CN109520974A - A kind of on-line detecting system and detection method of drainage pipeline Heavy Metals in Sludge - Google Patents
A kind of on-line detecting system and detection method of drainage pipeline Heavy Metals in Sludge Download PDFInfo
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- CN109520974A CN109520974A CN201910092257.7A CN201910092257A CN109520974A CN 109520974 A CN109520974 A CN 109520974A CN 201910092257 A CN201910092257 A CN 201910092257A CN 109520974 A CN109520974 A CN 109520974A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The present invention provides the on-line detecting systems and detection method of a kind of drainage pipeline Heavy Metals in Sludge.The on-line detecting system includes sludge pretreatment device and detection device；The sludge of extraction can be carried out impurity and screened out by sludge pretreatment device, can guarantee Heavy Metals in Sludge Elemental redistribution to be measured uniformly and in the detection using stirring module and spray module can be improved the repeatability of detection, the detection limit for reducing element, improves the sensitivity of element to be measured.The present invention for the first time combines laser induced breakdown spectroscopy with technologies such as sprayings, realizes the on-line checking to drainage pipeline Heavy Metals in Sludge element.Spraying technology is used to make sample, highly sensitive, low detection limit, the vertical distribution quick testing requirements of super low concentration can be achieved under the premise of guaranteeing sample homogeneity, unique technological means can be provided for quickly detection Heavy Metals in Sludge constituent content etc..
Description
Technical field
The present invention relates to Heavy Metals in Sludge detection technique field, specifically a kind of drainage pipeline Heavy Metals in Sludge
On-line detecting system and detection method.
Background technique
Current common Heavy Metals in Sludge detection method is broadly divided into two kinds: atomic absorption spectrophotometry (AAS) and
Inductively coupled plasma mass spectrometry (ICP-MS).The former has the characteristics that detection accuracy height, strong antijamming capability, but needs
Normal pressure is cleared up and cannot detect multiple element simultaneously；The latter analyzes speed fastly and can detect multiple element simultaneously, but price
It is expensive and cumbersome.In contrast, laser induced breakdown spectroscopy (LIBS) because have can on-line analysis, can be simultaneously
The advantages that detecting multiple element, is more and more applied in environment measuring.
The principle of laser induced breakdown spectroscopy method (LIBS) is that laser focuses on sample to be tested and sample to be tested is punctured gas
Change forms plasma, and spectrometer collects plasma and it is changed into electric signal transmission to computer by optical signal, according to
Heavy metal concentration contained by the characteristic spectral line and sample of heavy metal element contained by sample to be tested and spectral intensity matched curve carry out
Qualitative and quantitative analysis.
Laser induced breakdown spectroscopy its advantage lies in being able to quick real-time online detection compared with other detection techniques
Multiple element.And it detects limit and reaches ppm magnitude, meets the national standard of detection Heavy Metals in Sludge.But it is by test sample
The influence of moral character matter, aqueous solution contained by sludge can accelerate the dieing out of plasma generation with laser, contained heavy metal member in sludge
Element, which is unevenly distributed, to impact spectrometer collection plasma signal.
Summary of the invention
It is an object of the invention to provide the on-line detecting system and detection method of a kind of drainage pipeline Heavy Metals in Sludge,
So as to it is real-time, efficient, quickly and accurately to drainage pipeline Heavy Metals in Sludge carry out qualitative and quantitative detection analysis.
The present invention is implemented as follows: a kind of on-line detecting system of drainage pipeline Heavy Metals in Sludge, including sludge are pre-
Processing unit and detection device；
The sludge pretreatment device includes grid, sludge pump, vibrating screen, Mortar spraying machine and automatic specimen heating holder；It is described
Grid is used to carry out coarse filtration to the sludge in drainage pipeline, and the sludge pump through the sludge after the grid coarse filtration for that will extract
To the vibrating screen；The used by oscillating screen in the sludge pump it is decimated come sludge carry out fine filtering；The mortar spraying
Machine includes stirring module and spray module；The stirring module sludge after the vibrating screen fine filtering can be stirred so that
It is uniformly mixed, and the spray module is for will stir the sludge even application after module stirs to automatic heating sample through described
On platform；
The detection device includes YAG laser, total reflective mirror, condenser lens, fibre-optical probe, spectrometer and computer；The YAG
Laser is for emitting laser；The laser that the YAG laser is emitted is refracted to institute after total reflective mirror reflection with 45° angle
It states on condenser lens；On the sludge to be measured that laser is irradiated to automatic specimen heating holder after condenser lens focusing, and generate
Plasma；The fibre-optical probe is for being collected and transmitting to generated plasma in laser irradiation to sludge to be measured
To the spectrometer, the spectrometer is for receiving the collected plasma of the fibre-optical probe and converting light signals into electricity
Signal is then transmit to computer；The computer can the signal according to transmitted by the spectrometer in drainage pipeline sludge
Heavy metal carries out qualitative and quantitative detection analysis.
The automatic specimen heating holder is placed on rotating platform, and the rotating platform can drive the automatic specimen heating holder
It is rotated.
Motorized rails are equipped with below the rotating platform；The motorized rails are for driving the rotating platform and described
Automatic specimen heating holder shifts to the detection device, in order to the laser after condenser lens focusing can direct irradiation extremely
On the sludge to be measured of automatic specimen heating holder.
The grid in drainage pipeline sludge carry out coarse filtration when, it is used be drainage pipeline mud face or less four/
Sludge in one to half depth bounds.
The YAG laser is Nd:YAG laser.
The present invention also provides a kind of online test methods of drainage pipeline Heavy Metals in Sludge, include the following steps:
A, randomly select five sampled points, each sampled point in drainage pipeline the following a quarter in mud face to half depth
Sludge is taken in range；
B, so that taken sludge is carried out coarse filtration through grid, sludge is extracted to vibrating screen via sludge pump carry out fine filtering later；
C, the sludge after fine filtering is stirred through the stirring module in Mortar spraying machine first, by spray module that sludge is equal later
Even to be sprayed on automatic specimen heating holder, sludge is heated on automatic specimen heating holder and is dried to drying regime；Later by electricity
Dynamic guide rail carries rotating platform and automatic specimen heating holder moves to the position opposite with condenser lens；
D, YAG laser emits laser, and laser is refracted on condenser lens after total reflective mirror reflects with 45° angle；Line focus lens
In laser irradiation to the sludge to be measured of automatic specimen heating holder after focusing, laser breakdown sludge to be measured and gasify form plasma
Body；It drives automatic specimen heating holder to rotate by rotating platform, and then makes the laser uniform irradiation after line focus lens focus extremely
On the sludge to be measured of automatic specimen heating holder；
E, generated plasma and it is transmitted to spectrometer in fibre-optical probe acquisition step d, spectrometer reception optical fiber is popped one's head in institute
Collected plasma simultaneously converts light signals into electric signal and is then transmit to computer；Computer is according to transmitted by spectrometer
Signal in drainage pipeline sludge heavy metal carry out qualitative and quantitative detection analysis.
It is an advantage of the invention that laser induced breakdown spectroscopy is combined realization using sharp with technologies such as sprayings for the first time
Photoinduction breakdown spectral technology is to the heavy metal element on-line checking in drainage pipeline sludge.Spraying technology is used to make sample
It is fast that highly sensitive, low detection limit, the vertical distribution of super low concentration can be achieved in product under the premise of guaranteeing sample homogeneity
Fast testing requirements can provide unique technological means for quickly detection Heavy Metals in Sludge constituent content etc..It is examined compared to national standard
Survey method (AAS and ICP-MS), advantage are in particular in three aspects: (1) can be realized on-line checking: with traditional national standard
Detection method is compared, and the present invention mutually ties the technologies such as laser induced breakdown spectroscopy method and filtering, stirring, spraying, heating, transfer
It closes, simplifies cumbersome sample pretreatment process, on-line checking may be implemented.(2) mud sample has preferable uniformity:
It uses spraying technology to be equably sprayed on mud sample on sample stage after mud sample is carried out uniform stirring, improves detection
The parameters such as sensitivity as a result.(3) have real-time: on-site test and by mud sample spray progress flash baking,
It ensure that the real-time of testing result.
Detailed description of the invention
Fig. 1 is the on-line detecting system structural schematic diagram of drainage pipeline Heavy Metals in Sludge in the present invention.
In figure: 1, drainage pipeline；2, grid；3, sludge pump；4, vibrating screen；5, Mortar spraying machine；5-1, stirring module；5-
2, spray module；6, automatic specimen heating holder；7, rotating platform；8, YAG laser；9, total reflective mirror；10, condenser lens；11, light
Fibre probe；12, spectrometer；13, computer；14, motorized rails.
Specific embodiment
Embodiment 1, a kind of on-line detecting system of drainage pipeline Heavy Metals in Sludge.
Based on the requirement detected to drainage pipeline Heavy Metal Level In Sludge real-time online, the present invention is hit using induced with laser
Spectroscopic methodology is worn, using sludge as object to be measured, it is intended to design and build a huge sum of money in a real-time online detection drainage pipeline sludge
Belong to the system of ingredient and content, to provide efficient, fast and accurately measurement method for environment measuring and protection.
The on-line detecting system of drainage pipeline Heavy Metals in Sludge provided by the present invention include sludge pretreatment device and
Detection device；The sludge of extraction can be carried out impurity and screened out by sludge pretreatment device, can using stirring module and spray module
The repeatability of detection can be improved to guarantee Heavy Metals in Sludge Elemental redistribution to be measured uniformly and in the detection, reduce element
Detection limit, improves the sensitivity of element to be measured.
As shown in Figure 1, sludge pretreatment device includes grid 2, sludge pump 3, vibrating screen 4, Mortar spraying machine 5, adds automatically
Hot sample stage 6 and rotating platform 7.Sludge to be measured need to take out from drainage pipeline 1 first, when taking-up, can drainage pipeline 1 with
Machine chooses five sampled points, and each sampled point can sample in depth bounds of the following a quarter in mud face to half, so
The sample of five sampled points is mixed afterwards, as the mud sample for representing mean concentration.The sludge taken out by drainage pipeline 1
Coarse filtration is carried out through grid 2 first, in order to remove the relatively large impurity such as the rubbish in sludge, wooden unit.After 2 coarse filtration of grid
Sludge is extracted by sludge pump 3 to vibrating screen 4.The next sludge decimated to sludge pump 3 of vibrating screen 4 carries out filtering again, this
Belong to fine filtering for the secondary coarse filtration for filtering opposite grid 2, it may be assumed that the fine impurities in sludge can be rejected after vibrating screen 4.Through lattice
After grid 2 and vibrating screen 4 filter twice, the impurity in sludge is removed completely substantially, it is subsequent by Mortar spraying machine 5 to sludge into
Row stirring and spraying.
Mortar spraying machine 5 includes stirring module 5-1 and spray module 5-2.It is initially entered through the filtered sludge of vibrating screen 4
Stirring module 5-1 is stirred, and stirring module 5-1 is sufficiently mixed sludge by stirring, so that ingredient is uniform in sludge.
The sludge stirred evenly is admitted to spray module 5-2, and the sludge stirred evenly is sprayed into automatic heating sample by spray module 5-2
In sample platform 6.The spray range of spray module 5-2 is relatively large, and radius can reach one meter or so.Make automatic specimen heating holder 6
The center of face spray module 5-2 spray range can guarantee that spraying is uniform.Automatic specimen heating holder 6 its actually one automatic
Heating device, the sludge being sprayed into thereon can be heated drying to reach drying regime.Automatic specimen heating holder 6 in the present invention
It is placed on rotating platform 7, rotating platform 7 can realize automatic rotation, and rotating platform 7 can drive automatic specimen heating holder 6 to be revolved
Turn, to strike laser equably on the sludge to be measured of automatic specimen heating holder 6 in subsequent detection.
The present invention is equipped with motorized rails 14 in the lower section of rotating platform 7.Rotating platform 7 can be driven by motorized rails 14
Mobile with automatic specimen heating holder 6, in sample preparation and later period cleaning sample platform, motorized rails can make sample stage separate
Detection device can effectively avoid the dirt caused by detection device due to sputtering etc. in sample preparation and cleaning process
Dye.
Detection device includes YAG laser 8, total reflective mirror 9, condenser lens 10, fibre-optical probe 11, spectrometer 12 in the present invention
With computer 13.YAG laser 8 is Nd:YAG laser, and YAG laser 8 is for emitting laser.What YAG laser 8 was emitted
Laser is refracted on condenser lens 10 after the reflection of total reflective mirror 9 with 45° angle, and condenser lens 10 is for being focused laser.Electricity
Dynamic guide rail 14 moves to mud sample to be measured at the position of face condenser lens 10, and the laser after line focus lens 10 focus is direct
Irradiation strikes the sludge to be measured on automatic specimen heating holder 6, and laser breakdown sludge to be measured simultaneously forms plasma.It needs to illustrate
It is that when laser detection, rotating platform 7 is in rotation status, laser can be made equably to irradiate impact in heating sample automatically in this way
On the sludge to be measured of sample platform 6.Fibre-optical probe 11 on sludge to be measured and punctures the plasma that sludge to be measured is formed to laser irradiation
Body is collected, and is transmitted to spectrometer 12 later.12 reception optical fiber of spectrometer probe, 11 collected plasmas of institute and by light
Signal is changed into electric signal and is then transmit to computer 13；Computer 13 receives signal transmitted by spectrometer 12, utilizes
The spectral analysis softwares such as Oceamview, MATLAB, Origin carry out data processing, to the heavy metal in drainage pipeline sludge into
The analysis of row qualitative and quantitative detection.
Embodiment 2, a kind of online test method of drainage pipeline Heavy Metals in Sludge.
In order to overcome the shortcomings of that the prior art detects sludge, the present invention to be accomplished that based in extraction drainage pipeline
Sludge and handled, the spraying and laser induced breakdown spectroscopy of sludge the characteristics of, its advantage is combined together,
The ingredient and content of drainage pipeline Heavy Metals in Sludge are detected real-time, quickly to realize.
The online test method of drainage pipeline Heavy Metals in Sludge provided by the present invention, includes the following steps:
A, five sampled points are randomly selected, (are referred in the following a quarter to half depth bounds of mud face in drainage pipeline
In depth bounds away from mud identity distance from a quarter for sludge total height to half) take mud sample.Then by five parts
Mud sample is mixed, as mud sample to be measured.
B, so that the taken mud sample of step a is carried out coarse filtration through grid, later extract sludge to vibrating screen via sludge pump
Carry out fine filtering.What coarse filtration generally filtered out is the relatively large impurity such as rubbish, wooden unit, and what fine filtering generally filtered out is gravel, stone etc.
Lesser impurity.
C, the sludge after fine filtering is stirred through the stirring module in Mortar spraying machine first, after mixing evenly, by spraying
Module is dried to dry shape on sludge even application to automatic specimen heating holder, sludge is heated on automatic specimen heating holder
State, motorized rails carry rotating platform later and automatic specimen heating holder moves to the sludge to be measured position opposite with condenser lens.
D, YAG laser emits laser, and laser is refracted on condenser lens after total reflective mirror reflects with 45° angle；Line focus
In laser irradiation to the sludge to be measured of automatic specimen heating holder after lens focus, laser breakdown sludge to be measured simultaneously forms plasma
Body.When laser irradiation sludge to be measured, automatic specimen heating holder should be driven to rotate by rotating platform, and then strike laser uniformly
On sludge to be measured.
E, generated plasma and it is transmitted to spectrometer in fibre-optical probe acquisition step d, spectrometer reception optical fiber is visited
The head collected plasma of institute simultaneously converts light signals into electric signal and is then transmit to computer；Computer is according to spectrometer institute
The signal of transmission carries out data processing using spectral analysis softwares such as Oceamview, MATLAB, Origin, to drainage pipeline dirt
Heavy metal in mud carries out qualitative and quantitative detection analysis.
Claims (7)
1. a kind of on-line detecting system of drainage pipeline Heavy Metals in Sludge, characterized in that including sludge pretreatment device and inspection
Survey device；
The sludge pretreatment device includes grid, sludge pump, vibrating screen, Mortar spraying machine and automatic specimen heating holder；It is described
Grid is used to carry out coarse filtration to the sludge in drainage pipeline, and the sludge pump through the sludge after the grid coarse filtration for that will extract
To the vibrating screen；The used by oscillating screen in the sludge pump it is decimated come sludge carry out fine filtering；The mortar spraying
Machine includes stirring module and spray module；The stirring module sludge after the vibrating screen fine filtering can be stirred so that
It is uniformly mixed, and the spray module is for will stir the sludge even application after module stirs to the automatic heating through described
On sample stage；
The detection device includes YAG laser, total reflective mirror, condenser lens, fibre-optical probe, spectrometer and computer；The YAG
Laser is for emitting laser；The laser that the YAG laser is emitted is refracted to institute after total reflective mirror reflection with 45° angle
It states on condenser lens；On the sludge to be measured that laser is irradiated to automatic specimen heating holder after condenser lens focusing, and generate
Plasma；The fibre-optical probe is for being collected and transmitting to generated plasma in laser irradiation to sludge to be measured
To the spectrometer, the spectrometer is for receiving fibre-optical probe plasma collected and converting light signals into electricity
Signal is then transmit to computer；The computer can the signal according to transmitted by the spectrometer in drainage pipeline sludge
Heavy metal carries out qualitative and quantitative detection analysis.
2. the on-line detecting system of drainage pipeline Heavy Metals in Sludge according to claim 1, characterized in that described automatic
Specimen heating holder is placed on rotating platform, and the rotating platform can drive the automatic specimen heating holder to be rotated.
3. the on-line detecting system of drainage pipeline Heavy Metals in Sludge according to claim 1, characterized in that in the rotation
Turn to be equipped with motorized rails below platform；The motorized rails are for driving the rotating platform and the automatic specimen heating holder to move
To the detection device, in order to the laser after condenser lens focusing can direct irradiation to automatic specimen heating holder
On sludge to be measured.
4. the on-line detecting system of drainage pipeline Heavy Metals in Sludge according to claim 1, characterized in that the grid
When carrying out coarse filtration to the sludge in drainage pipeline, used is the following a quarter in drainage pipeline mud face to half depth
Sludge in range.
5. a kind of online test method of drainage pipeline Heavy Metals in Sludge, characterized in that include the following steps:
A, randomly select five sampled points, each sampled point in drainage pipeline the following a quarter in mud face to half depth
Sludge is taken in range；
B, so that taken sludge is carried out coarse filtration through grid, sludge is extracted to vibrating screen via sludge pump carry out fine filtering later；
C, the sludge after fine filtering is stirred through the stirring module in Mortar spraying machine first, by spray module that sludge is equal later
Even to be sprayed on automatic specimen heating holder, sludge is heated on automatic specimen heating holder and is dried to drying regime；
D, YAG laser emits laser, and laser is refracted on condenser lens after total reflective mirror reflects with 45° angle；Line focus lens
In laser irradiation to the sludge to be measured of automatic specimen heating holder after focusing, laser breakdown sludge to be measured forms plasma；
E, generated plasma and it is transmitted to spectrometer in fibre-optical probe acquisition step d, spectrometer reception optical fiber probe is adopted
The plasma that collects simultaneously converts light signals into electric signal and is then transmit to computer；Computer is according to transmitted by spectrometer
Signal carries out qualitative and quantitative detection analysis to the heavy metal in drainage pipeline sludge.
6. the online test method of drainage pipeline Heavy Metals in Sludge according to claim 5, characterized in that in step d,
Automatic specimen heating holder is placed on rotating platform, drives automatic specimen heating holder to rotate by rotating platform, and then can make through poly-
On laser uniform irradiation to the sludge to be measured of automatic specimen heating holder after focus lens focusing.
7. the online test method of drainage pipeline Heavy Metals in Sludge according to claim 6, characterized in that step c it
Afterwards, rotating platform is carried by motorized rails and automatic specimen heating holder moves to the position opposite with condenser lens, so as to line focus
Laser after lens focus can be on direct irradiation to the sludge to be measured of automatic specimen heating holder.
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| CN110357382A (en) * | 2019-07-19 | 2019-10-22 | 中矿（天津）岩矿检测有限公司 | A kind of Treatment of Sludge conveying device and its application method may filter that moisture |
| CN110426347A (en) * | 2019-09-04 | 2019-11-08 | 中绿环保科技股份有限公司 | Anti-attenuation photoelectricity regulating water quality monitor |
| CN113866205A (en) * | 2021-12-06 | 2021-12-31 | 天津海关动植物与食品检测中心 | Chinese herbal medicine fluorescence spectrum heavy metal detection device and detection method |
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| CN113866205A (en) * | 2021-12-06 | 2021-12-31 | 天津海关动植物与食品检测中心 | Chinese herbal medicine fluorescence spectrum heavy metal detection device and detection method |
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| CN109520974B (en) | 2023-10-17 |
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