CN109520974B - Online detection system and detection method for heavy metals in drainage pipeline sludge - Google Patents
Online detection system and detection method for heavy metals in drainage pipeline sludge Download PDFInfo
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- CN109520974B CN109520974B CN201910092257.7A CN201910092257A CN109520974B CN 109520974 B CN109520974 B CN 109520974B CN 201910092257 A CN201910092257 A CN 201910092257A CN 109520974 B CN109520974 B CN 109520974B
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
Abstract
The invention provides an online detection system and a detection method for heavy metals in drainage pipeline sludge. The online detection system comprises a sludge pretreatment device and a detection device; the sludge pretreatment device can screen out the extracted sludge by impurities, and the stirring module and the spraying module can ensure that heavy metal elements in the sludge to be detected are uniformly distributed and can improve the repeatability of detection in detection, reduce the detection limit of the elements and improve the sensitivity of the elements to be detected. According to the invention, the laser-induced breakdown spectroscopy technology is combined with the spraying technology for the first time, so that the on-line detection of heavy metal elements in the drainage pipeline sludge is realized. The spraying technology is used for preparing samples, the requirements of high sensitivity, low detection limit and ultra-low concentration heavy metal pollution element rapid detection can be met on the premise of guaranteeing the uniformity of the samples, and a unique technical means can be provided for rapid detection of the heavy metal element content in the sludge.
Description
Technical Field
The invention relates to the technical field of heavy metal detection in sludge, in particular to an online detection system and method for heavy metal in drainage pipeline sludge.
Background
Currently, the commonly used methods for detecting heavy metals in sludge are generally divided into two types: atomic Absorption Spectrophotometry (AAS) and inductively coupled plasma mass spectrometry (ICP-MS). The former has the characteristics of high detection precision, strong anti-interference capability and the like, but needs normal pressure digestion and cannot detect multiple elements at the same time; the latter has high analysis speed and can detect multiple elements at the same time, but is expensive and cumbersome to operate. In contrast, laser Induced Breakdown Spectroscopy (LIBS) is increasingly used in environmental detection because of its advantages such as real-time online analysis and simultaneous detection of multiple elements.
The principle of the Laser Induced Breakdown Spectroscopy (LIBS) is that laser is focused on a sample to be tested, the sample to be tested is broken down and gasified to form plasma, a spectrometer collects the plasma and converts an optical signal into an electric signal to be transmitted to a computer, and qualitative and quantitative analysis is carried out according to characteristic spectral lines of heavy metal elements contained in the sample to be tested and a fitting curve of the concentration and spectral intensity of heavy metal contained in the sample.
Compared with other detection technologies, the laser-induced breakdown spectroscopy technology has the advantage of being capable of rapidly detecting various elements on line in real time. And the detection limit reaches ppm level, and meets the national standard of detecting heavy metals in sludge. However, the method is affected by the property of the sample to be measured, the aqueous solution contained in the sludge accelerates laser to generate plasma, and uneven distribution of heavy metal elements contained in the sludge can affect the collection of plasma signals by the spectrometer.
Disclosure of Invention
The invention aims to provide an online detection system and an online detection method for heavy metals in drainage pipeline sludge, so that qualitative and quantitative detection and analysis of the heavy metals in the drainage pipeline sludge can be performed in real time, efficiently, quickly and accurately.
The invention is realized in the following way: an online detection system for heavy metals in drainage pipeline sludge comprises a sludge pretreatment device and a detection device;
the sludge pretreatment device comprises a grid, a sludge pump, a vibrating screen, a mortar spraying machine and an automatic heating sample stage; the grid is used for carrying out rough filtration on sludge in the drainage pipeline, and the sludge pump is used for extracting the sludge subjected to rough filtration by the grid to the vibrating screen; the vibrating screen is used for carrying out fine filtration on the sludge pumped by the sludge pump; the mortar spraying machine comprises a stirring module and a spraying module; the stirring module can stir the sludge after being finely filtered by the vibrating screen to uniformly mix the sludge, and the spraying module is used for uniformly spraying the sludge after being stirred by the stirring module onto the automatic heating sample stage;
the detection device comprises a YAG laser, a total reflection mirror, a focusing lens, an optical fiber probe, a spectrometer and a computer; the YAG laser is used for emitting laser; the laser emitted by the YAG laser is reflected by the total reflection mirror and then refracted to the focusing lens at an angle of 45 degrees; the laser irradiates the sludge to be detected of the automatic heating sample stage after being focused by the focusing lens, and generates plasma; the optical fiber probe is used for collecting plasma generated by irradiating laser onto sludge to be detected and transmitting the plasma to the spectrometer, and the spectrometer is used for receiving the plasma collected by the optical fiber probe, converting an optical signal into an electric signal and transmitting the electric signal to the computer; the computer can perform qualitative and quantitative detection analysis on heavy metals in the drainage pipeline sludge according to signals sent by the spectrometer.
The automatic heating sample stage is arranged on the rotating platform, and the rotating platform can drive the automatic heating sample stage to rotate.
An electric guide rail is arranged below the rotary platform; the electric guide rail is used for driving the rotary platform and the automatic heating sample stage to move towards the detection device, so that laser focused by the focusing lens can directly irradiate on sludge to be detected of the automatic heating sample stage.
When the grid is used for carrying out rough filtration on the sludge in the drainage pipeline, the sludge in the depth range from one quarter to one half of the depth below the sludge surface of the drainage pipeline is adopted.
The YAG laser is Nd: YAG laser.
The invention also provides an online detection method of heavy metals in the drainage pipeline sludge, which comprises the following steps:
a. randomly selecting five sampling points, wherein each sampling point is used for taking sludge within a depth range from one quarter to one half below the sludge surface in the drainage pipeline;
b. coarse filtering the sludge through a grid, and then pumping the sludge to a vibrating screen through a sludge pump for fine filtering;
c. stirring the finely filtered sludge through a stirring module in a mortar spraying machine, uniformly spraying the sludge onto an automatic heating sample table through a spraying module, and heating and drying the sludge on the automatic heating sample table to a dry state; then the electric guide rail carries the rotary platform and the automatic heating sample stage to move to a position opposite to the focusing lens;
d. the YAG laser emits laser, and the laser is reflected by the total reflection mirror and then is refracted to the focusing lens at an angle of 45 degrees; the laser focused by the focusing lens irradiates on the sludge to be tested of the automatic heating sample table, and the laser breaks down the sludge to be tested and is gasified to form plasma; the automatic heating sample stage is driven to rotate by the rotating platform, so that laser focused by the focusing lens is uniformly irradiated to sludge to be detected of the automatic heating sample stage;
e. the optical fiber probe collects the plasmas generated in the step d and transmits the plasmas to the spectrometer, and the spectrometer receives the plasmas collected by the optical fiber probe, converts optical signals into electric signals and then transmits the electric signals to the computer; and the computer performs qualitative and quantitative detection and analysis on heavy metals in the sewage pipeline sludge according to signals sent by the spectrometer.
The invention has the advantages that the laser-induced breakdown spectroscopy technology is combined with the spraying technology for the first time to realize the on-line detection of the heavy metal elements in the drainage pipeline sludge by adopting the laser-induced breakdown spectroscopy technology. The spraying technology is used for preparing samples, the requirements of high sensitivity, low detection limit and ultra-low concentration heavy metal pollution element rapid detection can be met on the premise of guaranteeing the uniformity of the samples, and a unique technical means can be provided for rapid detection of the heavy metal element content in the sludge. Compared with the national standard detection method (AAS and ICP-MS), the method has the advantages of three aspects: (1) enabling on-line detection: compared with the traditional national standard detection method, the invention combines the laser-induced breakdown spectroscopy with the technologies of filtration, stirring, spraying, heating, transferring and the like, simplifies the complex sample pretreatment process and can realize on-line detection. (2) the sludge sample has better uniformity: after the sludge sample is uniformly stirred, the sludge sample is uniformly sprayed on the sample table by adopting a spraying technology, so that parameters such as sensitivity of a detection result are improved. (3) real-time performance: and the spot detection and the quick drying of the sprayed sludge sample ensure the real-time performance of the detection result.
Drawings
FIG. 1 is a schematic diagram of an on-line detection system for heavy metals in drainage pipeline sludge.
In the figure: 1. a drainage pipe; 2. a grille; 3. a sludge pump; 4. a vibrating screen; 5. a mortar spraying machine; 5-1, a stirring module; 5-2, a spraying module; 6. automatically heating the sample stage; 7. rotating the platform; 8. a YAG laser; 9. a total reflection mirror; 10. a focusing lens; 11. an optical fiber probe; 12. a spectrometer; 13. a computer; 14. an electric guide rail.
Detailed Description
Embodiment 1, an on-line detection system for heavy metals in drainage pipeline sludge.
Based on the requirement of real-time on-line detection of heavy metal content in drainage pipeline sludge, the invention adopts a laser-induced breakdown spectroscopy method, takes sludge as an object to be detected, and aims to design and build a system for real-time on-line detection of heavy metal components and content in drainage pipeline sludge so as to provide an efficient, rapid and accurate measurement method for environment detection and protection.
The invention provides an on-line detection system for heavy metals in drainage pipeline sludge, which comprises a sludge pretreatment device and a detection device; the sludge pretreatment device can screen out the extracted sludge by impurities, and the stirring module and the spraying module can ensure that heavy metal elements in the sludge to be detected are uniformly distributed and can improve the repeatability of detection in detection, reduce the detection limit of the elements and improve the sensitivity of the elements to be detected.
As shown in fig. 1, the sludge pretreatment device comprises a grid 2, a sludge pump 3, a vibrating screen 4, a mortar sprayer 5, an automatic heating sample stage 6 and a rotary platform 7. When the sludge to be measured is taken out from the drainage pipeline 1, five sampling points can be randomly selected from the drainage pipeline 1, each sampling point can sample in the depth range from one fourth to one half below the mud surface, and then samples of the five sampling points are mixed to be used as sludge samples representing average concentration. The sludge taken out from the drainage pipeline 1 is firstly subjected to rough filtration through the grating 2 so as to remove larger impurities such as garbage, wood blocks and the like in the sludge. The sludge after being strained by the grille 2 is pumped to the vibrating screen 4 by the sludge pump 3. The vibrating screen 4 filters the sludge pumped by the sludge pump 3 again, and the filtering belongs to fine filtering relative to the coarse filtering of the grating 2, namely: after passing through the vibrating screen 4, the fine impurities in the sludge can be removed. After twice filtration through the grid 2 and the vibrating screen 4, impurities in the sludge are basically removed, and the sludge is stirred and sprayed by a mortar sprayer 5.
Mortar sprayer 5 includes a stirring module 5-1 and a spraying module 5-2. The sludge filtered by the vibrating screen 4 firstly enters the stirring module 5-1 for stirring, and the stirring module 5-1 sufficiently mixes the sludge by stirring so as to make the components contained in the sludge uniform. The sludge stirred uniformly is sent to a spraying module 5-2, and the spraying module 5-2 sprays the sludge stirred uniformly onto an automatic heating sample stage 6. The spray coating range of the spray coating module 5-2 is relatively large, and the radius can reach about one meter. The self-heating sample stage 6 is opposite to the center of the spraying range of the spraying module 5-2, so that the spraying uniformity can be ensured. The self-heating sample stage 6 is embodied as a self-heating device, and the sludge sprayed thereon can be heated and dried to achieve a dry state. According to the invention, the automatic heating sample stage 6 is arranged on the rotary platform 7, the rotary platform 7 can automatically rotate, and the rotary platform 7 can drive the automatic heating sample stage 6 to rotate, so that laser can be uniformly impacted on sludge to be detected of the automatic heating sample stage 6 in a subsequent detection link.
The invention is provided with an electric guide rail 14 below the rotary platform 7. The rotary platform 7 and the automatic heating sample table 6 can be driven to move through the electric guide rail 14, and the electric guide rail can enable the sample table to be far away from the detection device during sample preparation and later cleaning of the sample table, so that pollution to the detection device due to sputtering and other reasons during sample preparation and cleaning can be effectively avoided.
The detection device comprises a YAG laser 8, a total reflection mirror 9, a focusing lens 10, an optical fiber probe 11, a spectrometer 12 and a computer 13. The YAG laser 8 is Nd: YAG laser 8 is used for emitting laser light. The laser light emitted from the YAG laser 8 is reflected by the total reflection mirror 9 and then refracted at an angle of 45 ° to the focusing lens 10, and the focusing lens 10 is used for focusing the laser light. The electric guide rail 14 moves the sludge sample to be measured to a position opposite to the focusing lens 10, and laser focused by the focusing lens 10 directly irradiates and hits the sludge to be measured on the automatic heating sample table 6, so that the laser breaks down the sludge to be measured and forms plasma. In the laser detection, the rotary table 7 is rotated, so that the laser light can be uniformly irradiated and hit on the sludge to be measured on the self-heating sample table 6. The optical fiber probe 11 irradiates laser on the sludge to be measured and breaks down plasma formed by the sludge to be measured to collect, and then transmits the plasma to the spectrometer 12. The spectrometer 12 receives the plasma collected by the optical fiber probe 11, converts the optical signal into an electric signal and transmits the electric signal to the computer 13; the computer 13 receives the signals sent by the spectrometer 12, performs data processing by utilizing spectrum analysis software such as Oceamview, MATLAB, origin and the like, and performs qualitative and quantitative detection and analysis on heavy metals in the drainage pipeline sludge.
Example 2, an on-line detection method of heavy metals in drainage pipeline sludge.
In order to overcome the defects of the prior art in sludge detection, the invention aims to realize the real-time and rapid detection of the components and the content of heavy metals in the sludge of the drainage pipeline based on the characteristics of the technology of extracting and treating the sludge in the drainage pipeline, spraying the sludge and laser-induced breakdown spectroscopy.
The invention provides an on-line detection method for heavy metals in drainage pipeline sludge, which comprises the following steps:
a. five sampling points are randomly selected, and sludge samples are taken within a depth range of one quarter to one half below the sludge surface in the drainage pipeline (namely, within a depth range of one quarter to one half of the total height of the sludge from the sludge surface). And mixing the five sludge samples to obtain a sludge sample to be measured.
b. And c, coarsely filtering the sludge sample obtained in the step a through a grid, and then pumping the sludge to a vibrating screen through a sludge pump for fine filtration. Coarse filtration generally filters out larger impurities such as garbage and wood blocks, and fine filtration generally filters out smaller impurities such as gravel and stones.
c. The sludge after fine filtration is stirred by a stirring module in the mortar spraying machine, after the stirring is uniform, the sludge is uniformly sprayed onto an automatic heating sample stage by a spraying module, the sludge is heated and dried on the automatic heating sample stage to a dry state, and then the electric guide rail carries a rotating platform and the automatic heating sample stage to move to a position where the sludge to be detected is opposite to a focusing lens.
d. The YAG laser emits laser, and the laser is reflected by the total reflection mirror and then is refracted to the focusing lens at an angle of 45 degrees; the laser focused by the focusing lens irradiates the sludge to be tested of the automatic heating sample stage, and the laser breaks down the sludge to be tested and forms plasma. When the laser irradiates the sludge to be measured, the automatic heating sample table is driven to rotate through the rotating platform, so that the laser is uniformly hit on the sludge to be measured.
e. The optical fiber probe collects the plasmas generated in the step d and transmits the plasmas to the spectrometer, and the spectrometer receives the plasmas collected by the optical fiber probe, converts optical signals into electric signals and then transmits the electric signals to the computer; and the computer performs data processing by utilizing spectrum analysis software such as Oceamview, MATLAB, origin and the like according to signals sent by the spectrometer, and performs qualitative and quantitative detection and analysis on heavy metals in the sewage pipeline sludge.
Claims (4)
1. An online detection system for heavy metals in drainage pipeline sludge is characterized by comprising a sludge pretreatment device and a detection device;
the sludge pretreatment device comprises a grid, a sludge pump, a vibrating screen, a mortar spraying machine and an automatic heating sample stage; the grid is used for carrying out rough filtration on sludge in the drainage pipeline, and the sludge pump is used for extracting the sludge subjected to rough filtration by the grid to the vibrating screen; the vibrating screen is used for carrying out fine filtration on the sludge pumped by the sludge pump; the mortar spraying machine comprises a stirring module and a spraying module; the stirring module can stir the sludge after being finely filtered by the vibrating screen to uniformly mix the sludge, and the spraying module is used for uniformly spraying the sludge after being stirred by the stirring module onto the self-heating sample stage;
the detection device comprises a YAG laser, a total reflection mirror, a focusing lens, an optical fiber probe, a spectrometer and a computer; the YAG laser is used for emitting laser; the laser emitted by the YAG laser is reflected by the total reflection mirror and then refracted to the focusing lens at an angle of 45 degrees; the laser irradiates the sludge to be detected of the automatic heating sample stage after being focused by the focusing lens, and generates plasma; the optical fiber probe is used for collecting plasma generated by irradiating laser onto sludge to be detected and transmitting the plasma to the spectrometer, and the spectrometer is used for receiving the plasma collected by the optical fiber probe, converting an optical signal into an electric signal and transmitting the electric signal to the computer; the computer can perform qualitative and quantitative detection analysis on heavy metals in the drainage pipeline sludge according to signals sent by the spectrometer;
the automatic heating sample platform is arranged on a rotating platform, and the rotating platform can drive the automatic heating sample platform to rotate;
an electric guide rail is arranged below the rotary platform; the electric guide rail is used for driving the rotary platform and the automatic heating sample stage to move towards the detection device so that laser focused by the focusing lens can directly irradiate on sludge to be detected of the automatic heating sample stage;
when the grid is used for carrying out rough filtration on the sludge in the drainage pipeline, the sludge in the depth range from one quarter to one half of the depth below the sludge surface of the drainage pipeline is adopted.
2. The on-line detection method for heavy metals in drainage pipeline sludge is characterized by comprising the following steps of:
a. randomly selecting five sampling points, wherein each sampling point is used for taking sludge within a depth range from one quarter to one half below the sludge surface in the drainage pipeline;
b. coarse filtering the sludge through a grid, and then pumping the sludge to a vibrating screen through a sludge pump for fine filtering;
c. stirring the finely filtered sludge through a stirring module in a mortar spraying machine, uniformly spraying the sludge onto an automatic heating sample table through a spraying module, and heating and drying the sludge on the automatic heating sample table to a dry state;
d. the YAG laser emits laser, and the laser is reflected by the total reflection mirror and then is refracted to the focusing lens at an angle of 45 degrees; the laser focused by the focusing lens irradiates the sludge to be tested of the automatic heating sample table, and the laser breaks down the sludge to be tested to form plasma;
e. the optical fiber probe collects the plasmas generated in the step d and transmits the plasmas to the spectrometer, and the spectrometer receives the plasmas collected by the optical fiber probe, converts optical signals into electric signals and transmits the electric signals to the computer; and the computer performs qualitative and quantitative detection and analysis on heavy metals in the sewage pipeline sludge according to signals sent by the spectrometer.
3. The method for on-line detection of heavy metals in drainage pipeline sludge according to claim 2, wherein in the step d, the automatic heating sample stage is arranged on the rotating platform, and the automatic heating sample stage is driven to rotate by the rotating platform, so that laser focused by the focusing lens can be uniformly irradiated on sludge to be detected of the automatic heating sample stage.
4. The method for on-line detection of heavy metals in drainage pipeline sludge according to claim 3, wherein after step c, the electric guide rail carries the rotary platform and the self-heating sample stage to a position opposite to the focusing lens, so that the laser focused by the focusing lens can directly irradiate the sludge to be detected on the self-heating sample stage.
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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 |
| CN113866205B (en) * | 2021-12-06 | 2022-02-18 | 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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