CN102495222B - Online stibium analyzer and method for detecting concentration of stibium of different forms in water sample - Google Patents
Online stibium analyzer and method for detecting concentration of stibium of different forms in water sample Download PDFInfo
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- CN102495222B CN102495222B CN 201110418617 CN201110418617A CN102495222B CN 102495222 B CN102495222 B CN 102495222B CN 201110418617 CN201110418617 CN 201110418617 CN 201110418617 A CN201110418617 A CN 201110418617A CN 102495222 B CN102495222 B CN 102495222B
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Abstract
The invention provides an online stibium analyzer and a method for detecting the concentration of stibium of different forms in water samples, wherein the analyzer comprises a control device, a quantitative sampling device, a reaction device, a detecting device, a water sample storage device and a reagent storage device. The control device is used for controlling the quantitative sampling device to obtain the water samples and reagents from the water sample storage device and the reagent storage device respectively, and filling the water samples and the reagents into the reaction device; the control device is also used for controlling the detecting device to detect the absorbance of complex generated in the reaction device, and feeding detecting results back to an analytical processing module; and the analytical processing module is used for analyzing the absorbance to obtain the concentration of the stibium of different forms in the water samples. The online stibium analyzer can be used for directly and automatically analyzing free stibium, total stibium, +3-valence stibium and +5-valence stibium in the water samples, so that the water samples can be monitored on line. In addition, owing to an extraction function, the online stibium analyzer is capable of detecting low-concentration stibium.
Description
Technical field
The present invention relates to the enviromental monitoring equipment field, especially, relate to the antimony in-line analyzer of the concentration of the free antimony in a kind of on-line monitoring water quality, total antimony, antimony (III) or antimony (V).In addition, the invention still further relates to a kind of method that detects the concentration of different shape antimony in the water sample.
Background technology
Antimony is the biosome non-essential element.The simple substance of antimony and compound are mostly poisonous, and wherein antimonious toxicity is than high ten times of quinquevalence antimonies.Antimony can stimulate people's eye, nose, throat and skin, and continuous contact can destroy heart and liver function, and the antimony that sucks high-load can cause antimony poisoning, and symptom comprises vomiting, headache, expiratory dyspnea, and severe patient may be dead.Some studies show that antimony has chronic toxicity and carcinogenicity to biological and human body, and the antimony pollution problem can not be ignored.EPA and European Union classify antimony as top-priority pollutant 1979 and 1976 respectively, and the pollutant of close attention is also classified it as in the Japanese environmental sanitation Room.Strict environmental standard has all been formulated to antimony in countries in the world.The every per day suction antimony of Germany's regulation human body is limited the quantity of and is 23ug.The maximum acceptable concentration (MPC) of antimony is 5 μ g/L in European Union's regulation potable water.Japan is defined as 2 μ g/L.EPA is with the MCLG(maximum contaminant level goal of antimony in the potable water) and MCL(maximum contaminant level) value all is decided to be 6 μ g/L.The World Health Organization (WHO) is based on the pathogenic antimony amount that contains of the 0.43mg/ that observes with it from home mouse (kgd), and the antimony content in the regulation potable water should be lower than 5 μ g/L.China has also made corresponding limit value regulation to the antimony in the environment.China's " water environment quality standard " (GB3838-2002) and in " Drinking Water hygienic practice " (Ministry of Public Health, calendar year 2001) all is decided to be 5 μ g/L with the limit value of antimony." water supply engineering planning standard " (GB50282-98) stipulated also to stipulate simultaneously antimony in the drinking water source＜50 μ g/L by antimony in water factory's water outlet＜10 μ g/L.
As known from the above, be very important to the mensuration of the content of antimony in the water.Yet prior art is difficult to realize the automatic on-line monitoring to various form antimony in the water.
Summary of the invention
The method that the object of the invention is to provide a kind of antimony in-line analyzer and detects the concentration of different shape antimony in the water sample can't be to the technical matters of the realization of the antimony in water sample on-line monitoring to solve existing antimony detection method.
For achieving the above object, according to an aspect of the present invention, provide a kind of antimony in-line analyzer, comprised that control device, quantitative sampling device, reaction unit, pick-up unit, water sample storing apparatus reach the reagent storing apparatus that is used for storing reagent; Control device also comprises analysis and processing module, and pick-up unit is electrically connected with analysis and processing module; Pick-up unit is installed on the reaction unit, and the entrance of reaction unit is connected with the outlet of quantitative sampling device; The water sample storing apparatus is connected with the entrance of quantitative sampling device with the reagent storing apparatus and is connected; Wherein, control device control quantitative sampling device is obtained water sample and reagent respectively from water sample storing apparatus and reagent storing apparatus, and water sample and reagent are injected reaction unit; Control device control pick-up unit detects the absorbance of the complex compound that generates in the reaction unit, and testing result is fed back to analysis and processing module; Analysis and processing module obtains the concentration of the different shape antimony in the water sample to absorbance analysis.
Further, control device also comprise be respectively applied to control detect in the water sample+the first control module of the concentration of valency antimony, be used for concentration the second control module that control detects the free antimony of water sample, be used for control and detect density control three control modules of water sample+valency antimony and be used for density control four control modules that control detects the total antimony of water sample; The first control module, the second control module, the 3rd control module and the 4th control module all are electrically connected with quantitative sampling device.
Further, reagent comprises multiple, quantitative sampling device is under the control of the first control module or the second control module or the 3rd control module or the 4th control module, selectivity extracts one or more reagent from plurality of reagents, wherein, plurality of reagents comprises acid solution, reductive agent and developer.
Further, reagent also comprises extractant, and quantitative sampling device extracts extractant under the control of the first control module or the second control module or the 3rd control module or the 4th control module.
Further, the antimony in-line analyzer comprises that also reaction unit comprises the cross pipeline in reaction tank and coupled reaction pond for the waste liquid storing apparatus of collecting waste liquid, and cross pipeline comprises first end, the second end, the 3rd end and the 4th end; First end is connected with the outlet of quantitative sampling device, and the second end is connected with reaction tank, and the 3rd end is connected with the waste liquid storing apparatus.
Further, quantitative sampling device comprises the propulsion system of hyperchannel selector valve, proportioning device and connection proportioning device; The hyperchannel selector valve is provided with an outlet and a plurality of entrance, and outlet and each porch are provided with valve, and proportioning device is connected with an entrance of hyperchannel selector valve; The reagent storing apparatus has a plurality of, and each reagent storing apparatus is connected with an entrance respectively, and reaction tank is connected with the outlet of hyperchannel selector valve; Propulsion system are peristaltic pump or ram pump.
Further, also be provided with temperature sensor and heating arrangement in the reaction tank, temperature sensor and heating arrangement all are electrically connected with control device.
Further, reaction unit also comprises cold hydrazine and stirring apparatus, and cold hydrazine is connected in reaction tank with connecting; Stirring apparatus is connected with the 4th end of cross pipeline.
Further, pick-up unit comprises light source and the photoelectric detection system that relatively is arranged at the reaction tank both sides, and light source and photoelectric detection system all are connected with control device.
According to another aspect of the present invention, a kind of method that detects the concentration of different shape antimony in the water sample is provided, use above-mentioned antimony in-line analyzer, the method in turn includes the following steps: the concentration of step 1, the form antimony that detects as required, the first control module of device for selection controlling or the second control module or the 3rd control module or the 4th control module; Step 2, quantitative sampling device are obtained water sample and corresponding reagent from water sample storing apparatus and reagent storing apparatus under the control of the selected control module of step 1, and water sample and reagent injection reaction unit are reacted, and generate complex compound after the reaction; Step 3, the selected control module control of step 1 pick-up unit detect the absorbance of the complex compound in the reaction unit, and testing result are fed back to the analysis and processing module of antimony in-line analyzer; Step 4, analysis and processing module go out the concentration of form antimony in water sample that needs detect according to Analysis of test results.
Further, in step 1, select be the first control module the time, the detailed process of step 2 is as follows: the first control module control quantitative sampling device is obtained water sample and is obtained respectively the reaction tank that acid solution and developer inject reaction unit successively and react from the acid solution storage container of reagent storing apparatus and developer storage container from the water sample storing apparatus, generate complex compound after the reaction.
Further, in step 1, select be the second control module the time, the detailed process of step 2 is as follows: the second control module control quantitative sampling device is obtained water sample and is obtained respectively the reaction tank that acid solution, reductive agent and developer inject reaction unit successively and react from acid solution storage container, reductive agent storage container and the developer storage container of reagent storing apparatus from the water sample storing apparatus, generate complex compound after the reaction.
Further, in step 1, select be the 3rd control module the time, step 2 comprises the first step and the second step that separately carries out: the first step: the first control module control quantitative sampling device is obtained water sample and is obtained respectively the reaction tank that acid solution and developer inject reaction unit successively and react from the acid solution storage container of reagent storing apparatus and developer storage container from the water sample storing apparatus; Second step: the second control module control quantitative sampling device is obtained water sample and is obtained respectively the reaction tank that acid solution, reductive agent and developer inject reaction unit successively and react from acid solution storage container, reductive agent storage container and the developer storage container of reagent storing apparatus from the water sample storing apparatus; Between the first step and second step, obtain in the water sample+concentration of valency antimony by step 3 and step 4 successively; After second step, again obtain successively the concentration of free antimony in the water sample by step 3 and step 4; Analysis and processing module according to the concentration of free antimony deduct+concentration of valency antimony obtains+concentration of valency antimony.
Further, in step 1, select be the 4th control module the time; The detailed process of step 2 is as follows successively: the 4th control module control quantitative sampling device is obtained respectively water sample and acid solution and injected the reaction tank of reaction unit from the acid solution storage container of water sample storing apparatus and reagent storing apparatus after, control device control reaction unit is cleared up water sample; The 4th control module control quantitative sampling device reacts from the reaction tank that the reductive agent storage container of reagent storing apparatus and developer storage container are obtained reductive agent and developer and injected reaction unit respectively, generates complex compound after the reaction.
Further, in the process of step 2, quantitative sampling device is also obtained extractant in the extractant storage container from the reagent storing apparatus, and extractant is injected in the reaction unit, and extractant extracts complex compound.
The present invention has following beneficial effect:
Antimony in-line analyzer of the present invention directly the free antimony in the automatic analysis water sample, total antimony ,+antimony of 3 valencys and the antimony of+5 valencys, thereby can reach the on-line monitoring of water sample.In addition, antimony in-line analyzer of the present invention owing to possess the extraction function, can be realized the detection of low concentration antimony.
Except purpose described above, feature and advantage, the present invention also has other purpose, feature and advantage.The below is with reference to figure, and the present invention is further detailed explanation.
Description of drawings
The accompanying drawing that consists of the application's a part is used to provide a further understanding of the present invention, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not consist of improper restriction of the present invention.In the accompanying drawings:
Fig. 1 is the structural representation of the antimony in-line analyzer of the preferred embodiment of the present invention; And
Fig. 2 is the structural representation of the preferred embodiment of quantitative sampling device among Fig. 1, water sample memory storage, reagent storing apparatus, reaction unit, pick-up unit and waste liquid storing apparatus.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated, but the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
Referring to Fig. 1, antimony in-line analyzer of the present invention can realize in the water sample+3 valency antimony, free antimony ,+detection of the concentration of 5 valency antimony and total antimony, it comprises control device 1, quantitative sampling device 2, reaction unit 3, pick-up unit 4, water sample storing apparatus 5 and reagent storing apparatus 6.Wherein, control device 1 control quantitative sampling device 2 is obtained respectively water sample to be measured and reagent and water sample and reagent injection reaction unit 3 in turn from water sample storing apparatus 5 and reagent storing apparatus 6 after, so that the antimony in the water sample and reagent are at these reaction unit 3 internal reactions, at this moment, control device 1 can be controlled the reaction conditions of reaction unit 3 as required.When water sample and reagent react generate complex compound after, after control device 1 control pick-up unit 4 was realized detections to the absorbance of complex compound, control pick-up unit 4 also sent to analysis and processing module 19 in the control device 1 with testing result.The analysis and processing module 19 of control device 1 can analyze the concentration of different shape antimony in the water sample according to testing result.
Control device 1 comprises alternative the first control module 11, the second control module 13, the 3rd control module 15 and the 4th control module 17.The concentration of wherein, the first control module 11 is used for controlling antimony in-line analyzer of the present invention right+3 valency antimony detects; The second control module 13 detects for controlling the concentration of antimony in-line analyzer of the present invention to free antimony; The concentration of the 3rd control module 15 is used for controlling antimony in-line analyzer of the present invention right+5 valency antimony detects; The 4th control module 17 detects for controlling the concentration of antimony in-line analyzer of the present invention to total antimony.
Please in conjunction with referring to Fig. 2, in the present embodiment, quantitative sampling device 2 comprises hyperchannel selector valve 21, proportioning device 22, sampling propulsion system 23.Wherein, the hyperchannel selector valve 21 preferred selector valves that adopt eight passages or ten passages, it comprises that arranging valvular one exports and a plurality of entrance.Valve is preferably solenoid valve.Preferably, the entrance of this hyperchannel selector valve 21 comprises the first entrance, the second entrance, the 3rd entrance, the 4th entrance, the 5th entrance, the 6th entrance, and outlet and the switching of each entrance are achieved by the control of 1 pair of valve of control device.Sampling propulsion system 23 connect proportioning device 22, for proportioning device 22 samplings provide power.Proportioning device 22 is connected with hyperchannel selector valve 21 through the first entrance of hyperchannel selector valve 21.Proportioning device 22 preferred peristaltic pump and/or the ram pumps of adopting.Reaction unit 3 is connected in the outlet of this hyperchannel selector valve 21.
Reagent storing apparatus 6 comprises acid solution storage container 61, developer storage container 63, reductive agent storage container 65 and extractant storage container 67.Wherein, acid solution storage container 61, developer storage container 63, reductive agent storage container 65 and extractant storage container 67 store respectively acid solution, developer, reductive agent and extractant.Preferably, acid solution can be sulfuric acid solution or salpeter solution, and its concentration can be 50%～100%.Reductive agent is preferably one or more the combination in thiocarbamide, potassium iodide, oxammonium hydrochloride, stannous chloride, anti-ization hematic acid, the tartrate, and its concentration can be 1～20%.Developer is preferably the 2-(5-Bromo-2-pyridylazo)-potpourri of 5-diethylamino phenol (be called for short 5-Br-PADAP) and alcohol, wherein, the massfraction of 5-Br-PADAP is preferably 0.01～2%, and the concentration of alcohol is preferably 40～100%.Extractant can be one or more the combination in toluene, benzene, the methenyl choloride.
Water sample storing apparatus 5, acid solution storage container 61, developer storage container 63, reductive agent storage container 65 and extractant storage container 67 connect respectively the second entrance, the 3rd entrance, the 4th entrance, the 5th entrance and the 6th entrance of above-mentioned hyperchannel selector valve 21.Like this, under the control of control device 1, the corresponding entrance of this hyperchannel selector valve 21 can be opened, again under the driving of sampling propulsion system 23, proportioning device 22 can extract quantitative water sample and corresponding reagent from water sample memory storage 5 and reagent storing apparatus 6, and again under the control of control device 1, the water sample that this is quantitative and corresponding reagent inject reaction unit 3 by the outlet of this hyperchannel selector valve 21 and react.
Reaction unit 3 comprises the reaction tank 31 that is connected with the outlet of above-mentioned hyperchannel selector valve 21, and the reaction tank 31 preferred glass materials that adopt certainly, adopt other transparent material also to be fine.Preferably, reaction tank 31 is connected with the outlet of hyperchannel selector valve 21 through a cross pipeline 35.Preferably, cross pipeline 35 comprises first end, the second end, the 3rd end and the 4th end.The first end of cross pipeline 35 is connected with the outlet of hyperchannel selector valve 21, and the second end of hyperchannel selector valve 21 is connected with reaction tank 31.Reaction tank 31 is used for holding water sample and corresponding reagent, and so that water sample and corresponding reagent react accordingly within it.Preferably, in order to improve the reaction rate of reaction tank 31 internal reaction things, be connected with a stirring apparatus 34 at the 3rd end of cross pipeline 35; The combination of any one or more in stirring apparatus 34 preferred employing magnetic agitation, air pump stirring, the mechanical raking, stirring apparatus 34 can intelligence be regulated the intensity that stirs.Preferably, the present invention also is provided with a waste liquid storing apparatus 7 that is communicated with reaction tank 31, with the water sample in the recovery reaction unit 3 and the waste liquid behind the reagent reacting.Waste liquid storing apparatus 7 is connected to the 4th end of cross pipeline 35.More preferably, for the ease of control, be provided with operation valve at the position that connects between waste liquid storing apparatus 7 and the reaction tank 31.Preferably, reaction unit 3 also comprises temperature sensor 32 and the heating arrangement 33 that is arranged in the reaction tank 31.Temperature sensor 32 and heating arrangement 33 all are connected with control device 1, so that accept the control of control device 1.Wherein, the real time temperature of temperature sensor 32 in the control device 1 feedback response pond 31, control device 1 can be controlled by reaction conditions the heating-up temperature of heating arrangement 33.The top of reaction tank 31 is connected with a cold hydrazine 37 with also connecting, so that the reactant condensation of gasification.
Pick-up unit 4 comprises light source 41 and photoelectric detection system 43.Preferably, light source 41 and photoelectric detection system 43 are arranged at the both sides of reaction tank 31 accordingly.Wherein, complex compound in the control device 1 control light source 41 luminous irradiation reaction tanks 31, photoelectric detection system 43 can detect the absorbance of complex compound like this, and the analysis and processing module 19 that testing result sends to control device 1 analyzed, to draw the concentration of different shape antimony in the water sample.Preferably, light source 41 can adopt any in light emitting diode, Halogen lamp LED, the xenon lamp; The light that light source 41 sends can be monochromatic light, also can be the composite light source with beam splitting system.Photoelectric detection system 43 is preferred to adopt any in photodiodes, phototriode, photoresistance, ccd array detecting device and the photomultiplier.
The below elaborates and how to utilize antimony in-line analyzer of the present invention to monitor the concentration of different shape antimony in the water sample to be measured:
The first situation: when needs detect in the water sample+during 3 valency antimony, at first, the first control module 11 of device for selection controlling 1, so that the first control module 11 control quantitative sampling devices 2 are obtained respectively water sample to be measured, acid solution and developer in turn from water sample storing apparatus 5, acid solution storage container 61, developer storage container 63, and successively water sample, acid solution and developer are injected the reaction tank 31 of reaction unit 3.In the water sample+colour developing occurs with developer and occurs in 3 valency antimony in acid solution, generate stable complex compound.Complex compound is slightly soluble in acid solution, forms therein floccus.In order to improve the absorbance of complex compound, preferably, the first control module 11 is also controlled quantitative sampling device 2 and take out extractant from extractant storage container 67, and is injected in the reaction tank 31.Like this, extractant can extract the complex compound in the acid solution, to improve the absorbance of complex compound.
Then, after reaction tank 31 internal reactions are finished, complex compound in the light source 41 luminous irradiation reaction tanks 31 of the first control module 11 control pick-up units 4 of control device 1, and the absorbance of 43 pairs of complex compounds of control photoelectric detection system detects, thereby the testing result of obtaining, and testing result is sent to the analysis and processing module 19 of control device 1.
At last, can analyze in the water sample to be measured+concentration of 3 valency antimony according to the testing result of photoelectric detection system 43 by analysis and processing module 19.
The second situation: when needs detect the concentration of the free antimony in the water sample, at first, the second control module 13 of device for selection controlling 1, so that the second control module 13 control quantitative sampling devices 2 are obtained respectively water sample to be measured, acid solution, reductive agent and developer in turn from water sample storing apparatus 5, acid solution storage container 61, reductive agent storage container 65, developer storage container 63, and successively water sample, acid solution, reductive agent and developer are injected the reaction tank 31 of reaction unit 3.At this moment, in the water sample+5 valency antimony are reduced under the effect of reductive agent+3 valency antimony, and colour developing occurs with developer and occurs in all in the water sample+3 valency antimony in acid solution, generate stable complex compound.Same, in order to improve the second absorbance of complex compound, quantitative sampling device 2 also takes out extractant from extractant storage container 67, and is injected in the reaction tank 31.
Then, after reaction tank 31 internal reactions are finished, complex compound in the light source 41 luminous irradiation reaction tanks 31 of the second control module 13 control pick-up units 4 of control device 1, and the absorbance of 43 pairs of complex compounds of control photoelectric detection system detects, thereby the testing result of obtaining, and testing result is sent to the analysis and processing module 19 of control device 1.
At last, go out the concentration of free antimony in the water sample to be measured according to Analysis of test results by analysis and processing module 19.
The third situation: when needs detect in the water sample+during the concentration of 5 valency antimony because+content that the content of 5 valency antimony equals free antimony deducts+content of 3 valency antimony, so, the concentration of free antimony in the water sample is deducted in the water sample+concentration of 3 valency antimony can obtain+5 concentration.Be specially: at first, the first step: the method for describing according to above-mentioned the first situation measures in the water sample+concentration of 3 valency antimony; Secondly, second step: the method for describing according to situation in above-mentioned second measure with the first step in the concentration of free antimony in the identical water sample; At last, the 3rd step: the concentration of the free antimony that second step is obtained deducts that the first step obtains+concentration of 3 valency antimony can draw in the water sample+concentration of 5 valency antimony.
The 4th kind of situation: when needs detected the concentration of the total antimony in the water sample, concrete steps were as follows:
At first, water sample is cleared up.
Because include insoluble solid-state antimony in the water sample, therefore, need first the solid-state antimony in the water sample to be cleared up.Be specially: the 4th control module 17 of device for selection controlling 1, so that the 4th control module 17 control quantitative sampling devices 2 are obtained respectively water sample to be measured and acid solution and water sample and acid solution are injected the reaction tank 31 of reaction unit 3 from water sample storing apparatus 5, acid solution storage container 61 in turn.In reaction tank 31, the solid-state antimony in the water sample is cleared up.Preferably, digestion process is: the 33 pairs of water samples of heating arrangement in the 4th control module 17 control reaction tanks 31 and the potpourri of acid solution heat, and the temperature of heating is preferably 80 ℃-100 ℃.In the process of heating, in order to realize the real-time control to temperature, temperature sensor 32 in the reaction tank 31 to the real time temperature of the 4th control module 17 feedback heating, maintains between 80 ℃-100 ℃ so that the 4th control module 17 can be controlled the heating-up temperature of heating arrangement 33 in real time.
When adopting above-mentioned type of heating that the solid-state antimony in the water sample is cleared up, the cold hydrazine 37 that the top of reaction tank 31 connects can carry out condensation to the reactant of vaporization, and it is back in the reaction tank 31.In other embodiment of the present invention, the solid-state antimony in the water sample can not cleared up in reaction tank 31 yet, and the digestion pool of a special use can be set, and first water sample is cleared up in digestion pool, and the water sample after will clearing up again is injected in the reaction tank 31.
Then, the water sample after clearing up is carried out the detection of total antimony concentration.Detailed process is: after water sample has been cleared up, the 4th control module 17 control quantitative sampling devices 2 are obtained reductive agent and developer from reductive agent storage container 65 and developer storage container 63, and control quantitative sampling device 2 injects reductive agent and the developer of obtaining in the reaction tank 31.Colour developing occurs with developer and occurs in water sample in acid solution, generate stable complex compound.Same, in order to improve the 4th absorbance of the 4th complex compound, quantitative sampling device 2 also takes out extractant from extractant storage container 67, and is injected in the reaction tank 31.
After reaction tank 31 internal reactions are finished, complex compound in the light source 41 luminous irradiation reaction tanks 31 of the 4th control module 17 control pick-up units 4 of control device 1, and the absorbance of 43 pairs of complex compounds of control photoelectric detection system detects, thereby the testing result of obtaining, and testing result is sent to the analysis and processing module 19 of control device 1.At last, go out the content of total antimony in the water sample to be measured according to Analysis of test results by analysis and processing module 19.
In summary, antimony in-line analyzer of the present invention directly the free antimony in the automatic analysis water sample, total antimony ,+antimony of 3 valencys and the antimony of+5 valencys, thereby can reach on-line monitoring to the various form antimony of water sample.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (14)
1. an antimony in-line analyzer is characterized in that, comprises that control device (1), quantitative sampling device (2), reaction unit (3), pick-up unit (4), water sample storing apparatus (5) reach the reagent storing apparatus (6) that is used for storing reagent;
Described control device (1) also comprises analysis and processing module (19), and described pick-up unit (4) is electrically connected with described analysis and processing module (19);
Described pick-up unit (4) is installed on the described reaction unit (3), and the entrance of described reaction unit (3) is connected with the outlet of described quantitative sampling device (2);
Described water sample storing apparatus (5) is connected 6 with the reagent storing apparatus) respectively the entrance with described quantitative sampling device (2) be connected;
Wherein, described control device (1) is controlled described quantitative sampling device (2) and is obtained water sample and reagent respectively from described water sample storing apparatus (5) and described reagent storing apparatus (6), and described water sample and described reagent are injected described reaction unit (3);
Described control device (1) is controlled described pick-up unit (4) absorbance of the complex compound that generates in the described reaction unit (3) is detected, and testing result is fed back to described analysis and processing module (19);
Described analysis and processing module (19) obtains the concentration of the different shape antimony in the described water sample to described absorbance analysis;
Described control device (1) also comprise be respectively applied to control detect in the described water sample+first control module (11) of the concentration of 3 valency antimony, be used for concentration the second control module (13) that control detects the free antimony of described water sample, be used for control and detect density control three control modules (15) of described water sample+5 valency antimony and be used for density control four control modules (17) that control detects the total antimony of described water sample; Described the first control module (11), described the second control module (13), described the 3rd control module (15) and described the 4th control module (17) all are electrically connected with described quantitative sampling device (2).
2. antimony in-line analyzer according to claim 1, it is characterized in that, described reagent comprises multiple, described quantitative sampling device (2) is under the control of described the first control module (11) or described the second control module (13) or described the 3rd control module (15) or described the 4th control module (17), selectivity extracts one or more reagent from described plurality of reagents, wherein, described plurality of reagents comprises acid solution, reductive agent and developer.
3. antimony in-line analyzer according to claim 2, it is characterized in that, described reagent also comprises extractant, and described quantitative sampling device (2) extracts described extractant under the control of described the first control module (11) or described the second control module (13) or described the 3rd control module (15) or described the 4th control module (17).
4. antimony in-line analyzer according to claim 2, it is characterized in that, described antimony in-line analyzer also comprises for the waste liquid storing apparatus (7) of collecting waste liquid, described reaction unit (3) comprises reaction tank (31) and connects the cross pipeline (35) of described reaction tank (31) that described cross pipeline (35) comprises first end, the second end, the 3rd end and the 4th end; Described first end is connected with the outlet of described quantitative sampling device (2), and described the second end is connected with described reaction tank (31), and described the 3rd end is connected with described waste liquid storing apparatus (7).
5. antimony in-line analyzer according to claim 4 is characterized in that, described quantitative sampling device (2) comprises hyperchannel selector valve (21), proportioning device (22) and connects the propulsion system (23) of described proportioning device (22); Described hyperchannel selector valve (21) is provided with an outlet and a plurality of entrance, and described outlet and each described porch are provided with valve, and described proportioning device (22) is connected with a described entrance of described hyperchannel selector valve (21); Described reagent storing apparatus (6) has a plurality of, and each described reagent storing apparatus (6) is connected with a described entrance respectively, and described reaction tank (31) is connected with the outlet of described hyperchannel selector valve (21); Described propulsion system (23) are peristaltic pump or ram pump.
6. antimony in-line analyzer according to claim 4, it is characterized in that, also be provided with temperature sensor (32) and heating arrangement (33) in the described reaction tank (31), described temperature sensor (32) and described heating arrangement (33) all are electrically connected with described control device (1).
7. antimony in-line analyzer according to claim 4 is characterized in that, described reaction unit (3) also comprises cold hydrazine (37) and stirring apparatus (34), and described cold hydrazine (37) is connected in described reaction tank (31) with connecting; Described stirring apparatus (34) is connected with the 4th end of described cross pipeline (35).
8. antimony in-line analyzer according to claim 4, it is characterized in that, described pick-up unit (4) comprises light source (41) and the photoelectric detection system (43) that relatively is arranged at described reaction tank (31) both sides, and described light source (41) and described photoelectric detection system (43) all are connected with described control device (1).
9. method that detects the concentration of different shape antimony in the water sample, right to use requires each described antimony in-line analyzer in 1 to 8, it is characterized in that described method in turn includes the following steps:
The concentration of step 1, the form antimony that detects is as required selected the first control module (11) or the second control module (13) or the 3rd control module (15) or the 4th control module (17) of described control device (1);
Step 2, described quantitative sampling device (2) are obtained water sample and corresponding reagent from described water sample storing apparatus (5) and described reagent storing apparatus (6) under the control of the selected control module of described step 1, and described water sample and described reagent injected described reaction unit (3) reaction, generate complex compound after the reaction;
Step 3, the selected control module of described step 1 are controlled described pick-up unit (4) absorbance of the complex compound in the described reaction unit (3) are detected, and testing result are fed back to the analysis and processing module (19) of described antimony in-line analyzer;
Step 4, described analysis and processing module (19) go out the concentration of form antimony in described water sample that described needs detect according to described Analysis of test results.
10. the method for the concentration of different shape antimony in the detection water sample according to claim 9, it is characterized in that, in described step 1, select be described the first control module (11) time, the detailed process of described step 2 is as follows: described the first control module (11) is controlled described quantitative sampling device (2) and is obtained water sample and obtain respectively reaction tank (31) reaction that acid solution and developer inject described reaction unit (3) successively from described water sample storing apparatus (5) from the acid solution storage container (61) of described reagent storing apparatus (6) and developer storage container (63), generates described complex compound after the reaction.
11. the method for the concentration of different shape antimony in the detection water sample according to claim 9, it is characterized in that, in described step 1, select be described the second control module (13) time, the detailed process of described step 2 is as follows: described the second control module (13) controls that described quantitative sampling device (2) is obtained water sample from described water sample storing apparatus (5) and respectively from the acid solution storage container (61) of described reagent storing apparatus (6), obtain acid solution in reductive agent storage container (65) and the developer storage container (63), reductive agent and developer inject reaction tank (31) reaction of described reaction unit (3) successively, generate described complex compound after the reaction.
12. the method for the concentration of different shape antimony in the detection water sample according to claim 9, it is characterized in that, in described step 1, select be described the 3rd control module (15) time, described step 2 comprises the first step and the second step that separately carries out: the first step: described the first control module (11) is controlled described quantitative sampling device (2) and is obtained water sample and obtain respectively reaction tank (31) reaction that acid solution and developer inject described reaction unit (3) successively from described water sample storing apparatus (5) from the acid solution storage container (61) of described reagent storing apparatus (6) and developer storage container (63);
Second step: described the second control module (13) is controlled described quantitative sampling device (2) and is obtained water sample and obtain respectively reaction tank (31) reaction that acid solution, reductive agent and developer inject described reaction unit (3) successively from described water sample storing apparatus (5) from acid solution storage container (61), reductive agent storage container (65) and the developer storage container (63) of described reagent storing apparatus (6);
Between the described first step and described second step, obtain in the described water sample+concentration of 3 valency antimony by described step 3 and described step 4 successively;
After described second step, again obtain successively the concentration of free antimony in the described water sample by described step 3 and described step 4;
The concentration that described analysis and processing module (19) deducts described+3 valency antimony according to the concentration of described free antimony obtains the concentration of described+5 valency antimony.
13. the method for the concentration of different shape antimony is characterized in that in the detection water sample according to claim 9, in described step 1, select be described the 4th control module (17) time; The detailed process of described step 2 is as follows successively:
After described the 4th control module (17) was controlled described quantitative sampling device (2) and obtained respectively described water sample and acid solution and inject the reaction tank (31) of described reaction unit (3) from the acid solution storage container (61) of described water sample storing apparatus (5) and described reagent storing apparatus (6), described control device (1) was controlled described reaction unit (3) described water sample is cleared up;
Described the 4th control module (17) is controlled reaction tank (31) reaction that described quantitative sampling device (2) is obtained reductive agent and developer and injected described reaction unit (3) from reductive agent storage container (65) and the developer storage container (63) of described reagent storing apparatus (6) respectively, generates complex compound after the reaction.
14. the method for the concentration of different shape antimony to 13 described each described detection water samples according to claim 9, in the process of described step 2, described quantitative sampling device (2) is also obtained extractant in the extractant storage container (67) from described reagent storing apparatus (6), and described extractant injected in the described reaction unit (3), described extractant extracts described complex compound.
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| CN102721588A (en) * | 2012-06-28 | 2012-10-10 | 贵州师范大学 | Rapid in-situ measurement method for content of antimony in acid mine waste water |
| CN102778576A (en) * | 2012-08-16 | 2012-11-14 | 力合科技（湖南）股份有限公司 | Water-quality organic-matter monitoring car, system and method |
| CN102980862B (en) * | 2012-12-03 | 2015-10-21 | 力合科技（湖南）股份有限公司 | A kind of auto extractive separation detecting device and a kind of auto extractive method for separating and detecting |
| CN108445243A (en) * | 2017-03-05 | 2018-08-24 | 泉州泉港璟冠信息科技有限公司 | A kind of water quality automatic detection analysis instrument |
| CN108051429B (en) * | 2017-11-15 | 2020-06-02 | 芜湖乐佳自动化机械有限公司 | Water quality online detector with multiple detection functions and use method thereof |
| CN112903612A (en) * | 2021-01-26 | 2021-06-04 | 杭州绿洁环境科技股份有限公司 | Online analyzer for anionic surfactant |
| CN116338221B (en) * | 2023-05-24 | 2023-08-11 | 河北华清环境科技集团股份有限公司 | Quality control equipment for online automatic monitoring of water quality |
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| CN201344921Y (en) * | 2009-02-03 | 2009-11-11 | 北京吉天仪器有限公司 | Interface device for high performance liquid chromatogram-atomic fluorescence to detect antimony valence state |
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