CN114324805A - Online monitoring system and method for contraband in sewage - Google Patents
Online monitoring system and method for contraband in sewage Download PDFInfo
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Abstract
The invention provides an online monitoring system and a method for contraband in sewage, wherein the online monitoring system for the contraband in the sewage comprises an analyzer; the pretreatment device filters collected sewage; the inlet of the sample cell is connected with the pretreatment device, and the outlet of the sample cell is connected with the first multi-channel direction selection valve; the first pump is connected with the common end of the first multi-channel direction selection valve, and the ports of the first multi-channel direction selection valve are communicated with a plurality of containers; the port of the first multi-way valve is respectively connected with the ports of the first multi-way direction selection valve and the second multi-way valve; the port of the second multi-way valve is connected with an analyzer; the port of the second multi-channel option valve is connected with a plurality of mobile phases, and the common end of the second multi-channel option valve is connected with the port of the first multi-way valve; one end of the enrichment unit is connected with the second multi-way valve, and the other end of the enrichment unit is connected with the third multi-way valve; the first quantitative ring is arranged between the first pump and the common end of the second multi-channel option valve, and two ends of the second quantitative ring are respectively connected with the port of the first multi-way valve; and the ports of the third multi-way valve are communicated with carrier liquid. The invention has the advantages of automation, accuracy and the like.
Description
Technical Field
The invention relates to sewage monitoring, in particular to an online monitoring system and method for contraband in sewage.
Background
The sewage virus inspection is a novel virus inhibition scientific and technological means, can calculate data such as the types, consumption, the sizes of virus addicts and the like of abused drugs in a specific area in a reverse mode, can provide necessary guidance for public security virus inhibition work, and has important significance in promoting the development of the whole-society virus inhibition work.
In order to accurately estimate the drug consumption, the key link is to quickly obtain the accurate content of the drugs in the sewage. The existing sewage drug detection is completed in a laboratory, and the method for detecting the drug content in the sewage in the laboratory usually adopts off-line SPE extraction purification, so that the technology has many defects, such as:
1. the sample pretreatment operation process is complex, the operation time is long, the analysis efficiency is low, sewage samples need to be collected at regular intervals at sewage treatment plants in cities and sewage channels and other places in remote areas, the sampling environment is severe, the sample storage is difficult, the data has serious hysteresis, and the real-time tracing can not be realized.
2. Due to long-term working in drug tests or samples containing drug components, cross contamination of trace samples, such as biological samples and sewage, may occur, and the health of laboratory testing personnel may be affected.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an online monitoring method for contraband in sewage.
The purpose of the invention is realized by the following technical scheme:
the method for monitoring contraband in sewage on line comprises the following steps:
(A1) collecting sewage, conveying the sewage to a pretreatment device, removing particulate matters in the sewage, and then conveying the sewage to a sample pool;
(A2) by switching a first multi-channel direction selection valve, a first pump respectively extracts an internal standard and acid and sends the internal standard and the acid into the sample cell;
(A3) the first multi-channel direction selection valve is switched with the first multi-way valve, the first pump pumps the mixed liquid in the sample tank and sends the mixed liquid to the second quantitative ring, and two ends of the second quantitative ring are respectively connected with the port of the first multi-way valve;
(A4) the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, the mixed liquid in the second quantitative ring is sent into the activated enrichment unit by using carrier liquid, and two ends of the enrichment unit are respectively connected with ports of the second multi-way valve and the third multi-way valve;
(A5) and the second multi-way valve and the third multi-way valve are switched, the mobile phase elutes the sample in the enrichment unit to an analyzer, and the analyzer outputs forbidden object information in the sewage.
The invention also aims to provide an online monitoring system for contraband in sewage, and the invention aims to be realized by the following technical scheme:
the online monitoring system for contraband in sewage comprises an analyzer; the online monitoring system for contraband in sewage further comprises:
the pretreatment device is used for filtering the collected sewage;
the inlet of the sample cell is connected with the pretreatment device, and the outlet of the sample cell is connected with the port of the first multi-channel direction selection valve;
the multi-channel control system comprises a first multi-channel selector valve and a first pump, wherein the first pump is connected with a common end of the first multi-channel selector valve, and ports of the first multi-channel selector valve are communicated with a plurality of containers;
the port of the first multi-way valve is respectively connected with the ports of the first multi-way direction selection valve and the second multi-way valve; the port of the second multi-way valve is connected with the analyzer;
the port of the second multi-channel option valve is connected with multiple mobile phases, and the common end of the second multi-channel option valve is connected with the port of the first multi-way valve;
one end of the first enrichment unit is connected with the second multi-way valve, and the other end of the first enrichment unit is connected with the third multi-way valve;
the first quantitative ring is arranged between the common ends of the first pump and the second multi-channel option valve, and two ends of the second quantitative ring are respectively connected with the ports of the first multi-way valve;
and the ports of the third multi-way valve are communicated with carrier liquid.
Compared with the prior art, the invention has the beneficial effects that:
1. automation;
the full process is highly automated: automatic water collection, automatic pretreatment, automatic data processing and uploading, and real unattended sewage contraband detection is realized;
2. real-time and efficient;
the whole process only needs 40min from water collection to data output, the content of contraband in the sewage can be fed back in real time, and the drug consumption can be accurately estimated;
3. the accuracy is high;
the sample is collected and measured, so that the degradation of the sample can be effectively reduced; the full-automatic pretreatment can reduce human errors, and the detection result is more accurate and closer to the true value.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a schematic flow chart of a method for on-line monitoring contraband in sewage according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of explaining the technical solution of the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
the method for monitoring contraband in sewage on line comprises the following steps:
(A1) collecting sewage, conveying the sewage to a pretreatment device, removing impurities such as particulate matters in the sewage through sedimentation, multi-stage filtration and the like, and then conveying the sewage to a sample pool;
(A2) by switching a first multi-channel direction selection valve, a first pump respectively extracts an internal standard and acid and sends the internal standard and the acid into the sample cell; the structure and working mode of the multi-channel direction selection valve are the prior art in the field;
(A3) the first multi-channel direction selection valve is switched with the first multi-way valve, the first pump pumps the mixed liquid in the sample tank and sends the mixed liquid to the second quantitative ring, and two ends of the second quantitative ring are respectively connected with the port of the first multi-way valve;
(A4) the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, the mixed liquid in the second quantitative ring is sent into the activated enrichment unit by using carrier liquid, and two ends of the enrichment unit are respectively connected with ports of the second multi-way valve and the third multi-way valve;
(A5) the second and third multi-way valves are switched and the mobile phase elutes the sample in the enrichment cell to an analyzer, such as a mass spectrometer, which outputs contraband information in the wastewater.
In order to ensure that the monitoring can be carried out normally, further, the online monitoring method for contraband in sewage further comprises the following steps:
switching a first multi-channel selection valve, and pumping a quality control sample by a first pump;
the first multi-channel direction selection valve and the first multi-way valve are switched, and the first pump sends the extracted quality control sample to the second quantitative ring;
the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, and the carrier liquid sends the quality control sample in the second quantitative ring to the enrichment unit;
the third multi-way valve and the second multi-way valve are switched, the mobile phase elutes the quality control sample in the enrichment unit to an analyzer, and the analyzer outputs quality control sample information;
and if the deviation between the quality control sample information and the nominal information is in a set range, carrying out normal monitoring on the sewage.
In order to ensure the accuracy of the monitoring result, further, before the first pump pumps the quality control sample or the internal standard, the first multi-channel selector valve is switched, the first pump pumps pure water, and the pipeline is cleaned; thereafter, the first pump extracts a quality control sample.
In order to allow the reaction to proceed sufficiently, in step (a2), the first multi-channel selector valve is switched, the first pump draws air and sends the air to the sample cell, and the mixture is stirred.
For activating the enrichment unit, further, the activation mode of the enrichment unit is:
and by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, the methanol and the pure water are respectively discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve, so that the enrichment unit is activated.
In order to push the mixed liquid, further, pure water is discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, so that the mixed liquid in the second quantitative ring is sent to the enrichment unit.
To rinse the enrichment unit, further, in step (a4), the methanol water is discharged through the second multi-channel selector valve, the second multi-way valve, the enrichment unit, and the third multi-way valve by switching the second multi-channel selector valve, the first multi-way valve, the second multi-way valve, and the third multi-way valve, thereby completing the rinsing.
The online monitoring system for contraband in sewage comprises:
analyzers, such as mass spectrometers, or combined chromatography and mass spectrometers;
a pretreatment device such as a combination of a grit chamber and a filter for filtering the collected sewage;
the inlet of the sample cell is connected with the pretreatment device, and the outlet of the sample cell is connected with the port of the first multi-channel direction selection valve;
the multi-channel directional control device comprises a first multi-channel directional control valve and a first pump, wherein the first pump is connected with a common end of the first multi-channel directional control valve, a port of the first multi-channel directional control valve is communicated with a plurality of containers, and the containers are respectively used for containing quality control samples, hydrochloric acid, waste liquid, standard liquid and pure water;
the port of the first multi-way valve is respectively connected with the ports of the first multi-way direction selection valve and the second multi-way valve; the port of the second multi-way valve is connected with the analyzer;
the port of the second multi-channel option valve is connected with a plurality of mobile phases such as pure water, methanol and methanol water, and the common end of the second multi-channel option valve is connected with the port of the first multi-way valve;
one end of the first enrichment unit is connected with the second multi-way valve, and the other end of the first enrichment unit is connected with the third multi-way valve;
the first quantitative ring is arranged between the common ends of the first pump and the second multi-channel option valve, and two ends of the second quantitative ring are respectively connected with the ports of the first multi-way valve;
and the ports of the third multi-way valve are communicated with carrier liquid, such as pure water.
Example 2:
the system and the method for monitoring contraband in sewage on line are applied to the embodiment 1 of the invention.
In this application example, as shown in fig. 1, the method for on-line monitoring contraband in sewage includes the following steps:
(A1) collecting sewage, conveying the sewage to a pretreatment device, standing in a sedimentation tank for 10-20min, then removing impurities such as particulate matters in the sewage through filters with filtering precision of 100 micrometers and 0.45 micrometers respectively, and then conveying the sewage to a sample tank;
when sewage is pretreated, the first multi-channel direction selection valve is switched, the first pump pumps pure water, and the pipeline is repeatedly cleaned;
switching a first multi-channel direction selection valve, pumping a quality control sample by a first pump, and enabling the quality control sample to enter a first quantitative ring;
the first multi-channel direction selection valve and the first multi-way valve are switched, the first pump sends the quality control sample in the first quantitative ring to the second quantitative ring, and two ends of the second quantitative ring are respectively communicated with the port of the first multi-way valve;
the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, and the carrier liquid sends the quality control sample in the second quantitative ring to the activated enrichment unit; the enrichment unit adopts an SPE column, and two ends of the enrichment unit are respectively connected with a second multi-way valve and a third multi-way valve;
the third multi-way valve and the second multi-way valve are switched, the flow phase flows through the third multi-way valve, the enrichment unit and the second multi-way valve in turn, the quality control sample in the enrichment unit is eluted to an analyzer-mass spectrometer, and the analyzer outputs quality control sample information;
if the deviation between the quality control sample information and the nominal information is in a set range, carrying out normal monitoring on the sewage;
(A2) the first multi-channel direction selection valve is switched, the first pump pumps pure water, and the pipeline is repeatedly cleaned;
by switching the first multi-channel direction selection valve, the first pump respectively pumps the internal standard, the acid and the air and sends the internal standard, the acid and the air into the sample cell, and the air entering the sample cell stirs the mixed solution, so that the reaction is promoted; the structure and working mode of the multi-channel direction selection valve are the prior art in the field;
(A3) the first multi-channel direction selection valve is switched with the first multi-way valve, and the first pump pumps the mixed liquid in the sample pool and sends the mixed liquid to the second quantitative ring;
(A4) the first multi-way valve, the second multi-way valve, the third multi-way valve and the second multi-way direction selection valve are used for switching, and the methanol and the pure water sequentially pass through the second multi-way direction selection valve, the first multi-way valve, the second multi-way valve, the enrichment unit and the third multi-way valve for two times to complete the activation of the enrichment unit;
the first multi-way valve, the second multi-way valve, the third multi-way valve and the second multi-way direction selection valve are switched, and pure water passes through the second multi-way direction selection valve to push the mixed liquid in the second quantitative ring to sequentially pass through the first multi-way valve and the second multi-way valve and enter the activated enrichment unit;
(A5) by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, methanol water is discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve, so that leaching of the enrichment unit is completed;
and switching the second multi-way valve and the third multi-way valve, carrying out gradient elution, eluting the sample in the enrichment unit to an analyzer by using a mobile phase, and outputting forbidden object information in the sewage by the analyzer.
The results obtained for the multiple tests are shown in the following table;
the online monitoring system for contraband in sewage of the embodiment of the invention, namely the system for realizing the online monitoring method of the embodiment of the invention, comprises:
an analyzer, using a mass spectrometer;
the combination of a pretreatment device, a grit chamber and a secondary filter is used for filtering impurities such as particles in sewage, and the filtering precision of the secondary filter is 100 micrometers and 0.45 micrometer respectively;
the inlet of the sample cell is connected with the pretreatment device, and the outlet of the sample cell is connected with the port of the first multi-channel direction selection valve;
the multi-channel directional control device comprises a first multi-channel directional control valve and a first pump, wherein the first pump is connected with a common end of the first multi-channel directional control valve, a port of the first multi-channel directional control valve is communicated with air and a plurality of containers, and the containers are respectively used for containing quality control samples, hydrochloric acid, waste liquid, standard liquid and pure water;
the port of the first multi-way valve is respectively connected with the ports of the first multi-way direction selection valve and the second multi-way valve; the port of the second multi-way valve is connected with the analyzer;
the port of the second multi-channel option valve is connected with a plurality of mobile phases such as pure water, methanol and methanol water, and the common end of the second multi-channel option valve is connected with the port of the first multi-way valve;
the first enrichment unit adopts an SPE column, one end of the first enrichment unit is connected with the second multi-way valve, and the other end of the first enrichment unit is connected with the third multi-way valve;
the first quantitative ring is arranged between the common ends of the first pump and the second multi-channel option valve, and two ends of the second quantitative ring are respectively connected with the ports of the first multi-way valve;
and the ports of the third multi-way valve are communicated with carrier liquid, such as pure water.
The above embodiments are merely exemplary, as the analyzer employs a mass spectrometer, although other scenarios are possible, such as a combination of a chromatography column and a mass spectrometer.
Claims (10)
1. The method for monitoring contraband in sewage on line comprises the following steps:
(A1) collecting sewage, conveying the sewage to a pretreatment device, removing particulate matters in the sewage, and then conveying the sewage to a sample pool;
(A2) by switching a first multi-channel direction selection valve, a first pump respectively extracts an internal standard and acid and sends the internal standard and the acid into the sample cell;
(A3) the first multi-channel direction selection valve is switched with the first multi-way valve, the first pump pumps the mixed liquid in the sample tank and sends the mixed liquid to the second quantitative ring, and two ends of the second quantitative ring are respectively connected with the port of the first multi-way valve;
(A4) the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, the mixed liquid in the second quantitative ring is sent into the activated enrichment unit by using carrier liquid, and two ends of the enrichment unit are respectively connected with ports of the second multi-way valve and the third multi-way valve;
(A5) and the second multi-way valve and the third multi-way valve are switched, the mobile phase elutes the sample in the enrichment unit to an analyzer, and the analyzer outputs forbidden object information in the sewage.
2. The method for on-line monitoring of contraband in wastewater according to claim 1, further comprising:
switching a first multi-channel selection valve, and pumping a quality control sample by a first pump;
the first multi-channel direction selection valve and the first multi-way valve are switched, and the first pump sends the extracted quality control sample to the second quantitative ring;
the first multi-way valve, the second multi-way valve and the third multi-way valve are switched, and the carrier liquid sends the quality control sample in the second quantitative ring to the enrichment unit;
the third multi-way valve and the second multi-way valve are switched, the mobile phase elutes the quality control sample in the enrichment unit to an analyzer, and the analyzer outputs quality control sample information;
and if the deviation between the quality control sample information and the nominal information is in a set range, carrying out normal monitoring on the sewage.
3. The method of claim 2, wherein the first pump switches the first multi-channel selector valve before the quality control sample or the internal standard is pumped, the first pump pumps pure water and cleans the pipeline; thereafter, the first pump extracts a quality control sample.
4. The method for on-line monitoring contraband in sewage of claim 1, wherein in step (A2), the first multi-channel selector valve is switched, the first pump pumps air and sends the air to the sample pool, and the mixed liquid is stirred.
5. The method for on-line monitoring contraband in sewage according to claim 1, wherein the activation mode of the enrichment unit is as follows:
and by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, the methanol and the pure water are respectively discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve, so that the enrichment unit is activated.
6. The method of claim 1, wherein pure water is discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, so that the mixed liquid in the second quantitative ring is delivered to the enrichment unit.
7. The method for on-line monitoring of contraband in wastewater as claimed in claim 1, wherein in step (a4), the methanol water is discharged through the second multi-channel direction selection valve, the second multi-way valve, the enrichment unit and the third multi-way valve by switching the second multi-channel direction selection valve, the first multi-way valve, the second multi-way valve and the third multi-way valve, thereby completing the leaching.
8. The online monitoring system for contraband in sewage comprises an analyzer; the system is characterized in that the online monitoring system for contraband in sewage further comprises:
the pretreatment device is used for filtering the collected sewage;
the inlet of the sample cell is connected with the pretreatment device, and the outlet of the sample cell is connected with the port of the first multi-channel direction selection valve;
the multi-channel control system comprises a first multi-channel selector valve and a first pump, wherein the first pump is connected with a common end of the first multi-channel selector valve, and ports of the first multi-channel selector valve are communicated with a plurality of containers;
the port of the first multi-way valve is respectively connected with the ports of the first multi-way direction selection valve and the second multi-way valve; the port of the second multi-way valve is connected with the analyzer;
the port of the second multi-channel option valve is connected with multiple mobile phases, and the common end of the second multi-channel option valve is connected with the port of the first multi-way valve;
one end of the first enrichment unit is connected with the second multi-way valve, and the other end of the first enrichment unit is connected with the third multi-way valve;
the first quantitative ring is arranged between the common ends of the first pump and the second multi-channel option valve, and two ends of the second quantitative ring are respectively connected with the ports of the first multi-way valve;
and the ports of the third multi-way valve are communicated with carrier liquid.
9. The system of claim 8, wherein the plurality of containers are configured to hold quality control samples, hydrochloric acid, waste solutions, standard solutions, and purified water.
10. The system of claim 8, wherein the pre-treatment device comprises a settling tank and a filter.
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