CN205786321U - A kind of device of on-line checking Ammonia In Sea Water nitrogen content - Google Patents
A kind of device of on-line checking Ammonia In Sea Water nitrogen content Download PDFInfo
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- CN205786321U CN205786321U CN201620463178.4U CN201620463178U CN205786321U CN 205786321 U CN205786321 U CN 205786321U CN 201620463178 U CN201620463178 U CN 201620463178U CN 205786321 U CN205786321 U CN 205786321U
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Abstract
The utility model discloses the device of a kind of on-line checking Ammonia In Sea Water nitrogen content, realize the detection of ammonia-nitrogen content in sea water solution based on fluorospectrophotometry, including the first three-way magnetic valve, the second three-way magnetic valve, peristaltic pump, hybrid heating device, fluorescence floating cuvette, light source, optical receiver and signal processing system.Flow Injection Technique is combined by this utility model with fluorospectrophotometry, by controlling two three-way magnetic valves, peristaltic pump order sample introduction, it is achieved that Ammonia In Sea Water nitrogen content on-line checking, integrated level is high, and simple to operate, mix reagent is single, response time is short, and timeliness is fast.By using hybrid heating device to heat being pumped into seawater sample solution and OPA mix reagent in stream, and realize being sufficiently mixed of the two during heating, it is achieved thereby that mixing unites two into one with heating, while reducing volume, ensure that the completeness of reaction, be favorably improved the accuracy of testing result.
Description
Technical field
This utility model belongs to sewater chemistry analysis technical field, specifically, relates to a kind of detection device for measuring Ammonia In Sea Water nitrogen content.
Background technology
Ammonia nitrogen inorganic nutrient salt be a kind of in water with free ammonia (NH3) and ammonium ion (NH4 +) form exist nitrogen, typically use symbol NH4 +-N represents, is mainly derived from itrogenous organic substance in sanitary sewage by industrial wastewater and agricultural drains etc. such as the catabolite of microbial action, synthesis ammonia.Measure the ammonia-nitrogen content in water quality, contribute to evaluating water body and be contaminated and " self-cleaning " situation.In water quality, traditional assay method of ammonia-nitrogen content is Nessler's reagent photometer, but owing to sea water including substantial amounts of calcium, magnesium ion, these calcium, magnesium ion are easy to react with nessler reagent, cause water sample muddy and interference measurement, it is thus desirable to carry out corresponding pretreatment, complex operation is complicated, and includes cytotoxic compound in reagent used, environment can be caused certain pollution, therefore be unsuitable for sea water detection.
At present, the detection for Ammonia In Sea Water inorganic nutrients salt content mainly carries out spot sampling according to the hypobromite oxidation method in marine monitoring specification (GB 17378-2007) and indigo spectrophotometry, experimental determination.But, all there is the shortcomings such as preparation of reagents loaded down with trivial details, response time length, poor real in both assay methods.
In recent years, use fluorescence method to measure the technology of ammonia-nitrogen content in water body to be developed rapidly.The method utilizes o-phthalaldehyde(OPA) (OPA) to react with ammonia nitrogen in alkaline medium, under conditions of being heated to 45 DEG C, generation has epipolic isoindole derivatives, by detecting the fluorescence intensity that this isoindole derivatives produces, to calculate the ammonia-nitrogen content in sea water.The method uses single mix reagent, reagent is nontoxic, good stability, but need to carry out fluorescence spectrometry by instrument after complete to sea water to be measured and o-phthalaldehyde(OPA) (OPA) reagent hybrid reaction the most artificially during measuring, therefore automaticity is low, operate relative complex, poor in timeliness, it is impossible to the ammonia-nitrogen content in sea water is realized on-line determination.
Summary of the invention
The purpose of this utility model is to provide a kind of device that ammonia-nitrogen content in sea water can realize on-line checking, simple to operate, and automaticity is high, and real-time is good.
For solving above-mentioned technical problem, this utility model is achieved by the following technical solutions:
The device of a kind of on-line checking Ammonia In Sea Water nitrogen content, including the first three-way magnetic valve, the second three-way magnetic valve, peristaltic pump, hybrid heating device, fluorescence floating cuvette, light source, optical receiver and signal processing system；The normal open entrance of described first three-way magnetic valve is used for receiving seawater sample solution, and its normally closed entrance is used for receiving distilled water；The normal open entrance of described second three-way magnetic valve connects the outlet of the first three-way magnetic valve, and its normally closed entrance is used for receiving o-phthalaldehyde(OPA) mix reagent；The entrance of described peristaltic pump connects the outlet of the second three-way magnetic valve；Described hybrid heating device includes heating rod and the fluid delivery tube being wrapped on described heating rod, the entrance connection wriggling delivery side of pump of described fluid delivery tube；The entrance of described fluorescence floating cuvette connects the outlet of described fluid delivery tube, and its outlet is used for discharging waste liquid；Being provided with light incidence window and light exit window on described fluorescence floating cuvette, the central axis of described smooth incidence window and light exit window is perpendicular；Described light source launches the laser beam of specific wavelength, and the light incidence window through described fluorescence floating cuvette irradiates the liquid in described floating cuvette；Described optical receiver receives the fluorescence penetrated by the light exit window of described fluorescence floating cuvette, and is converted into the corresponding signal of telecommunication according to the fluorescence intensity received；Described signal processing system receives the signal of telecommunication of described optical receiver output.
In order to reduce the impact that testing result is caused by bubble, the chamber being internally provided with for accommodating described liquid at described fluorescence floating cuvette, the entrance of described fluorescence floating cuvette connects the bottom of described chamber via the interior fluid passage lost in the wall body of fluorescence floating cuvette, the top of chamber described in the outlet of described fluorescence floating cuvette, flow the most from bottom to top by controlling liquid, so that the bubble produced in liquid flow process all concentrates on the top of test point, it is to avoid testing result is impacted；Also it is enclosed with black polyethylene lucifuge shell in the outside of described fluorescence floating cuvette, to avoid ambient light to irradiate the liquid in described chamber, testing result is interfered.
Preferably, described chamber is preferably designed to cuboid or column type, to facilitate light incidence window and the laying of light exit window.
Preferably, on adjacent two sides of the left-right and front-back surrounding that described smooth incidence window and light exit window are opened in fluorescence floating cuvette.
Further, the LED that described light source can use emission center wavelength to be 365nm exciting light light beam, just light incidence window to described fluorescence floating cuvette, the exciting light light beam with the liquid propellant wavelength in fluorescence floating cuvette as 365nm by its exiting surface.
Further, between the light incidence window of described LED and fluorescence floating cuvette, the optical filter that centre wavelength is 365nm it is additionally provided with, to filter veiling glare.
Preferably, described optical receiver preferably employs photodiode, the fluorescence penetrated by the light exit window of described fluorescence floating cuvette is via the photodiode described in the bandpass filter directive of 400nm-480nm, to detect the fluorescence intensity in the range of 400-480nm.
In order to ensure that the temperature flowing through the liquid of hybrid heating device can stably arrive required temperature, in described hybrid heating device, the shell of described heating rod is stainless steel casing, described fluid delivery tube is wound around 10-50 circle on the shell of described heating rod, is enclosed with heat insulation adhesive tape in the outside of described fluid delivery tube.
The overall assembling of each parts in detection device for convenience, a fluid manifold valve plate it is additionally provided with in the device of described on-line checking Ammonia In Sea Water nitrogen content, it is carved with fluid passage in the inside of described fluid manifold valve plate, described first three-way magnetic valve, the second three-way magnetic valve, peristaltic pump, fluorescence floating cuvette, light source and optical receiver are arranged on described fluid manifold valve plate, described first three-way magnetic valve, are connected by described fluid passage between the second three-way magnetic valve and peristaltic pump.
Compared with prior art, advantage of the present utility model and good effect are:
1, Flow Injection Technique is combined by this utility model with fluorospectrophotometry, the ammonia-nitrogen content in on-line checking sea water, and by controlling three-way magnetic valve, peristaltic pump order sample introduction, integrated level is high, and simple to operate, volume is little, is suitable for on-line analysis；
2, in detection device of the present utility model, fluorescence floating cuvette uses the mode that liquid flows from bottom to top, and the bubble produced during making liquid flowing all concentrates on the top of test point, and testing result is formed without interference, and testing result is stable；
3, hybrid heating device of the present utility model, unites two into one liquid mixing with heating, ensure that the completeness of reaction while reducing volume；
4, Flow injection fluorometry of the present utility model, uses single mix reagent, and preparation is simple, low toxicity, and reagent waste is few, and reaction condition is gentle, and the response time is short, and timeliness is fast.
After reading in conjunction with the accompanying the detailed description of this utility model embodiment, other features of the present utility model and advantage will become clearer from.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of a kind of embodiment of the device of the on-line checking Ammonia In Sea Water nitrogen content that this utility model is proposed.
Detailed description of the invention
Below in conjunction with the accompanying drawings detailed description of the invention of the present utility model is described in detail.
The detection device of the present embodiment is mainly for detection of the ammonia-nitrogen content in the sample solutions such as sea water, the key component such as including the first three-way magnetic valve V1, the second three-way magnetic valve V2, peristaltic pump P, hybrid heating device MH, fluorescence floating cuvette C, light source L, optical receiver PM and signal processing system PC, as shown in Figure 1.
Fixing for the ease of the installation of each parts in detection device, the present embodiment preferably centers a fluid manifold valve plate (not shown) at described detection dress, it is preferred to use lucite is made, in case the erosion of the solution such as antacid, alkali, high salt.Being etched with a plurality of fluid passage in the inside of described fluid manifold valve plate, these fluid passages are used for connecting three-way magnetic valve V1, V2 and peristaltic pump P as a part for stream, to shorten the length of stream, reduce interface and leak source.The present embodiment offers screwed hole and drain through hole on described fluid manifold valve plate, described screwed hole is for using the miscellaneous part in threaded mode fixed test device, such as three-way magnetic valve V1, V2, peristaltic pump P, fluorescence floating cuvette C, light source L, optical receiver PM and fluid delivery tube etc..Described drain through hole is for connecting three-way magnetic valve V1, V2 and the fluid passage within valve plate.
Described two three-way magnetic valves V1, V2 are two-position three way, and an aperture on first is to be connected on stream always, can be as outlet, it is also possible to as entrance；Having two apertures on second, one is normal open mouth, and another is normally closed port, and the two aperture must be simultaneously as entrance or outlet.For two apertures being on second, defining described three-way magnetic valve V1, V2 and being in the aperture of connected state when power-off is closed with the aperture on first is that to be in the aperture of state of isolation be normally closed port to the aperture on normal open mouth, with first.Three-way magnetic valve V1, V2 energising open time, described normal open mouth with first on aperture completely cut off, described normally closed port connects with the aperture on first.Changing the power on/off state of three-way magnetic valve V1, V2, flow direction and the selectivity that can control fluid flow into.In the present embodiment, the aperture that described first, second three-way magnetic valve V1, V2 is on first as entrance, is called normal open entrance and normally closed entrance as outlet, two apertures being on second.Three-way magnetic valve V1, V2 of the present embodiment preferably employs PEEK material and makes, in case the erosion of the solution such as antacid, alkali, high salt, operating pressure is in (2～3) × 105Between Pa.
Below in conjunction with Fig. 1, the concrete annexation between all parts in the seawater ammonia-nitrogen content detection device of the present embodiment is described in detail.
As it is shown in figure 1, the normal open entrance of the first three-way magnetic valve V1 is connected with the vessel containing seawater sample solution by the present embodiment by fluid delivery tube, for receiving seawater sample solution S to be measured.The normally closed entrance of the first three-way magnetic valve V1 is connected distilled water DIW via fluid delivery tube, for introduction to distilled water DIW, cleans the stream of device.The outlet of the first three-way magnetic valve V1 is connected through the fluid passage of the internal etching of described fluid manifold valve plate the normal open entrance of the second three-way magnetic valve V2.Described fluid delivery tube preferably employ external diameter be 1-4mm, internal diameter be polyfluortetraethylene pipe or the silica gel tube of 0.5-2mm, quickly flow while requirement meeting liquid, the corrosion of the solution such as strong acid, highly basic, high salt can be tolerated.For described second three-way magnetic valve V2, its normally closed entrance is connected with the vessel containing o-phthalaldehyde(OPA) mix reagent, for receiving o-phthalaldehyde(OPA) mix reagent.The outlet of the second three-way magnetic valve V2 is connected by the entrance of fluid delivery tube with peristaltic pump P, described peristaltic pump P outlet by fluid delivery tube connect described in hybrid heating device MH.In the present embodiment, described peristaltic pump P preferably employs 6 rotor pulse pumps, and pump discharge is between 0.4～24ml/min.Heating rod and the fluid delivery tube being wrapped on described heating rod it is provided with in described hybrid heating device MH, the liquid pumped out by peristaltic pump P is flowed around described heating rod via described fluid delivery tube, realizing while sample solution mixes with OPA reagent, absorb the heat that heating rod produces, the temperature making mixed solution is increased to design temperature, to meet reaction condition.In the present embodiment, the shell of described heating rod preferably employs stainless steel, a diameter of 8mm, a length of 50-150mm, and controlling temperature is 45 DEG C, can be wound around fluid delivery tube 10-50 circle.After being wrapped on heating rod by fluid delivery tube, wrap up one layer of heat insulation adhesive tape in the outside of fluid delivery tube, to keep the temperature of mixed solution.Mixed solution after being heated by heater MH enters in the chamber within fluorescence floating cuvette C via the entrance of fluorescence floating cuvette C, to carry out illumination detection.In the present embodiment, described fluorescence floating cuvette C preferably employs quartz material and makes, what it was internally formed is preferably designed to cuboid or column type for accommodating the chamber of liquid, it is enclosed with black polyethylene lucifuge shell in the outside of fluorescence floating cuvette C, to avoid ambient light to inject chamber, testing result is interfered.On adjacent two sidewall of fluorescence floating cuvette C, such as on left side wall and front side wall, offer two orthogonal windows of central axis respectively, using as light incidence window and light exit window.The light path designing described fluorescence floating cuvette C is 1-5cm, width is 10-25mm, height is 20-50mm, and the width of window is 1-10mm, height is 2-20mm.The entrance and exit of fluorescence floating cuvette C is arranged at the top of fluorescence floating cuvette C, and on the wall body of fluorescence floating cuvette C, lose fluid passage, described fluid passage is connected with the entrance of fluorescence floating cuvette C and the bottom of described chamber respectively, makes the liquid entered by entrance be full of whole chamber from bottom to top via the bottom of chamber.Top by chamber described in the outlet of described fluorescence floating cuvette C, flow the most from bottom to top by controlling liquid, so that the bubble produced in liquid flow process is all gathered in the top of chamber, incident light will not be produced interference, thus can stop the impact that testing result is caused by bubble, improve the accuracy of testing result.The outlet of fluorescence floating cuvette C is connected fluid delivery tube, is used for discharging waste liquid W.
In the present embodiment, described light source L preferably employs the LED of the exciting light light beam that emission center wavelength is 365nm to irradiate the mixed solution in fluorescence floating cuvette C.Specifically, can by the exiting surface of light source L just light incidence window to fluorescence floating cuvette C, the optical filter F1 that centre wavelength is 365nm can also be set between the light incidence window of described light source L and fluorescence floating cuvette C further, to filter the veiling glare of other wavelength, the laser beam only making 365nm wavelength injects described light incidence window via fiber optic conduction, irradiate the mixed solution in fluorescence floating cuvette C, to excite generation fluorescence signal.The just light exit window to fluorescence floating cuvette C by the sensitive surface of optical receiver PM, and between the sensitive surface and the light exit window of fluorescence floating cuvette C of described optical receiver PM, set up the bandpass filter F2 of 400nm-480nm, optical receiver PM is made to receive wavelength fluorescence in the range of 400nm-480nm, and generating the corresponding signal of telecommunication according to the intensity of the fluorescence signal received, transmission to signal processing system PC carries out the mensuration of ammonia-nitrogen content.
In the present embodiment, described optical receiver PM preferably employs photodiode and carries out collection and the conversion of fluorescence signal, signal processing system PC is calculated the fluorescence intensity of seawater sample solution generated contrast with the fluorescence intensity-concentration relationship curve of Ammonia nitrogen standard liquid, just can obtain the concentration of seawater sample ammonia nitrogen in solution.
Certainly, the detection device of the present embodiment can also arrange controller further, to carry out described three-way magnetic valve V1, V2, peristaltic pump P, heater MH, light source L and optical receiver PM opening and closing control.
When utilizing the seawater ammonia-nitrogen content detection device shown in Fig. 1 that seawater sample carries out ammonia-nitrogen content detection, the first three-way magnetic valve V1, peristaltic pump P and light source L can be first turned on, coutroi velocity is 5ml/min, pump into distilled water DIW, rinse the stream of detection device, until after there is no fluorescence signal, closing the first three-way magnetic valve V1, peristaltic pump P and LED.
Then, opening peristaltic pump P, LED, hybrid heating device MH, coutroi velocity is 5 ml/min, pumps into the seawater sample solution S of 1min；Open the second three-way magnetic valve V2, pump into OPA mix reagent 10s；It is then shut off the second three-way magnetic valve V2；Being turned down by flow velocity to 3ml/min, reactant liquor is by fluorescence floating cuvette C and fluorescence signal occurs.After signal is more stable, closes peristaltic pump P, is received by photodiode PM after resting on filtered F2 of fluorescence that the reactant liquor in fluorescence floating cuvette C is launched, and be converted into signal of telecommunication output to signal processing system PC, to obtain corresponding fluorescence intensity Is.Closing hybrid heating device MH, open peristaltic pump P and the first three-way magnetic valve V1, coutroi velocity is 5 ml/min, and flusher stream discharges waste liquid W simultaneously.After substantially not having fluorescence signal, closing peristaltic pump P, close LED, detection terminates.
Now, utilize fluorescence intensity Is detected, in conjunction with the fluorescence intensity-concentration relationship curve of known ammonia nitrogen, to obtain the ammonia-nitrogen content in seawater sample solution S.
Thus, just can complete the mensuration of ammonia-nitrogen content in seawater sample solution S.
Certainly; the above is only a kind of preferred implementation of the present utility model; should be understood that; for those skilled in the art; on the premise of without departing from this utility model principle; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection domain of the present utility model.
Claims (8)
1. the device of an on-line checking Ammonia In Sea Water nitrogen content, it is characterised in that including:
First three-way magnetic valve, its normal open entrance is used for receiving seawater sample solution, and its normally closed entrance is used for receiving distilled water；
Second three-way magnetic valve, its normal open entrance connects the outlet of the first three-way magnetic valve, and its normally closed entrance is used for receiving o-phthalaldehyde(OPA) mix reagent；
Peristaltic pump, its entrance connects the outlet of the second three-way magnetic valve；
Hybrid heating device, it includes heating rod and the fluid delivery tube being wrapped on described heating rod, the entrance connection wriggling delivery side of pump of described fluid delivery tube；
Fluorescence floating cuvette, its entrance connects the outlet of described fluid delivery tube, and its outlet is used for discharging waste liquid；Being provided with light incidence window and light exit window on described fluorescence floating cuvette, the central axis of described smooth incidence window and light exit window is perpendicular；
Light source, it launches the laser beam of specific wavelength, through the liquid in the light incidence window described floating cuvette of irradiation of described fluorescence floating cuvette；
Optical receiver, it is received the fluorescence penetrated by the light exit window of described fluorescence floating cuvette, and is converted into the corresponding signal of telecommunication according to the fluorescence intensity received；
Signal processing system, it receives the signal of telecommunication of described optical receiver output.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 1, it is characterized in that, the chamber being internally provided with for accommodating described liquid at described fluorescence floating cuvette, the entrance of described fluorescence floating cuvette connects the bottom of described chamber via the interior fluid passage lost in the wall body of fluorescence floating cuvette, the top of chamber described in the outlet of described fluorescence floating cuvette；Outer wrap at described fluorescence floating cuvette has black polyethylene lucifuge shell.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 2, it is characterized in that, described chamber is cuboid or column type, and described smooth incidence window and light exit window are opened on adjacent two sides of the left-right and front-back surrounding of fluorescence floating cuvette.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 1, it is characterised in that described light source be emission center wavelength be the LED of 365nm exciting light light beam, its exiting surface just light incidence window to described fluorescence floating cuvette.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 4, it is characterised in that be additionally provided with the optical filter that centre wavelength is 365nm between the light incidence window of described LED and fluorescence floating cuvette.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 1, it is characterized in that, described optical receiver is photodiode, by the fluorescence of the light exit window injection of described fluorescence floating cuvette via the photodiode described in the bandpass filter directive of 400nm-480nm.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to claim 1, it is characterized in that, in described hybrid heating device, the shell of described heating rod is stainless steel casing, described fluid delivery tube is wound around 10-50 circle on the shell of described heating rod, is enclosed with heat insulation adhesive tape in the outside of described fluid delivery tube.
The device of on-line checking Ammonia In Sea Water nitrogen content the most according to any one of claim 1 to 7, it is characterized in that, also include a fluid manifold valve plate, it is carved with fluid passage in the inside of described fluid manifold valve plate, described first three-way magnetic valve, the second three-way magnetic valve, peristaltic pump, fluorescence floating cuvette, light source and optical receiver are arranged on described fluid manifold valve plate, described first three-way magnetic valve, are connected by described fluid passage between the second three-way magnetic valve and peristaltic pump.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105866088A (en) * | 2016-05-20 | 2016-08-17 | 山东省科学院海洋仪器仪表研究所 | Device and method for on-line detection of content of ammonia nitrogen in seawater |
| CN106770123A (en) * | 2017-01-04 | 2017-05-31 | 新疆维吾尔自治区产品质量监督检验研究院 | Flow injection fluorometry differentiates the devices and methods therefor of waste oil |
| CN107328749A (en) * | 2017-08-31 | 2017-11-07 | 河海大学 | A kind of water quality fluorescent solutions apparatus for measuring concentration and measuring method |
| CN109827919A (en) * | 2019-04-15 | 2019-05-31 | 嘉兴学院 | A kind of Quick testing instrument and its detection method of chroming waste liquor trivalent chromium content |
| CN110095418A (en) * | 2019-04-08 | 2019-08-06 | 北京时代新维测控设备有限公司 | A kind of photoelectric colorimetry measuring device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105866088A (en) * | 2016-05-20 | 2016-08-17 | 山东省科学院海洋仪器仪表研究所 | Device and method for on-line detection of content of ammonia nitrogen in seawater |
| CN105866088B (en) * | 2016-05-20 | 2019-01-11 | 山东省科学院海洋仪器仪表研究所 | A kind of device and method of on-line checking Ammonia In Sea Water nitrogen content |
| CN106770123A (en) * | 2017-01-04 | 2017-05-31 | 新疆维吾尔自治区产品质量监督检验研究院 | Flow injection fluorometry differentiates the devices and methods therefor of waste oil |
| CN106770123B (en) * | 2017-01-04 | 2021-06-18 | 新疆维吾尔自治区产品质量监督检验研究院 | Device and method for identifying illegal cooking oil by flow injection fluorescence method |
| CN107328749A (en) * | 2017-08-31 | 2017-11-07 | 河海大学 | A kind of water quality fluorescent solutions apparatus for measuring concentration and measuring method |
| CN110095418A (en) * | 2019-04-08 | 2019-08-06 | 北京时代新维测控设备有限公司 | A kind of photoelectric colorimetry measuring device |
| CN109827919A (en) * | 2019-04-15 | 2019-05-31 | 嘉兴学院 | A kind of Quick testing instrument and its detection method of chroming waste liquor trivalent chromium content |
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