Method and system for detecting elements in sewage
By separating sewage samples and combining different testing equipment, the problem of incomplete element detection in sewage is solved, fast and accurate sewage element analysis is achieved, and accurate locking of the source of pollution is promoted.
Patent Information
- Application Number
- CN202510389015.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-31
- Publication Date
- 2025-07-11
AI Technical Summary
The prior art is difficult to quickly and comprehensively detect elements in sewage, resulting in inaccurate detection results and inefficient efficiency.
By filtering the sewage sample, the supernatant and insoluble matter are separated, and the element detection is carried out using different detection equipment and methods, including the use of inductively coupled plasma atomic emission spectrometer and fluorescence spectrometer, combined with standard curve correction and data integration, to achieve comprehensive detection of elements in the sewage.
It realizes rapid and comprehensive sewage element detection, shortens the detection time to within 3 hours, and the accuracy reaches the ppm level, which can accurately determine the source of pollution, and improves detection efficiency and accuracy.
Smart Images
Figure CN120294279A_ABST
Abstract
Description
Technical Field
[0001] The present disclosure relates to the technical field of sewage treatment, and particularly to a method and system for detecting elements in sewage. Background Art
[0002] In the field of environmental governance, efficient and convenient detection of the elemental composition and accurate content of polluted water quality can more accurately locate the pollution source, and at the same time can judge the development speed and direction of the pollution source, which is of great significance for sewage treatment. Since the sources of sewage are complex and there are many types of elements, such as conventional ions, heavy metals, radioactive elements, organic substances, etc., how to quickly and efficiently analyze the sewage quality accurately is a difficult problem that needs to be solved urgently. Summary of the Invention
[0003] One technical problem to be solved by the present disclosure is to quickly and comprehensively detect elements in sewage.
[0004] To solve the above technical problem, an embodiment of the present disclosure provides a method for detecting elements in sewage, including the following steps: filtering a sewage sample to obtain a supernatant and insoluble matter; detecting elements in the supernatant to obtain a first detection result; detecting elements in the insoluble matter to obtain a second detection result; integrating the first detection result and the second detection result to obtain the types and contents of elements in the sewage sample.
[0005] In some embodiments, before filtering the sewage sample, the sewage sample is weighed to make it greater than a preset weight.
[0006] In some embodiments, detecting elements in the supernatant to obtain a first detection result includes the following steps: using the supernatant to prepare spiked samples and parallel samples, and simultaneously preparing a blank sample; establishing a standard curve with the spiked samples and correcting the standard curve with the blank sample; obtaining the first detection result according to the matching situation between the parallel samples and the corrected standard curve.
[0007] In some embodiments, using the supernatant to prepare spiked samples includes the following steps: equally dividing the supernatant into multiple volumetric flasks; adding a standard solution with a preset concentration into each volumetric flask; making up the volume with ultrapure water, shaking well and standing still to obtain multiple spiked samples.
[0008] In some embodiments, an inductively coupled plasma atomic emission spectrometer is used to detect elements in the supernatant.
[0009] In some embodiments, detecting elements in the insoluble matter to obtain a second detection result includes the following steps: making the insoluble matter into a sample; using a fluorescence spectrometer to detect the sample to obtain a second detection result.
[0010] In some embodiments, the fluorescence spectrometer is an X-ray fluorescence spectrometer, and the Quant As method is used to detect the sample.
[0011] In some embodiments, the insoluble matter is made into a sample, including the following steps: laying boric acid, the insoluble matter, and boric acid in sequence in the sample ring of the press; pressing for a set time to obtain the sample.
[0012] In some embodiments, integrating the first detection result and the second detection result to obtain the types and contents of elements in the sewage sample, including the following process: accumulating the types of elements in the first detection result and the second detection result; accumulating the contents of elements with the same type of element.
[0013] The embodiments of the present disclosure also provide a detection system for elements in sewage, including a memory, a processor, and a computer program stored on the memory. The processor executes the computer program to implement the steps of the above-mentioned method for detecting elements in sewage.
[0014] Through the above technical solutions, the method for detecting elements in sewage provided by the present disclosure takes into account the diverse types of elements in sewage, the different existing forms of the same element, and the complex matrix. First, the sewage is separated to obtain the supernatant and the insoluble matter, and then the elements in the supernatant and the insoluble matter are detected respectively. The methods and equipment used in the two detection processes are different, so they can be carried out in parallel, greatly shortening the detection time, improving the detection efficiency, avoiding missed detection of elements, making the detection more comprehensive, and analyzing the sample with high-precision instruments to make the detection results more accurate. Description of the Drawings
[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present disclosure or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present disclosure. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.
[0016] Figure 1 It is a schematic diagram of the basic process of the method for detecting elements in sewage disclosed in the embodiments of the present disclosure;
[0017] Figure 2 It is a schematic diagram of the process of obtaining the first detection result disclosed in the embodiments of the present disclosure;
[0018] Figure 3 It is a schematic diagram of the process of obtaining the second detection result disclosed in the embodiments of the present disclosure. Detailed Embodiments
[0019] The following further describes in detail the embodiments of the present disclosure in conjunction with the accompanying drawings and examples. The detailed description and drawings of the following examples are used to exemplarily illustrate the principles of the present disclosure, but cannot be used to limit the scope of the present disclosure. The present disclosure can be implemented in many different forms, not limited to the specific embodiments disclosed herein, but including all technical solutions falling within the scope of the claims.
[0020] The present disclosure provides these examples to make the present disclosure thorough and complete, and to fully convey the scope of the present disclosure to those skilled in the art. It should be noted that: unless otherwise specifically stated, the relative arrangements of components and steps, the components of materials, numerical expressions and values set forth in these examples should be construed as merely exemplary, rather than as limitations.
[0021] It should be noted that in the description of the present disclosure, unless otherwise specified, "a plurality of" means greater than or equal to two; the orientation or positional relationships indicated by terms such as "upper", "lower", "left", "right", "inner", "outer", etc. are only for the convenience of describing the present disclosure and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus cannot be construed as a limitation of the present disclosure. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.
[0022] In addition, the "first", "second" and similar terms used in the present disclosure do not denote any order, quantity or importance, but are only used to distinguish different parts. "Vertical" is not strictly vertical, but within the allowable error range. "Parallel" is not strictly parallel, but within the allowable error range. Terms such as "comprising" or "including" mean that the elements before the term cover the elements listed after the term, and do not exclude the possibility of also covering other elements.
[0023] It should also be noted that in the description of the present disclosure, unless otherwise clearly specified and limited, the terms "mounted", "connected" and "coupled" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected, or indirectly connected through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present disclosure can be understood according to specific circumstances. When it is described that a specific device is located between a first device and a second device, there may or may not be an intermediate device between the specific device and the first device or the second device.
[0024] All terms used in this disclosure have the same meanings as those understood by those of ordinary skill in the art to which this disclosure pertains, unless otherwise specifically defined. It should also be understood that terms defined in a general dictionary, such as those, should be interpreted to have meanings consistent with their meanings in the context of the relevant art, and should not be interpreted in an idealized or overly formal sense, unless specifically defined as such herein.
[0025] Technologies, methods, and devices known to those of ordinary skill in the relevant art may not be discussed in detail, but where appropriate, the technologies, methods, and devices should be regarded as part of the specification.
[0026] Sewage mainly comes from domestic sewage (feces, detergents, food residues) and industrial wastewater (heavy metals, petroleum, organic solvents), resulting in a diverse variety of elements it contains, such as metals (lead, cadmium), non-metals (sulfur, phosphorus), radioactive isotopes (iodine-129, cesium-137), and organic pollutants. Among them, under the action of microorganisms, the elemental forms will change (for example, ammonia nitrogen can become nitrate nitrogen). In addition, the concentration differences of different elements are very large. For example, the concentrations of radioactive elements (tritium, cesium-137) can be as low as ppt level, while ammonia nitrogen exceeds 1000 mg / L, and suspended particles will also cause local enrichment of elements (such as heavy metals adsorbed on sludge), thus making the elemental distribution uneven. At the same time, in addition to the above elements, sewage also contains suspended solids, oils, microorganisms, etc.
[0027] From the above description, it can be seen that the coexisting substances in sewage are numerous, making the matrix complex, and thus the matrix effect is significant when detecting the elemental content in sewage. For example, high salinity (Cl - 、SO 2- ) interferes with mass spectrometry detection, and organic substances cause background absorption or chromatographic column contamination. Among them, background absorption is the absorption or scattering of the light source radiation by non-target elements or molecules, resulting in the measurement signal deviating from the true value; chromatographic column contamination refers to the irreversible deposition of analytes, matrix components, or environmental impurities on the inner wall of the stationary phase / column tube during the analysis process, resulting in a decrease in column efficiency, retention time drift, and attenuation of detection sensitivity. Therefore, when detecting the elements in sewage, it is necessary to focus on the complexity of sewage. Otherwise, the accuracy of the detection results will be greatly affected.
[0028] In view of the above situation, in order to accurately and quickly obtain the composition and content of elements in sewage, please refer to Figures 1 to 3 , and the following detection scheme of steps S0 to S3 is proposed.
[0029] S0. Obtain a sewage sample. After obtaining the sewage sample, first weigh it. Only when the weighed weight is greater than the preset weight can the detection be carried out. Since there are components with relatively large masses such as sediment and heavy metals in the sewage, when the weight is insufficient, other elements may be missed, and a complete sample cannot be obtained, thus making it impossible to accurately detect the elements. Therefore, the detection needs to be carried out under the condition of meeting the preset weight requirement. In this embodiment, the preset weight is 500 ml. When the total weight of the sewage sample ≥ 500 ml, the following detection steps are carried out.
[0030] S1. Filter the sewage sample to obtain supernatant and insoluble substances. Specifically, first use a centrifuge to centrifuge the sewage sample to separate the suspended matter and the liquid, and then use a filter to filter to obtain filter residue and filtrate. The supernatant is obtained from the filtrate, and the insoluble substances are obtained from the filter residue. In this embodiment, the centrifuge is a centrifuge. The pretreatment of the sample such as centrifugation and filtration takes about 10 minutes.
[0031] Since it is considered that the same element may exist in different forms, the sewage sample is separated. For example, metal elements exist in the form of free ions (such as Cu 2+ ), complexes (such as combined with humic acid), or particulate state (such as adsorbed by suspended matter), etc., and nitrogen elements exist in the form of ammonia nitrogen (NH / NH4 + ), nitrate nitrogen (NO3 - / NO2 - ), and organic nitrogen (such as proteins, urea). Therefore, the sewage sample is separated and filtered to obtain liquid and solid forms, and then the elements in the supernatant and insoluble substances are detected simultaneously, and the obtained detection results are more comprehensive and accurate. For example, in addition to obtaining its water-soluble trace elements, the elemental composition in the sediment can also be obtained. Compared with only considering the element content in the supernatant, the method proposed by the present invention considers more comprehensively and has higher detection accuracy.
[0032] S2. Treat the supernatant and insoluble substances simultaneously, and detect their element contents and types respectively. The present invention uses different treatment processes and equipment to detect the supernatant and insoluble substances respectively, which can be carried out simultaneously, thereby improving the efficiency of element detection.
[0033] Among them, please refer to Figure 2 , detect the elements in the supernatant to obtain the first detection result. The steps are as follows:
[0034] First, prepare spiked samples and parallel samples using the supernatant, and also prepare blank samples. Among them, the standard addition method is used to prepare spiked samples. Specifically: divide the supernatant equally into multiple volumetric flasks. In this embodiment, 100 mL volumetric flasks are used, and 5 volumetric flasks are set. Add a standard solution with a preset concentration to each volumetric flask. In this embodiment, the standard solution with a preset concentration refers to the mixed standard solution preparation table obtained from Table 1 below, with the unit of μL. Dilute to the mark with ultrapure water so that the volume in each volumetric flask reaches 500 mL, and then shake well and let stand to obtain multiple spiked samples, that is, 5 spiked samples. In addition, parallel samples are prepared using the supernatant, and blank samples are prepared using ultrapure water. In this embodiment, 2 parallel samples are set, which are obtained by adding the supernatant to two 100 mL volumetric flasks; 1 blank sample is set, which is obtained by adding ultrapure water to a 100 mL volumetric flask.
[0035] Table 1 Mixed standard solution preparation table
[0036] Absorb the elements of the standard sample Standard sample 1 Standard sample 2 Standard sample 3 Standard sample 4 Standard sample 5 Na 0 10 20 50 100 K 0 10 20 50 100 Al 0 10 20 50 100 Ti 0 10 20 50 100 Cr 0 10 20 50 100 Mn 0 10 20 50 100 Fe 0 10 20 50 100 Co 0 10 20 50 100 Ni 0 10 20 50 100 Cu 0 10 20 50 100 Pb 0 10 20 50 100 Cd 0 10 20 50 100 Mg 0 200 500 1000 1500 Ba 0 10 20 50 100 Sr 0 50 100 300 500 Zn 0 10 20 50 100 Hg 0 10 20 50 100 As 0 10 20 50 100 Sb 0 10 20 50 100 Li 0 10 20 50 100
[0037] After that, establish a standard curve using the spiked samples and correct the standard curve using the blank samples. Finally, obtain the first test result according to the matching situation between the parallel samples and the corrected standard curve. In this embodiment, an inductively coupled plasma atomic emission spectrometer (ICP-OES) is used to analyze the spiked samples to obtain the standard curve, analyze the blank samples to correct the standard curve, and then analyze the matching situation between the parallel samples and the corrected standard curve to obtain the first test result. Correcting the standard curve and setting multiple spiked samples and parallel samples reduce the measurement error and accidental factors of the sample to be tested, making the obtained test result more accurate. In the embodiment, it takes about 2 - 2.5 h to detect the components of the filtrate using an inductively coupled plasma atomic emission spectrometer (ICP-OES).
[0038] In this embodiment, the first test result includes the first element types and the first element contents. Among them, the first element types are all the element types in the supernatant obtained from the first test result, and the first element contents are the contents of each element among all the element types in the supernatant obtained from the first test result. Of course, the first test result can also be in other forms as needed, such as the element distribution, concentration ratio, etc., so as to quickly determine the pollution source.
[0039] Please refer to Figure 3 , detect the elements in the insoluble matter to obtain the second test result, including the following steps:
[0040] First, prepare a sample from the insoluble substance. The specific steps are as follows: Lay boric acid, the insoluble substance, and boric acid in sequence in the sample ring of the press. Specifically, prepare the sample ring on the press in advance, use boric acid as an adhesive to form a base, spread the obtained insoluble substance evenly in the middle, and then cover a layer of boric acid on the insoluble substance to complete the sample preparation. After completing the sample preparation, press for a set time to obtain the sample. In this embodiment, use a force of 150 kN on the press and press for 30 s to obtain the final sample.
[0041] After that, use a fluorescence spectrometer to detect the sample to obtain the second detection result. The fluorescence spectrometer performs qualitative and semi-quantitative detection on the sample to obtain the distribution and content data of all elements in the insoluble substance. In this embodiment, the fluorescence spectrometer uses an X-ray fluorescence spectrometer, and calls the Quant As method in the X-ray fluorescence spectrometer to detect the sample. The Quant As method is a detection method built into the X-ray fluorescence spectrometer. In this embodiment, it takes about 30 min to detect the filter residue composition using the X-ray fluorescence spectrometer.
[0042] In this embodiment, the second detection result includes the second element types and the second element contents. For specific content, please refer to the first element types and the first element contents. Referring to the first detection result, similarly, the second detection result can also be in other forms as needed, such as the distribution of elements, concentration ratios, etc.
[0043] S3. Integrate the first detection result and the second detection result to obtain the element types and contents in the sewage sample, including the following process:
[0044] First, accumulate the element types in the first detection result and the second detection result. That is, add up all the element types in the first element types and the second element types. Of course, before adding, the data can be preprocessed, such as removing outliers and retaining normal values. After that, accumulate the element contents with the same element types. That is, add the first element content and the second element content corresponding to the same element. Similarly, before adding, the data can be preprocessed to make the detection result more accurate. Finally, obtain all the element types and contents in the sewage sample.
[0045] The detection system for elements in sewage of the present invention includes a memory, a processor, and a computer program stored on the memory. The processor executes the computer program to implement the steps of the method for detecting elements in sewage.
[0046] Traditional analytical methods cannot quickly and comprehensively analyze the total element content of polluted water sources, and thus cannot accurately and efficiently determine the content and distribution of all their elements. The element content method proposed in the present invention is highly efficient and accurate, can quickly obtain accurate data within 3 hours, and the accuracy can reach the ppm level. It can accurately analyze polluted water quality, thus facilitating the rapid locking of the pollution source, and greatly promoting the accuracy and precision of point-to-point treatment of polluted water quality. In this embodiment, the pretreatment such as centrifugation and filtration of the sample takes 10 minutes; it takes about 30 minutes to detect the composition of the filter residue using an X-ray fluorescence spectrometer; it takes 2 - 2.5 hours to detect the composition of the filtrate using an inductively coupled plasma atomic emission spectrometer (ICP-OES), and all analyses can be completed in about 3 hours, while traditional sewage detection takes 2 - 3 days to obtain all results.
[0047] So far, the embodiments of the present disclosure have been described in detail. To avoid obscuring the concept of the present disclosure, some details well known in the art have not been described. Those skilled in the art can fully understand how to implement the technical solutions disclosed herein based on the above description.
[0048] Although some specific embodiments of the present disclosure have been described in detail by way of examples, those skilled in the art should understand that the above examples are only for illustration and not for limiting the scope of the present disclosure. Those skilled in the art should understand that the above embodiments can be modified or partial technical features can be equivalently replaced without departing from the scope and spirit of the present disclosure. In particular, as long as there is no structural conflict, the various technical features mentioned in each embodiment can be combined in any way.
Claims
1. A method for detecting elements in sewage, characterized in that, Including the following steps: Filter the sewage sample to obtain the supernatant and insoluble substances; Detect the elements in the supernatant to obtain the first detection result; Detect the elements in the insoluble substances to obtain the second detection result; Integrate the first detection result and the second detection result to obtain the types and contents of the elements in the sewage sample.
2. The detection method of elements in sewage according to claim 1, characterized in that, Before filtering the sewage sample, weigh the sewage sample to make it greater than the preset weight.
3. The detection method of elements in sewage according to claim 1, characterized in that, The detecting the elements in the supernatant to obtain the first detection result includes the following steps: Use the supernatant to prepare spiked samples and parallel samples, and simultaneously prepare blank samples; Establish a standard curve with the spiked samples and correct the standard curve with the blank samples; Obtain the first detection result according to the matching situation between the parallel samples and the corrected standard curve.
4. The detection method of elements in sewage according to claim 3, characterized in that, Using the supernatant to prepare spiked samples includes the following steps: Divide the supernatant equally into multiple volumetric flasks; Add a standard solution with a preset concentration to each volumetric flask; Make up the volume with ultrapure water, shake well and let stand to obtain multiple spiked samples.
5. The detection method of elements in sewage according to claim 1, characterized in that Use an inductively coupled plasma atomic emission spectrometer to detect the elements in the supernatant.
6. The detection method of elements in sewage according to claim 1, characterized in that, The detecting the elements in the insoluble substances to obtain the second detection result includes the following steps: Make the insoluble substances into samples; Use a fluorescence spectrometer to detect the samples to obtain the second detection result.
7. The detection method of elements in sewage according to claim 6, characterized in that, The fluorescence spectrometer is an X-ray fluorescence spectrometer, and the Quant As method is used to detect the samples.
8. The detection method of elements in sewage according to claim 6, wherein, The making the insoluble substances into samples includes the following steps: Lay boric acid, the insoluble substances, and boric acid in sequence in the sample ring of the press; Press for a set time to obtain the sample.
9. The detection method of elements in sewage according to claim 1, characterized in that, Integrating the first detection result and the second detection result to obtain the types and contents of the elements in the sewage sample includes the following process: Accumulate the types of elements in the first detection result and the second detection result; Accumulate the element contents with the same element types.
10. A detection system for elements in sewage, characterized in that Including a memory, a processor, and a computer program stored on the memory, and the processor executes the computer program to implement the steps of the method according to any one of claims 1 to 9.