CN105388309B - The automatic quick determination method of trace iron ions and system and application in Power Plant Water Vapor - Google Patents
The automatic quick determination method of trace iron ions and system and application in Power Plant Water Vapor Download PDFInfo
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- CN105388309B CN105388309B CN201510764964.8A CN201510764964A CN105388309B CN 105388309 B CN105388309 B CN 105388309B CN 201510764964 A CN201510764964 A CN 201510764964A CN 105388309 B CN105388309 B CN 105388309B
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- 238000000034 method Methods 0.000 title claims abstract description 116
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 97
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 68
- -1 iron ions Chemical class 0.000 title claims abstract description 45
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 86
- 239000002131 composite material Substances 0.000 claims abstract description 69
- 238000001514 detection method Methods 0.000 claims abstract description 49
- 238000005070 sampling Methods 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 239000007853 buffer solution Substances 0.000 claims abstract description 40
- 238000006722 reduction reaction Methods 0.000 claims abstract description 39
- 238000004401 flow injection analysis Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 19
- 239000002699 waste material Substances 0.000 claims description 17
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 238000007599 discharging Methods 0.000 claims description 13
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 12
- 230000002572 peristaltic effect Effects 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000002798 spectrophotometry method Methods 0.000 claims description 5
- ALSPKRWQCLSJLV-UHFFFAOYSA-N azanium;acetic acid;acetate Chemical compound [NH4+].CC(O)=O.CC([O-])=O ALSPKRWQCLSJLV-UHFFFAOYSA-N 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000007689 inspection Methods 0.000 claims description 2
- 150000000182 1,3,5-triazines Chemical class 0.000 claims 1
- 238000004458 analytical method Methods 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 10
- 238000010586 diagram Methods 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000012491 analyte Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000005375 photometry Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 235000014171 carbonated beverage Nutrition 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000000673 graphite furnace atomic absorption spectrometry Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000002133 sample digestion Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides the automatic quick determination method of trace iron ions and system and application in a kind of Power Plant Water Vapor.The system includes go back original reagent bottle (1), colour reagent bottle (2), buffer solution 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 detector (15)；Wherein described flow injection analyzer (9) includes main pump (6), auxiliary pump (7), eight channel sample valves (8) and sampling ring (12).Application present invention also offers the automatic quick determination method of trace iron ions in Power Plant Water Vapor and its in Power Plant Water Vapor in trace iron ions detection.The method and system that the present invention is provided can realize that trace iron ions are automatic, quick in Power Plant Water Vapor, accurately and reliably determine, and detection is limited to 0.5 μ g/L.
Description
Technical field
The present invention relates to the detection of Power Plant Water Vapor, specifically, it is related to trace iron ions in a kind of Power Plant Water Vapor automatically fast
Fast detection method and system and application.
Background technology
The iron content of Power Plant Water Vapor system is a very important monitor control index, and it is to evaluate operating unit therrmodynamic system
The important evidence of corrosion and scaling situation, is one of daily production regular monitoring index of power plant.
At present, the method for determining full iron in power generation feedwater, stove water is Phen AAS (GB/T
14427-2008) with graphite oven atomic absorption (DL/T 955-2005).Phen AAS is analyzed for traditional-handwork
Method, this method trivial operations, analysis efficiency is low, acid mist can be produced in water sample digestion process, to working environment and health
Cause harm.And the instrument that graphite oven atomic absorption is used involves great expense, Operation and Maintenance requires high.
The method that will be described in detail several measure iron contents commonly used in the art below.
1st, boiler feed water and cooling water analysis method (GB/T 14427-2008)
The analysis method uses the content of spectrophotometric determination o-phenanthroline iron.Fe (II) ferrosin complex compound is in pH
2.5-9.0 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
It is linear with absorbance.Maximum light absorption value is at 510nm wavelength.But this method is artificial detection method, sample is in behaviour
Make repeatedly be shifted in container, so that the accuracy and reliability of test result can be influenceed, and the water sample of this method consumption
Amount and amount of reagent are larger, cause the waste of water sample and reagent.
2nd, in graphite furnace atomic absorption spectrometry thermal power plant water, vapour copper and iron (DL/T 955-2005)
Graphite oven atomic absorption, its detection line is 0-100 μ g/L, and the Determination Limit of this method is less than modern unit steam
Full iron newest standards value, this meets existing technical requirements, but is due to that the instrument of graphite oven atomic absorption involves great expense, property
Can reliable import instrument unit price of about 600,000 yuan, and Operation and Maintenance requires high, higher to personnel qualifications, power plant apply compared with
It is few.
3rd, full iron in FIA-TPTZ water by Spectrophotometry
The method is the complex reaction and stream based on Fe (II) with (2- the pyridine radicals) -1,3,5- triazines of 2,4,6- tri- (TPTZ)
The analysis method that dynamic injection technique is set up, the detection of this method is limited to 22.7 μ g/L, and its Determination Limit can not meet modern unit
The full iron newest standards value of steam (5 μ g/L), therefore, this method is not suitable for the monitoring of Trace Iron in Power Plant Water Vapor.
It is more with the detection method that spectrophotomelric assay technology is combined research and development based on Flow Injection Technique, for example with stream
Total iron content in dynamic injection AAS on-line analysis water, it, which is detected, is limited to 40 μ g/L, and its Determination Limit can not meet existing
For the full iron newest standards value of unit steam (5 μ g/L)；Fe (II) and Fe is determined using Flow Injection Spectrophotometry simultaneously
(III), its detection limit is respectively 0.0012 μ g/L and 0.0018 μ g/L, and this method uses the reduction of single valve biobelt cadmium plating zinc metal sheet
The valve body stream of post band isolation, flow path system is complicated, is also unsuitable for the use of power plant.
4th, iron in catalytic Spectrophotometric Determination carbonated drink
Such detection method needs to select a suitable catalytic oxidation system of the range of linearity, simultaneously as catalytic kinetic
Learn photometry and need manual control time to complete heating, cooling process, therefore the poor anti jamming capability of this method, temperature and when
Between on measurement result influence it is larger, realize on-line monitoring require it is higher.
5th, chemiluminescence determination trace and ultra trace iron
For current research level, the technical stability of this method is poor, and determination data stability is not high, if big face
Product applies this method, it is necessary to have higher automaticity, sensitivity, the more preferable instrument of stability, therefore the technology of this method
Route is immature, it is impossible to be used as national standard method popularization and application.
6th, Fluorimetric Determination of Trace iron
Because iron has paramagnetism, therefore this area seldom determines iron content in water using this method, be typically it is anti-its
Road and go it, using the method indirect determination iron content of fluorescent quenching, but this method is in realization, it is necessary to using dual wavelength,
First excite, first determine, it is comparatively laborious, the difficulty that on-line monitoring is realized certainly will be increased, and this method determines the range of linearity
Narrower, this method is in terms of iron is surveyed, and extension potentiality are little.
As can be seen here, develop it is a kind of it is automatic, quick, accurate, be reliable, easy to realize onlineization, workable power plant
The analyzing detecting method of trace iron ions is very necessary in steam (or other aqueous systems).
Flowing injecting analysis technology (Flow Injection Analysis, abbreviation FIA) is based on physics imbalance and changed
Learn dynamic that is uneven and carrying out and determine micro wet-chemical analysis technology.The outstanding feature of the technology is that analyze speed is fast, precision
It is high, save reagent and sample, applicability be wide, equipment and simple to operate, easy to use and be easily achieved on-line monitoring, it is realization
Analysis automated and research chemical theory the effective means of solution chemistry.FIA is combined with AAS, in trace analysis
Quite big proportion is accounted in, the automation mechanized operation that the high sample treatment efficiency of FIA technologies and height are reappeared can be by sample
Onlineization is realized in the detection of product, whole analysis process is completed in enclosed system.FIA- AAS on-line analysis,
Multiple transfer of the sample in process container is avoided, so as to greatly reduce human error, and sample and reagent is saved,
It is more convenient operation, succinct.Importantly, this automatic on-line analysis method, whole analysis detecting system is all the time in automatic
Working condition, work station records detection baseline in real time, quantitative objectively to have reacted testing result, so as to eliminate manual
Uncertain factor, improves the reliability and accuracy of detection data.
The content of the invention
To solve the above problems, it is an object of the present invention to provide trace iron ions in a kind of Power Plant Water Vapor are automatically fast
Fast detection method.
Exist it is another object of the present invention to provide the automatic quick determination method of trace iron ions in the Power Plant Water Vapor
Application in Power Plant Water Vapor in trace iron ions detection.
It is yet a further object of the present invention to provide the automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor.
Up to above-mentioned purpose, the invention provides the automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor, to be somebody's turn to do
System includes go back original reagent bottle 1, colour reagent bottle 2, buffer solution bottle 3, current-carrying bottle 4, water sample bottle 5, flow injection analyzer 9, group
Matched moulds block 10, Y-type three way type 11, chromogenic reaction coil pipe 13, reduction reaction coil pipe 14 and detector 15；Wherein described flow injection point
Analyzer 9 includes main pump 6, auxiliary pump 7, eight channel sample valves 8 and sampling ring 12；
Wherein, when the system is in sample states, the go back original reagent bottle 1 is by pipeline via main pump 6 and combination die
The first port c1 of block 10 is connected；
Colour reagent bottle 2, buffer solution bottle 3 by pipeline via main pump 6 after Y-type three way type 11 converges again by pipeline
It is connected with the fifth port c5 of composite module 10；
The current-carrying bottle 4 is connected by pipeline via auxiliary pump 7 with the outer ring second port d2 of eight channel sample valves 8, and eight lead to
The inner ring second port e2 of road sampling valve 8 is connected by pipeline with the port e8 of inner ring the 8th, the outer ring the 8th of eight channel sample valves 8
Port d8 is connected by pipeline with the second port c2 of composite module 10；
The water sample bottle 5 is connected by pipeline via auxiliary pump 7 with the port d7 of outer ring the 7th of eight channel sample valves 8, and eight lead to
The port e7 of inner ring the 7th of road sampling valve 8 is connected via sampling ring 12 with inner ring first port e1；
4th port c4 of the composite module 10 passes through reduction reaction coil pipe 14 and the 3rd port c3 of composite module 10
It is connected；
6th port c6 of the composite module 10 is connected by pipeline with the entrance of chromogenic reaction coil pipe 13, chromogenic reaction
The outlet of coil pipe 13 is connected by pipeline with detector 15；
When the system is in injection state, the go back original reagent bottle 1 is by pipeline via main pump 6 and composite module 10
First port c1 is connected；
Colour reagent bottle 2, buffer solution bottle 3 by pipeline via main pump 6 after Y-type three way type 11 converges again by pipeline
It is connected with the fifth port c5 of composite module 10；
The current-carrying bottle 4 is connected by pipeline via auxiliary pump 7 with the outer ring second port d2 of eight channel sample valves 8, and eight lead to
The inner ring first port e1 of road sampling valve 8 is connected via sampling ring 12 with the port e7 of inner ring the 7th, the outer ring of eight channel sample valves 8
8th port d8 is connected by pipeline with the second port c2 of composite module 10；
The water sample bottle 5 is connected by pipeline via auxiliary pump 7 with the port d7 of outer ring the 7th of eight channel sample valves 8；
4th port c4 of the composite module 10 passes through reduction reaction coil pipe 14 and the 3rd port c3 of composite module 10
It is connected；
6th port c6 of the composite module 10 is connected by pipeline with the entrance of chromogenic reaction coil pipe 13, chromogenic reaction
The outlet of coil pipe 13 is connected by pipeline with detector 15.
According to system of the present invention, eight channel sample valves 8 used in the present invention are the conventional sampling valve in this area, should
Eight channel sample valves 8 include 16 ports, i.e. outer ring first port d1, outer ring second port d2, the port d3 of outer ring the 3rd, outer
Enclose the 4th port d4, outer ring fifth port d5, the port d6 of outer ring the 6th, the port d7 of outer ring the 7th and the port d8 of outer ring the 8th；
Inner ring first port e1, inner ring second port e2, the port e3 of inner ring the 3rd, the port e4 of inner ring the 4th, inner ring the 5th
Port e5, the port e6 of inner ring the 6th, the port e7 of inner ring the 7th and the port e8 of inner ring the 8th.
According to system of the present invention, it is preferable that the internal diameter of the pipeline is 0.5mm；It is understood that institute here
The pipeline stated is whole pipelines for connecting between each component of the invention, i.e. water sample, go back original reagent, colour reagent, buffer solution and load
The flowed through pipeline of stream.
According to system of the present invention, it is preferable that the length of the reduction reaction coil pipe 14 is 6-160cm；
The length of the reduction reaction coil pipe 14 is more preferably 5-20cm.
According to system of the present invention, it is preferable that the length of the chromogenic reaction coil pipe 13 is 100-390cm, internal diameter
For 0.5mm.
According to system of the present invention, it is preferable that the eight channel samples valve 8 is that can make water sample by water in sample states
Sample bottle 5 enters sampling ring 12 from bottom to top by pipeline via auxiliary pump 7, and current-carrying is by current-carrying bottle 4 by the way that pipeline is via auxiliary pump 7 and goes back
Original reagent is collected by pipeline by go back original reagent bottle 1 via main pump 6 in composite module 10, passes through reduction reaction coil pipe 14
Afterwards, with colour reagent, buffer solution respectively by colour reagent bottle 2, buffer solution bottle 3 by pipeline via main pump 6 in Y-type three way type 11
Collected again by pipeline in composite module 10 after collecting；
And current-carrying can be made to enter sampling ring from top to bottom via auxiliary pump 7 by pipeline by current-carrying bottle 4 in the state of injection
12, then via pipeline enter composite module 10, with go back original reagent by go back original reagent bottle 1 by pipeline via main pump 6 in combination die
Collect in block 10, pass through after reduction reaction coil pipe 14, with colour reagent, buffer solution respectively by colour reagent bottle 2, buffer solution bottle
3 collected by pipeline via main pump 6 in Y-type three way type 11 after eight channel samples collected again by pipeline in composite module 10
Valve.
According to system of the present invention, it is preferable that the system also includes the first discharging of waste liquid end 17 and the second waste liquid is arranged
Put end 18；The first discharging of waste liquid end 17 is connected by pipeline with the detector 15；The second discharging of waste liquid end 18 leads to
Outer ring first port d1, inner ring sixth port e6 of the pipeline respectively with eight channel sample valves 8 is crossed to be connected.
According to system of the present invention, it is preferable that the system also includes work station 16, the work station 16 and detector
15 electrical connections.
Described work station is this area conventional equipment, can be used for the testing result of detector is handled and shown
Show, it might even be possible to carry out the input of data to be controlled the equipment such as detector by alternating interface between man and computer.
According to system of the present invention, it is preferable that the detector 15 is UV-vis spectroscopy detector；Described
UV-vis spectroscopy detector can be UV-vis spectroscopy detector any in the prior art, use preferred for this invention
Be light path be 10-50mm, pond body product for 10-100 μ L UV-vis spectroscopy detector.
According to system of the present invention, it is preferable that the conventional pumps that the 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 the 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 the auxiliary pump 7 is 0.5-1.5mm；Rotating speed is 30-60r/min,
Flow is 1.0-3.0mL/min.
According to system of the present invention, the sampling ring used in the present invention is this area conventional equipment.
Present invention also offers the automatic quick determination method of trace iron ions in a kind of Power Plant Water Vapor, methods described is to use
The automatic rapid detection system of trace iron ions realizes that this method is using flow injection-spectrophotometric point in above-mentioned Power Plant Water Vapor
Analysis method, sampling volume is 30-1000 μ L；
Go back original reagent used is aqueous ascorbic acid, and concentration is 1-50mg/L；
Colour reagent used is 2,4,6- tri- (2- pyridine radicals) -1,3,5-triazines (TPTZ) aqueous solution, and concentration is 1-
50mg/L；
Buffer solution used is that the pH value that pH value is water sample used in 2.5-3.5 buffer solution is 2.0-7.0；
Current-carrying used is high purity water, and the effect of current-carrying is the current-carrying conduct when eight channel sample valves are in sampling location
Background, detection signal is background signal；When eight channel sample valves are in injection phase, current-carrying promotes the water to be measured in sampling ring
Sample is the response peak height of sample with entering detector, detection signal after go back original reagent, colour reagent reaction.Wherein, it is described high-purity
Water is the conventional substances that this area is used, in the preferred embodiment of the present invention, and high purity water used is that resistivity is 18.3M
Ω high purity water.
According to method of the present invention, go back original reagent used is the stronger material of reproducibility, currently preferred
In embodiment, the go back original reagent is aqueous ascorbic acid.
According to method of the present invention, colour reagent used is complexing that can be with Fe (II) formation colored complexs
Agent, in the preferred embodiment of the present invention, the colour reagent is 2,4,6- tri- (2- pyridine radicals) -1,3,5-triazines (TPTZ) water
Solution.
According to method of the present invention, the present invention is to go back original reagent used, colour reagent, buffer solution, current-carrying and water sample
Flow be not required；In sample states or injection state, go back original reagent, colour reagent, buffer solution, the flow of current-carrying and water sample
It is identical with the flow for the pump (main pump or auxiliary pump) that it is flowed through.
According to method of the present invention, the temperature of the reduction reaction is normal temperature, and the reduction reaction time flows through for reagent
The time of whole reduction reaction coil pipe, it is determined by the length of reduction reaction coil pipe；
The temperature of the chromogenic reaction be normal temperature, the chromogenic reaction time be reagent flow through whole chromogenic reaction coil pipe when
Between, it is determined by the length of chromogenic reaction coil pipe.The flow injection analysis of the present invention is carried out under non-equilibrium condition, right
Whether reaction does not require completely, as long as ensureing that sensitivity and reappearance reach technical requirements.
According to method of the present invention, it is preferable that the sampling volume is 200-800 μ L.
According to method of the present invention, it is preferable that the concentration of the go back original reagent aqueous ascorbic acid is 5-25mg/
L。
According to method of the present invention, it is preferable that described 2,4,6- tri- (2- pyridine radicals) -1,3,5-triazines aqueous solution show
The concentration of color reagent is 10-40mg/L.
According to method of the present invention, it is preferable that the buffer solution is acetic acid-ammonium acetate buffer solution.
According to method of the present invention, it is preferable that the pH value of the water sample is 2.0-4.5.
According to method of the present invention, it is preferable that methods described comprises the following steps：
A, sampling process：Water sample enters sampling ring by auxiliary pump driving through eight channel sample valves by the road, meanwhile, auxiliary pump driving
The go back original reagent that current-carrying drives via eight channel sample valves with main pump is collected in composite module, passes through after reduction reaction coil pipe,
The colour reagent and the mixed solution of buffer solution driven with main pump flows through chromogenic reaction coil pipe and enters inspection after composite module collects
Survey device to be detected, detection signal carries out real-time data acquisition and processing by work station, obtains background signal；
B, injection process：After the completion of sampling process, current-carrying promotes water sample after composite module is mixed with go back original reagent, stream
Reduction reaction is carried out through reduction reaction coil pipe, then with the mixed solution of colour reagent and buffer solution after composite module collects, stream
Chromogenic reaction is carried out through chromogenic reaction coil pipe, after chromogenic reaction terminates, is detected into detector.
According to method of the present invention, it is preferable that the detector is UV-vis spectroscopy detector；
The light path of more preferably described UV-vis spectroscopy detector is 10-50mm, and pond body product is 10-100 μ L.
According to method of the present invention, it is preferable that methods described also includes walking baseline process before sampling process：Current-carrying
Through eight channel sample valves enter sampling ring by auxiliary pump driving by the road, meanwhile, auxiliary pump drive current-carrying via eight channel sample valves with
Main pump driving go back original reagent collect in composite module, pass through after reduction reaction coil pipe, with main pump drive colour reagent and
The mixed solution of buffer solution flows through chromogenic reaction coil pipe and detected into detector after composite module collects, and detects signal
Real-time data acquisition and processing, the background signal stablized (signal shown on work station recorder) are carried out by work station.
According to method of the present invention, it is preferable that the length of the reduction reaction coil pipe is 6-160cm；
The length of more preferably described reduction reaction coil pipe is 5-20cm.
According to method of the present invention, it is preferable that the length of the chromogenic reaction coil pipe is 100-390cm, internal diameter is
0.5mm。
According to method of the present invention, it is preferable that the internal diameter of the pipeline is 0.5mm.
According to method of the present invention, it is preferable that the main pump is peristaltic pump；The pump line internal diameter of the main pump is 0.5-
1.5mm, rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min.
According to method of the present invention, it is preferable that the auxiliary pump is peristaltic pump, and the pump line internal diameter of the 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 automatic quick determination method of trace iron ions trace in Power Plant Water Vapor in above-mentioned Power Plant Water Vapor
Measure the application in iron ion detection.Wherein, described " iron " is the full iron in Power Plant Water Vapor.
In summary, the invention provides the automatic quick determination method of trace iron ions and system in a kind of Power Plant Water Vapor.
Flow injection (FIA) analytical technology and light splitting detection technique are successfully applied in Power Plant Water Vapor (or other aqueous systems) by the present invention
In the automatic detection of trace iron ions；FIA technologies have high sample treatment efficiency, while height reproduction can also be carried out
Automation mechanized operation, and then this method can be made to be carried out in a kind of online, closed analysis system, it is to avoid in manual operations
The multiple transfer of sample in a reservoir, so as to greatly reduce human error, and saves sample and reaction reagent, it is seen that the party
Method operation more facilitates, succinctly, improves the reliability and accuracy of detection data.
In addition, the automatic quick determination method of trace iron ions and system have filled up water in Power Plant Water Vapor provided by the present invention
The blank of middle trace iron ions chemical analysis automatic technology, is that the development of underwater trace iron ion on-Line Monitor Device is established
Solid method basis, with great scientific research value and actual application value.
The automatic quick determination method of trace iron ions in the Power Plant Water Vapor of the present invention and system are applied in Power Plant Water Vapor
The detection of trace iron ions, it is possible to achieve trace iron ions are automatic, quick in Power Plant Water Vapor, accurately and reliably determine, detection limit
For 0.5 μ g/L.
Brief description of the drawings
Fig. 1 is (initial for the automatic embodiment of rapid detection system one of trace iron ions in the Power Plant Water Vapor of the present invention
State)；
Fig. 2 is the automatic embodiment of rapid detection system one of trace iron ions (work in the Power Plant Water Vapor of the present invention
State)；
Fig. 3 is (initial for the automatic embodiment of rapid detection system one of trace iron ions in the Power Plant Water Vapor of the present invention
State) under eight channel sample valves specific annexation schematic diagram；
Fig. 4 is the automatic embodiment of rapid detection system one of trace iron ions (work in the Power Plant Water Vapor of the present invention
State) under eight channel sample valves specific annexation schematic diagram；
Fig. 5 is respectively holds on the composite module in the Power Plant Water Vapor of the present invention used in the automatic rapid detection system of trace iron ions
The schematic diagram of mouth；
Fig. 6 is the standard working curve figure of iron ion in test case of the present invention；
Fig. 7 is detection signal spectrogram when trace iron ions in Power Plant Water Vapor are determined using the method for the present invention.
Main Reference label declaration
The passage of 6 auxiliary pump of go back original reagent bottle 1 colour reagent bottle 2 buffer solutions bottle 3 current-carrying bottle 4 water samples, 5 main pump of bottle 7 eight
The reduction reaction of 12 chromogenic reaction coil pipe of sampling valve 8 flow injection analyzer, 9 composite module, 10 Y-type three way type, 11 sampling ring 13
The discharging of waste liquid end 18 of 14 detector of coil pipe, 15 work station, 16 first discharging of waste liquid end 17 second；
Eight channel sample valves 8 include 16 ports, i.e. outer ring first port d1, outer ring second port d2, outer ring the 3rd
Port d3, the port d4 of outer ring the 4th, outer ring fifth port d5, the port d6 of outer ring the 6th, the port d7 of outer ring the 7th and outer ring the 8th
Port d8；
Inner ring first port e1, inner ring second port e2, the port e3 of inner ring the 3rd, the port e4 of inner ring the 4th, inner ring the 5th
Port e5, the port e6 of inner ring the 6th, the port e7 of inner ring the 7th and the port e8 of inner ring the 8th；
Composite module 10 includes six ports：That is first port c1, second port c2, the 3rd port c3, the 4th port c4,
Fifth port c5, the 6th port c6.
Embodiment
The beneficial of the implementation process and generation of specific embodiment and the Figure of description detailed description present invention will be passed through below
Technique effect, it is intended to help reader to be best understood from the essence and feature of the present invention, but not as can practical range to this case
Restriction.
1st, equipment
The automatic rapid detection system of trace iron ions in a kind of Power Plant Water Vapor is present embodiments provided, wherein, the system bag
Include：Go back original reagent bottle 1, colour reagent bottle 2, buffer solution bottle 3, current-carrying bottle 4, water sample bottle 5, flow injection analyzer 9, composite module
10th, Y-type three way type 11, chromogenic reaction coil pipe 13, reduction reaction coil pipe 14, detector 15, work station 16, the first discharging of waste liquid end 17
And the second discharging of waste liquid end 18；
Wherein described flow injection analyzer 9 includes main pump 6, auxiliary pump 7, eight channel sample valves 8 and sampling ring 12；
Wherein described eight channel samples valve 8 includes 16 ports, i.e. outer ring first port d1, outer ring second port d2,
The port d3 of outer ring the 3rd, the port d4 of outer ring the 4th, outer ring fifth port d5, the port d6 of outer ring the 6th, the port d7 of outer ring the 7th and
The port d8 of outer ring the 8th；
Inner ring first port e1, inner ring second port e2, the port e3 of inner ring the 3rd, the port e4 of inner ring the 4th, inner ring the 5th
Port e5, the port e6 of inner ring the 6th, the port e7 of inner ring the 7th and the port e8 of inner ring the 8th；
The composite module 10 includes six ports：That is first port c1, second port c2, the 3rd port c3, the 4th end
Mouth c4, fifth port c5, the 6th port c6, the schematic diagram of each port of composite module are as shown in Figure 5；
Wherein, when the system is in sample states (state diagram is as shown in Figure 1, Figure 3), the go back original reagent bottle 1 passes through
Pipeline is connected via main pump 6 with the first port c1 of composite module 10；
Colour reagent bottle 2, buffer solution bottle 3 by pipeline via main pump 6 after Y-type three way type 11 converges again by pipeline
It is connected with the fifth port c5 of composite module 10；
The current-carrying bottle 4 is connected by pipeline via auxiliary pump 7 with the outer ring second port d2 of eight channel sample valves 8, and eight lead to
The inner ring second port e2 of road sampling valve 8 is connected by pipeline with the port e8 of inner ring the 8th, the outer ring the 8th of eight channel sample valves 8
Port d8 is connected by pipeline with the second port c2 of composite module 10；
The water sample bottle 5 is connected by pipeline via auxiliary pump 7 with the port d7 of outer ring the 7th of eight channel sample valves 8, and eight lead to
The port e7 of inner ring the 7th of road sampling valve 8 is connected by sampling ring 12 with inner ring first port e1；
4th port c4 of the composite module 10 passes through reduction reaction coil pipe 14 and the 3rd port c3 of composite module 10
It is connected；
6th port c6 of the composite module 10 is connected by pipeline with the entrance of chromogenic reaction coil pipe 13, chromogenic reaction
The outlet of coil pipe 13 is connected by pipeline with detector 15；
When the system is in injection state (state diagram is as shown in Figure 2, Figure 4 shows), the go back original reagent bottle 1 is passed through by pipeline
It is connected by main pump 6 with the first port c1 of composite module 10；
Colour reagent bottle 2, buffer solution bottle 3 by pipeline via main pump 6 after Y-type three way type 11 converges again by pipeline
It is connected with the fifth port c5 of composite module 10；
The current-carrying bottle 4 is connected by pipeline via auxiliary pump 7 with the outer ring second port d2 of eight channel sample valves 8, and eight lead to
The inner ring first port e1 of road sampling valve 8 is connected with the port e7 of inner ring the 7th by the road again by pipeline via sampling ring 12, and eight
The port d8 of outer ring the 8th of channel sample valve 8 is connected by pipeline with the second port c2 of composite module 10；
The water sample bottle 5 is connected by pipeline via auxiliary pump 7 with the port d7 of outer ring the 7th of eight channel sample valves 8；
4th port c4 of the composite module 10 passes through reduction reaction coil pipe 14 and the 3rd port c3 of composite module 10
It is connected；
6th port c6 of the composite module 10 is connected by pipeline with the entrance of chromogenic reaction coil pipe 13, chromogenic reaction
The outlet of coil pipe 13 is connected by pipeline with detector 15；
The first discharging of waste liquid end 17 is connected by pipeline with the detector 15；The second discharging of waste liquid end 18 leads to
Outer ring first port d1, inner ring sixth port e6 of the pipeline respectively with eight channel sample valves 8 is crossed to be connected；
The work station 16 is electrically connected with detector 15；
The internal diameter of the pipeline is 0.5mm；
The length of the reduction reaction coil pipe 14 is 6-160cm；
The length of the chromogenic reaction coil pipe 13 is 100-390cm, and internal diameter is 0.5mm；
The detector 15 is UV-vis spectroscopy detector；The light path of the UV-vis spectroscopy detector is 10-
50mm, pond body product is 10-100 μ L；
The 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, 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。
2nd, analysis process
According to the automatic rapid detection system of trace iron ions in the Power Plant Water Vapor that provides of the present invention establish flow injection-point
Light photometric analysis system.The system can carry out the programming of operation sequence, setting pump speed, flow etc., sample " sampling " and " note
Enter " automatically switch by setup program, realize the Automated condtrol of whole pipe-line system.
Walk baseline process：Flow chart is as shown in figure 1, eight channel sample valves are in " sampling " state (original state), current-carrying
Through eight channel sample valves enter sampling ring by auxiliary pump driving by the road, meanwhile, auxiliary pump drive current-carrying via eight channel sample valves with
Main pump driving go back original reagent collect in composite module, pass through after reduction reaction coil pipe, with main pump drive colour reagent and
Buffer solution mixed solution (before composite module collects, colour reagent and buffer solution driven through main pump after first in Y-type three way type
In converge) after composite module collects, flow through chromogenic reaction coil pipe and detected into detector, detection signal entered by work station
Row real-time data acquisition and processing, the background signal stablized (signal shown on work station recorder)；
Sampling process：Flow chart is as shown in figure 1, eight channel sample valves are in " sampling " state (original state), water sample warp
Pipeline is driven by auxiliary pump enters sampling ring through eight channel sample valves, meanwhile, auxiliary pump drives current-carrying via eight channel sample valves and master
The go back original reagent of pump driving is collected in composite module, passes through after reduction reaction coil pipe, the colour reagent that is driven with main pump and slow
The mixed solution of fliud flushing flows through chromogenic reaction coil pipe and detected into detector after composite module collects, detection signal by
Work station carries out real-time data acquisition and processing, obtains background signal；
Injection and detection process：After the completion of sampling process, eight channel sample valves are automatically brought to " injection " state (work shape
State), flow chart is as shown in Fig. 2 current-carrying promotion water sample flows through reduction reaction coil pipe and entered after composite module is mixed with go back original reagent
Row reduction reaction, then flow through chromogenic reaction coil pipe (interior after composite module collects with the mixed solution of colour reagent and buffer solution
Footpath is 0.5mm) chromogenic reaction is carried out, after chromogenic reaction terminates, detected into detector, waste liquid is discharged into waste liquid barrel.It is whole
Iron concentration detection signal is acquired in real time by work station in individual " injection " state, water sample；
Current-carrying used is high purity water, and its resistivity is 18.3M Ω；
Colour reagent used is 2,4,6- tri- (2- pyridine radicals) -1,3,5- triazine aqueous solution；
Go back original reagent used is aqueous ascorbic acid；
Buffer solution used is acetic acid-ammonium acetate buffer solution.
Embodiment is shown in Table 1：
The embodiment of table 1
| 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 detector light path (mm) | 10 | 20 | 30 |
| UV-vis spectroscopy detector cell volume (μ L) | 12 | 40 | 60 |
Test example
1st, the measure of standard working curve
Under the experiment condition of embodiment 1, a series of ferric ion standards have been prepared in the range of 0.5-80 μ g/L
Solution, determines the standard working curve in this concentration range, as a result as shown in fig. 6, from fig. 6 it can be seen that working curve
The concentration of peak height and standard liquid iron ion be in good linear relationship.Trace in Power Plant Water Vapor is determined using the method for the present invention
Detection signal spectrogram when measuring iron ion is as shown in Figure 7.
2nd, the measure of reappearance
Parallel determination more than 7 times is distinguished to 5.0 μ g/L and 50 μ g/L iron ion standard liquid, to the reappearance of this method
It is determined, measurement result is shown in Table 2.The relative standard deviation difference of 5.0 μ g/L and 50 μ g/L iron ion standard liquids
For 0.69% and 0.74%, the relative standard deviation of the two is respectively less than 1.0%, it can be seen that, the reappearance of this method is good.
The reappearance measurement result of table 2
3rd, the measure of lower limit is detected
In this method, detection limit refers under the peak height for the analyte being clearly discernible on work station signal record figure
Limit, it is generally recognized that the response signal peak height that be able to be distinguished, minimum should be 3 times of baseline noise, the corresponding analyte of this signal
Concentration.
The detection of this method is limited to：C=0.5 μ g/L.
Other performance indications of this method are shown in Table 3.
The performance indications of this method of table 3
| Sequence number | Performance indications | Control standard | 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 drift | <0.002AU/h | <0.002AU/h |
| 9 | Analyze speed | 60 | 60s/ samples |
4th, practical application
The trace iron content in some Power Plant Water Vapor samples is determined using this project approach, measurement result is shown in Table
Shown in 4.
The measure of the rate of recovery of table 4
As can be seen from Table 4, the measured value of the rate of recovery is in the range of 90-110%, this show in water sample it is other from
Son, pH value etc. do not form interference to detection, demonstrate the accuracy and reliability of this method.
Claims (24)
1. the automatic quick determination method of trace iron ions in a kind of Power Plant Water Vapor, it is characterised in that methods described is to use power plant
The automatic rapid detection system of trace iron ions realizes that this method uses water by Flow Injection-Spectrophotometry method in steam, its
In, sampling volume is 30-1000 μ L；
Go back original reagent used is aqueous ascorbic acid, and concentration is 1-50mg/L；
Colour reagent used is 2,4,6- tri- (2- pyridine radicals) -1,3,5-triazines aqueous solution, and concentration is 1-50mg/L；
Buffer solution used is the buffer solution that pH value is 2.5-3.5；
The pH value of water sample used is 2.0-7.0；
Current-carrying used is high purity water；
Wherein, the automatic rapid detection system of trace iron ions includes go back original reagent bottle (1), colour reagent bottle in the Power Plant Water Vapor
(2), buffer solution 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 detector (15)；Wherein described flow injection analyzer (9)
Including main pump (6), auxiliary pump (7), eight channel sample valves (8) and sampling ring (12)；
Wherein, when the system is in sample states, the go back original reagent bottle (1) is by pipeline via main pump (6) and combination die
The first port (c1) of block (10) is connected；
The colour reagent bottle (2), buffer solution bottle (3) are passed through again by pipeline via main pump (6) after Y-type three way type (11) converges
Pipeline is connected with the fifth port (c5) of composite module (10)；
The current-carrying bottle (4) is connected by pipeline via auxiliary pump (7) with the outer ring second port (d2) of eight channel sample valves (8),
The inner ring second port (e2) of eight channel sample valves (8) is connected by pipeline with the port (e8) of inner ring the 8th, eight channel sample valves
(8) the port (d8) of outer ring the 8th is connected by pipeline with the second port (c2) of composite module (10)；
The water sample bottle (5) is connected by pipeline via auxiliary pump (7) with the port (d7) of outer ring the 7th of eight channel sample valves (8),
The port (e7) of inner ring the 7th of eight channel sample valves (8) is connected via sampling ring (12) with inner ring first port (e1)；
The 3rd end that 4th port (c4) of the composite module (10) passes through reduction reaction coil pipe (14) and composite module (10)
Mouth (c3) is connected；
6th port (c6) of the composite module (10) is connected by pipeline with the entrance of chromogenic reaction coil pipe (13), and colour developing is anti-
The outlet of coil pipe (13) is answered to be connected by pipeline with detector (15)；
When the system is in injection state, the go back original reagent bottle (1) is by pipeline via main pump (6) and composite module (10)
First port (c1) be connected；
The colour reagent bottle (2), buffer solution bottle (3) are passed through again by pipeline via main pump (6) after Y-type three way type (11) converges
Pipeline is connected with the fifth port (c5) of composite module (10)；
The current-carrying bottle (4) is connected by pipeline via auxiliary pump (7) with the outer ring second port (d2) of eight channel sample valves (8),
The inner ring first port (e1) of eight channel sample valves (8) is connected via sampling ring (12) with the port (e7) of inner ring the 7th, eight passages
The port (d8) of outer ring the 8th of sampling valve (8) is connected by pipeline with the second port (c2) of composite module (10)；
The water sample bottle (5) is connected by pipeline via auxiliary pump (7) with the port (d7) of outer ring the 7th of eight channel sample valves (8)；
The 3rd end that 4th port (c4) of the composite module (10) passes through reduction reaction coil pipe (14) and composite module (10)
Mouth (c3) is connected；
6th port (c6) of the composite module (10) is connected by pipeline with the entrance of chromogenic reaction coil pipe (13), and colour developing is anti-
The outlet of coil pipe (13) is answered to be connected by pipeline with detector (15).
2. according to the method described in claim 1, it is characterised in that the sampling volume is 200-800 μ L.
3. according to the method described in claim 1, it is characterised in that go back original reagent used is aqueous ascorbic acid, concentration
For 5-25mg/L.
4. according to the method described in claim 1, it is characterised in that colour reagent used be 2,4,6- tri- (2- pyridine radicals)-
The 1,3,5-triazines aqueous solution, concentration is 10-40mg/L.
5. according to the method described in claim 1, it is characterised in that the buffer solution is acetic acid-ammonium acetate buffer solution.
6. according to the method described in claim 1, it is characterised in that the pH value of water sample used is 2.0-4.5.
7. according to the method described in claim 1, it is characterised in that methods described comprises the following steps：
A, sampling process：Water sample enters sampling ring by auxiliary pump driving through eight channel sample valves by the road, meanwhile, auxiliary pump driving current-carrying
The go back original reagent driven via eight channel sample valves with main pump is collected in composite module, passes through after reduction reaction coil pipe, with master
The colour reagent of pump driving and the mixed solution of buffer solution flow through chromogenic reaction coil pipe and enter detector after composite module collects
Detected, detection signal carries out real-time data acquisition and processing by work station, obtains background signal；
B, injection process：After the completion of sampling process, current-carrying promotes water sample after composite module is mixed with go back original reagent, flows through also
Original reaction coil pipe carries out reduction reaction, then is flowed through aobvious after composite module collects with the mixed solution of colour reagent and buffer solution
Colour response coil pipe carries out chromogenic reaction, after chromogenic reaction terminates, is detected into detector.
8. method according to claim 7, it is characterised in that methods described also includes walking baseline mistake before sampling process
Journey：Current-carrying enters sampling ring by auxiliary pump driving through eight channel sample valves by the road, meanwhile, auxiliary pump driving current-carrying is adopted via eight passages
The go back original reagent that sample valve drives with main pump is collected in composite module, passes through after reduction reaction coil pipe, the colour developing driven with main pump
The mixed solution of reagent and buffer solution flows through chromogenic reaction coil pipe and detected into detector after composite module collects, inspection
Survey signal and real-time data acquisition and processing, the background signal stablized are carried out by work station.
9. method according to claim 7, it is characterised in that the length of the reduction reaction coil pipe is 6-160cm.
10. method according to claim 9, it is characterised in that the length of the reduction reaction coil pipe is 5-20cm.
11. method according to claim 7, it is characterised in that the length of the chromogenic reaction coil pipe is 100-390cm,
Internal diameter is 0.5mm.
12. method according to claim 7, it is characterised in that the internal diameter of the pipeline is 0.5mm.
13. the method according to claim any one of 1-12, it is characterised in that the detector is UV-vis spectroscopy
Detector.
14. method according to claim 13, it is characterised in that the light path of the UV-vis spectroscopy detector is 10-
50mm, pond body product is 10-100 μ L.
15. the method according to claim any one of 1-12, it is characterised in that the main pump is peristaltic pump；The main pump
Pump line internal diameter is 0.5-1.5mm, and rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min.
16. method according to claim 13, it is characterised in that the main pump is peristaltic pump；The pump line internal diameter of the main pump
For 0.5-1.5mm, rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min.
17. method according to claim 14, it is characterised in that the main pump is peristaltic pump；The pump line internal diameter of the main pump
For 0.5-1.5mm, rotating speed is 10-50r/min, and flow is 0.2-3.0mL/min.
18. the method according to claim any one of 1-12, it is characterised in that the auxiliary pump is peristaltic pump, the auxiliary pump
Pump line internal diameter is 0.5-1.5mm；Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
19. method according to claim 13, it is characterised in that the auxiliary pump is peristaltic pump, the pump line internal diameter of the auxiliary pump
For 0.5-1.5mm；Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
20. method according to claim 14, it is characterised in that the auxiliary pump is peristaltic pump, the pump line internal diameter of the auxiliary pump
For 0.5-1.5mm；Rotating speed is 30-60r/min, and flow is 1.0-3.0mL/min.
21. the method according to claim any one of 1-12, it is characterised in that the eight channel samples valve (8) is to adopt
Sample state can make water sample enter sampling ring (12) from bottom to top via auxiliary pump (7) by pipeline by water sample bottle (5), and current-carrying is by current-carrying
Bottle (4) by pipeline via auxiliary pump (7) and go back original reagent by go back original reagent bottle (1) by pipeline via main pump (6) in combination die
Block collects in (10), passes through after reduction reaction coil pipe (14), with colour reagent, buffer solution respectively by colour reagent bottle (2), slow
Fliud flushing bottle (3) is converged by pipeline in composite module (10) again after being collected by pipeline via main pump (6) in Y-type three way type (11)
Collection；
And current-carrying can be made to enter sampling ring from top to bottom via auxiliary pump (7) by pipeline by current-carrying bottle (4) in the state of injection
(12), then via pipeline enter composite module (10), with go back original reagent by go back original reagent bottle (1) by pipeline via main pump (6)
Collect in composite module (10), pass through after reduction reaction coil pipe (14), with colour reagent, buffer solution respectively by colour reagent
Bottle (2), buffer solution bottle (3) collected by pipeline via main pump (6) in Y-type three way type (11) after again by pipeline in composite module
(10) the eight channel sample valves collected in.
22. the method according to claim any one of 1-12, it is characterised in that in the Power Plant Water Vapor trace iron ions from
Dynamic rapid detection system also includes the first discharging of waste liquid end (17) and the second discharging of waste liquid end (18)；The first discharging of waste liquid end
(17) it is connected by pipeline with the detector (15)；The second discharging of waste liquid end (18) is adopted with eight passages respectively by pipeline
The outer ring first port (d1) of sample valve (8), the port (e6) of inner ring the 6th are connected.
23. the method according to claim any one of 1-12, it is characterised in that in the Power Plant Water Vapor trace iron ions from
Dynamic rapid detection system also includes work station (16), and the work station (16) electrically connects with detector (15).
24. the automatic quick determination method of trace iron ions is in Water of Power Plant in the Power Plant Water Vapor described in claim 1-23 any one
Application in vapour in trace iron ions detection.
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| CN106769954B (en) * | 2017-03-30 | 2024-02-02 | 华北电力科学研究院有限责任公司 | Automatic rapid analysis method and system for trace/trace chloride ions in water vapor of power plant |
| CN109752375A (en) * | 2019-03-18 | 2019-05-14 | 天津市环境保护科学研究院 | A kind of device and method of real-time detection ferrous ion concentration |
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| CN112179861A (en) * | 2020-11-15 | 2021-01-05 | 西安热工研究院有限公司 | Online trace iron determination device and method based on phenanthroline spectrophotometry |
| CN112945953B (en) * | 2021-02-05 | 2024-03-01 | 南京工业大学 | Flow path system of continuous flow turbidimetry analyzer |
| CN113567376A (en) * | 2021-07-29 | 2021-10-29 | 北京京能电力股份有限公司 | Device and method for measuring concentration of trace iron ions in water vapor of power plant |
| CN114036756A (en) * | 2021-11-10 | 2022-02-11 | 西安热工研究院有限公司 | Method and device for evaluating furnace shutdown protection anti-corrosion effect of thermal power generating unit |
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| CN205080143U (en) * | 2015-11-11 | 2016-03-09 | 华北电力科学研究院有限责任公司 | Automatic quick detecting system of trace iron ion in power plant's steam |
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