CN115266627B - Ultraviolet detection method for rapidly measuring mixed micro-plastic and lead - Google Patents
Ultraviolet detection method for rapidly measuring mixed micro-plastic and lead Download PDFInfo
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- 229920003023 plastic Polymers 0.000 title claims abstract description 58
- 239000004033 plastic Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000000825 ultraviolet detection Methods 0.000 title claims abstract description 20
- 238000002835 absorbance Methods 0.000 claims abstract description 51
- 229920000426 Microplastic Polymers 0.000 claims abstract description 43
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000011161 development Methods 0.000 claims abstract description 18
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- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 48
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- 239000004793 Polystyrene Substances 0.000 claims description 31
- 229920002223 polystyrene Polymers 0.000 claims description 31
- 125000000524 functional group Chemical group 0.000 claims description 27
- 239000012086 standard solution Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
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- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
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- 239000003344 environmental pollutant Substances 0.000 abstract description 5
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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Abstract
The invention discloses an ultraviolet detection method for rapidly measuring mixed micro-plastic and lead, which relates to the technical field of detection of pollutants in the environment and comprises the following steps: mixing the micro plastic and a lead sample to be detected, performing ultraviolet full scanning, respectively determining the absorbance of the sample to be detected at the wavelength of 485nm, 460nm and 494nm according to the full scanning result, and calculating to obtain the concentration of the micro plastic in the sample to be detected according to the established absorbance and a standard curve between the concentrations of the three micro plastics coexisting with the lead; the method comprises the steps of filtering a solution to be measured, detecting lead by adopting a xylenol orange color development method, measuring the absorbance of the solution to be measured at the wavelength of 568nm, calculating the concentration of lead in a sample to be measured according to the established standard curve between the absorbance and the lead concentration, eliminating the mutual interference of the absorbance and the lead in a mixed system of the micro-plastic and the lead, and accurately measuring the micro-plastic and the lead by utilizing an ultraviolet spectrophotometer in a proper range.
Description
Technical Field
The invention relates to the technical field of detection of pollutants in the environment, in particular to an ultraviolet detection method for rapidly measuring mixed micro-plastic and lead.
Background
Plastic granules with a size of 1 μm to 5mm are defined as microplastics, most of which are microplastics with indefinite size and shape resulting from the breaking of larger plastic fragments by mechanical action, UV irradiation, weathering, etc. Polystyrene is one of the most commonly used plastics, and polystyrene particles modified with different functional groups also have different degrees of influence on the coagulation of human body.
Lead, as one of heavy metal elements, is widely used in the electroplating industry, the steel industry, the electrical industry and the like. In recent years, due to the exploitation of lead-zinc ores, the stacking of the tailing slag causes different pollution to the environment. Such contamination can cause lead content in surface waters, sediments, soils near the lead-zinc mine to exceed background values.
The coexistence of micro-plastics and lead in the environment changes the respective migration behavior and environmental exposure risks. At present, common detection methods for micro-plastics in the environment comprise visual detection, raman spectroscopy, infrared spectroscopy and the like, but have some limitations, particles with too small particle size cannot be detected by visual detection, the detection efficiency of the Raman spectroscopy is low, and the infrared spectroscopy can only detect large-size particles. Laboratory lead detection methods often use large precision instruments and require cumbersome pre-processing. For detecting mixed pollutants, a high performance liquid chromatography-mass spectrometry combined method is often used, but the problems of high price, easy failure of instruments and the like also exist.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, adopts a simple, quick and accurate method to quantify the micro-plastics and heavy metals existing in water at the same time, provides an ultraviolet detection method for quickly and accurately quantifying mixed polystyrene micro-plastics and lead, and meets the requirement of pollutant quantification in the environmental field.
In order to achieve the purpose, the invention provides the following scheme:
an ultraviolet detection method for rapidly measuring mixed micro-plastic and lead comprises the following steps:
mixing the micro plastic with a lead sample to be detected, carrying out ultraviolet full scanning (ultraviolet full-wavelength scanning, the same below), respectively determining the absorbance of the sample to be detected at the wavelength of 485nm, 460nm and 494nm according to the full scanning result, and calculating to obtain the concentration of the micro plastic in the sample to be detected according to the established absorbance and a standard curve between the concentrations of the three micro plastics when the micro plastic coexists with the lead;
and filtering the solution to be detected, detecting lead by adopting a xylenol orange color development method, determining the absorbance of the solution to be detected at the wavelength of 568nm, and calculating to obtain the concentration of the lead in the sample to be detected according to the established standard curve between the absorbance and the lead concentration.
The detection method has the advantages of small volume of the required solution to be detected (only 1mL of the solution to be detected is needed when the method is used for detecting lead, but dozens of milliliters of the solution to be detected is needed when the method is used for detecting lead in the prior art, for example, 10.0mL of the solution to be detected is used in the research on simultaneous determination of lead and selenium in water by a hydride atomic fluorescence method published in 2018 by Zhaoyong et al, 40.0mL of the solution to be chemically plated with nickel by xylenol orange spectrophotometry published in 2011 by Jing national gold and the like, low cost, simple and convenient instrument operation, high analysis speed, good accuracy in a certain concentration range and the like, and has wide application prospect.
Further, the ultraviolet detection method for rapidly measuring the mixed micro-plastic and the lead specifically comprises the following steps:
(1) Establishing a standard curve of the single micro-plastic and the single lead when the single micro-plastic and the lead coexist in the ultraviolet detection
The first step is as follows: preparing standard solutions of three different microplastics with the concentrations of 0.15mg/L, 0.45mg/L, 0.75mg/L, 1.2mg/L, 1.5mg/L, 4.5mg/L, 7.5mg/L, 12mg/L and 15mg/L respectively, carrying out ultraviolet full scanning on the standard solutions of the microplastics with different concentrations, respectively measuring the absorbances of the standard solutions with different concentrations at 485nm, 460nm and 494nm according to an absorption spectrogram obtained by full scanning, and drawing a standard curve of the microplastics under a single system;
the second step: diluting the mixed solution of the micro-plastic with the concentration of 15mg/L and the lead with the concentration of 10mg/L to different times (0.01 time, 0.03 time, 0.05 time, 0.08 time, 0.1 time, 0.3 time, 0.5 time, 0.8 time and 1 time), respectively measuring the absorbances of MS w/Pb, CMS w/Pb and SMS w/Pb at 485nm, 460nm and 494nm, and drawing a standard curve of the micro-plastic under a composite system;
the third step: respectively preparing standard solutions of lead with the concentrations of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L, respectively taking 1mL of the solutions according to a xylenol orange color development method, sequentially adding deionized water, a xylenol orange solution and a HAC-NaAC buffer solution, uniformly mixing, then carrying out ultraviolet full-sweep, respectively measuring the absorbance of the lead solution after xylenol orange color development at 568nm according to the full-sweep result, and drawing a standard curve of the lead under a single system;
(2) Measuring the concentration of the micro-plastic and the lead in the mixed solution to be measured
The first step is as follows: diluting or concentrating a mixed sample to be detected containing the micro plastic and the lead, so that the concentrations of the micro plastic and the lead in the diluted or concentrated solution are in a linear range of a standard curve;
the second step: under the same conditions of the step (1), measuring the absorbance of the diluted or concentrated solution at 485nm, 460nm and 494nm, and obtaining the polystyrene fluorescent Microspheres (MS) without functional groups, the polystyrene fluorescent microspheres (CMS) with carboxyl functional groups and the polystyrene fluorescent microspheres (SMS) with sulfonic functional groups in the mixed solution by utilizing the absorbance, wherein the concentrations of the polystyrene fluorescent Microspheres (MS) with the sulfonic functional groups are respectively C MS 、C CMS 、C SMS (ii) a Filtering 1mL of the solution to be detected, measuring the absorbance of the solution after the xylenol orange color development at 568nm according to a xylenol orange color development method, and obtaining the concentration of lead in the mixed solution by using the absorbance (C) Pb )。
Further, the diameter of the micro plastic is 1 μm.
Further, the absorbance is measured by an ultraviolet-visible spectrophotometer, preferably a UV2000 ultraviolet-visible spectrophotometer is used.
Further, a 0.22 μm needle filter was used for the filtration.
Further, the three different micro-plastics in the step (1) are polystyrene fluorescent microspheres without functional groups, polystyrene fluorescent microspheres with carboxyl functional groups and polystyrene fluorescent microspheres with sulfonic functional groups.
The invention discloses the following technical effects:
(1) The invention provides an ultraviolet detection method for quickly, accurately and quantitatively mixing micro plastic and lead, which does not need to use a microscope for observation and a large instrument, and has the advantages of simple operation, high analysis speed and low cost.
(2) In the mixed system of the micro plastic and the lead, when the lead concentration is detected, the method separates the micro plastic and the lead by using simple and easy-to-operate filtration, and eliminates the mutual interference of the micro plastic and the lead. Accurate measurement of the micro plastic and the lead by using the ultraviolet spectrophotometer is realized in a proper range, the required original solution to be measured is less, and the efficiency is higher.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph of the UV absorption spectra of MS (a), CMS (b) and SMS (c) at different concentration multiples and a representative standard curve (d);
FIG. 2 is a representative standard graph of a micro-plastic in the presence of lead;
FIG. 3 is a graph (a) showing the ultraviolet absorption spectrum of lead at different concentration multiples and a standard curve (b) showing lead at 568 nm;
FIG. 4 is a graph of the transmission of MS (a), CMS (b) and SMS (c) in G20/25 medium at different ionic strengths in a two-substance system;
FIG. 5 is a graph of lead penetration curves (a, b, c) in G20/25 medium at different ionic strengths co-migrating with the micro-plastic.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated or intervening value in a stated range, and every other stated or intervening value in that stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The embodiment of the invention provides an ultraviolet detection method for rapidly measuring mixed micro-plastic and lead, which comprises the following steps:
mixing the micro plastic and a lead sample to be detected, performing ultraviolet full scanning (ultraviolet full-wavelength scanning, the same below), respectively determining the absorbance of the sample to be detected at the wavelength of 485nm, 460nm and 494nm according to the full scanning result, and calculating to obtain the concentration of the micro plastic in the sample to be detected according to the established absorbance and a standard curve between the concentrations of the three micro plastic when the micro plastic coexists with the lead;
and filtering the solution to be detected, detecting lead by adopting a xylenol orange color development method, determining the absorbance of the solution to be detected at the wavelength of 568nm, and calculating to obtain the concentration of the lead in the sample to be detected according to the established standard curve between the absorbance and the lead concentration.
The detection method has the advantages of small volume of the required solution to be detected (only 1mL of the solution to be detected is needed when the method is used for detecting lead, but dozens of milliliters of the solution to be detected is needed when the lead is detected in the prior art, for example, 10.0mL of the solution to be detected is used in the research on simultaneous determination of lead and selenium in water by a hydride atomic fluorescence method published in 2018 by Zhaoyong et al, 40.0mL of the solution to be detected by xylenol orange spectrophotometry published in 2011 by sinus national gold and the like), low cost, simple and convenient instrument operation, high analysis speed, good accuracy in a certain concentration range and the like, and has wide application prospect.
In the embodiment of the invention, the ultraviolet detection method for rapidly measuring the mixed micro plastic and the lead specifically comprises the following steps:
(1) Establishing a standard curve of the single micro-plastic and the single lead when the single micro-plastic and the lead coexist in the ultraviolet detection
The first step is as follows: respectively preparing standard solutions of three different types of micro-plastics with the concentrations of 0.15mg/L, 0.45mg/L, 0.75mg/L, 1.2mg/L, 1.5mg/L, 4.5mg/L, 7.5mg/L, 12mg/L and 15mg/L, carrying out ultraviolet full scanning on the micro-plastic standard solutions with different concentrations, respectively determining the absorbances of the standard solutions with different concentrations at 485nm, 460nm and 494nm according to an absorption spectrogram obtained by full scanning, and drawing a standard curve of the micro-plastics under a single system;
the second step: diluting the mixed solution of the micro-plastic with the concentration of 15mg/L and the lead with the concentration of 10mg/L to different times (0.01 time, 0.03 time, 0.05 time, 0.08 time, 0.1 time, 0.3 time, 0.5 time, 0.8 time and 1 time), respectively measuring the absorbances of MS w/Pb, CMS w/Pb and SMS w/Pb at 485nm, 460nm and 494nm, and drawing a standard curve of the micro-plastic under a composite system;
the third step: respectively preparing standard solutions of lead with the concentrations of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L, respectively taking 1mL of the solutions according to a xylenol orange color development method, sequentially adding deionized water, a xylenol orange solution and an HAC-NaAC buffer solution, uniformly mixing, then carrying out ultraviolet full-sweep, respectively measuring the absorbance of the xylenol orange colored lead solution at 568nm according to a full-sweep result, and drawing a standard curve of the lead in a single system;
(2) Measuring the concentration of the micro-plastic and the lead in the mixed solution to be measured
The first step is as follows: diluting or concentrating a mixed sample to be detected containing the micro plastic and the lead, and enabling the concentrations of the micro plastic and the lead in the diluted or concentrated solution to be in the linear range of a corresponding standard curve;
the second step: under the same conditions of the step (1), measuring the absorbance of the diluted or concentrated solution at 485nm, 460nm and 494nm, and obtaining the polystyrene fluorescent Microspheres (MS) without functional groups in the mixed solution by using the absorbance, wherein the polystyrene fluorescent microspheres have carboxyl functional groupsThe concentration of the polystyrene fluorescent microsphere (CMS) with sulfonic group functional group is C MS 、C CMS 、C SMS (ii) a Filtering 1mL of the solution to be detected, measuring the absorbance of the solution after the xylenol orange color development at 568nm according to a xylenol orange color development method, and obtaining the concentration of lead in the mixed solution by using the absorbance (C) Pb )。
In the present example, the diameter of the micro plastic was 1 μm.
In the examples of the present invention, the absorbance is measured by an ultraviolet-visible spectrophotometer, preferably a UV2000 ultraviolet-visible spectrophotometer.
In the present example, a 0.22 μm needle filter was used for filtration.
In the embodiment of the present invention, the three different micro-plastics in step (1) are polystyrene fluorescent microspheres without functional groups, polystyrene fluorescent microspheres with carboxyl functional groups, and polystyrene fluorescent microspheres with sulfonic functional groups.
The process of ultraviolet full scan in the embodiments of the present invention is a conventional technical means in the art, and is not the focus of the present invention, and is not described herein again.
Example 1
(1) Establishing a standard curve of the single micro-plastic and the single lead when the single micro-plastic and the lead coexist in the ultraviolet detection
The first step is as follows: preparing standard solutions of three different types of micro-plastics (non-functional group polystyrene fluorescent Microspheres (MS), carboxyl-functional group polystyrene fluorescent microspheres (CMS) and sulfonic-functional group polystyrene fluorescent microspheres (SMS)) with concentrations of 0.15mg/L, 0.45mg/L, 0.75mg/L, 1.2mg/L, 1.5mg/L, 4.5mg/L, 7.5mg/L, 12mg/L and 15mg/L respectively, performing full ultraviolet scanning on the micro-plastic standard solutions with different concentrations, measuring absorbances of the micro-plastic standard solutions with different concentrations at 485nm, 460nm and 494nm respectively according to absorption spectrum graphs obtained by full scanning, and drawing standard curves of the micro-plastics under a single system, wherein the standard curves are shown in Table 1 and figure 1.
TABLE 1 Absorbance value recordings of individual microplastic Standard solutions
The second step is that: the mixed solution of the micro plastic with the concentration of 15mg/L and the lead with the concentration of 10mg/L is diluted to different times (0.01 time, 0.03 time, 0.05 time, 0.08 time, 0.1 time, 0.3 time, 0.5 time, 0.8 time and 1 time), the absorbances of MS w/Pb, CMS w/Pb and SMS w/Pb at 485nm, 460nm and 494nm are respectively measured, and a standard curve of the micro plastic under a composite system is drawn, as shown in the table 2 and the figure 2.
TABLE 2 recording of absorbance values of the microplastic standard solutions under the composite system
The third step: lead standard solutions with concentrations of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L were prepared, respectively. According to a xylenol orange color development method, respectively taking 1mL of the solution, sequentially adding deionized water, a xylenol orange solution and an HAC-NaAC buffer solution, uniformly mixing, carrying out ultraviolet full-scan, respectively measuring the absorbance of the lead solution after xylenol orange color development at 568nm according to the full-scan result, and drawing a standard curve of lead under a single system, wherein the standard curve is shown in table 3 and figure 3.
TABLE 3 Absorbance value recording of lead Standard solution alone
(2) Measuring the concentration of the micro-plastic and the lead in the mixed solution to be measured
The first step is as follows: diluting or concentrating a mixed sample to be detected containing the micro plastic and the lead, and enabling the concentrations of the micro plastic and the lead in the diluted or concentrated solution to be in a linear range of a standard curve;
the second step: under the same conditions in the step (1), measuring the absorbance of the diluted or concentrated solution at 485nm, 460nm and 494nm by using a UV2000 ultraviolet-visible spectrophotometer, and obtaining the polystyrene fluorescent Microspheres (MS) without functional groups, the polystyrene fluorescent microspheres (CMS) with carboxyl functional groups and the polystyrene fluorescent microspheres (SMS) with sulfonic functional groups in the mixed solution by using the absorbance, wherein the concentration of the polystyrene fluorescent microspheres (SMS) with sulfonic functional groups is respectively C MS 、C CMS 、C SMS (ii) a Filtering 1mL of diluted or concentrated solution to be detected with 0.22 μm needle filter, measuring absorbance of the solution at 568nm according to xylenol orange color development method, and obtaining concentration C of lead in the mixed solution by using absorbance Pb 。
Example 2
The method for measuring the mixed micro-plastic and the lead by using the ultraviolet spectrophotometry is applied to practice, and the change of the concentrations of the micro-plastic and the free lead in the penetration experiment in the column migration experiment along with the time is tested in order to explore the migration rule of pollutants in a porous medium.
The first step is as follows: under two background solutions with different ionic strengths (1 mM and 100 mM), a mixed solution of the micro plastic and the lead is prepared, wherein the concentrations of the micro plastic and the lead are 15mg/L and 10mg/L respectively.
The second step is that: glass media with a particle size of G20/25 were packed into the column with a calibrated flow rate of 5mL/min.
The third step: the system was equilibrated by feeding a background electrolyte solution of at least 20PVs to the column using a peristaltic pump, followed by a microplastic-lead mixed solution of 6PVs, followed by a background electrolyte solution of 12PVs, so that the concentration of contaminants in the effluent approached 0. One water sample was collected every 56s in the experiment.
The fourth step: according to the procedure of example 1, the concentration of the micro-plastic in each water sample is measured according to the ultraviolet spectrophotometry method, and the penetration curves of the micro-plastic with different functional groups under different background conditions are obtained, namely, fig. 4; 1mL of each water sample was filtered through a 0.22 μm needle filter, and then the concentration of free lead was determined according to the UV detection method for rapid measurement of mixed micro-plastics and lead of the present invention, resulting in lead penetration curves under different background conditions, i.e., FIG. 5. From fig. 4 and 5, it can be seen that the detection method of the present invention is applicable in the experimental process, and the data obtained within a certain error range is repeatable, indicating that the method is widely applicable.
The above-described embodiments are only intended to illustrate the preferred embodiments of the present invention, and not to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (5)
1. An ultraviolet detection method for rapidly measuring mixed micro plastic and lead is characterized by comprising the following steps:
mixing the micro plastic and a lead sample to be detected, performing ultraviolet full scanning, respectively determining the absorbance of the sample to be detected at the wavelength of 485nm, 460nm and 494nm according to the full scanning result, and calculating to obtain the concentration of the micro plastic in the sample to be detected according to the established absorbance and a standard curve between the concentrations of the three micro plastics coexisting with the lead;
filtering the solution to be detected, detecting lead by adopting a xylenol orange color development method, determining the absorbance of the solution to be detected at the wavelength of 568nm, and calculating to obtain the concentration of lead in the sample to be detected according to the established standard curve between the absorbance and the lead concentration;
the three types of micro-plastics are polystyrene fluorescent microspheres without functional groups, polystyrene fluorescent microspheres with carboxyl functional groups and polystyrene fluorescent microspheres with sulfonic functional groups.
2. The ultraviolet detection method for rapidly measuring mixed micro-plastic and lead according to claim 1, is characterized by comprising the following steps:
(1) Establishing a standard curve of the single micro-plastic and the single lead when the single micro-plastic and the lead coexist in the ultraviolet detection
The first step is as follows: respectively preparing standard solutions of three different micro-plastics with the concentrations of 0.15mg/L, 0.45mg/L, 0.75mg/L, 1.2mg/L, 1.5mg/L, 4.5mg/L, 7.5mg/L, 12mg/L and 15mg/L, carrying out ultraviolet full scan on the standard solutions of the micro-plastics with different concentrations, respectively measuring the absorbances of the standard solutions with different concentrations at 485nm, 460nm and 494nm according to an absorption spectrogram obtained by full scan, and drawing a standard curve of the micro-plastics under a single system;
the second step: diluting the mixed solution of the micro-plastic with the concentration of 15mg/L and the lead with the concentration of 10mg/L to different times, respectively measuring the absorbances of MS w/Pb, CMS w/Pb and SMS w/Pb at 485nm, 460nm and 494nm, and drawing a standard curve of the micro-plastic under a composite system;
the third step: respectively preparing standard solutions of lead with the concentrations of 0.1mg/L, 0.3mg/L, 0.5mg/L, 0.8mg/L, 1.0mg/L, 3.0mg/L, 5.0mg/L, 8.0mg/L and 10.0mg/L, respectively taking 1mL of the solutions according to a xylenol orange color development method, sequentially adding deionized water, a xylenol orange solution and a HAC-NaAC buffer solution, uniformly mixing, then carrying out ultraviolet full-sweep, respectively measuring the absorbance of the lead solution after xylenol orange color development at 568nm according to the full-sweep result, and drawing a standard curve of the lead under a single system;
(2) Measuring the concentration of micro-plastics and lead in the mixed solution to be measured
The first step is as follows: diluting or concentrating a mixed sample to be detected containing the micro plastic and the lead, and enabling the concentrations of the micro plastic and the lead in the diluted or concentrated solution to be in a linear range of a standard curve;
the second step: under the same condition of the step (1), measuring the absorbance of the diluted or concentrated solution at 485nm, 460nm and 494nm, and obtaining the polystyrene fluorescent microspheres without functional groups, the polystyrene fluorescent microspheres with carboxyl functional groups and the polystyrene fluorescent microspheres with sulfonic functional groups in the mixed solution by utilizing the absorbance, wherein the concentrations of the polystyrene fluorescent microspheres with carboxyl functional groups and the polystyrene fluorescent microspheres with sulfonic functional groups are respectively C MS 、C CMS 、C SMS (ii) a And (3) filtering 1mL of solution to be detected, measuring the absorbance of the solution after the xylenol orange color development at 568nm according to a xylenol orange color development method, and obtaining the concentration of lead in the mixed solution by utilizing the absorbance.
3. The UV detection method for rapid measurement of mixed micro-plastics and lead according to claim 2, wherein the diameter of the micro-plastics is 1 μm.
4. The UV detection method for rapid measurement of mixed micro-plastic and lead according to claim 2, characterized in that the absorbance is measured by UV-visible spectrophotometer.
5. The UV detection method for the rapid measurement of mixed micro-plastics and lead according to claim 1, characterized in that the filtration uses a 0.22 μm needle filter.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294554A (en) * | 1991-03-01 | 1994-03-15 | C. Uyemura & Co., Ltd. | Analysis of tin, lead or tin-lead alloy plating solution |
| CN107402204A (en) * | 2016-05-20 | 2017-11-28 | 无锡创晨科技有限公司 | A kind of lead ion detection method |
| CN107421899A (en) * | 2017-06-28 | 2017-12-01 | 重庆市宇驰检测技术有限公司 | Determine the detection method of water quality aniline, formaldehyde simultaneously based on ultraviolet-visible absorption spectroscopy |
| CN111948167A (en) * | 2020-08-18 | 2020-11-17 | 天津大学 | Method for quickly quantifying concentration of polystyrene microspheres and tetracycline in water |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5294554A (en) * | 1991-03-01 | 1994-03-15 | C. Uyemura & Co., Ltd. | Analysis of tin, lead or tin-lead alloy plating solution |
| CN107402204A (en) * | 2016-05-20 | 2017-11-28 | 无锡创晨科技有限公司 | A kind of lead ion detection method |
| CN107421899A (en) * | 2017-06-28 | 2017-12-01 | 重庆市宇驰检测技术有限公司 | Determine the detection method of water quality aniline, formaldehyde simultaneously based on ultraviolet-visible absorption spectroscopy |
| CN111948167A (en) * | 2020-08-18 | 2020-11-17 | 天津大学 | Method for quickly quantifying concentration of polystyrene microspheres and tetracycline in water |
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