. 5 is a schematic structural diagram of an absorption detection cup and a fixing tube according to an embodiment of the present disclosure.
As shown in fig. 1 to 5, an embodiment of the present application provides an online automatic detection device for a water environment, which mainly includes: metering mechanism 1, eviction mechanism 2 and color comparison mechanism 3, wherein:
the metering mechanism 1 mainly comprises a metering pipe 11, a peristaltic pump 12 communicated with a first end of the metering pipe 11 and a multi-way discharge valve 13 communicated with a second end of the metering pipe 11. Specifically, be provided with photoelectric sensor on the measurement pipe 11 for liquid in the measurement pipe 11, liquid is the water sample that awaits measuring, is used for oxidant, reductant, colour developing agent, buffer etc. that the water sample colorimetric detection that awaits measuring. In the specific use, at first open through a certain solenoid valve of many through valves, through peristaltic pump work with liquid suction in the measurement pipe, then measure the intraductal liquid of measurement through photoelectric sensor, reach required volume after, through the peristaltic pump back discharge effect with the liquid pump in the measurement pipe in expelling mechanism or the color comparison mechanism.
The expelling mechanism 2 comprises a reaction cup 21 communicated with the multi-way exhaust valve 13, a water-gas separator 22 communicated with the output end of the reaction cup 21 and an absorption tube assembly 23 communicated with the output end of the water-gas separator 22, wherein the water-gas separator 22 comprises an external tube body 221 and an internal tube body 222 arranged inside the external tube body 221, the internal tube body 222 is communicated with an external cooling water source, and a gas channel 223 is reserved between the internal tube body 222 and the external tube body 221. Specifically, the reaction cup is also called as an expulsion pool and is mainly used for converting arsenic in a water sample to be detected into arsine gas and expelling the arsine gas into an absorption detection cup in a colorimetric mechanism for colorimetric detection, and the gas channel is communicated with the absorption tube assembly and is used for introducing the arsine gas generated in the reaction cup into the absorption detection cup.
Specifically, the inner tube 222 and the outer tube 221 are coaxially arranged, and the gas channel 223 is an annular channel with the same width, so that gas can uniformly circulate in the gas channel 223, and the gas in the gas channel can be effectively cooled by a cooling water source in the inner tube.
The colorimetric mechanism 3 includes an absorption detection cup 31 communicating with the multi-way exhaust valve 13, and the output end of the absorption tube assembly 23 extends into the absorption detection cup 31.
In the application, the arsine gas generated in the reaction cup 21 and the steam enter the gas channel 223 of the water-gas separator 22 together, the arsine gas and the steam flow in the gas channel 223 in an ascending mode, the inner pipe body 222 is communicated with an external cooling water source, so that the inner pipe body 222 has a lower temperature, the steam meets the inner pipe body 222 and the outer pipe body 221 with the lower temperature when the steam rises in the gas channel 223 and is condensed into liquid water and flows back to the reaction cup 21 along the water-gas separator 22, the generated arsine gas and the generated steam can be fully separated, the influence of the steam on contrast color detection is reduced or avoided, the detection accuracy is improved, and the practicability is improved.
In some embodiments, the outer tube body 221 comprises a middle tube 2211, a funnel structure 2212 in communication with the bottom of the middle tube 2211, and a converging tube 2213 in communication with the top of the middle tube 2211, the funnel structure 2212 extending into the interior of the reaction cup 21.
In this application, the funnel structure 2212 of outside body 221 stretches into the inside to reaction cup 21, inside that gaseous arsine and vapor in the reaction cup 21 passed through the bottom opening of funnel structure 2212 get into outside body 221, vapor meets the surface of funnel structure 2212, make partly vapor condensation flow back to in the reaction cup 21, remaining vapor and gaseous arsine pass through funnel structure 2212 and get into in the gas passage 223 of water gas separator 22, vapor condenses the backward flow once more in gas passage 223, thereby guarantee the separation effect to gaseous arsine and vapor.
In some embodiments, the moisture separator 22 further includes a spin flow guiding structure 224 disposed inside the gas channel 223, and the gas in the gas channel 223 flows along the spin flow guiding structure 224 in a rotating manner.
In this application, arsine gas and vapor rise along the rotatory flow of spin water conservancy diversion structure 224 in gas passage 223, have increased the flow length of vapor in gas passage 223 to improve the condensation effect to vapor, rotatory rising vapor is in addition easier and microthermal outside body 221 or inside body 222 contact, further improves the condensation effect to vapor.
In some embodiments, the spin flow guiding structure 224 is a helical blade disposed on the outer circumference of the inner tube 222, and the outer circumference of the helical blade abuts against the inner surface of the middle tube 2211.
Specifically, the helical blade is fixedly disposed on the outer circumferential side of the inner tube 222, and the outer end of the helical blade abuts against the inner surface of the middle tube 2211, so that the self-rotating flow guiding structure 224 is formed inside the gas passage 223, and the gas rises along the gas passage 223 of the self-rotating flow guiding structure 224.
In some embodiments, intermediate tube 2211 is integrally formed with funnel structure 2212, and intermediate tube 2211 is connected to converging tube 2213 by threads or a connecting flange.
In this application, middle pipe 2211 and funnel structure 2212 integrated into one piece, middle pipe 2211 and the pipe 2213 that converges pass through threaded connection, conveniently will converge pipe 2213 and middle pipe 2211 split to pack interior body 222 and helical blade into in the middle pipe 2211 of outside body 221. The middle tube 2211 and the converging tube 2213 can be connected through a connecting flange, the effect of conveniently installing the inner tube 222 and the helical blades into the outer tube 221 is achieved, a sealing ring is arranged at the joint of the converging tube and the middle tube for sealing, the sealing performance of the joint of the converging tube and the middle tube is guaranteed, and gas leakage is prevented.
Specifically, the converging tube 2213 is a tubular structure with a small upper part and a large lower part, and can converge the arsine gas after water vapor separation, then the arsine gas is guided to the colorimetric mechanism 3 through the absorption tube component 23, meanwhile, the close structure with a small upper part and a big lower part can further increase the contact condition of the water vapor and the inner surface of the outer tube body, thereby further condensing the water vapor, fully separating the arsenic hydride gas and the water vapor, effectively coping with the situation of different gas speeds generated in the driving reaction process, because the expelling reaction is more violent in the early period and generates more gas, the expelling reaction gradually becomes slow, and only the water vapor evaporates, the arsine gas in the reaction cup can be completely pressed into the water-gas separator, thereby ensuring that the generated arsine gas can completely enter a subsequent colorimetric mechanism for colorimetric detection.
The middle pipe and the reaction cup are integrally formed, so that the sealing performance of the joint of the water-gas separator and the reaction cup is ensured. Prevent the leakage of the arsine gas and improve the safety in the operation process.
In some embodiments, the two ends of the inner tube 222 are sealed, and the inner tube 222 is provided with a liquid inlet tube 2221 and a liquid return tube 2222 in a communication manner.
In this application, during cooling water source passed through feed liquor pipe 2221 and gets into inside body 222, carry out cooling to the vapor in gas passage 223, cooling water source heaies up the back and flows out through liquid return pipe 2222, guarantees to have lower temperature in the inside body 222, can effectively cool off the vapor in gas passage 223.
Specifically, the liquid inlet tube 2221 and the liquid return tube 2222 are communicated with the top of the inner tube body 222, and the bottom of the liquid inlet tube 2221 is straightened at the bottom of the inner tube body 222, so that the input end of the gas channel 223 has a lower temperature, and the water vapor is more easily condensed.
Optionally, a plurality of baffles may be disposed inside the inner tube 222, and the cooling water source may be bent and flow inside the inner tube 222 through the plurality of baffles, so as to increase a heat exchange effect between the cooling water source and the inner tube 222.
Among the correlation technique, thereby the output of absorption tube directly stretches into and absorbs in detecting cup 31 and let in the absorption with arsine gas and detect cup 31, in order to make arsine gas fully absorbed, the output of absorption tube is located the bottom that absorbs and detects cup 31, when carrying out the color comparison and detecting, the part that the absorption tube is located absorption and detects cup 31 shelters from the color comparison and detects the light path easily, causes test result repeatability and the degree of accuracy to hang down.
As shown in fig. 1, 2 and 5, in some embodiments, the colorimetric mechanism 3 further comprises: a fixed tube 32, a dual optical path transmitter 33 and a signal receiver 34. The fixing tube 32 is disposed on the inner sidewall of the absorption detection cup 31 for fixing the output end of the absorption tube assembly 23. The dual light path emitter 33 is disposed at one side of the absorption detection cup 31. The signal receiver 34 is disposed on one side of the absorption detection cup 31 and opposite to the dual light path emitter 33.
In this application, through set up a fixed pipe 32 on absorbing the inside wall that detects cup 31, the tip of absorption tube subassembly 23 passes fixed pipe 32, it is spacing to be located the part that absorbs and detect cup 31 absorption tube subassembly 23 for absorption tube subassembly 23 hugs closely the inside wall that absorbs and detects cup 31, keeps away from the central detection pipeline that absorbs and detects cup 31, thereby the condition of sheltering from the colorimetric detection light path can not appear, improves the repeatability and the degree of accuracy of test result.
In addition, the output end of the absorption tube assembly 23 is fixed through the fixing tube 32, so that the output end of the absorption tube assembly 23 can be ensured to extend into the specified depth below the liquid level of the absorption liquid, the absorption effect of the absorption liquid on the arsine gas is ensured, and the stability of the absorption reaction is ensured.
Specifically, the dual-optical path emitter 33 emits dual-optical path light, the signal receiver 34 receives a detection signal, the absorbance of the mixed solution in the absorption detection cup 31 is measured, and the amount of arsine gas is calculated according to the absorbance, so that the content of arsenic in the water sample to be detected is obtained.
Wherein the inner diameter of the top of the absorption test cup 31 is larger than the inner diameter of the bottom, so as to facilitate the insertion of the end of the absorption tube assembly 23 into the absorption test cup 31.
In some embodiments, the colorimetric mechanism 3 further comprises an evacuation pipe 35 communicating with the top of the absorption detection cup 31, and an evacuation valve 36 provided on the evacuation pipe 35.
In the present application, when pumping liquid into the absorption detection cup 31, the evacuation valve 36 is opened, so that the inside and the outside of the absorption detection cup 31 are communicated, thereby ensuring that the liquid can be pumped into the absorption detection cup 31.
The colorimetric mechanism 3 in the present application further includes a fixing frame for fixing the absorption detection cup 31, the dual optical path emitter 33, and the signal receiver 34.
In some embodiments, the absorption pipe assembly 23 includes a solenoid valve 231, a first absorption pipe 232 communicating with one end of the solenoid valve 231, and a second absorption pipe 233 communicating with the other end of the solenoid valve 231, one end of the first absorption pipe 232 remote from the solenoid valve 231 communicates with the convergence pipe 2213 of the moisture separator 22, and one end of the second absorption pipe 233 remote from the solenoid valve 231 extends into the absorption detection cup 31 and is fixed in the fixing pipe 32.
Specifically, the solenoid valve 231 is a three-way valve, and a first end of the solenoid valve 231 is communicated with the first absorption pipe 232, a second end of the solenoid valve is communicated with the second absorption pipe 233, and a third end of the solenoid valve is communicated with the outside. The third end is communicated with the outside, so that the reaction cup is communicated with the outside, and the liquid can be pumped into the reaction cup 21 through the metering mechanism 1.
Wherein the third end of solenoid valve stretches into in the absorption liquid again with outside intercommunication, and the output of evacuation pipe stretches into in the absorption liquid again with outside intercommunication equally, and the harmful gas that produces in the absorption liquid can the effective absorption reaction process to guarantee the security of operation in-process.
In the present application, the end of the first absorption tube 232 is inserted into the moisture separator 22, the end of the second absorption tube 233 extends into the absorption detection cup 31 and is fixed by the fixing tube 32, and the arsine gas generated in the reaction cup 21 is introduced into the absorption detection cup 31 through the first absorption tube 232 and the second absorption tube 233 for colorimetric detection.
In some embodiments, the ejection mechanism 2 further includes a first heating assembly 24 disposed on an outer peripheral side of the reaction cup 21; the colorimetric mechanism 3 further includes a second heating unit 37 provided on the outer peripheral side of the absorption detection cup 31.
Specifically, a second fixing column is arranged on the outer side of the absorption detection cup 31, the second heating assembly 37 is a second heating resistance wire, and the second heating resistance wire is wound on the outer side of the second fixing column to fix and limit the second heating resistance wire.
In this application, the first heating assembly 24 is used for heating the reaction cup 21, and the second heating assembly 37 is used for heating the absorption detection cup 31.
As shown in fig. 3, in some embodiments, the first heating element 24 is a semiconductor cooling plate 241 disposed at an outer peripheral side of the reaction cup, and the semiconductor cooling plate 241 has a heat dissipating surface closely attached to an outer surface of the reaction cup and a heat absorbing surface opposite to the heat dissipating surface; the moisture separator 22 further includes: a water tank 225, a heat exchanger 226, and a circulation pump 227, wherein:
the water tank 225 has a cavity, and a liquid return port and a liquid supply port which are communicated with the cavity, and the liquid return port is communicated with one end of the liquid return pipe 2222 which is far away from the inner pipe body.
The heat exchanger 226 is disposed at a heat absorbing surface of the semiconductor chilling plate 241, and is configured to provide heat to the semiconductor chilling plate 241, and the heat exchanger 226 has an input port and an output port, where the output port is communicated with one end of the liquid inlet pipe 2221, which is far away from the inner pipe body 222.
One end of the circulating pump 227 is communicated with a liquid supply port of the water tank 225, and the other end is communicated with an input port of the heat exchanger 226.
In this application, the reaction cup is hugged closely to semiconductor refrigeration piece 241's cooling surface, be used for heating for the reaction cup, provide suitable temperature for the expulsion of arsine gas in the water sample that awaits measuring, semiconductor refrigeration piece 241's heat-absorbing surface and heat exchanger 226 carry out the heat transfer simultaneously, circulating pump 227 lets in the water tank 225 in the heat exchanger 226, thereby carry out cooling to the water in the heat exchanger 226, let in the condensation that is arranged in gas channel vapor in the inside body through the feed liquor pipe after the water cooling, water after rising temperature returns in the inside body returns water tank 225 through the liquid return pipe, realize cooling water source's circulation, can reach the difference in temperature fast, and the energy consumption is low.
Specifically, the quantity of semiconductor refrigeration piece 241 is a plurality of, set up in the periphery side of reaction cup, the outside of the refrigeration piece of every semiconductor sets up a heat exchanger 226, heat exchanger 226 adopts finned heat exchanger 226, the one end of heat transfer fin is connected with the heat absorption face of semiconductor refrigeration piece 241, the other end is located the casing of heat exchanger 226, cooling water source flows in the casing of heat exchanger 226, the realization is to cooling water source's cooling, it is specific, heat transfer fin still has the effect of water conservancy diversion in heat exchanger 226 casing, increase the distance that cooling water source flows in heat exchanger 226 casing, guarantee the heat transfer effect.
As shown in fig. 4, optionally, a first fixing column is disposed on an outer side of the reaction cup 21, the first heating assembly 24 is a first heating resistance wire, and the first heating resistance wire is wound on the outer side of the first fixing column to fix and limit the first heating resistance wire.
The arsine gas generated by the water environment online automatic detection device in the reaction cup 21 is communicated with the steam and enters the gas channel 223 of the water-gas separator 22 together, the arsine gas and the steam flow in the gas channel 223 in an ascending mode, the inner pipe body 222 is communicated with an external cooling water source, so that the inner pipe body 222 has a lower temperature, the steam meets the inner pipe body 222 and the outer pipe body 221 with the lower temperature when rising in the gas channel 223 and is condensed into liquid water and flows back to the reaction cup 21 along the water-gas separator 22, the generated arsine gas and the steam can be fully separated, the influence of the steam on color contrast detection is reduced or avoided, the detection accuracy is improved, and the practicability is improved.
The water environment on-line automatic detection device is not only suitable for detecting arsenic in a water sample, but also suitable for detecting other gaseous components of a target object.
The embodiment of the application also provides a water environment detection method, and the water environment online automatic detection device comprises the following steps:
pumping a certain amount of oxidant into an absorption detection cup through a metering mechanism 1;
pumping a quantitative water sample to be measured into the reaction cup 21 through the metering mechanism 1;
pumping a certain amount of buffer solution into the reaction cup 21 through the metering mechanism 1;
slowly adding a quantitative reducing agent into the reaction cup 21 through the metering mechanism 1, completely converting arsenic in a water sample to be detected into arsine gas, separating water vapor in the reaction cup 21 through the water vapor separator 22, introducing the arsine gas into the absorption detection cup through the absorption tube assembly 23, and standing;
quantitative color developing agent and reducing agent are sequentially added into the absorption detection cup 31 through the metering mechanism 1 for color development detection, and the arsenic content in the water sample to be detected is obtained through analysis.
Example 1:
step one, a peristaltic pump is started, meanwhile, a certain electromagnetic valve in a multi-way exhaust valve is opened, an oxidant (the oxidant is 20g/L potassium persulfate solution) of a connecting pipeline of the peristaltic pump is pumped into a metering pipe, when a photoelectric sensor senses that a water sample reaches a specific liquid level, the peristaltic pump is stopped, an exhaust valve at the top of an absorption detection cup is opened and communicated with an air end, the peristaltic pump reversely exhausts the oxidant into the absorption detection cup to finish quantitative sampling of the oxidant, and the absorption detection cup is started to heat and is kept at 50 ℃;
step two, the peristaltic pump is started, meanwhile, one path of electromagnetic valve in the multi-way drain valve is opened, a water sample to be detected of a connecting pipeline of the multi-way drain valve is pumped into the metering pipe, when the photoelectric sensor senses that the water sample reaches a specific liquid level, the peristaltic pump is stopped, the electromagnetic valves at the bottom and the top of the reaction cup are opened, the peristaltic pump reversely drains the water sample to be detected and enters the reaction cup, and quantitative sampling of the water sample to be detected is completed;
adding a buffer solution (a mixed solution of 0.25mol/L sulfuric acid and 30g/L tartaric acid) into a reaction cup, and keeping the temperature of the reaction cup at 30 ℃;
step four, slowly adding a reducing agent (mixed solution of potassium hydroxide with the concentration of 3g/L and potassium borohydride with the concentration of 80 g/L) into a reaction cup, completely converting arsenic in a water sample to be detected into arsine gas, allowing the arsine gas to enter an absorption detection cup through a water-gas separator and an absorption tube assembly, and reacting the absorption detection cup for 5min at the constant temperature of 70 ℃;
opening an emptying valve at the top end of the absorption detection cup to be communicated with air, starting a peristaltic pump to sequentially add a color developing agent and a reducing agent into the absorption detection cup, carrying out color development at the constant temperature of 50 ℃ for 15min, sending out detection light of 840nm by using a double-light-path emitter, receiving a detection signal by using a signal receiver, and measuring the absorbance of a mixed solution in the absorption detection cup; the control system calculates the content of arsenic in the water sample to be detected according to the absorbance;
and step six, respectively pumping the mixed solution in the absorption detection cup and the mixed solution in the reaction cup to a metering pipe, discharging the mixed solution to a waste liquid barrel, and then cleaning and emptying the waste liquid barrel to finish the detection of arsenic in a once complete water sample.
Example 2:
step one, a peristaltic pump is started, meanwhile, a certain electromagnetic valve in a multi-way exhaust valve is opened, an oxidant (the oxidant is 30g/L potassium persulfate solution) of a connecting pipeline of the peristaltic pump is pumped into a metering pipe, when a photoelectric sensor senses that a water sample to be detected reaches a specific liquid level, the peristaltic pump is stopped, an exhaust valve at the top of an absorption detection cup is opened and communicated with an air end, the peristaltic pump reversely exhausts the oxidant to enter the absorption detection cup, quantitative sampling of the oxidant is completed, and the absorption detection cup is started to heat and is kept at 65 ℃;
opening a peristaltic pump, simultaneously opening a certain electromagnetic valve in a multi-way drain valve, pumping a water sample to be detected of a connecting pipeline into a metering pipe, stopping the peristaltic pump when a photoelectric sensor senses that the water sample reaches a specific liquid level, opening electromagnetic valves at the bottom and the top of a reaction cup, reversely discharging the water sample to be detected by the peristaltic pump, and entering the reaction cup to finish quantitative sampling of the water sample;
adding a buffer solution (a mixed solution of 0.5mol/L sulfuric acid and 60g/L tartaric acid) into a reaction cup, and keeping the temperature of the reaction cup at 40 ℃;
step four, slowly adding a reducing agent (mixed solution of potassium hydroxide with the concentration of 6g/L and potassium borohydride with the concentration of 100 g/L) into a reaction cup, completely converting arsenic in a water sample into arsine gas, allowing the arsine gas to enter an absorption detection cup through a water-gas separator and an absorption tube assembly, and reacting the absorption detection cup for 10min at the constant temperature of 50 ℃;
opening an emptying valve at the top end of the absorption detection cup to be communicated with air, starting a peristaltic pump to sequentially add a color developing agent and a reducing agent into the absorption reaction tank, carrying out color development at the constant temperature of 50 ℃ for 5min, sending out detection light of 840nm by using a double-light-path emitter, receiving a detection signal by using a signal receiver, and measuring the absorbance of a mixed solution in the absorption detection cup; the control system calculates the content of arsenic in the water sample through absorbance;
and step six, respectively absorbing the mixed solution in the detection cup and the mixed solution in the reaction cup, pumping the mixed solution to a metering pipe, discharging the mixed solution to a waste liquid barrel, and then cleaning and emptying the waste liquid barrel to finish the detection of arsenic in the complete water sample once.
It should be noted that references in the specification to "one embodiment," "an example embodiment," "some embodiments," etc., indicate that the embodiment described may include a particular feature, structure, or characteristic, but every embodiment may not necessarily include the particular feature, structure, or characteristic. Moreover, such phrases are not necessarily referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with an embodiment, it is within the knowledge of one skilled in the art to effect such feature, structure, or characteristic in connection with other embodiments whether or not explicitly described.
It should be readily understood that "on … …", "above … …" and "above … …" in this disclosure should be interpreted in the broadest sense such that "on … …" means not only "directly on something", but also includes the meaning of "on something" with intervening features or layers therebetween, and "above … …" or "above … …" includes not only the meaning of "above something" or "above" but also includes the meaning of "above something" or "above" with no intervening features or layers therebetween (i.e., directly on something).
Furthermore, spatially relative terms, such as "below," "lower," "above," "upper," and the like, may be used herein for ease of description to describe one element or feature's illustrated relationship to another element or feature. Spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. The device may have other orientations (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly as well.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in the process, method, article, or apparatus that comprises the element.
Finally, it should be noted that: the above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
Claims (12)
1. An online automatic detection device for water environment is characterized by comprising:
the metering mechanism (1) comprises a metering pipe (11), a peristaltic pump (12) communicated with a first end of the metering pipe (11) and a multi-way discharge valve (13) communicated with a second end of the metering pipe (11);
the driving-out mechanism (2) comprises a reaction cup (21) communicated with the multi-way exhaust valve (13), a water-gas separator (22) communicated with the output end of the reaction cup (21) and an absorption pipe assembly (23) communicated with the output end of the water-gas separator (22), the water-gas separator (22) comprises an external pipe body (221) and an internal pipe body (222) arranged inside the external pipe body (221), the internal pipe body (222) is communicated with an external cooling water source, and a gas channel (223) is reserved between the internal pipe body (222) and the external pipe body (221);
the colorimetric mechanism (3), colorimetric mechanism (3) including with absorption detection cup (31) that multi-pass valve (13) communicate, the output of absorption tube subassembly (23) stretches into inside absorption detection cup (31).
2. The online automatic detection device for the water environment according to claim 1, wherein the external pipe body (221) comprises a middle pipe (2211), a funnel structure (2212) communicated with the bottom of the middle pipe (2211), and a convergence pipe (2213) communicated with the top of the middle pipe (2211), and the funnel structure (2212) extends into the reaction cup (21).
3. The online automatic detection device for the water environment according to claim 2, characterized in that the moisture separator (22) further comprises a spin flow guiding structure (224) arranged inside the gas channel (223), and the gas in the gas channel (223) flows along the spin flow guiding structure (224) in a rotating manner.
4. The water environment online automatic detection device according to claim 3, wherein the self-rotating flow guiding structure (224) is a helical blade arranged on the outer periphery of the inner pipe body (222), and the outer periphery of the helical blade abuts against the inner surface of the intermediate pipe (2211).
5. The water environment online automatic detection device according to claim 2, characterized in that the middle pipe (2211) and the funnel structure (2212) are integrally formed, and the middle pipe (2211) and the convergence pipe (2213) are connected through a thread or a connecting flange.
6. The water environment online automatic detection device according to claim 1, wherein two ends of the inner pipe body (222) are respectively sealed, and a liquid inlet pipe (2221) and a liquid return pipe (2222) are communicated with the inner pipe body (222).
7. The water environment on-line automatic detection device according to claim 2, characterized in that the colorimetric mechanism (3) further comprises:
the fixed pipe (32) is arranged on the inner side wall of the absorption detection cup (31) and is used for fixing the output end of the absorption pipe component (23);
a dual light path emitter (33) disposed on one side of the absorption detection cup (31);
and the signal receiver (34) is arranged on one side of the absorption detection cup (31) and is opposite to the dual-light-path emitter (33).
8. The water environment online automatic detection device according to claim 1, wherein the colorimetric mechanism (3) further comprises an emptying pipe (35) communicated with the top of the absorption detection cup (31) and an emptying valve (36) arranged on the emptying pipe (35).
9. The water environment online automatic detection device according to claim 7, characterized in that the absorption tube assembly (23) comprises a solenoid valve (231), a first absorption tube (232) communicated with one end of the solenoid valve (231), and a second absorption tube (233) communicated with the other end of the solenoid valve (231), one end of the first absorption tube (232) far away from the solenoid valve (231) is communicated with the convergence tube (2213) of the moisture separator (22), and one end of the second absorption tube (233) far away from the solenoid valve (231) extends into the absorption detection cup (31) and is fixed in the fixed tube (32).
10. The water environment online automatic detection device according to claim 6, characterized in that the drive-out mechanism (2) further comprises a first heating assembly (24) arranged on the outer circumferential side of the reaction cup (21); the colorimetric mechanism (3) further comprises a second heating member (37) provided on the outer peripheral side of the absorption detection cup (31).
11. The water environment online automatic detection device according to claim 10, wherein the first heating component (24) is a semiconductor cooling plate (241) disposed on the outer peripheral side of the reaction cup, and the semiconductor cooling plate (241) has a heat dissipation surface attached to the outer surface of the reaction cup and a heat absorption surface opposite to the heat dissipation surface;
the moisture separator (22) further comprises:
the water tank (225) is provided with a cavity, a liquid return port and a liquid supply port which are communicated with the cavity, and the liquid return port is communicated with one end of the liquid return pipe, which is far away from the inner pipe body;
the heat exchanger (226) is arranged at the heat absorption surface of the semiconductor refrigeration piece (241) and is used for providing heat for the semiconductor refrigeration piece (241), the heat exchanger (226) is provided with an input port and an output port, and the output port is communicated with one end, far away from the inner tube body, of the liquid inlet tube;
and one end of the circulating pump (227) is communicated with a liquid supply port of the water tank (225), and the other end of the circulating pump is communicated with an input port of the heat exchanger (226).
12. A method for detecting a water environment by using the device for automatically detecting the water environment on line according to any one of claims 1 to 11, which is characterized by comprising the following steps:
pumping a certain amount of oxidant into an absorption detection cup through a metering mechanism (1);
pumping a quantitative water sample to be measured into a reaction cup (21) through a metering mechanism (1);
pumping a certain amount of buffer solution into a reaction cup (21) through a metering mechanism (1);
a quantitative reducing agent is slowly added into the reaction cup (21) through the metering mechanism (1), arsenic in a water sample to be detected is completely converted into arsine gas, water vapor in the reaction cup (21) is separated through the water vapor separator (22), and the arsine gas is introduced into the absorption detection cup through the absorption tube assembly (23) and stands still;
quantitative color developing agent and reducing agent are sequentially added into the absorption detection cup (31) through the metering mechanism (1) for color development detection, and the arsenic content in the water sample to be detected is obtained through analysis.
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