CN105203575B - Water quality heavy metal online analyzer and analysis method based on XRF technology - Google Patents
Water quality heavy metal online analyzer and analysis method based on XRF technology Download PDFInfo
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- CN105203575B CN105203575B CN201510618547.2A CN201510618547A CN105203575B CN 105203575 B CN105203575 B CN 105203575B CN 201510618547 A CN201510618547 A CN 201510618547A CN 105203575 B CN105203575 B CN 105203575B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 54
- 238000005516 engineering process Methods 0.000 title claims abstract description 26
- 238000004458 analytical method Methods 0.000 title claims abstract description 16
- 238000005070 sampling Methods 0.000 claims abstract description 63
- 238000000889 atomisation Methods 0.000 claims abstract description 50
- 230000005540 biological transmission Effects 0.000 claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 13
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 17
- 230000002572 peristaltic effect Effects 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 239000013618 particulate matter Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 8
- 239000000443 aerosol Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 230000033001 locomotion Effects 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 claims description 2
- 230000007423 decrease Effects 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 claims description 2
- 230000003111 delayed effect Effects 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000012544 monitoring process Methods 0.000 abstract description 5
- 238000012423 maintenance Methods 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009659 non-destructive testing Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A kind of water quality heavy metal online analyzer and analysis method based on XRF technology, belong to environmental monitoring technology field.Water quality heavy metal online analyzer includes：Water sample atomization system, example enrichment system, detecting system, strainer transmission system and control acquisition system.Atomized sample caused by water sample atomization system, example enrichment system is transferred to by silicone tube or metal tube, complete strainer transmission system after example enrichment and will be enriched with spot and be sent to detecting system, the control of above-mentioned each system and the collection of data and pass through built-in intelligence software automatic synchronization by control acquisition system to complete.Water sample atomization system, example enrichment system, strainer transmission system and detecting system are connected by data wire with control acquisition system.Analysis method includes：Water sampling, atomization and example enrichment, water sample discharge, sample detection.Advantage is have ultralow test limit, determined while can realizing water quality detection device for multi metallic elements.Also, reduce maintenance cost, avoid secondary pollution.
Description
Technical field
The invention belongs to environmental monitoring technology field, and in particular to a kind of water quality heavy metal based on XRF technology
In-line analyzer and analysis method.
Background technology
With the quickening of China's process of industrialization, the heavy metal pollution that water pollution problems is particularly wide basin turns into system
The about main Environmental Problems of socio-economic development, it would be highly desirable to solved from source.And thus derivative crop heavy metal excessive problem
Also strong influence has been carried out for mankind's health care belt.Therefore, the exploitation for water quality heavy metal online analyzer and analysis method has
There is important meaning.
The water quality heavy metal online analyzer of main flow in the market, mainly using photometry or Anodic stripping.
Luminosity law technology relative maturity, stability are good.But method sensitivity is not high, Element detection selectivity is not strong, easily by coexisting ion
Interference, developer have response to many metal ions sometimes, can not be directed to various heavy and be detected simultaneously, and chemistry
Reagent can not meet the detection of low concentration complexity water sample there may be secondary pollution.Anodic stripping is to be based on electrochemical method,
Complicated mechanism is detected, method is sensitive, and repeatability wants specific luminosity method poor.Sensitivity and selectivity are good, and test limit, can up to μ g/L
The detection of the various heavies such as lead, cadmium, copper is realized simultaneously.But instrument maintenance requires higher, especially electrode polishing is safeguarded, is safeguarded
Personnel need to grasp by professional training and prolonged practice.
In addition, mainly there are XOS companies of the U.S. in the producer for realizing heavy metal analysis technology in water quality based on XRF technologies at present,
Using X ray single-wavelength light spectral technology, it can be monitored on-line at present for Pb and As, detection is limited to 30 μ g/L.But this
Kind instrument needs to use the analyzing crystal of costliness to realize the light splitting of X incident rays and fluorescence signal, and is limited to analyzing crystal,
Not all element can detection.Meanwhile instrument cost is higher, light path is relative complex, and environmental suitability is slightly worse.
The content of the invention
It is an object of the invention to provide a kind of based on the water quality heavy metal online analyzer of XRF technology and analysis
Method, XRF non-destructive testing technology is combined using water sample atomization, water quality heavy metal can be directed to and carry out on-line analysis, spirit
Sensitivity, stability, reappearance are outstanding.
To achieve the above object, technical scheme is as follows：
The water quality heavy metal online analyzer of the present invention includes：Water sample atomization system, example enrichment system, detecting system,
Strainer transmission system and control acquisition system.Atomized sample caused by water sample atomization system, pass through silicone tube (or metal
Pipe) example enrichment system is transferred to, strainer transmission system is sent to detecting system by spot is enriched with after completing example enrichment, above-mentioned
The control of each system and the collection of data are completed by control acquisition system by built-in intelligence software automatic synchronization.Water sample mist
Change system, example enrichment system, strainer transmission system and detecting system are connected by data wire with control acquisition system.
Water sample atomization system of the present invention includes：Sample peristaltic pump 1, sample cell 2, first liquid level gauge 3, the second liquid level
Meter 4, ultrasonic atomizer 5, the first magnetic valve 6, second solenoid valve 7, air compressor 8, venturi scrubber 9, drier 10；Adopt
Sample peristaltic pump 1, the first magnetic valve 6, sample cell 2 are connected by flexible pipe.Ultrasonic atomizer 5 is fixed on sample cell by fixed screw
2 bottoms.First liquid level gauge 3 is individually fixed in sample cell upper and lower part with second liquid level gauge 4, can determine to adopt by difference in height
The atomization volume of sample liquid body.Pass through silicone tube between sample cell 2, second solenoid valve 7, venturi scrubber 9, drier 10
(or metal tube) connects, and the position that silicone tube (or metal tube) enters sample cell 2 will be less than second liquid level gauge 4, guarantee
Enough extract water sample atomization.Air compressor 8 provides atomization of the pure air for water sample by flexible pipe to venturi scrubber 9.
The system mainly realizes the gathering of water sample, quantitatively atomization forms aerosol particle, by after drying by the heavy metal salt in water
Form dry particulate matter.
Example enrichment system of the present invention includes：3rd magnetic valve 11, sampling pipe lifting motor 12, sample stage 13,
Particulate filter 14, flow-control module 15, sampling pump 16.It is that metal tube connects between drier 10, the 3rd magnetic valve 11
Connect, sampling pipe lower end under the action of sampling pipe lifting motor 12, sampling pipe by extrude strainer 28 can with sample stage 13 it
Between form closed sample space.Pass through between sample stage 13, particulate filter 14, flow-control module 15, sampling pump 16
Flexible pipe connects.Enrichment system is enriched with by the way that the particulate matter dried caused by atomization system is drawn into strainer surface, is realized
The enrichment of heavy metal substance in water.
Described detecting system includes：X ray light pipe 17, light pipe high voltage power supply 18 and XRF detector 19.X is penetrated
Linear light pipe 17 is connected with light pipe high voltage power supply 18 by high-tension bus-bar.Light pipe high voltage power supply 18 and XRF detector 19,
It is connected with industrial PC 31 by data wire, is controlled by intelligence software.Detecting system is located at the right side of sample stage 13, strainer 28
Top, by XRF technology, realize the detection to different heavy metals.
The strainer transmission system includes：Feed belt wheel 20, take-up pulley 21, smooth wheel 22-25, pinch roller 26, power transmission shaft 27,
Strainer 28.Hello belt wheel 20, the first smooth 22 and the 3rd smooth wheel 24 of wheel, pinch roller 26, transmission take out 27 on the left of sample stage 13,
Strainer can constantly be released by feeding belt wheel 20, then be transmitted strainer 28 into example enrichment system by the coordination rotation of each several part.The
Four smooth 25 and second smooth wheels 23 of wheel, take-up pulley 21 are located at the right side of sample stage 13.Take-up pulley 21 can be continuous by rotating
Pack up the strainer by detection.The both ends of strainer 28, which are wound in, feeds on belt wheel 20 and take-up pulley 21, and the motion of the collaboration of the two can
Realize the continuous folding and unfolding of strainer 28.Realize that strainer sample is in enrichment by the frictional force between pinch roller 26 and power transmission shaft 27
Transmission between system and detecting system.Belt wheel 20, take-up pulley 21 are fed as the transmission of strainer carries out corresponding folding and unfolding strainer, it is flat
Whole wheel 22-25 ensures strainer 28 in the smooth of whole transmission process.
Control acquisition system of the present invention includes：Water sample is atomized control board 29, is enriched with transmission control circuit plate
30, industrial PC 31 and intelligence software.Water sample is atomized control board 29, and enrichment driving circuit plate 30 passes through data wire and work
Control computer 31 is connected, and intelligence software is installed in industrial PC 31.
X ray light pipe 17 is 10-100W using power；XRF detector 19 is SDD types.
The test limit for most of heavy metal elements of the analyzer can reach 1 μ g/L.
A kind of water quality heavy metal on-line analysis based on XRF technology described in use comprises the following steps：
1) water sampling, atomization and example enrichment：The first magnetic valve 6, second solenoid valve 7 are in open mode first,
Sampling peristaltic pump 1 squeezes into water sample in sample cell 2 by sampling pipe, until the liquid level in sample cell 2 is detected by first liquid level gauge 3
After arriving, close sampling peristaltic pump 1 and stop sampling, turn off the first magnetic valve 6, it is ensured that the uniformity of each sampling quantity.Then open
Dynamic ultrasonic atomizer 5, which starts, starts primary atomization, and subsequent air compressor 8, which starts, drives venturi scrubber 9 to be further atomized.
The water produced in aerosol particle is removed by drier 10, forms dry particulate matter, heavy metal thing by the air-flow after atomization
Matter can be resided in particle phase.It is synchronous to open the 3rd magnetic valve 11, sampling pipe lifting motor 12 when venturi scrubber 9 is opened
Decline, clamp strainer 28 between sample stage 13, form confined space.Sampling pump 16 is opened, particulate matter is synchronously dried
Example enrichment.Flow controller 15 controls the gas circuit speed of evacuation, ensures the stability of sampling.Particulate filter 14 is used to protect
Flow controller is protected, prevents from blocking.With the progress of atomization, when the liquid level in sample cell 2 drops at second liquid level gauge 4,
Ultrasonic atomizer 5, air compressor 8, second solenoid valve 7 are first closed.(20s is usually set to after delay certain time), the 3rd
Magnetic valve 11, sampling pump 16 are closed successively.Sampling pipe lifting motor 12 rises.Complete collection, atomization and the enrichment process of sample.
2) water sample is discharged：After the completion of water sample is atomized and is enriched with, the first magnetic valve 6 and second solenoid valve 7 are opened, sampling is compacted
Dynamic pump 1 discharges all liq in sample cell 2, completes this sampling, and evacuated tube road, prepares the collection of next water sample.
3) sample detection：The strainer of enrichment is completed, test position is run to by transmission device, industrial PC 31 is controlled automatically
System opens light pipe high voltage power supply 18, X ray light pipe 17 and XRF detector 19.The software of industrial PC 31 completes spectrogram
Collection and processing, according to built-in working curve, it finally can be calculated heavy metal corresponded in water sample with reference to the data of collection
Concentration.
X ray light pipe 17, the detection time of XRF detector 19 are by industrial PC 31 in above-mentioned steps
Software systems are configured.Using Non-Destructive Testing, the sample being stored on strainer, it can retain and further be examined for laboratory
Survey.
The beneficial effects of the present invention are：
1st, the present invention is to be based on XRF technology water quality heavy metal online analyzer, the feature of different heavy metal elements
Spectrum does not have to, therefore this method can realize the same detection of water quality detection device for multi metallic elements.Without any chemical reagents, reduce
Maintenance cost, while it also avoid the secondary pollution problem of chemical reagent；
2nd, present invention employs water sample atomization and enrichment method, there is the Monitoring lower-cut of μ g/L magnitudes, and pass through regulation
Enrichment ratio, the detection (μ g/L-g/L) of wide dynamic detection range can be realized, surface water and pollution sources can be met simultaneously
On-line monitoring needs；
3rd, the XRF detection technique that the present invention uses, can compared with existing main stream approach for lossless detection method
Test sample is reclaimed, the recovery, retention and laboratory for being easy to implement same sample are rechecked；
4th, sampling of the invention and detection part physical isolation, operating mode scene is more suitable for, can greatly reduce maintenance
Cost；
Brief description of the drawings
Fig. 1 is the water quality heavy metal online analyzer system schematic of the invention based on XRF technology.Wherein, adopt
Sample peristaltic pump 1, sample cell 2, first liquid level gauge 3, second liquid level gauge 4, ultrasonic atomizer 5, the first magnetic valve 6, second solenoid valve
7th, air compressor 8, venturi scrubber 9, drier 10, include the 3rd magnetic valve 11, sampling pipe lifting motor 12, sample stage
13rd, particulate filter 14, flow-control module 15, sampling pump 16, X ray light pipe 17, light pipe high voltage power supply 18, X ray are glimmering
Photodetector 19, hello belt wheel 20, take-up pulley 21, the first smooth smooth the 23, the 3rd smooth wheel the 24, the 4th of wheel of wheel 22, second are smooth
Wheel 25, pinch roller 26, power transmission shaft 27, strainer 28, water sample atomization control board 29, enrichment transmission control circuit plate 30, industry control
Computer 31.
Fig. 2 is certain lead waste water of the measure of the water quality heavy metal online analyzer based on XRF technology of the present invention
The spectrogram of middle content of heavy metal lead.
Embodiment
The water quality heavy metal online analyzer of the present invention includes：Water sample atomization system, example enrichment system, detecting system,
Strainer transmission system and control acquisition system.Atomized sample caused by water sample atomization system, pass through silicone tube (or metal
Pipe) example enrichment system is transferred to, strainer transmission system is sent to detecting system by spot is enriched with after completing example enrichment, above-mentioned
The control of each system and the collection of data are completed by control acquisition system by built-in intelligence software automatic synchronization.Water sample mist
Change system, example enrichment system, strainer transmission system and detecting system are connected by data wire with control acquisition system.
Below in conjunction with the accompanying drawings, the embodiment of the present invention is described in further detail.
The present invention is the water quality heavy metal online analyzer based on XRF technology, system include water sample atomization system,
Example enrichment system, detecting system, strainer transmission system and control acquisition system.
Water sample atomization system mainly realizes the gathering of water sample, quantitatively atomization forms aerosol particle, after further drying
Form the dry particle thing of heavy metal salt.
As shown in figure 1, sampling peristaltic pump 1, sample cell 2, first liquid level gauge 3, second liquid level gauge 4, ultrasonic atomizer 5, the
One magnetic valve 6, second solenoid valve 7, air compressor 8, venturi scrubber 9, drier 10.Pass through between above-mentioned each part
Flexible pipe connects, and the flexible pipe lower end in sample cell 2 needs to be placed in the lower section of second liquid level gauge 4, ensures to be in whole atomization process
Below liquid level, water sample can be extracted and be atomized.
Example enrichment system is used to heavy metal salt particulate matter caused by water sample atomization system being enriched in strainer surface, carries
The concentration of high measurand, improve the Monitoring lower-cut and stability of global analysis instrument.
As shown in figure 1, example enrichment system mainly include the 3rd magnetic valve 11, sampling pipe lifting motor 12, sample stage 13,
Particulate filter 14, flow-control module 15, sampling pump 16.Drier 10, the 3rd magnetic valve 11, sampling pipe lifting motor 12
Between for flexible pipe connect.The lower end of sampling pipe lifting motor 12 is metal tube, ensures to be formed between sample stage 13 after declining
Sealing.Sample stage 13, particulate filter 14, flow-control module 15 and sampling pump 16 are connected by flexible pipe.
The principle that water quality heavy metal is enriched with strainer is as follows：Using water sample atomization system, pass through designed sequential control
System, the concrete water quality that guarantee is atomized every time are consistent.By air suction sampling, by the heavy metal particles thing enrichment after atomization drying and strainer
Surface.In enrichment process, industrial PC 31 can record the volume V of water quality atomizationl, wherein certain water quality heavy metal detected
Concentration is Cl.Then, the concentration obtained by detecting system is Cs, the area of particle concentrations is S on strainers.Wherein Cs, Cl,
Ss, VlMeet formula below：
Cs×Ss=Cl×Vl
Due to Ss, Vl, it is known that C is obtained by detecting systems, so that it may C is calculated by above-mentioned formulal, that is, obtained reality
The concentration of heavy metal is corresponded in the water sample of border.
Detecting system is based on online XRF technology, including the use of the X ray light pipe 17 that power is 10-100W
With SDD types detector 19, SDD types detector 19 is freezed using electricity, and integrated level is high, technology maturation, has higher detection efficient
And energy resolution, it disclosure satisfy that the effective detection of most of Characteristics of Heavy Metals XRF；X ray light pipe 17 and detector
19 are individually fixed in above strainer.X ray light pipe 17 is connected with light pipe high voltage power supply 18 by high voltage insulated cable, light pipe high-tension electricity
Source 18 is connected with industrial PC 31 by data wire.Detector 19 is connected by data wire with industrial PC 31, industrial PC 31
The software of inside installation can automatically control X ray light pipe 17, light pipe high voltage power supply 18 and detector 19, realize detecting system
Normal work.
The principle of X-ray detection heavy metal element is as follows：X-ray bombardment is on sample, contained heavy metal in sample
Element can be excited, characteristic fluorescence corresponding to generation, fluorescent energy and Atom of Elements Z square directly proportional, member to be measured
The content of element is relevant with the feature X-fluorescence intensity that it is launched；By the FPGA data process circuit built in detector 19 to collection,
Data signal after amplification, A/D conversions is handled, and is carried out data transmission and controlled with industrial PC 31 by data-interface
Communication.During analysis, software can automatic identification difference heavy metal element spectral peak, and carry out smooth, the spectrum such as buckle back scape automatically
Figure processing, whole spectrogram real-time display is on the screen of industrial PC 31.The data processing of this method uses peak area method, leads to
The characteristic peak that automatic identification corresponds to heavy metal is crossed, after carrying out buckle back scape, obtains net peak intensity I0 m, then interference school carried out by software
After just, new correction intensity I can obtainm.By using corresponding heavy metal element standard sample, obtain corresponding spectral peak Im
Data；The sample of n heavy metal element different content is taken, obtains one group of Im(n), wherein n >=3；Draw ImWith the element in sample
Concentration CmFunctional arrangement, obtain working curve.Weight by being enriched with the relative intensity inverse strainer that obtains in actually detected again
Metal concentration (Cs).C is calculated by above-mentioned formula againl, that is, obtained the concentration of heavy metal in water.This method passes through software, light path
The upgrading selection of hardware, can extend the quantitative analysis for realizing the different elements such as cadmium, lead, arsenic, copper, chromium, zinc.
Strainer transmission system includes feeding belt wheel 20, take-up pulley 21, smooth wheel 22-25, pinch roller 26, power transmission shaft 27, strainer
28.Strainer 28 is clamped between pinch roller 26 and power transmission shaft 27, passes through the forward and reverse rotation of power transmission shaft 27.Realize strainer 28 each
Transmission between system.Feed belt wheel 20, take-up pulley 21, power transmission shaft 27 with enrichment transmission control circuit plate 30 to be connected, enrichment transmission
Control board 30 is connected with industrial PC 31 by data wire, the sequential movement control of final strainer 28, is controlled by software.
Acquisition system is controlled to include water sample atomization control board 29, enrichment transmission control circuit plate 30, industrial PC 31
And intelligence software.The processes such as stream in total system, circuit are realized by the software in industrial PC 31 and logic circuit
Automatically control and system in Various types of data collection, processing and storage.
The water quality heavy metal online analyzer and analysis method based on XRF technology of the present invention includes following step
Suddenly：
1) water sampling, atomization and example enrichment：The first magnetic valve 6, second solenoid valve 7 are in opening first,
Sampling peristaltic pump 1 squeezes into water sample in sample cell 2 by sampling pipe, until the liquid level in sample cell 2 is detected by first liquid level gauge 3
After arriving, close sampling peristaltic pump 1 and stop sampling, turn off the first magnetic valve 6, it is ensured that the uniformity of each sampling quantity.Then open
Dynamic ultrasonic atomizer 5, which starts, starts primary atomization, and air compressor 8, which starts, drives venturi scrubber 9 to be further atomized.Atomization
The water produced in aerosol particle is removed by drier 10, forms dry particulate matter, heavy metal substance meeting by air-flow afterwards
Reside in particle phase.When atomization starts, open the 3rd magnetic valve 11, sampling pipe lifting motor 12 declines, with sample stage 13 it
Between strainer 28 is clamped, formed confined space.Sampling pump 16 is opened, the example enrichment of particulate matter is synchronously dried.Flow control
Device 15 processed controls the gas circuit speed of evacuation, ensures the stability of sampling.As the liquid level in sample cell 2 drops to second liquid level gauge 4
During place, ultrasonic atomizer 5, air compressor 8, second solenoid valve 7 are first closed.(20s is usually set to after delay certain time),
3rd magnetic valve 11, sampling pump 16 are closed successively.Sampling pipe lifting motor 12 rises.Complete collection, atomization and the enrichment of sample
Process.
2) water sample is discharged：After the completion of water sample is atomized and is enriched with, the first magnetic valve 6 and second solenoid valve 7 are opened, sampling is compacted
Dynamic pump 1 discharges all liq in sample cell 2, completes this sampling, and evacuated tube road, prepares the collection of next water sample.
3) sample detection：The strainer of enrichment is completed, test position is run to by transmission device, industrial PC 31 is controlled automatically
System opens light pipe high voltage power supply 18, X ray light pipe 17 and XRF detector 19.The software of industrial PC 31 completes spectrogram
Collection and processing, according to built-in working curve, it finally can be calculated heavy metal corresponded in water sample with reference to the data of collection
Concentration.
The water quality heavy metal online analyzer based on XRF technology and analysis method of the present invention passes through software, light
The upgrading of road hardware combines, and can realize the different heavy metal elements such as K (potassium, No. 19 elements)-U (uranium, No. 92 elements) in theory
Expanded application, application is extremely wide.
The water quality heavy metal online analyzer and analysis method based on XRF technology of the present invention, for water quality weight
The detection of metal is limited to 1 μ g/L or so, meet in all existing national environmental standards be directed to water quality heavy metal in lead, cadmium, mercury,
The requirement of the limit values such as arsenic, chromium, nickel, copper, zinc discharge.
Claims (6)
- A kind of 1. water quality heavy metal online analyzer based on XRF technology, it is characterised in that including：Water sample atomization system System, example enrichment system, detecting system, strainer transmission system and control acquisition system；It is atomized caused by water sample atomization system Sample, example enrichment system is transferred to by silicone tube or metal tube, strainer transmission system will be enriched with after completing example enrichment Spot is sent to detecting system, and the control of above-mentioned each system and the collection of data pass through built-in intelligence by control acquisition system Software automatic synchronization is completed；Water sample atomization system, example enrichment system, strainer transmission system and detecting system pass through data wire It is connected with control acquisition system；Described water sample atomization system includes：Sample peristaltic pump (1), sample cell (2), first liquid level gauge (3), second liquid level gauge (4), ultrasonic atomizer (5), the first magnetic valve (6), second solenoid valve (7), air compressor (8), venturi scrubber (9), Drier (10)；Sampling peristaltic pump (1), the first magnetic valve (6), sample cell (2) are connected by flexible pipe；Ultrasonic atomizer (5) is logical Cross fixed screw and be fixed on sample cell (2) bottom；First liquid level gauge (3) is individually fixed on sample cell with second liquid level gauge (4) Portion and bottom, the atomization volume of sample liquid can be determined by difference in height；Sample cell (2), second solenoid valve (7), venturi Connected between atomizer (9), drier (10) by silicone tube or metal tube, silicone tube or metal tube enter sample cell (2) position will be less than second liquid level gauge (4), guarantee to extract water sample atomization；Air compressor (8) is by flexible pipe to literary mound In atomizer (9) provide pure air be used for water sample atomization；The system realizes the gathering of water sample, quantitatively atomization forms aerosol Particle, by the way that the heavy metal salt in water is formed into dry particulate matter after drying.
- 2. in-line analyzer according to claim 1, it is characterised in that described example enrichment system includes：3rd electricity Magnet valve (11), sampling pipe lifting motor (12), sample stage (13), particulate filter (14), flow-control module (15), sampling Pump (16)；It is metal tube connection between drier (10), the 3rd magnetic valve (11), sampling pipe lower end is in sampling pipe lifting motor (12) under action, sampling pipe can form closed sample space by extruding strainer (28) between sample stage (13)；Sample Sample platform (13), particulate filter (14), flow-control module (15), sampling pump are connected between (16) by flexible pipe；Sample is rich Collecting system is enriched with by the way that the particulate matter dried caused by atomization system is drawn into strainer surface, realizes heavy metal thing in water The enrichment of matter.
- 3. in-line analyzer according to claim 1, it is characterised in that described detecting system includes：X ray light pipe (17), light pipe high voltage power supply (18) and XRF detector (19)；X ray light pipe (17) is logical with light pipe high voltage power supply (18) Cross high-tension bus-bar connection；Light pipe high voltage power supply (18) and XRF detector (19) pass through data wire and industrial PC (31) connect；Detecting system is located at the right side of sample stage (13), the top of strainer (28), passes through XRF technology, realization pair The detection of different heavy metals.
- 4. in-line analyzer according to claim 1, it is characterised in that described strainer transmission system includes：Feed belt wheel (20), take-up pulley (21), smooth wheel, pinch roller (26), power transmission shaft (27), strainer (28)；Feed belt wheel (20), the first smooth wheel (22) (27) are taken out and are located on the left of sample stage (13) with the 3rd smooth wheel (24), pinch roller (26), transmission, feeding belt wheel (20) can not It is disconnected to release strainer, then transmitted strainer 28 into example enrichment system by the coordination rotation of each several part；4th it is smooth wheel (25) and Second smooth wheel (23), take-up pulley (21) are located on the right side of sample stage (13)；Take-up pulley (21) can be packed up constantly by rotating By the strainer of detection；Strainer (28) both ends, which are wound in, feeds on belt wheel (20) and take-up pulley (21), the motion of the collaboration of the two, energy Enough realize the continuous folding and unfolding of strainer (28)；Strainer sample is realized by the frictional force between pinch roller (26) and power transmission shaft (27) Transmission between enrichment system and detecting system；Feed belt wheel (20), take-up pulley (21) is carried out accordingly with the transmission of strainer Folding and unfolding strainer, it is smooth wheel ensure strainer (28) in the smooth of whole transmission process.
- 5. in-line analyzer according to claim 1, it is characterised in that described control acquisition system includes：Water sample mist Change control board 29, enrichment transmission control circuit plate 30, industrial PC 31 and intelligence software；Water sample is atomized control board (29), it is enriched with driving circuit plate (30) to be connected with industrial PC (31) by data wire, intelligence software is installed on industrial PC (31) in.
- 6. a kind of method of analyzer on-line analysis using described in claim 1, it is characterised in that comprise the following steps：1) water sampling, atomization and example enrichment：First magnetic valve first (6), second solenoid valve (7) are in open mode, Sampling peristaltic pump (1) squeezes into water sample in sample cell (2) by sampling pipe, until the liquid level in sample cell (2) is by the first liquid level After meter (3) detects, close sampling peristaltic pump (1) and stop sampling, turn off the first magnetic valve (6), it is ensured that each sampling quantity Uniformity；Then start ultrasonic atomizer (5) and start beginning primary atomization, subsequent air compressor (8), which starts, drives venturi Atomizer (9) is further atomized；Air-flow after atomization is removed the water produced in aerosol particle, shape by drier (10) Into dry particulate matter, heavy metal substance can be resided in particle phase；It is synchronous to open the 3rd when venturi scrubber (9) is opened Magnetic valve (11), sampling pipe lifting motor (12) decline, and clamp strainer (28) between sample stage (13), form confined air Between；Sampling pump (16) is opened, the example enrichment of particulate matter is synchronously dried；Flow controller (15) control gas circuit pumping speed Degree, ensure the stability of sampling；Particulate filter (14) is used to protect flow controller, prevents from blocking；With entering for atomization OK, when the liquid level in sample cell (2) drops to second liquid level gauge (4) place, ultrasonic atomizer (5), air compressor (8), Two magnetic valves (7) are first closed；It is delayed after 20s, the 3rd magnetic valve (11), sampling pump (16) are closed successively；Sampling pipe lifting motor (12) rise；Complete collection, atomization and the enrichment process of sample；2) water sample is discharged：After the completion of water sample is atomized and is enriched with, the first magnetic valve (6) and second solenoid valve (7) are opened, sampling is compacted Dynamic pump (1) discharges all liq in sample cell (2), completes this sampling, and evacuated tube road, prepares adopting for next water sample Collection；3) sample detection：The strainer of enrichment is completed, test position is run to by transmission device, industrial PC (31) automatically controls Open light pipe high voltage power supply (18), X ray light pipe (17) and XRF detector 19；Industrial PC (31) software completes spectrum The collection and processing of figure, according to built-in working curve, finally it is calculated in water sample with reference to the data of collection and corresponds to heavy metal Concentration.
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| CN105866153A (en) * | 2016-03-31 | 2016-08-17 | 北方工业大学 | Atmosphere heavy metal detection system |
| CN106442591A (en) * | 2016-09-14 | 2017-02-22 | 钢研纳克检测技术有限公司 | Component control and signal exploration system for WEDXRF spectrometer |
| CN107247013A (en) * | 2017-06-29 | 2017-10-13 | 苏州浪声科学仪器有限公司 | Atmosphere heavy metal in-line analyzer |
| CN108593694A (en) * | 2018-05-10 | 2018-09-28 | 深圳市西凡谨顿科技有限公司 | The x-ray fluorescence online test method of increasing material manufacturing |
| CN110873727A (en) * | 2018-09-04 | 2020-03-10 | 河北地质大学 | XRF-based analysis method for in-situ determination of water body metals |
| CN109709126B (en) * | 2019-02-21 | 2021-11-02 | 中国科学院合肥物质科学研究院 | Automatic detection device and method for heavy metals in water body by algae enrichment-X-ray fluorescence spectrum |
| CN114935638A (en) * | 2022-07-05 | 2022-08-23 | 南通艾森传感技术有限公司 | Novel online environment-friendly special water quality detector |
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| JP2012093151A (en) * | 2010-10-26 | 2012-05-17 | Hitachi High-Tech Control Systems Corp | Fluorescent x-ray water quality meter and water quality management system |
| CN104483339B (en) * | 2014-12-30 | 2017-03-22 | 钢研纳克检测技术有限公司 | On-line analyzer and analysis method of mercury in flue gas based on wet enrichment |
| CN104569017B (en) * | 2014-12-31 | 2017-05-31 | 聚光科技(杭州)股份有限公司 | Heavy metal analysis device and its method of work in water |
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