CN105388309A - Automatic and rapid detection method and system for trace iron ions in power plant water vapor and application - Google Patents
Automatic and rapid detection method and system for trace iron ions in power plant water vapor and application Download PDFInfo
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- CN105388309A CN105388309A CN201510764964.8A CN201510764964A CN105388309A CN 105388309 A CN105388309 A CN 105388309A CN 201510764964 A CN201510764964 A CN 201510764964A CN 105388309 A CN105388309 A CN 105388309A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention provides an automatic and rapid detection method and system for trace iron ions in power plant water vapor and application. The system comprises a reducing reagent bottle (1), a color reagent bottle (2), a buffer liquid bottle (3), a current-carrying bottle (4), a water sample bottle (5), a flow injection analyzer (9), a combination module (10), a Y-type tee joint (11), a color reaction disk tube (13), a reducing reaction disk tube (14) and a detection device (15), wherein the flow injection analyzer (9) comprises a main pump (6), an auxiliary pump (7), an eight-channel sampling valve (8) and a sampling ring (12). The invention further provides an automatic and rapid detection method for trace iron ions in power plant water vapor and application of the method in detection of trace iron ions in power plant water vapor. The method and the system provided by the invention can realize automatic, rapid, accurate and reliable determination of trace iron ions in power plant water vapor, and the detection limit is 0.5mu g/L.
Description
Technical field
The present invention relates to the detection of Power Plant Water Vapor, specifically, relate to the automatic method for quick of trace iron ions and system and application in a kind of Power Plant Water Vapor.
Background technology
The iron content of Power Plant Water Vapor system is a very important monitor control index, and it is the important evidence evaluating operating unit therrmodynamic system corrosion and scaling situation, is one of power plant's daily production regular monitoring index.
At present, the method measuring full iron in electrical production feedwater, stove water is Phen spectrophotometric method (GB/T14427-2008) and graphite oven atomic absorption (DL/T955-2005).Phen spectrophotometric method is traditional-handwork analytical approach, the method trivial operations, and analysis efficiency is low, can produce acid mist in water sample digestion process, works the mischief to working environment and health.And the instrument that graphite oven atomic absorption uses involves great expense, Operation and Maintenance requires high.
The method of the mensuration iron content commonly used several this area will be introduced in detail below.
1, boiler feed water and chilled water analytical approach (GB/T14427-2008)
This analytical approach adopts the content of spectrophotometric determination o-phenanthroline iron.Fe (II) ferrosin complex compound is 2.5-9.0 at pH is stable, and the intensity of its color is directly proportional to Fe (II) amount.When concentration of iron is below 5.0mg/L, concentration and absorbance linear.Maximum light absorption value is at 510nm wavelength place.But the method is artificial detection method, and sample can repeatedly shift in process container, thus accuracy and the reliability of test result can be affected, and the water sample amount of the method consumption and amount of reagent are all comparatively large, cause the waste of water sample and reagent.
2, the copper iron (DL/T955-2005) in graphite furnace atomic absorption spectrometry fuel-burning power plant water, vapour
Graphite oven atomic absorption, its detection line is 0-100 μ g/L, the Determination Limit of the method is lower than modern unit steam full iron newest standards value, this meets existing technical requirement, but because the instrument of graphite oven atomic absorption involves great expense, the import instrument unit price of dependable performance reaches about 600,000 yuan, and Operation and Maintenance requires high, higher to personnel qualifications, power plant's application is less.
3, full iron in FIA-TPTZ water by Spectrophotometry
The method is based on Fe (II) and 2,4,6-tri-(2-pyridine radicals)-1,3, the analytical approach that the complex reaction of 5-triazine (TPTZ) and Flow Injection Technique are set up, detecting of the method is limited to 22.7 μ g/L, and its Determination Limit can not meet modern unit steam full iron newest standards value (5 μ g/L), therefore, the method is not suitable for the monitoring of Trace Iron in Power Plant Water Vapor.
More based on to combine with the spectrophotomelric assay technology detection method researched and developed of Flow Injection Technique, such as adopt the total iron content in Flow Injection Spectrophotometry on-line analysis water, it detects and is limited to 40 μ g/L, and its Determination Limit can not meet modern unit steam full iron newest standards value (5 μ g/L); Adopt Flow Injection Spectrophotometry Simultaneously test Fe (II) and Fe (III), its detection limit is respectively 0.0012 μ g/L and 0.0018 μ g/L, what the method adopted is the valve body stream that single valve biobelt cadmium plating zinc metal sheet reduction cornice is isolated, flow path system is complicated, is also unsuitable for the use of power plant.
4, iron in catalytic Spectrophotometric Determination carbonated drink
This type of detection method needs the catalytic oxidation system that selection range of linearity is suitable, simultaneously, because Catalytic-Kinetic Spectrophotometric needs the Non-follow control time to complete heating, cooling process, therefore the poor anti jamming capability of the method, temperature and time is comparatively large on measurement result impact, realizes on-line monitoring requirement higher.
5, chemiluminescence determination trace and ultratrace iron
With regard to current research level, the technical stability of the method is poor, determination data stability is not high, if large-area applications the method, must have that automaticity is higher, sensitivity, the better instrument of stability, therefore the technology path of the method is immature, can not apply as national standard method.
6, Fluorimetric Determination of Trace iron
Because iron has paramagnetism, therefore this area seldom adopts the method to measure iron content in water, normally acts in a diametrically opposite way, the method indirect determination iron content of application fluorescent quenching, but the method in realization, need to apply dual wavelength, excite first, measure first, more loaded down with trivial details, the difficulty that on-line monitoring realizes certainly will be increased, and the method mensuration range of linearity is narrower, the method is in survey iron, and expansion potentiality are little.
As can be seen here, a kind of analyzing detecting method that is automatic, quick, accurate, reliable, that be easy to realize at linearize, the middle trace iron ions of workable Power Plant Water Vapor (or other aqueous systems) is developed very necessary.
Flowing injecting analysis technology (FlowInjectionAnalysis is called for short FIA) is that physically based deformation is uneven and chemistry is uneven and the micro-wet-chemical analysis technology of dynamic measurement that is that carry out.The outstanding feature of this technology is that analysis speed is fast, precision is high, save reagent and sample, applicability is wide, equipment and simple to operate, easy to use and be easy to realize on-line monitoring, and it is the effective means realizing the analysis automated and specializes in chemistry theory of solution chemistry.FIA combines with spectrophotometric method, quite large proportion is accounted in trace analysis chemistry, the sample preparation efficiency that FIA technology is high and the automation mechanized operation highly reappeared, can realize the detection of sample in linearize, whole analytic process is completed in enclosed system.FIA-spectrophotometric method on-line analysis, avoids the repeatedly transfer of sample in process container, thus greatly reduces personal error, and save sample and reagent, more convenient operation, succinct.The more important thing is, this automatic on-line analytical approach, whole analysis detection system is in automatic mode all the time, workstation real time record detects baseline, quantitatively objectively react testing result, thus eliminate manual uncertain factor, improve the reliability and accuracy that detect data.
Summary of the invention
For solving the problem, one object of the present invention is to provide the automatic method for quick of trace iron ions in a kind of Power Plant Water Vapor.
Application during another object of the present invention is to provide the automatic method for quick of trace iron ions trace iron ions in Power Plant Water Vapor in described Power Plant Water Vapor to detect.
Another object of the present invention is to provide the automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor.
For reaching above-mentioned purpose, the invention provides the automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor, this system comprises reduction reagent bottle 1, chromogenic reagent bottle 2, damping fluid bottle 3, current-carrying bottle 4, water sample bottle 5, flow injection analyzer 9, composite module 10, Y-type three way type 11, chromogenic reaction coil pipe 13, reduction reaction coil pipe 14 and detecting device 15; Wherein said flow injection analyzer 9 comprises main pump 6, auxiliary pump 7, eight channel sample valve 8 and sampling ring 12;
Wherein, when this system is in sample states, described reduction reagent bottle 1 is connected with the first port c1 of composite module 10 via main pump 6 by pipeline;
Described chromogenic reagent bottle 2, damping fluid bottle 3 are connected by the five-port c5 of pipeline with composite module 10 via main pump 6 by pipeline after Y-type three way type 11 converges again;
Described current-carrying bottle 4 is connected with the outer ring second port d2 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, the inner ring second port e2 of eight channel sample valves 8 is connected with inner ring the 8th port e8 by pipeline, and outer ring the 8th port d8 of eight channel sample valves 8 is connected with the second port c2 of composite module 10 by pipeline;
Described water sample bottle 5 is connected with outer ring the 7th port d7 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, and inner ring the 7th port e7 of eight channel sample valves 8 is connected with inner ring first port e1 via sampling ring 12;
4th port c4 of described composite module 10 is connected with the 3rd port c3 of composite module 10 by reduction reaction coil pipe 14;
6th port c6 of described composite module 10 is connected by the entrance of pipeline with chromogenic reaction coil pipe 13, and the outlet of chromogenic reaction coil pipe 13 is connected with detecting device 15 by pipeline;
When this system is in injection state, described reduction reagent bottle 1 is connected with the first port c1 of composite module 10 via main pump 6 by pipeline;
Described chromogenic reagent bottle 2, damping fluid bottle 3 are connected by the five-port c5 of pipeline with composite module 10 via main pump 6 by pipeline after Y-type three way type 11 converges again;
Described current-carrying bottle 4 is connected with the outer ring second port d2 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, the inner ring first port e1 of eight channel sample valves 8 is connected with inner ring the 7th port e7 via sampling ring 12, and outer ring the 8th port d8 of eight channel sample valves 8 is connected with the second port c2 of composite module 10 by pipeline;
Described water sample bottle 5 is connected with outer ring the 7th port d7 of eight channel sample valves 8 via auxiliary pump 7 by pipeline;
4th port c4 of described composite module 10 is connected with the 3rd port c3 of composite module 10 by reduction reaction coil pipe 14;
6th port c6 of described composite module 10 is connected by the entrance of pipeline with chromogenic reaction coil pipe 13, and the outlet of chromogenic reaction coil pipe 13 is connected with detecting device 15 by pipeline.
According to system of the present invention, the present invention's eight channel sample valves 8 used are the sampling valve of this area routine, this eight channel sample valve 8 comprises 16 ports, i.e. outer ring first port d1, outer ring second port d2, outer ring the 3rd port d3, outer ring the 4th port d4, outer ring five-port d5, outer ring the 6th port d6, outer ring the 7th port d7 and outer ring the 8th port d8;
Inner ring first port e1, inner ring second port e2, inner ring the 3rd port e3, inner ring the 4th port e4, inner ring five-port e5, inner ring the 6th port e6, inner ring the 7th port e7 and inner ring the 8th port e8.
According to system of the present invention, preferably, the internal diameter of described pipeline is 0.5mm; Be understandable that, pipeline described here is the whole pipelines connected between each assembly of the present invention, namely water sample, go back the pipeline that original reagent, chromogenic reagent, damping fluid and current-carrying flow through.
According to system of the present invention, preferably, the length of described reduction reaction coil pipe 14 is 6-160cm;
The length of described reduction reaction coil pipe 14 is more preferably 5-20cm.
According to system of the present invention, preferably, the length of described chromogenic reaction coil pipe 13 is 100-390cm, and internal diameter is 0.5mm.
According to system of the present invention, preferably, described eight channel sample valves 8 are for can make water sample from bottom to top enter sampling ring 12 by pipeline via auxiliary pump 7 by water sample bottle 5 in sample states, current-carrying by current-carrying bottle 4 by pipeline via auxiliary pump 7 with go back original reagent and collected in composite module 10 via main pump 6 by pipeline by reducing reagent bottle 1, after flowing through reduction reaction coil pipe 14 again, collected in composite module 10 by pipeline again after being collected in Y-type three way type 11 via main pump 6 by pipeline by chromogenic reagent bottle 2, damping fluid bottle 3 respectively with chromogenic reagent, damping fluid;
And current-carrying can be made to enter sampling ring 12 by pipeline from top to bottom via auxiliary pump 7 by current-carrying bottle 4 when the state of injection, composite module 10 is entered again via pipeline, with go back original reagent and collected in composite module 10 via main pump 6 by pipeline by reducing reagent bottle 1, after flowing through reduction reaction coil pipe 14 again, with chromogenic reagent, damping fluid respectively by chromogenic reagent bottle 2, damping fluid bottle 3 after being collected in Y-type three way type 11 via main pump 6 by pipeline again by eight channel sample valves that pipeline collects in composite module 10.
According to system of the present invention, preferably, this system also comprises the first discharging of waste liquid end 17 and the second discharging of waste liquid end 18; Described first discharging of waste liquid end 17 is connected with described detecting device 15 by pipeline; Described second discharging of waste liquid end 18 is connected with outer ring first port d1, inner ring the 6th port e6 of eight channel sample valves 8 respectively by pipeline.
According to system of the present invention, preferably, this system also comprises workstation 16, and described workstation 16 is electrically connected with detecting device 15.
Described workstation is this area conventional equipment, may be used for processing and displaying the testing result of detecting device, even can carry out the input of data to control equipment such as detecting devices by alternating interface between man and computer.
According to system of the present invention, preferably, described detecting device 15 is UV-vis spectroscopy detecting device; Described UV-vis spectroscopy detecting device can be UV-vis spectroscopy detecting device any in prior art, employing preferred for this invention be light path be 10-50mm, pond volume is the UV-vis spectroscopy detecting device of 10-100 μ L.
According to system of the present invention, preferably, the conventional pumps that described main pump 6, auxiliary pump 7 can use for this area, main pump 6 is peristaltic pump in the present invention; The pump line internal diameter of this main pump 6 is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min;
Auxiliary pump 7 used is also peristaltic pump, and the pump line internal diameter of this auxiliary pump 7 is 0.5-1.5mm; Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
According to system of the present invention, the present invention's sampling ring used is this area conventional equipment.
Present invention also offers the automatic method for quick of trace iron ions in a kind of Power Plant Water Vapor, described method adopts the automatic rapid detection system of trace iron ions in above-mentioned Power Plant Water Vapor to realize, the method adopts water by Flow Injection-Spectrophotometry method, and sampling volume is 30-1000 μ L;
Used original reagent of going back is aqueous ascorbic acid, and concentration is 1-50mg/L;
Chromogenic reagent used is 2,4,6-tri-(2-pyridine radicals)-1,3,5-triazines (TPTZ) aqueous solution, and concentration is 1-50mg/L;
The pH value of damping fluid used to be pH value the be damping fluid water sample used of 2.5-3.5 is 2.0-7.0;
Current-carrying used is high purity water, and the effect of current-carrying is when eight channel sample valves are in sampling location, and current-carrying is as background, and detection signal is background signal; When eight channel sample valves are in injection phase, current-carrying promote water sample to be measured in sampling ring and go back original reagent, chromogenic reagent enters detecting device after reacting, detection signal is the response peak height of sample.Wherein, described high purity water is the conventional substances that this area uses, in the preferred embodiment of the present invention, and the high purity water of high purity water used to be resistivity be 18.3M Ω.
According to method of the present invention, used original reagent of going back is the material that reductibility is stronger, and in the preferred embodiment of the present invention, this goes back original reagent is aqueous ascorbic acid.
According to method of the present invention, chromogenic reagent used is can form the complexing agent of colored complex, in the preferred embodiment of the present invention with Fe (II), this chromogenic reagent is 2,4,6-tri-(2-pyridine radicals)-1,3,5-triazine (TPTZ) aqueous solution.
According to method of the present invention, the present invention does not do requirement to the flow going back original reagent, chromogenic reagent, damping fluid, current-carrying and water sample used; In sample states or the state of injection, the flow of the pump (main pump or auxiliary pump) that the flow going back original reagent, chromogenic reagent, damping fluid, current-carrying and water sample all flows through with it is identical.
According to method of the present invention, the temperature of described reduction reaction is normal temperature, and the reduction reaction time is the time that reagent flows through whole reduction reaction coil pipe, and it is determined by the length of reduction reaction coil pipe;
The temperature of described chromogenic reaction is normal temperature, and the chromogenic reaction time is the time that reagent flows through whole chromogenic reaction coil pipe, and it is determined by the length of chromogenic reaction coil pipe.Whether completely flow injection analysis of the present invention is carried out under non-equilibrium condition, to reaction not requirement, as long as ensure that sensitivity and reappearance reach technical requirement.
According to method of the present invention, preferably, described sampling volume is 200-800 μ L.
According to method of the present invention, preferably, the concentration of going back original reagent aqueous ascorbic acid described in is 5-25mg/L.
According to method of the present invention, preferably, the concentration of described 2,4,6-tri-(2-pyridine radicals)-1,3,5-triazines aqueous solution chromogenic reagents is 10-40mg/L.
According to method of the present invention, preferably, described damping fluid is acetic acid-ammonium acetate buffer solution.
According to method of the present invention, preferably, the pH value of described water sample is 2.0-4.5.
According to method of the present invention, preferably, described method comprises the steps:
A, sampling process: water sample is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtains background signal;
B, injection process: after sampling process completes, current-carrying promote water sample composite module with go back after original reagent mixes, flow through reduction reaction coil pipe and carry out reduction reaction, again with the mixed solution of chromogenic reagent and damping fluid after composite module collects, flow through chromogenic reaction coil pipe and carry out chromogenic reaction, after chromogenic reaction terminates, enter detecting device and detect.
According to method of the present invention, preferably, described detecting device is UV-vis spectroscopy detecting device;
More preferably the light path of described UV-vis spectroscopy detecting device is 10-50mm, and pond volume is 10-100 μ L.
According to method of the present invention, preferably, described method also comprises walking baseline process before sampling process: current-carrying is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtain stable background signal (signal that workstation registering instrument shows).
According to method of the present invention, preferably, the length of described reduction reaction coil pipe is 6-160cm;
More preferably the length of described reduction reaction coil pipe is 5-20cm.
According to method of the present invention, preferably, the length of described chromogenic reaction coil pipe is 100-390cm, and internal diameter is 0.5mm.
According to method of the present invention, preferably, the internal diameter of described pipeline is 0.5mm.
According to method of the present invention, preferably, described main pump is peristaltic pump; The pump line internal diameter of this main pump is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min.
According to method of the present invention, preferably, described auxiliary pump is peristaltic pump, and the pump line internal diameter of this auxiliary pump is 0.5-1.5mm; Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
Present invention also offers the application of the automatic method for quick of trace iron ions in Power Plant Water Vapor in trace iron ions detection in above-mentioned Power Plant Water Vapor.Wherein, described " iron " is the full iron in Power Plant Water Vapor.
In sum, the invention provides the automatic method for quick of trace iron ions and system in a kind of Power Plant Water Vapor.Flow injection (FIA) analytical technology and point optical detection technique are successfully applied in the automatic detection of trace iron ions in Power Plant Water Vapor (or other aqueous systems) by the present invention; FIA technology has high sample preparation efficiency, also can carry out the automation mechanized operation highly reappeared simultaneously, and then can make the method a kind of online, carry out in airtight analytic system, avoid sample repeatedly transfer in a reservoir in manual operations, thus greatly reduce personal error, and save sample and reaction reagent, visible the method is more convenient to operate, succinct, improve the reliability and accuracy that detect data.
In addition, in Power Plant Water Vapor provided by the present invention, the automatic method for quick of trace iron ions and system have filled up the blank of trace iron in water ion chemistry analysis automatic technology, solid method basis has been established in development for underwater trace ferric ion on-Line Monitor Device, has great scientific research value and actual application value.
The automatic method for quick of trace iron ions and system in Power Plant Water Vapor of the present invention are applied to the detection of trace iron ions in Power Plant Water Vapor, trace iron ions in Power Plant Water Vapor can be realized automatically, fast, accurately, reliably measure, detect and be limited to 0.5 μ g/L.
Accompanying drawing explanation
Fig. 1 is trace iron ions automatic rapid detection system one embodiment (original state) in Power Plant Water Vapor of the present invention;
Fig. 2 is trace iron ions automatic rapid detection system one embodiment (duty) in Power Plant Water Vapor of the present invention;
Fig. 3 is the concrete annexation schematic diagram of eight channel sample valves under trace iron ions automatic rapid detection system one embodiment (original state) in Power Plant Water Vapor of the present invention;
Fig. 4 is the concrete annexation schematic diagram of eight channel sample valves under trace iron ions automatic rapid detection system one embodiment (duty) in Power Plant Water Vapor of the present invention;
Fig. 5 is the schematic diagram of each port on composite module that in Power Plant Water Vapor of the present invention, the automatic rapid detection system of trace iron ions is used;
Fig. 6 is the standard working curve figure of ferric ion in test case of the present invention;
Fig. 7 is detection signal spectrogram when adopting trace iron ions in method of the present invention mensuration Power Plant Water Vapor.
Main Reference label declaration
Reduction reagent bottle 1 chromogenic reagent bottle 2 damping fluid bottle 3 current-carrying bottle 4 water sample bottle 5 main pump 6 auxiliary pump 7 eight channel sample valve 8 flow injection analyzer 9 composite module 10Y type threeway 11 sampling ring 12 chromogenic reaction coil pipe 13 reduction reaction coil pipe 14 detecting device 15 workstation 16 first discharging of waste liquid end 17 second discharging of waste liquid end 18;
Eight channel sample valves 8 comprise 16 ports, i.e. outer ring first port d1, outer ring second port d2, outer ring the 3rd port d3, outer ring the 4th port d4, outer ring five-port d5, outer ring the 6th port d6, outer ring the 7th port d7 and outer ring the 8th port d8;
Inner ring first port e1, inner ring second port e2, inner ring the 3rd port e3, inner ring the 4th port e4, inner ring five-port e5, inner ring the 6th port e6, inner ring the 7th port e7 and inner ring the 8th port e8;
Composite module 10 comprises six ports: i.e. the first port c1, the second port c2, the 3rd port c3, the 4th port c4, five-port c5, the 6th port c6.
Embodiment
To be described in detail the Advantageous Effects of implementation process of the present invention and generation by specific embodiment and Figure of description below, be intended to help reader better to understand essence of the present invention and feature, but not as can the restriction of practical range to this case.
1, equipment
Present embodiments provide the automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor, wherein, this system comprises: reduction reagent bottle 1, chromogenic reagent bottle 2, damping fluid bottle 3, current-carrying bottle 4, water sample bottle 5, flow injection analyzer 9, composite module 10, Y-type three way type 11, chromogenic reaction coil pipe 13, reduction reaction coil pipe 14, detecting device 15, workstation 16, first discharging of waste liquid end 17 and the second discharging of waste liquid end 18;
Wherein said flow injection analyzer 9 comprises main pump 6, auxiliary pump 7, eight channel sample valve 8 and sampling ring 12;
Wherein said eight channel sample valves 8 comprise 16 ports, i.e. outer ring first port d1, outer ring second port d2, outer ring the 3rd port d3, outer ring the 4th port d4, outer ring five-port d5, outer ring the 6th port d6, outer ring the 7th port d7 and outer ring the 8th port d8;
Inner ring first port e1, inner ring second port e2, inner ring the 3rd port e3, inner ring the 4th port e4, inner ring five-port e5, inner ring the 6th port e6, inner ring the 7th port e7 and inner ring the 8th port e8;
Described composite module 10 comprises six ports: i.e. the first port c1, the second port c2, the 3rd port c3, the 4th port c4, five-port c5, the 6th port c6, and the schematic diagram of each port of composite module as shown in Figure 5;
Wherein, when this system is in sample states (constitutional diagram as shown in Figure 1, Figure 3), described reduction reagent bottle 1 is connected with the first port c1 of composite module 10 via main pump 6 by pipeline;
Described chromogenic reagent bottle 2, damping fluid bottle 3 are connected by the five-port c5 of pipeline with composite module 10 via main pump 6 by pipeline after Y-type three way type 11 converges again;
Described current-carrying bottle 4 is connected with the outer ring second port d2 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, the inner ring second port e2 of eight channel sample valves 8 is connected with inner ring the 8th port e8 by pipeline, and outer ring the 8th port d8 of eight channel sample valves 8 is connected with the second port c2 of composite module 10 by pipeline;
Described water sample bottle 5 is connected with outer ring the 7th port d7 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, and inner ring the 7th port e7 of eight channel sample valves 8 is connected with inner ring first port e1 by sampling ring 12;
4th port c4 of described composite module 10 is connected with the 3rd port c3 of composite module 10 by reduction reaction coil pipe 14;
6th port c6 of described composite module 10 is connected by the entrance of pipeline with chromogenic reaction coil pipe 13, and the outlet of chromogenic reaction coil pipe 13 is connected with detecting device 15 by pipeline;
When this system is in injection state (constitutional diagram as shown in Figure 2, Figure 4 shows), described reduction reagent bottle 1 is connected with the first port c1 of composite module 10 via main pump 6 by pipeline;
Described chromogenic reagent bottle 2, damping fluid bottle 3 are connected by the five-port c5 of pipeline with composite module 10 via main pump 6 by pipeline after Y-type three way type 11 converges again;
Described current-carrying bottle 4 is connected with the outer ring second port d2 of eight channel sample valves 8 via auxiliary pump 7 by pipeline, the inner ring first port e1 of eight channel sample valves 8 is connected with inner ring the 7th port e7 via sampling ring 12 more by the road by pipeline, and outer ring the 8th port d8 of eight channel sample valves 8 is connected with the second port c2 of composite module 10 by pipeline;
Described water sample bottle 5 is connected with outer ring the 7th port d7 of eight channel sample valves 8 via auxiliary pump 7 by pipeline;
4th port c4 of described composite module 10 is connected with the 3rd port c3 of composite module 10 by reduction reaction coil pipe 14;
6th port c6 of described composite module 10 is connected by the entrance of pipeline with chromogenic reaction coil pipe 13, and the outlet of chromogenic reaction coil pipe 13 is connected with detecting device 15 by pipeline;
Described first discharging of waste liquid end 17 is connected with described detecting device 15 by pipeline; Described second discharging of waste liquid end 18 is connected with outer ring first port d1, inner ring the 6th port e6 of eight channel sample valves 8 respectively by pipeline;
Described workstation 16 is electrically connected with detecting device 15;
The internal diameter of described pipeline is 0.5mm;
The length of described reduction reaction coil pipe 14 is 6-160cm;
The length of described chromogenic reaction coil pipe 13 is 100-390cm, and internal diameter is 0.5mm;
Described detecting device 15 is UV-vis spectroscopy detecting device; The light path of this UV-vis spectroscopy detecting device is 10-50mm, and pond volume is 10-100 μ L;
Described main pump 6, auxiliary pump 7 are peristaltic pump; The pump line internal diameter of main pump 6 is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min; The pump line internal diameter of auxiliary pump 7 is 0.5-1.5mm; Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
2, analysis process
Flow injection-spectrophotometric analysis system is established according to the automatic rapid detection system of trace iron ions in Power Plant Water Vapor provided by the invention.This system can carry out the programming of running program, and setting pump speed, flow etc., sample " sampling " and " injection " are automatically switched by setup program, achieve the Automated condtrol of whole pipe system.
Walk baseline process: process flow diagram as shown in Figure 1, eight channel sample valves are in " sampling " state (original state), current-carrying is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are (before composite module collects, first chromogenic reagent and damping fluid converge after main pump drives in Y-type three way type) after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtain stable background signal (signal that workstation registering instrument shows),
Sampling process: process flow diagram as shown in Figure 1, eight channel sample valves are in " sampling " state (original state), water sample is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtain background signal,
Inject and testing process: after sampling process completes, eight channel sample valves are automatically brought to " injection " state (duty), process flow diagram as shown in Figure 2, current-carrying promote water sample composite module with go back after original reagent mixes, flow through reduction reaction coil pipe and carry out reduction reaction, again with the mixed solution of chromogenic reagent and damping fluid after composite module collects, flow through chromogenic reaction coil pipe (internal diameter is 0.5mm) and carry out chromogenic reaction, after chromogenic reaction terminates, enter detecting device to detect, waste liquid enters in waste liquid barrel.Whole " injection " state, in water sample, iron concentration detection signal is gathered in real time by workstation;
Current-carrying used is high purity water, and its resistivity is 18.3M Ω;
Chromogenic reagent used is 2,4,6-tri-(2-pyridine radicals)-1,3,5-triazines aqueous solution;
Used original reagent of going back is aqueous ascorbic acid;
Damping fluid used is acetic acid-ammonium acetate buffer solution.
Embodiment is in table 1:
Table 1 embodiment
| Experiment condition | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Main pump rotating speed (rpm) | 10 | 20 | 30 |
| Main pump pump line internal diameter (mm) | 0.89 | 1.04 | 1.26 |
| Auxiliary pump rotating speed (rpm) | 35 | 45 | 60 |
| Auxiliary pump pump line internal diameter (mm) | 0.89 | 1.04 | 1.26 |
| Sampling volume (μ L) | 300 | 400 | 500 |
| TPTZ concentration (mg/L) | 10 | 20 | 30 |
| PH of cushioning fluid | 2.5 | 3.0 | 3.5 |
| Ascorbic acid concentrations (mg/L) | 5 | 15 | 20 |
| The pH value of water sample | 2.0 | 2.5 | 3.0 |
| Chromogenic reaction coil lengths (cm) | 100 | 150 | 200 |
| Reduction reaction coil lengths (cm) | 5 | 10 | 15 |
| UV-vis spectroscopy detecting device light path (mm) | 10 | 20 | 30 |
| UV-vis spectroscopy detector cell volume (μ L) | 12 | 40 | 60 |
Test example
1, the mensuration of standard working curve
Under the experiment condition of embodiment 1, at a series of ferric ion standard solution of latitude of formulation of 0.5-80 μ g/L, be determined at the standard working curve in this concentration range, result as shown in Figure 6, as can be seen from Figure 6, the peak height of working curve and the concentration of standard solution ferric ion are good linear relationship.Detection signal spectrogram when adopting method of the present invention to measure trace iron ions in Power Plant Water Vapor as shown in Figure 7.
2, reproducible mensuration
To the ferric ion standard solution replicate determination more than 7 times respectively of 5.0 μ g/L and 50 μ g/L, measure the reappearance of this method, measurement result is shown in Table 2.The relative standard deviation of 5.0 μ g/L and 50 μ g/L ferric ion standard solution is respectively 0.69% and 0.74%, and the relative standard deviation of the two is all less than 1.0%, and as can be seen here, the reappearance of this method is good.
Table 2 reappearance measurement result
3, the mensuration of lower limit is detected
In this method, detection limit refers to the lower limit can knowing the peak height of the analyte distinguished on workstation signal record figure, it has been generally acknowledged that the response signal peak height that be able to distinguish, minimum 3 times of should be baseline noise, the concentration of the analyte that this signal is corresponding.
Detecting of this method is limited to: C=0.5 μ g/L.
Other performance index of this method are shown in Table 3.
The performance index of table 3 this method
| Sequence number | Performance index | Control criterion | Measured value |
| 1 | The range of linearity (μ g/L) | <100 | 0.5-80 |
| 2 | Linear coefficient | >0.999 | 0.999 |
| 3 | Precision (RSD) | <5％ | 0.69％ |
| 4 | Relative error | <20％ | <20％ |
| 5 | Recovery of standard addition | 90％-110％ | 93.96％-103.37％ |
| 6 | Sensitivity | / | / |
| 7 | Detect lower limit | <5 | 0.5 |
| 8 | Baseline wander | <0.002AU/h | <0.002AU/h |
| 9 | Analysis speed | 60 | 60s/ sample |
4, practical application
Adopt this project approach to measure the Trace Iron content in some Power Plant Water Vapor samples, measurement result is shown in Table 4.
The mensuration of table 4 recovery
As can be seen from Table 4, the measured value of the recovery is within the scope of 90-110%, and this shows that other ion, pH value etc. in water sample do not form interference to detection, demonstrates accuracy and the reliability of the method.
Claims (10)
1. the automatic rapid detection system of trace iron ions in a Power Plant Water Vapor, it is characterized in that, this system comprises reduction reagent bottle (1), chromogenic reagent bottle (2), damping fluid bottle (3), current-carrying bottle (4), water sample bottle (5), flow injection analyzer (9), composite module (10), Y-type three way type (11), chromogenic reaction coil pipe (13), reduction reaction coil pipe (14) and detecting device (15); Wherein said flow injection analyzer (9) comprises main pump (6), auxiliary pump (7), eight channel sample valves (8) and sampling ring (12);
Wherein, when this system is in sample states, described reduction reagent bottle (1) is connected with first port (c1) of composite module (10) via main pump (6) by pipeline;
Described chromogenic reagent bottle (2), damping fluid bottle (3) are connected by the five-port (c5) of pipeline with composite module (10) via main pump (6) by pipeline after Y-type three way type (11) converges again;
Described current-carrying bottle (4) is connected via the outer ring second port (d2) of auxiliary pump (7) with eight channel sample valves (8) by pipeline, inner ring second port (e2) of eight channel sample valves (8) is connected with inner ring the 8th port (e8) by pipeline, and the outer ring the 8th port (d8) of eight channel sample valves (8) is connected with second port (c2) of composite module (10) by pipeline;
Described water sample bottle (5) is connected via the outer ring seven port (d7) of auxiliary pump (7) with eight channel sample valves (8) by pipeline, and the inner ring the 7th port (e7) of eight channel sample valves (8) is connected with inner ring first port (e1) via sampling ring (12);
4th port (c4) of described composite module (10) is connected with the 3rd port (c3) of composite module (10) by reduction reaction coil pipe (14);
6th port (c6) of described composite module (10) is connected by the entrance of pipeline with chromogenic reaction coil pipe (13), and the outlet of chromogenic reaction coil pipe (13) is connected with detecting device (15) by pipeline;
When this system is in injection state, described reduction reagent bottle (1) is connected with first port (c1) of composite module (10) via main pump (6) by pipeline;
Described chromogenic reagent bottle (2), damping fluid bottle (3) are connected by the five-port (c5) of pipeline with composite module (10) via main pump (6) by pipeline after Y-type three way type (11) converges again;
Described current-carrying bottle (4) is connected via the outer ring second port (d2) of auxiliary pump (7) with eight channel sample valves (8) by pipeline, inner ring first port (e1) of eight channel sample valves (8) is connected with inner ring the 7th port (e7) via sampling ring (12), and the outer ring the 8th port (d8) of eight channel sample valves (8) is connected with second port (c2) of composite module (10) by pipeline;
Described water sample bottle (5) is connected via the outer ring seven port (d7) of auxiliary pump (7) with eight channel sample valves (8) by pipeline;
4th port (c4) of described composite module (10) is connected with the 3rd port (c3) of composite module (10) by reduction reaction coil pipe (14);
6th port (c6) of described composite module (10) is connected by the entrance of pipeline with chromogenic reaction coil pipe (13), and the outlet of chromogenic reaction coil pipe (13) is connected with detecting device (15) by pipeline;
The internal diameter of preferred described pipeline is 0.5mm;
Also the length of preferred described reduction reaction coil pipe (14) is 6-160cm, is more preferably 5-20cm;
Also the length of preferred described chromogenic reaction coil pipe (13) is 100-390cm, and internal diameter is 0.5mm;
Wherein also preferably described eight channel sample valves (8) for water sample can be made to enter sampling ring (12) by pipeline from bottom to top via auxiliary pump (7) by water sample bottle (5) in sample states, current-carrying by current-carrying bottle (4) by pipeline via auxiliary pump (7) with go back original reagent and collected in composite module (10) via main pump (6) by pipeline by reducing reagent bottle (1), after flowing through reduction reaction coil pipe (14) again, with chromogenic reagent, damping fluid is respectively by chromogenic reagent bottle (2), damping fluid bottle (3) is collected in composite module (10) by pipeline after being collected in Y-type three way type (11) via main pump (6) by pipeline again,
And current-carrying can be made to enter sampling ring (12) by pipeline from top to bottom via auxiliary pump (7) by current-carrying bottle (4) when the state of injection, composite module (10) is entered again via pipeline, with go back original reagent and collected in composite module (10) via main pump (6) by pipeline by reducing reagent bottle (1), after flowing through reduction reaction coil pipe (14) again, with chromogenic reagent, damping fluid is respectively by chromogenic reagent bottle (2), damping fluid bottle (3) after being collected in Y-type three way type (11) via main pump (6) by pipeline again by eight channel sample valves that pipeline collects in composite module (10).
2. system according to claim 1, is characterized in that, this system also comprises the first discharging of waste liquid end (17) and the second discharging of waste liquid end (18); Described first discharging of waste liquid end (17) is connected with described detecting device (15) by pipeline; Described second discharging of waste liquid end (18) is connected with the outer ring first port (d1) of eight channel sample valves (8), inner ring the 6th port (e6) respectively by pipeline.
3. system according to claim 1 and 2, is characterized in that, this system also comprises workstation (16), and described workstation (16) is electrically connected with detecting device (15).
4. system according to claim 1 and 2, is characterized in that, described detecting device (15) is UV-vis spectroscopy detecting device;
The light path of preferred described UV-vis spectroscopy detecting device is 10-50mm, and pond volume is 10-100 μ L.
5. the system according to any one of claim 1-4, is characterized in that, described main pump (6) is peristaltic pump; The pump line internal diameter of this main pump (6) is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min;
Preferred described auxiliary pump (7) is peristaltic pump; The pump line internal diameter of this auxiliary pump (7) is 0.5-1.5mm; Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
6. the automatic method for quick of trace iron ions in a Power Plant Water Vapor, it is characterized in that, described method adopts the automatic rapid detection system of trace iron ions in the Power Plant Water Vapor described in any one of claim 1-5 to realize, the method adopts water by Flow Injection-Spectrophotometry method, wherein, sampling volume is 30-1000 μ L, is preferably 200-800 μ L;
Used original reagent of going back is aqueous ascorbic acid, and concentration is 1-50mg/L, is preferably 5-25mg/L;
Chromogenic reagent used is 2,4,6-tri-(2-pyridine radicals)-1,3,5-triazines aqueous solution, and concentration is 1-50mg/L, is preferably 10-40mg/L;
The damping fluid of damping fluid used to be pH value be 2.5-3.5, preferred described damping fluid is acetic acid-ammonium acetate buffer solution;
The pH value of water sample used is 2.0-7.0, is preferably 2.0-4.5;
Current-carrying used is high purity water.
7. method according to claim 6, is characterized in that, described method comprises the steps:
A, sampling process: water sample is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtains background signal;
B, injection process: after sampling process completes, current-carrying promote water sample composite module with go back after original reagent mixes, flow through reduction reaction coil pipe and carry out reduction reaction, again with the mixed solution of chromogenic reagent and damping fluid after composite module collects, flow through chromogenic reaction coil pipe and carry out chromogenic reaction, after chromogenic reaction terminates, enter detecting device and detect;
Preferred described method also comprises walking baseline process before sampling process: current-carrying is driven by auxiliary pump by the road and enters sampling ring through eight channel sample valves, simultaneously, the original reagent of going back that auxiliary pump drives current-carrying to drive via eight channel sample valves and main pump collects at composite module, after flowing through reduction reaction coil pipe again, the chromogenic reagent driven with main pump and the mixed solution of damping fluid are after composite module collects, flow through chromogenic reaction coil pipe to enter detecting device and detect, detection signal carries out real-time data acquisition and process by workstation, obtains stable background signal;
Also the length of preferred described reduction reaction coil pipe is 6-160cm, is more preferably 5-20cm;
Also the length of preferred described chromogenic reaction coil pipe is 100-390cm, and internal diameter is 0.5mm;
Also the internal diameter of preferred described pipeline is 0.5mm.
8. the method according to claim 6 or 7, is characterized in that, described detecting device is UV-vis spectroscopy detecting device;
The light path of preferred described UV-vis spectroscopy detecting device is 10-50mm, and pond volume is 10-100 μ L.
9. the method according to claim 6-8 any one, is characterized in that, described main pump is peristaltic pump; The pump line internal diameter of this main pump is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min;
Preferred described auxiliary pump is peristaltic pump, and the pump line internal diameter of this auxiliary pump is 0.5-1.5mm; Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
10. the application of the automatic method for quick of trace iron ions in Power Plant Water Vapor in trace iron ions detection in the Power Plant Water Vapor described in claim 6-9 any one.
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