CN206583798U - The automatic quick analysis system of micro in Power Plant Water Vapor/trace chloro ion - Google Patents
The automatic quick analysis system of micro in Power Plant Water Vapor/trace chloro ion Download PDFInfo
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- CN206583798U CN206583798U CN201720322404.1U CN201720322404U CN206583798U CN 206583798 U CN206583798 U CN 206583798U CN 201720322404 U CN201720322404 U CN 201720322404U CN 206583798 U CN206583798 U CN 206583798U
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000004458 analytical method Methods 0.000 title claims abstract description 38
- 238000005070 sampling Methods 0.000 claims abstract description 61
- 239000002131 composite material Substances 0.000 claims abstract description 33
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 23
- 238000004401 flow injection analysis Methods 0.000 claims abstract description 10
- 230000008676 import Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 13
- 239000002699 waste material Substances 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 description 43
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- 238000004587 chromatography analysis Methods 0.000 description 18
- 229920001895 acrylonitrile-acrylic-styrene Polymers 0.000 description 15
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- 241000370738 Chlorion Species 0.000 description 14
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 13
- 229910052801 chlorine Inorganic materials 0.000 description 13
- 239000000460 chlorine Substances 0.000 description 13
- 238000005342 ion exchange Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- LJBWEZVYRBKOCI-UHFFFAOYSA-N 2,4,6-triaminoquinazoline Chemical compound N1=C(N)N=C(N)C2=CC(N)=CC=C21 LJBWEZVYRBKOCI-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 7
- 150000001450 anions Chemical class 0.000 description 7
- 239000012498 ultrapure water Substances 0.000 description 7
- 238000002798 spectrophotometry method Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000011088 calibration curve Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 230000002572 peristaltic effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- 238000004255 ion exchange chromatography Methods 0.000 description 3
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- 241000628997 Flos Species 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model provides the automatic quick analysis system of micro/trace chloro ion in a kind of Power Plant Water Vapor, it includes current-carrying bottle, reaction reagent bottle, water sample bottle, flow injection analyzer, composite module, sampling ring, react coil pipe and detector, wherein, the flow injection analyzer includes A pumps, B pumps and sampling valve, water sample bottle is connected by pipeline via B pumps with sampling valve, current-carrying bottle is connected by pipeline via A pumps with sampling valve, composite module sets at least two entrances and one outlet, reaction reagent bottle is connected by pipeline via the entrance of A pumps and composite module, sampling valve is connected by another entrance of pipeline and composite module, the outlet of composite module is connected by pipeline with reacting the entrance of coil pipe, the outlet of reaction coil pipe is connected by pipeline with detector, the import and export of the sampling ring are connected by pipeline with sampling valve respectively；The composite module and reaction coil pipe are located in insulating box.
Description
Technical field
The utility model is related to the detection of Power Plant Water Vapor, specifically, be related to a kind of micro in Power Plant Water Vapor/trace amounts of chlorine from
Sub automatic quick analysis system.
Background technology
Chlorion is that one of anion of maximum is endangered in generating set water-steam system, and trace level chlorion is contained in steam
The integrality of unit thermodynamic system metal inner surface oxide film can be destroyed, causes system corrosion to destroy, jeopardizes generating set
Safety economy stable operation.Domestic standard《GB-T12145-2016 thermal power generation units and apparatus of steam power plants Water Vapor Quality》It is right
Micro and trace chloro ion content is determined in the steam such as different capabilities, the boiler water of different types generating set, feedwater, steam
Specific control range requirement.Therefore, it is very to carry out accurate detection to micro, trace level chloride ion content in Power Plant Water Vapor
It is necessary.
At present, the chromatography of ions is usually used in determining the chlorion of micro in water and trace level.In power industry, chromatography of ions
Method is usually used in determining the trace chloro ion in unit steam, and the measure of trace chlorine uses AAS or electrode method,
The chlorine ion content determination of constant then uses mole titration.
At present, trace chlorine is carried out using methods such as the chromatography of ions, mercuric thiocyanate AASs more than this area
Measurement, but be present many drawbacks in these measuring methods, be specifically described as follows：
The chromatography of ions：
Chromatography of ions is a kind of pattern of high performance liquid chromatography, and it is mainly used in anion, cation analysis detection.From
Sub- chromatography is selectively good, and sensitivity is high, and multicomponent can be determined simultaneously.Ion chromatograph by mobile phase translator unit, splitter,
Detector and the part of data processing equipment four composition.Sulfate by ion chromatography chlorion generally comprises following steps：Determine first
The standard sample solution of known composition and concentration, generates calibration curve, then analyze by necessary pre-treatment by data handling system
Sample solution, its result and the calibration curve that is previously generated be compared by final data processing system, complete it is quantitative calculate,
Obtain the analysis result of sample.
One of critical component of chromatography of ions (IC) is splitter.Splitter is the retention characteristic that basis treats measured ion,
By the exchange column of detected ion isolation before detection.Analysis of the chromatography of ions to anion is one in analytical chemistry new prominent
It is broken, its can simultaneously, it is sensitive and determine a variety of anion exactly, 7 kinds of Common Anions can be typically completed in 15-30min
(F-、Cl-、NO3 -、Br-、NO2 -、PO4 3-、SO4 2-) and 6 kinds of Common Cations (Li+、Na+、NH4 +、K+、Mg2+、Ca2+) analysis.
The concentration range of ion chromatography is μ g/L-mg/L, and sampling volume is smaller, is less than 10 μ g/ to the detection limit of Common Anions
L, by optimizing analysis system and analysis condition, test limit is up to 10-12G/L or lower.
But, the chromatography of ions is there is also shortcomings, such as：
(1) system complex；
(2) maintenance workload is big；
(3) because of its system complex, to use environment and operation level requirement it is higher, so be more applicable for scientific research with experiment
The detection and analysis of room, and be not suitable for industry spot detection and analysis immediately or on-line monitoring analysis；
(4) instrument price is expensive.
Mercuric thiocyanate AAS：
Mercuric thiocyanate AAS is the classical analysis method for determining chlorion in water,《DL/T 1203-2013 sulphur
Mercuric cyanate-AAS》In standard, this method is Manual analysis method, and detection range is 25 μ g/L-1000 μ g/L.
Flow injection-mercuric thiocyanate AAS：
Flow injection-mercuric thiocyanate AAS can also determine trace chlorine content, this method in power plant's stove water
For autoanalyzer method, detection lower limit is 20 μ g/L.
Flow injection-ON-LINE ION-EXCHANGE preenrichment-AAS：
Flow injection-ON-LINE ION-EXCHANGE preenrichment-AAS can also determine trace chloro ion in Power Plant Water Vapor,
The detection lower limit of this method is 1.0 μ g/L, and analysis efficiency is 2-6 samples/hour.
Other detection methods：
The A of patent CN 102156101 disclose the method for continuous measuring and device of trace chloro ion in a kind of high purity water, its
Action principle is to take a certain amount of water sample to flow through specific device (built-in ion exchange resin), and chlorion is quantitatively enriched in resin
On, then select tens times smaller than volume of water sample certain solution to elute it from resin, so as to reach enrichment concentration chlorine
The purpose of ion, is then directly measured with spectrophotometer to the chlorion in concentration sample.
Concrete technical scheme is, in the high purity water continuous measuring device of trace chloro ion include water sample enrichment facility and with
Connection photodetector system, concentration systems are enriched with the chlorion of trace in high-purity water sample based on ion exchange principle.Work as water
When sample chloride ion content is more than 20 μ g/L, water sample is directly entered photodetector system and measured；Chloride Ion In Water content is small
When 20 μ g/L, system carries out the concentration of Chloride Ion In Water, elution by enrichment facility is automatically switched to, and eluent enters photoelectricity
System is measured, so that the Monitoring lower-cut of chlorion is down to below 1.0 μ g/L.
The detection lower limit of this method detection trace chlorine is 20 μ g/L, and the detection lower limit of detection trace chloro ion is less than
Time needed for 1.0 μ g/L, but one sample of enrichment, analysis efficiency was low at 1 more than hour.
In summary, at present, determining trace chlorine (100-1000 μ g/L) in Power Plant Water Vapor can be using mercuric thiocyanate point
Light photometry.In mercuric thiocyanate spectrophotometric method determines the research application of trace chlorine in water, flow injection-light splitting
The detection lower limit of photometry and continuous flowing colorimetric method is minimum, is 20 μ g/L.And the chlorion in water below 20 μ g/L needs to adopt
With sulfate by ion chromatography, chromatography of ions Monitoring lower-cut can reach below 1.0 μ g/L.In recent years, using Ion-exchange pretreatment
Method, flows with reference to flow injection-AAS or continuously AAS, can also realize to the automatic of underwater trace chlorion
Detection, detection lower limit is in below 1.0 μ g/L.It is worth noting that, the chromatography of ions, Ion-exchange pretreatment-continuous dynamic method
With trace chloro ion in flow injection-Ion-exchange pretreatment-water by Spectrophotometry, its analysis efficiency is 2-6 samples/small
When, analysis efficiency is relatively low, and the chromatography of ions is lab analysis detection method, Ion-exchange pretreatment-continuous dynamic method and
Flow injection-Ion-exchange pretreatment-AAS can realize on-line monitoring, but practical application effect is also unsatisfactory.
Utility model content
The purpose of this utility model is that provide a kind of micro in Power Plant Water Vapor/trace chloro ion quickly analyzes system automatically
System.
For up to above-mentioned purpose, the utility model provides micro/trace chloro ion in a kind of Power Plant Water Vapor and quickly divided automatically
Analysis system, it include current-carrying bottle 1, reaction reagent bottle 2, water sample bottle 3, flow injection analyzer 13, composite module 7, sampling ring 8,
Coil pipe 9 and detector 10 are reacted,
Wherein, the flow injection analyzer 13 includes A pumps 4, B pumps 5 and sampling valve 6, and water sample bottle 3 is by pipeline via B
Pump 5 is connected with sampling valve 6, and current-carrying bottle 1 is connected by pipeline via A pumps 4 with sampling valve 6, and composite module 7 sets at least two to enter
Mouth and one outlet, reaction reagent bottle 2 are connected by pipeline via A pumps 4 with the entrance of composite module 7, and sampling valve 6 passes through pipeline
It is connected with another entrance of composite module 7, the outlet of composite module 7 is connected by pipeline with reacting the entrance of coil pipe 9, reaction tray
The outlet of pipe 9 is connected by pipeline with detector 10, and the import and export of the sampling ring 8 are connected by pipeline with sampling valve 6 respectively；
The composite module 7 and reaction coil pipe 9 are located in insulating box 11.
According to the utility model specific embodiment, wherein the flow injection analyzer 13 is provided with control module,
It can be controlled programming and pump and sampling valve are automatically controlled by predetermined method operating procedure step with realizing.
According to the utility model specific embodiment, it is preferable that the system also includes work station 14, the work station 14
Electrically connected through the control module 13 with detector 10.Work station used in the utility model is the conventional equipment of this area,
It can be used for the testing result of detector is processed and displayed, it might even be possible to carry out the defeated of data by alternating interface between man and computer
Enter to be controlled the equipment such as detector.
According to the utility model specific embodiment, it is preferable that the system also includes discharging of waste liquid end 12, the waste liquid
Discharge end 12 is connected by pipeline with detector 10.
In described system, it is preferable that the sampling valve 6 is that in sample states water sample can be made to be passed through by water sample bottle 3
Pipeline can be such that current-carrying is adopted by current-carrying bottle 1 by pipeline via the entrance of A pumps 4 via the entrance sampling ring 8 of B pumps 5, and in injection state
Sample ring 8 simultaneously promotes the water sample in sampling ring 8 to enter composite module 7 via pipeline, and pipe is passed through by reaction reagent bottle 2 with reaction reagent
The sampling valve 6 that road is collected via A pumps 4 into composite module 7.
In described system, it is preferable that the sampling valve 6 is the groove Single-channel Rolling valve of six hole three or the hole of eight passage 16
Multifunctional rotary valve.
In described system, it is preferable that the length of the reaction coil pipe 9 is 100-500cm, and internal diameter is 0.5-1.5mm.
In described system, it is preferable that the internal diameter of the pipeline is 0.5-1.5mm.It is understood that described here
Pipeline be whole pipelines for connecting between each component of the utility model, i.e., the pipeline that water sample, current-carrying and reaction reagent are flowed through.
In described system, it is preferable that the detector 10 is photometric detector, its flow cell is constant temperature flow cell,
The flow cell light path is 5-50mm, and flow cell light path aperture is 1.0-3.0mm.Detector makes for this area used in the utility model
Conventional detector, the application is not improved to its structure, those skilled in the art can according to field operation needs,
With reference to the structure of photometric detector in the prior art, suitable photometric detector is selected, the utility model is only to the photometric detection
The parameters such as light path, the flow cell light path aperture of device flow cell are provided.
In described system, it is preferable that the pump speed of the A pumps is 10-50rpm, and flow is 0.5-5.0mL/min.
In described system, it is preferable that the pump speed of the B pumps is 10-80rpm, and flow is 1.0-10.0mL/min.Its
In, the A pumps, B pumps are peristaltic pump.
System described in the utility model goes for a variety of different methods and carries out micro/trace amounts of chlorine in Power Plant Water Vapor
Ion is quickly analyzed automatically, and in order to further be illustrated to system of the present utility model, the utility model additionally provides application
System of the present utility model is noted to the automatic rapid analysis method of micro/trace chloro ion in Power Plant Water Vapor, this method using flowing
- spectrophotometric analysis method is penetrated, wherein,
Sampling volume is 200-1000 μ L, and the flow of water sample is 1.0-10.0mL/min during sampling；
Calculated using the gross weight of the reaction reagent as 100%, it is less than 5.0% mercuric thiocyanate, concentration comprising concentration
High ferron less than 5.0%, and the reaction reagent is adjusted using aqueous solution of nitric acid or high chloro acid solution in process for preparation
PH value is less than 2.0, and surplus is high purity water；
The flow of the reaction reagent is 0.5-5.0mL/min, and the flow of current-carrying is 0.5-5.0mL/min；
The current-carrying is high purity water.
According to the utility model specific embodiment, it is preferable that this method specifically includes following steps：
Sampling process：Water sample drives sampled valve to enter sampling ring and discharged from floss hole by B pumps by the road；Meanwhile, carry
Stream drives combined module to converge by A pumps by the road with reaction reagent, enters after passing through reaction coil pipe into detector flow cell
Row detection, produced photosignal is gathered and handled in real time by work station, obtains background signal；
Injection process：After the completion of sampling process, current-carrying promotes the water sample in sampling ring to be tried in composite module with reaction
Enter reaction tray pipe after agent mixing, the mixed liquor after scattered, reaction, flows through detector flow cell and examined in reaction coil pipe
Survey, produced photosignal is gathered and handled in real time by work station.
In the analysis method, the length of the reaction coil pipe 9 is 100-500cm, and internal diameter is 0.5-1.5mm.
In the analysis method, the internal diameter of the pipeline is 0.5-1.5mm.
In the analysis method, the detector 10 is photometric detector, and its flow cell is constant temperature flow cell, the circulation
Pond light path is 5-50mm, and flow cell light path aperture is 1.0-3.0mm.
In the analysis method, the pump speed of the A pumps is 10-50rpm, and flow is 0.5-5.0mL/min.
In the analysis method, the pump speed of the B pumps is 10-80rpm, and flow is 1.0-10.0mL/min.
In the analysis method, the reaction carried out in reaction coil pipe is carried out at room temperature, and the constant room temperature is
Realized by insulating box.
In the analysis method, the utility model is not made specifically to the concentration of aqueous solution of nitric acid and high chloro acid solution
Ask, those skilled in the art can need reasonable selection aqueous solution of nitric acid and the concentration of high chloro acid solution according to field operation,
As long as the pH value of reaction reagent can be adjusted to be less than 2.0 by guarantee.
System and method provided by the utility model can be realized micro and trace chloro ion automatic in Power Plant Water Vapor
Quick analysis, is also easy to realize the analysis detection changed online；The actual detection lower limit of this method is 5.0 μ g/L, and analysis efficiency is
40-60 samples/hour, detection range is 5.0-2000 μ g/L, and good linear relation is presented between the absorbance and concentration of measure, and
And the Common Anions such as sulfate radical, the phosphate radical in Power Plant Water Vapor sample and pH value are not interfered with to this method.
Brief description of the drawings
The automatic quick analysis system one of micro/trace chloro ion is specific in the Power Plant Water Vapor that Fig. 1 provides for the utility model
Embodiment (sample states)；
The automatic quick analysis system one of micro/trace chloro ion is specific in the Power Plant Water Vapor that Fig. 2 provides for the utility model
Embodiment (injection state)；
Fig. 3 is trace chlorine standard working curve spectrum in FIA- water by Spectrophotometry provided by the utility model
Figure；
Fig. 4 is trace chlorine standard working curve in FIA- water by Spectrophotometry provided by the utility model.
Main Reference label declaration：
Current-carrying bottle 1, reaction reagent bottle 2, water sample bottle 3, A pumps 4, B pumps 5, sampling valve 6, composite module 7, sampling ring 8, reaction
Coil pipe 9, detector 10, insulating box 11, discharging of waste liquid end 12, flow injection analyzer 13, work station 14, a-f are respectively sampling
The first of valve 6 is to the 6th port.
Embodiment
Implementation process of the present utility model and having for producing are described in detail below by way of specific embodiment and Figure of description
Beneficial effect, it is intended to help reader to more fully understand essence of the present utility model and feature, not as can practical range to this case
Restriction.
Embodiment 1
A kind of automatic quick analysis system of micro in Power Plant Water Vapor/trace chloro ion is present embodiments provided, it includes：Carry
Flow bottle 1, reaction reagent bottle 2, water sample bottle 3, flow injection analyzer 13, composite module 7, sampling ring 8, reaction coil pipe 9 and detection
Device 10；
Wherein, the flow injection analyzer 13 includes A pumps 4, B pumps 5 and sampling valve 6；
The composite module 7 sets at least two entrances and one outlet；
When the system is in sample states, its schematic diagram is as shown in figure 1, from figure 1 it appears that water sample bottle 3 passes through
Pipeline is connected via B pumps (peristaltic pump) 5 with the first port a of sampling valve 6, and first port a is connected with second port b, sampling ring 8
Import and export be connected respectively by pipeline with second port b, the fifth port e of sampling valve 6, fifth port e and the 6th port f phases
Connect, and the 6th port f is leakage fluid dram；
Current-carrying bottle 1 is connected by pipeline via A pumps (peristaltic pump) 4 with the 4th port d of sampling valve 6, the 4th port d and the
Three port c are connected, and the 3rd port c of sampling valve 6 is connected by pipeline with an entrance of composite module 7, and reaction reagent bottle 2 leads to
Cross pipeline to be connected with another entrance of composite module 7 via A pumps 4, the outlet of composite module 7 passes through pipeline and reaction coil pipe 9
Entrance is connected, and the outlet of reaction coil pipe 9 is connected by pipeline with detector 10；
When the system is in injection state, its schematic diagram is as shown in Fig. 2 from figure 2 it can be seen that current-carrying bottle 1 passes through
Pipeline is connected via A pumps (peristaltic pump) 4 with the 4th port d of sampling valve 6, and the 4th port d is connected with fifth port e, sampling
The import and export of ring 8 are connected by pipeline with second port b, the fifth port e of sampling valve 6 respectively, second port b and the 3rd port
C is connected, and the 3rd port c of sampling valve 6 is connected by pipeline with an entrance of composite module 7, and reaction reagent bottle 2 is passed through by pipeline
It is connected by A pumps 4 with another entrance of composite module 7, the outlet of composite module 7 is connected by pipeline with reacting the entrance of coil pipe 9,
The outlet of reaction coil pipe 9 is connected by pipeline with detector 10；
The composite module 7 and reaction coil pipe 9 are located in insulating box 11；
The system also includes work station 14, and the work station 14 is electrically connected with detector 10；
The system also includes discharging of waste liquid end 12, and the discharging of waste liquid end 12 is connected by pipeline with detector 10；
The sampling valve 6 is the groove Single-channel Rolling valve of six hole three；
The detector 10 is photometric detector, and its flow cell is constant temperature flow cell, and the flow cell light path is 5-50mm, hole
Footpath is 1.0-3.0mm；
The pump speed of the A pumps is 15rpm, and flow is 2.5mL/min；
The pump speed of the B pumps is 50rpm, and flow is 3.0mL/min；
The length of the reaction coil pipe 9 is 450cm, and internal diameter is 0.5mm；
The internal diameter of the pipeline is 1.0mm.
Embodiment 2
A kind of automatic rapid analysis method of micro in Power Plant Water Vapor/trace chloro ion is present embodiments provided, it is to use
What the system that embodiment is provided was realized, this method comprises the following steps：
Sampling process：Water sample drives sampled valve to enter sampling ring and discharged from floss hole by B pumps by the road；Meanwhile, carry
Stream drives combined module to converge by A pumps by the road with reaction reagent, enters after passing through reaction coil pipe into detector flow cell
Row detection, produced photosignal is gathered and handled in real time by work station, obtains background signal；
Injection process：After the completion of sampling process, current-carrying promotes the water sample in sampling ring to be tried in composite module with reaction
Enter reaction tray pipe after agent mixing, the mixed liquor after scattered, reaction, flows through detector flow cell and examined in reaction coil pipe
Survey, produced photosignal is gathered and handled in real time by work station.
Wherein, sampling volume is 600 μ L；
Calculated using the gross weight of the reaction reagent as 100%, it includes the mercuric thiocyanate that concentration is 0.2%, concentration is
3.5% high ferron, and in process for preparation using certain density aqueous solution of nitric acid adjust the pH value of the reaction reagent to
1.65, surplus is high purity water；
The current-carrying is high purity water.
Test example
(1) measure of standard working curve
Compound concentration be respectively 5.0 μ g/L, 10 μ g/L, 20 μ g/L, 50 μ g/L, 100 μ g/L, 200 μ g/L, 400 μ g/L,
600 μ g/L and 800 μ g/L chlorion standard liquid, the system provided using the utility model embodiment 1, in above-mentioned experiment
Under the conditions of determine the corresponding detected value of each standard liquid (peak height absorbance), shown in measurement result as Fig. 3 and Fig. 4.
Trace chlorine standard working curve in the FIA- water by Spectrophotometry that the utility model embodiment 2 is provided
As shown in figure 4, figure 4, it is seen that its working curve is y=0.000019x+0.000307, r=0.9990.
(2) reappearance is determined
Parallel determination more than 7 times, the reproduction to this method are distinguished to 5.0 μ g/L and 100 μ g/L chlorion standard liquid
Property is determined, and measurement result is shown in Table 1.
Table 1
From table 1 it follows that concentration is respectively the relative standard of 5.0 μ g/L and 100 μ g/L chlorion standard liquid
Deviation is respectively 4.14% and 0.37%, and it shows：When standard liquid concentration is less than 10 μ g/L, relative standard deviation is less than 5.0%；
When standard liquid concentration is less than or equal to 100 μ g/L, relative standard deviation is less than 1.0%.As can be seen here, it is provided by the utility model
The reappearance of method is good.
(3) measure of lower limit is detected
Detection lower limit is calculated as follows：
In formula：S：For zero standard deviation, k：For calibration curve equation slope.
In the range of 5.0-1000 μ g/L, the calibration curve equation of measure is：
Y=0.000019x+0.000307；
To 5.0 μ g/L standard specimens replication 11 times, standard deviation s is：8.32×10-6AU。
It is computed, the detection lower limit of this method is：CL=1.31 μ g/L.
In terms of the actual test spectral data shown in Fig. 3, under optimal experiment condition, the actual detection of this method and system
Lower limit is 5.0 μ g/L.
Application examples
The method provided using the utility model embodiment 2 is to the micro and trace chloro ion in multiple Power Plant Water Vapor samples
Be determined, and by measurement result and use the chromatography of ions (conventional determining method that the chromatography of ions uses for this area,
Chromatography of ions used is that the U.S. wears peace ICS-2100 chromatography of ions) detected obtained by testing result contrasted, experiment
Data are shown in Table 2.
Table 2
From Table 2, it can be seen that being realized using system and method provided by the utility model micro in Power Plant Water Vapor
And the automatic quick detection of trace chloro ion content, and the utility model provides the detection lower limit of detection method for 5.0 μ g/L,
Analysis efficiency is 40-60 samples/hour, and detection range is 5.0-2000 μ g/L.
Method provided by the utility model is can also be seen that compared with the chromatography of ions from the testing result in table 2, is examined
Survey results contrast to approach, variation tendency is consistent.Because of the difference of detection method, data processing method etc., method of the present utility model
Certain difference is there is with the testing result of the chromatography of ions；It is relative to miss when Chloride Ion In Water content is less than 10 μ g/L
Difference is less than 20%；When Chloride Ion In Water content is more than 10 μ g/L, relative error is less than 10%, and measurement error is in allowed band
It is interior.
Comparative example
This comparative example is by FIA- AASs provided by the utility model and the existing flow injection-ion in this area
The test result and pros and cons for exchanging enrichment-AAS have carried out brief comparison explanation, the results are shown in Table shown in 3.
Table 3
From table 3 it is observed that using method and system provided by the utility model determine Power Plant Water Vapor in trace and
ON-LINE ION-EXCHANGE preenrichment processing need not be carried out during trace chlorine to water sample, but can direct adopting with certain volume
Detected after the sampling of sample ring.Therefore, method and system relative ease provided by the utility model, analyze speed is fast, still
Detect lower limit relatively higher.And from the point of view of the reappearance and antijamming capability of two methods, method provided by the utility model
And the stability and reliability of system are obviously improved compared with flow injection-Pro-concentration with ion exchange process-AAS, it is easy to accomplish
Onlineization, with preferable popularizing application prospect, scientific research value and social value are notable.
Claims (10)
1. a kind of automatic quick analysis system of micro in Power Plant Water Vapor/trace chloro ion, it includes current-carrying bottle (1), reaction reagent
Bottle (2), water sample bottle (3), flow injection analyzer (13), composite module (7), sampling ring (8), reaction coil pipe (9) and detector
(10),
Wherein, the flow injection analyzer (13) includes A pumps (4), B pumps (5) and sampling valve (6), and water sample bottle (3) passes through pipeline
It is connected via B pumps (5) with sampling valve (6), current-carrying bottle (1) is connected by pipeline via A pumps (4) with sampling valve (6), composite module
(7) at least two entrances and one outlet are set, and reaction reagent bottle (2) is by pipeline via A pumps (4) and composite module (7)
Entrance is connected, and sampling valve (6) is connected by pipeline with another entrance of composite module (7), and the outlet of composite module (7) passes through pipe
Road is connected with the entrance of reaction coil pipe (9), and the outlet of reaction coil pipe (9) is connected by pipeline with detector (10), the sampling
The import and export of ring (8) are connected by pipeline with sampling valve (6) respectively；
The composite module (7) and reaction coil pipe (9) are located in insulating box (11).
2. system according to claim 1, it is characterised in that the system also includes discharging of waste liquid end (12), the waste liquid
Discharge end (12) is connected by pipeline with detector (10).
3. system according to claim 1, it is characterised in that the system also includes work station (14), the work station
(14) electrically connected with detector (10).
4. system according to claim 1, it is characterised in that the detector (10) is photometric detector, its flow cell
For constant temperature flow cell, the flow cell light path is 5-50mm, and flow cell light path aperture is 1.0-3.0mm.
5. system according to claim 1, it is characterised in that the pump speed of the A pumps is 10-50rpm, and flow is 0.5-
5.0mL/min。
6. system according to claim 1, it is characterised in that the pump speed of the B pumps is 10-80rpm, and flow is 1.0-
10.0mL/min。
7. the system according to claim any one of 1-6, it is characterised in that the sampling valve (6) is in sample states energy
Water sample is entered sampling ring (8) via B pumps (5) by pipeline by water sample bottle (3), and can make current-carrying by carrying in injection state
Stream bottle (1), which enters sampling ring (8) via A pumps (4) by pipeline and promotes the water sample in sampling ring (8) to enter via pipeline, to be combined
Module (7), enters the sampling that composite module (7) collects by pipeline by reaction reagent bottle (2) with reaction reagent via A pumps (4)
Valve (6).
8. system according to claim 7, it is characterised in that the sampling valve (6) is the groove Single-channel Rolling valve of six hole three
Or the hole Multifunctional rotary valve of eight passage 16.
9. the system according to claim any one of 1-6, it is characterised in that the length of the reaction coil pipe (9) is 100-
500cm, internal diameter is 0.5-1.5mm.
10. the system according to claim any one of 1-6, it is characterised in that the internal diameter of the pipeline is 0.5-1.5mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110220856B (en) * | 2019-06-05 | 2021-07-27 | 常州大学 | Method for detecting content of chloride ions in electrodeposition liquid of electrolytic copper foil by flow injection method |
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