CN101819212B - On-line automatic monitoring device for water quality mercury - Google Patents

On-line automatic monitoring device for water quality mercury Download PDF

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Publication number
CN101819212B
CN101819212B CN 201010150252 CN201010150252A CN101819212B CN 101819212 B CN101819212 B CN 101819212B CN 201010150252 CN201010150252 CN 201010150252 CN 201010150252 A CN201010150252 A CN 201010150252A CN 101819212 B CN101819212 B CN 101819212B
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pipeline
mercury
gasification
sampling
oxidation
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CN101819212A (en
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马三剑
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Suzhou Kete Environmental Protection Co., Ltd.
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马三剑
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Abstract

The invention discloses an on-line automatic monitoring device for water quality mercury, which is characterized by comprising a PLC control system (5), and a sampling system (1), an oxidation reduction system (2), a gasification system (3) and a measuring system (4) which are connected orderly by a pipeline. The PLC control system is internally equipped with preset programming procedures for controlling operation of the sampling system, the oxidation reduction system, the gasification system and the measuring system; and after sampling by the sampling system, the water sample to be tested forms metallic mercury through treatment by the oxidation reduction system, and then the metallic mercury enters the measuring system for measuring after being gasified by the gasification system. Compared with similar products, the on-line automatic monitoring device has the advantages of lower fault rate, less maintenance, lower reagent consumption, higher price-to-performance ratio and higher accuracy.

Description

On-line automatic monitoring device for water quality mercury
Technical field
The invention belongs to the water quality monitoring technical field, be specifically related to a kind of on-line automatic monitoring device for water quality mercury.
Background technology
Having many uses of mercury made the catholyte salt solution with mercury and produced chlorine and caustic soda in chemical industry; Make mercury vapor lamp, vacuum pump, physics instrument (such as barometer, thermometer, sphygmomanometer etc.) with mercury; Make various mercurous medicines, reagent, agricultural chemicals, explosive etc.; Extract the precious metals such as gold and silver with amalgam process; Handicraft or the temple gold-plated or gold-plating of gold amalgam.In total consumption, mercury metal account for 30%, the mercury of compound state accounts for 70%.Metallurgical industry is commonly used amalgam process (mercury can dissolve other metal and form amalgam) and is extracted the metals such as gold, silver and thallium.Chemical industry is made negative electrode with mercury and is produced caustic soda and chlorine with electrolytic salt solution.Mercury is made pool tube, mercury vacuum pump, novel and alcohol, concentrated nitric acid solution Hybrid Heating are made.Some compounds of mercury are pharmaceutically having sterilization, diuresis and analgesic activity, and the mercury silver alloy is good dental material.On traditional Chinese medicine, mercury is disliked the raw material of sore, mange medicine as treatment.Mercury can be used as mold and the cooling medium of atomic pile and the constituent element of cadmium base bearing alloy etc. of hot investment casting.
But mercury and mercuric compounds belongs to extremely toxic substance, can accumulate in human body.The main source of these mercury is instrucment and meter plant, salt electrolysis, precious metal smelting, cosmetics, illuminator lamp, dental material, fire coal, hydrobiont etc.After mercury metal in the blood enters brain tissue, accumulate in brain tissue gradually, will cause damage to brain tissue when reaching certain amount, a part of mercury ion is transferred to kidney in addition.The inorganic mercury ion that enters water body can change the larger organic mercury of toxicity into, enters human body by food chain, causes the whole body intoxication; Vulnerable crowd has the women, especially ready-to-be mother, hobby seafood personage; Mercurous few in the natural water, generally be no more than 0.1 μ g/L.Mercury is one of index of China's enforcement total emission volumn control.
The environmental protection industry standard HJ/T 241-2007 of the People's Republic of China (PRC) discloses " the mensuration Cold Atomic Fluorescent Mercury method (trying) of water quality mercury " tentative standard, and its principle is: the mercury ion in the water sample is reduced agent and is reduced to Elemental Mercury, forms mercury vapour.Its ground state mercury atom is subject to the ultraviolet excitation of wavelength 253.7nm, just gives off the fluorescence of identical wavelength when excited state mercury atom deexcitation.Under given condition and in the lower concentration range, fluorescence intensity is directly proportional with the concentration of mercury.Under laboratory condition, the mensuration of water quality mercury realizes by the digital phosphor mercury vapor analyzer, yet still do not carry out the equipment of water quality online auto monitoring water quality mercury in the prior art.The present invention comes therefrom.
Summary of the invention
The object of the invention is to provide a kind of on-line automatic monitoring device for water quality mercury, has solved that the equipment that lacks online auto monitoring water quality mercury in the prior art causes that monitoring water quality on line work is loaded down with trivial details, program repeat, measurement result have problems such as human factor is accurate not.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of on-line automatic monitoring device for water quality mercury is characterized in that described device comprises the PLC control system and is connected sampling system, oxidation-reduction system, gasification system and the mensuration system that pipeline connects; Default program in the described PLC control system, control sampling system, oxidation-reduction system, gasification system and mensuration system works, water sample to be measured is processed through oxidation-reduction system and is formed mercury metal after the described sampling system sampling, and described mercury metal enters the mensuration system measurement after the gasification system gasification.
Preferably, described mensuration system comprises measuring cell, and described measuring cell one end arranges drying device, the other end arranges the mercury vapour absorption plant, described gasification system is measured the mercury metal gasification by entering measuring cell after the drying device drying, then enter the mercury vapour absorption plant and absorb, and residual air is discharged.
Preferably, described oxidation-reduction system comprises reaction bulb, described reaction bulb arranged outside attemperator, and described reaction bulb lower end is connected with gasification system by pipeline.
Preferably, described device also comprises waste liquid bottle, and described waste liquid bottle is communicated with reaction bulb control by pipeline, and after the mensuration system measurement was complete, waste liquid was collected into the waste liquid bottle discharge by the road in the reaction bulb.
Preferably, open and close pipeline connection by the multi-way selecting valve selectivity between described reaction bulb and waste liquid bottle, after the mensuration system measurement was complete, multi-way selecting valve was opened the pipeline connection effluent discharge of reaction bulb and waste liquid bottle.
Preferably, be communicated with by the multi-way selecting valve pilot piping between described reaction bulb and gasification system.
Preferably, described gasification system comprises air pump, and described air pump is communicated with the oxidation-reduction system pilot piping by multi-way selecting valve.
Preferably, described sampling system comprises the peristaltic pump for sample introduction in oxidation-reduction system, is provided for carrying out the photoelectrometer buret of accurate-metering water sample or reagent on the pipeline of described peristaltic pump; Described peristaltic pump passes through pump water sampling or reagent, and water sample or reagent are sent in the oxidation-reduction system.
Preferably, be communicated with by the multi-way selecting valve pilot piping between described peristaltic pump and water sample to be measured or reagent; Described multi-way selecting valve selectivity opens and closes water sample pipeline to be measured, standard model pipeline, distilled water pipeline, oxygenant reagent pipeline, rare HNO 3Solution reagent pipeline, the first reductive agent reagent pipeline and the second reductive agent reagent pipeline.
Preferably, be communicated with air pump by three-way solenoid valve control on the connecting line of described peristaltic pump and multi-way selecting valve; When sampling system was worked, three-way solenoid valve was opened the pipeline connection of sampling system and oxidation-reduction system; When gasification system was worked, three-way solenoid valve was opened the pipeline connection of gasification system and oxidation-reduction system.
Preferably, described peristaltic pump comprises stepper motor driven roller, and described roller is arranged on the outside of pipeline, and described stepper motor is got reagent or sample according to the order-driven roller rotation negative pressure pump of PLC control system.Described photoelectrometer buret comprises the gauge line of determining volume, the two ends scale arranged outside photoelectric detector of described gauge line; Described photoelectric detector is according to the volume that has or not accurate-metering reagent or sample of reagent in the gauge line or sample.
The present invention adopts the principle in " the mensuration cold atomic absorbent spectrophotometry of GB7468-87 water quality total mercury ": under the condition of sulfonitric medium and heating, with potassium permanganate and potassium persulfate under little condition of boiling, with sample digestion, make the mercurous dimercurion that all is converted in the sample.With the oxygenant reduction of oxammonium hydrochloride with surplus, with stannous chloride divalence mercury is reduced into mercury metal again.At room temperature pass into air, the mercury metal steam is written into absorption tube, measure it in the absorption value at 253.7nm wavelength place, within the specific limits, absorption value is directly proportional with the mercury vapour amount, can try to achieve accordingly Hg content in the sample.
After the measurement cyclic process begins, wash each pipeline, gauge line and reaction bulb with new water sample first, to remove residual chaff interference.The sampling of PLC control system control sampling system uses peristaltic pump with water sample, oxygenant, rare HNO 3Solution, the first reductive agent, the second reductive agent successively are added in the reaction bulb by the order of programming in advance and react under insulation (temperature constant) and acid condition; Pass into air with mercury vapour by gasification system after reacting completely, be written into measuring cell after the mercury vapour drying device internal desiccant drying; Then utilize cold-vapour atomic absorption method to measure absorbance, calculate the concentration of mercury in the water sample according to absorbance.The mercury vapour absorption cell of measuring cell one end setting absorbs the mercury vapour by measuring cell, the control mercury pollution.
In whole measurement cyclic process, owing to adopt peristaltic pump to carry out the sample introduction sampling, water sample and reagent solution just enter reaction bulb by pipeline, and liquid does not directly contact with peristaltic pump, prevent from corrosion and the chaff interference of peristaltic pump are polluted; And at the pipeline of peristaltic pump the photoelectrometer buret is set, can prevent the error of the liquid volume added that causes owing to the peristaltic pump fluctuations in discharge.Certainly, in order to react quickening or to react more complete, in reaction bulb, pass through the bubbling mixing material, thereby guarantee that the solution in the reaction bulb mixes fully.
With respect to scheme of the prior art, advantage of the present invention is:
1. on-line automatic monitoring device for water quality mercury of the present invention adopts cold-vapour atomic absorption method as the measuring method of online automatic monitor.Its sampling system adopts peristaltic pump sampling, and the reagent sample introduction adopts peristaltic pump negative pressure suction, guarantee the contact of liquid discord pump line, stopped pump line to the pollution of liquid, avoided the pump line corrosion.The photoelectrometer buret is set on the sampling line, utilizes the photoelectric metering guard system to overcome the error that the peristaltic pump instability of flow causes; Realize simultaneously the accurate quantification of trace reagent, greatly reduced using amount of reagent.
2, adopt the whole device of PLC control system control in the technical solution of the present invention, the PLC control system is programmed in advance, measuring cyclic process can carry out repeatedly, makes this product have less trouble more, lower maintenance, lower reagent consumption and higher cost performance and accuracy than like product.Oxidation-reduction system adopts temperature controlled reaction bulb, reduces temperature to the impact of measurement result, adopts the temperature conditions of strict control, guarantees that reaction conditions meets the requirements, even is better than manually-operated.
3, adopt multi-way selecting valve in the preferred technical solution of the present invention, versatile and flexible with communicating passage such as each reagent bottle, sample, waste liquids, abandoned expensive diaphragm electromagnetic valve, greatly reduce maintenance and maintenance cost, also make apparatus structure of the present invention compact, be convenient to preparation and production.Multi-way selecting valve is communicated with by PLC control system pilot piping, few consumable accessory, and failure rate is low, operating cost is low.In addition, by the PLC control system can fault, when exceeding standard active retrograde to warning.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1 is the schematic diagram of embodiment of the invention on-line automatic monitoring device for water quality mercury;
Fig. 2 is the pipeline connecting figure of embodiment of the invention on-line automatic monitoring device for water quality mercury.
Wherein: 1 is sampling system; 2 is oxidation-reduction system; 3 is gasification system; 4 is the mensuration system; 5 is the PLC control system; 6 is waste liquid bottle; 7 is three-way solenoid valve;
11 is peristaltic pump; 12 is the photoelectrometer buret; 13 is multi-way selecting valve; 21 is reaction bulb; 22 is attemperator; 31 is air pump; 41 is measuring cell; 42 is drying device; 43 is the mercury vapour absorption plant; 100 is water sample pipeline to be measured; 101 is that standard model pipeline, 102 is that distilled water pipeline, 103 is that oxygenant reagent pipeline, 104 is rare HNO 3Solution reagent pipeline, 105 is that the first reductive agent reagent pipeline, 106 is the second reductive agent reagent pipeline.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for explanation the present invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The embodiment on-line automatic monitoring device for water quality mercury
As depicted in figs. 1 and 2, this on-line automatic monitoring device for water quality mercury comprises PLC control system 5 and is connected sampling system 1, oxidation-reduction system 2, gasification system 3 and the mensuration system 4 that pipeline connects; Default program in the described PLC control system, control sampling system, oxidation-reduction system, gasification system and mensuration system works, water sample to be measured is processed through oxidation-reduction system and is formed mercury metal after the described sampling system sampling, and described mercury metal enters the mensuration system measurement after the gasification system gasification.
Sampling system comprises the peristaltic pump 11 for sample introduction in oxidation-reduction system, is provided for carrying out the photoelectrometer buret 12 of accurate-metering water sample or reagent on the pipeline of described peristaltic pump; Described peristaltic pump passes through pump water sampling or reagent, and water sample or reagent are sent in the oxidation-reduction system.Be communicated with by multi-way selecting valve 13 pilot piping between described peristaltic pump and water sample to be measured or reagent; Described multi-way selecting valve 13 selectivity open and close water sample pipeline 100 to be measured, standard model pipeline 101, distilled water pipeline 102, oxygenant reagent pipeline 103, rare HNO 3Solution reagent pipeline 104, the first reductive agent reagent pipeline 105, the second reductive agent reagent pipeline 106 and waste liquid bottle 6 pipelines.Peristaltic pump comprises stepper motor driven roller, and described roller is arranged on the outside of pipeline, and described stepper motor is got reagent or sample according to the order-driven roller rotation negative pressure pump of PLC control system.Described photoelectrometer buret comprises the gauge line of determining volume, the two ends scale arranged outside photoelectric detector of described gauge line; Described photoelectric detector is according to the volume that has or not accurate-metering reagent or sample of reagent in the gauge line or sample.
Oxidation-reduction system comprises reaction bulb 21, described reaction bulb 21 arranged outside attemperators 22, and described reaction bulb lower end is connected with gasification system 3 by pipeline.Described waste liquid bottle 6 is communicated with reaction bulb 21 controls by pipeline, and after the mensuration system measurement was complete, waste liquid was collected into the waste liquid bottle discharge by the road in the reaction bulb.6 of described reaction bulb 21 and waste liquid bottles pass through multi-way selecting valve 13 selectivity and open and close pipeline connection, and after the mensuration system measurement was complete, multi-way selecting valve was opened the pipeline connection effluent discharge of reaction bulb and waste liquid bottle.
Gasification system 3 comprises air pump 31, and described air pump is communicated with the oxidation-reduction system pilot piping by multi-way selecting valve 13.3 of described reaction bulb and gasification systems are communicated with by multi-way selecting valve 13 pilot piping.Be communicated with air pump 31 by three-way solenoid valve 7 controls on the connecting line of described peristaltic pump 11 and multi-way selecting valve 13; When sampling system was worked, three-way solenoid valve 7 was opened the pipeline connection of sampling system and oxidation-reduction system; When gasification system 3 work, three-way solenoid valve 7 is opened the pipeline connection of gasification system and oxidation-reduction system.
Mensuration system 4 comprises measuring cell 41, described measuring cell one end arranges drying device 42, and the other end arranges mercury vapour absorption plant 43, and described gasification system is measured the mercury metal gasification by entering measuring cell after the drying device drying, then enter the mercury vapour absorption plant and absorb, residual air is discharged.The measuring cell arranged outside detects the photoelectric detector of final mercury vapour absorbance, and described photoelectric detector is connected with the PLC control system by photoelectric switching circuit.Described photoelectric detector comprises the emissive source that is arranged on the reaction unit outside and accepts the source, and described acceptance sends the PLC control system to by photoelectric switching circuit behind the depleted light signal that source acceptable response device opposite side emissive source sends.
Pipeline adopts the fluorine tubes of material of 1.5mm internal diameter in the device.After the measurement cyclic process begins, wash each pipeline, gauge line and reaction bulb with new water sample first, to remove residual chaff interference.The sampling of PLC control system control sampling system uses peristaltic pump with water sample, oxygenant, rare HNO 3Solution, the first reductive agent, the second reductive agent successively are added in the reaction bulb by the order of programming in advance and react under insulation (temperature constant) and acid condition; Pass into air with mercury vapour by gasification system after reacting completely, be written into measuring cell after the mercury vapour drying device internal desiccant drying; Then utilize cold-vapour atomic absorption method to measure absorbance, calculate the concentration of mercury in the water sample according to absorbance.The mercury vapour absorption cell of measuring cell one end setting absorbs the mercury vapour by measuring cell, prevents and remedies pollution.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalent transformations that Spirit Essence is done according to the present invention or modification all should be encompassed within protection scope of the present invention.

Claims (6)

1. on-line automatic monitoring device for water quality mercury is characterized in that described device comprises PLC control system (5) and is connected sampling system (1), oxidation-reduction system (2), gasification system (3) and the mensuration system (4) that pipeline connects; Default program in the described PLC control system, control sampling system, oxidation-reduction system, gasification system and mensuration system works, water sample to be measured is processed through oxidation-reduction system and is formed mercury metal after the described sampling system sampling, and described mercury metal enters the mensuration system measurement after the gasification system gasification; Described oxidation-reduction system (2) comprises reaction bulb (21), described reaction bulb (21) arranged outside attemperator (22), and described reaction bulb lower end is connected with gasification system (3) by pipeline; Described gasification system (3) comprises air pump (31), and described air pump is communicated with the oxidation-reduction system pilot piping by multi-way selecting valve (13); Described sampling system comprises the peristaltic pump (11) for sample introduction in oxidation-reduction system, is provided for carrying out the photoelectrometer buret (12) of accurate-metering water sample or reagent on the pipeline of described peristaltic pump; Described peristaltic pump passes through pump water sampling or reagent, and water sample or reagent are sent in the oxidation-reduction system; Described mensuration system (4) comprises measuring cell (41), described measuring cell one end arranges drying device (42), the other end arranges mercury vapour absorption plant (43), described gasification system is measured the mercury metal gasification by entering measuring cell after the drying device drying, then enter the mercury vapour absorption plant and absorb, residual air is discharged.
2. on-line automatic monitoring device for water quality mercury according to claim 1, it is characterized in that described device also comprises waste liquid bottle (6), described waste liquid bottle is communicated with reaction bulb (21) control by pipeline, after the mensuration system measurement was complete, waste liquid was collected into the waste liquid bottle discharge by the road in the reaction bulb.
3. on-line automatic monitoring device for water quality mercury according to claim 2, it is characterized in that opening and closing pipeline connection by described multi-way selecting valve (13) selectivity between described reaction bulb (21) and waste liquid bottle (6), after the mensuration system measurement was complete, described multi-way selecting valve was opened the pipeline connection effluent discharge of reaction bulb and waste liquid bottle.
4. on-line automatic monitoring device for water quality mercury according to claim 1 is characterized in that being communicated with by described multi-way selecting valve (13) pilot piping between described reaction bulb and gasification system (3).
5. on-line automatic monitoring device for water quality mercury according to claim 1 is characterized in that being communicated with by described multi-way selecting valve (13) pilot piping between described peristaltic pump and water sample to be measured or reagent; Described multi-way selecting valve (13) selectivity opens and closes water sample pipeline to be measured (100), standard model pipeline (101), distilled water pipeline (102), oxygenant reagent pipeline (103), rare HNO 3Solution pipeline (104), the first reductive agent reagent pipeline (105) and the second reductive agent reagent pipeline (106).
6. on-line automatic monitoring device for water quality mercury according to claim 1 is characterized in that being communicated with air pump (31) by three-way solenoid valve (7) control on the connecting line of described peristaltic pump (11) and described multi-way selecting valve (13); When sampling system was worked, three-way solenoid valve (7) was opened the pipeline connection of sampling system and oxidation-reduction system; When gasification system (3) was worked, three-way solenoid valve (7) was opened the pipeline connection of gasification system and oxidation-reduction system.
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