CN110836797A - Method for preparing LIBS liquid detection sample based on chelating resin - Google Patents
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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- G01N21/718—Laser microanalysis, i.e. with formation of sample plasma
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/40—Concentrating samples
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a method for preparing a LIBS liquid detection sample based on chelating resin, which comprises the following steps: (1) putting a preset amount of chelate resin into a glass tube, sealing one side of the glass tube by using a filter screen, and connecting one side of the glass tube with a peristaltic pump tube; (2) the method comprises the following steps that (1) a solution to be detected containing metal elements passes through a glass tube placed with chelate resin at a preset flow rate under the driving of a peristaltic pump, (3) the peristaltic pump is suspended after a half volume of the solution to be detected is introduced into the glass tube, and the glass tube is reversely placed in a pipeline of the peristaltic pump so as to be adsorbed more uniformly; (4) continuously introducing the solution to be detected until the solution to be detected is completely introduced into the glass tube; (5) taking out the chelating resin from the glass tube and drying; (6) taking out the dried chelating resin, grinding, tabletting and preparing a LIBS liquid test sample; (7) and analyzing the prepared sample by adopting a laser-induced breakdown spectroscopy system to obtain the content analysis of the metal elements in the water body.
Description
Technical Field
The invention belongs to the technical field of atomic emission spectroscopy detection, and particularly relates to a method for preparing a LIBS liquid detection sample based on chelating resin.
Background
At present, in China, in the processes of mining, smelting and processing of heavy metals, a lot of heavy metals such as lead, mercury, cadmium, cobalt and the like enter the atmosphere, water and soil to cause serious environmental pollution. In environmental pollution, water body pollution, particularly heavy metal element pollution, is a topic which is very concerned by people in the real society, and even if the concentration of heavy metals in wastewater is low, the heavy metals can be accumulated in algae and bottom mud, and are adsorbed by the body surfaces of fishes and shellfishes to generate food chain concentration, so that the pollution is caused, and the detection significance on the heavy metal elements in the water body is great.
Laser-induced breakdown spectroscopy (LIBS) is an analysis technique for detecting the composition and content of a substance based on atomic emission spectroscopy, and utilizes high-energy-density laser pulses to breakdown a sample to induce and generate high-temperature plasma, and performs qualitative and quantitative analysis on the composition of elements by measuring atomic or ion spectral lines emitted by corresponding elements of the plasma during cooling. The LIBS technology has the advantages of no need of sampling and sample preparation, no destructiveness to samples, capability of carrying out element component detection on various types of samples, capability of rapidly detecting multiple elements on line in real time and the like, and is widely applied to the fields of material analysis, environmental monitoring, industrial production control, archaeology and the like. Meanwhile, the LIBS can be applied to component detection in environments including solid, liquid and gas.
However, when the LIBS technique is used to measure a liquid sample, due to the influence of complex factors such as liquid sputtering, liquid level fluctuation and laser quenching, the problems of low intensity of spectral signals, poor stability and rapid plasma quenching are generated, thereby affecting the detection sensitivity of the element to be measured. To overcome these problems, researchers have proposed methods for transferring analytes from a liquid phase to a solid phase by absorbing a liquid sample with a particular solid phase matrix, thereby adsorbing heavy metal elements in the liquid sample to the solid phase matrix, and then evaporating the sample solvent, thereby completing the matrix conversion from liquid to solid. Through such treatment, the determination of heavy metal elements in liquid samples can be realized by directly analyzing the solid matrix through LIBS, and the method is widely used for LIBS related research. For example, the forest celebration et al proposes that porous electrostatic spinning fibers are used as solid phase carriers, heavy metal elements in a solution to be detected are enriched in the porous electrostatic spinning fibers and then are detected by an LIBS technology, the detection limits of the obtained Cr element and Cu element are 1.8mg/L and 1.9mg/L, but the porous electrostatic spinning fibers are self-made in laboratories, and used instruments are expensive, so that the operation cost is increased; for another example, NiuGuanghui et al propose adding concentrated sulfuric acid into a beaker containing a proper amount of sucrose to form a carbon column, mixing the solution to be detected with carbon powder to make heavy metal elements contained in the solution to be detected adsorbed by the carbon powder, and tabletting the carbon powder after a series of treatments to perform LIBS detection, although the method can obtain a lower detection limit, a complex preparation procedure is required, and the time cost is increased; the detection limit of zinc obtained by analyzing the zinc in the solution after enrichment with graphite blocks is 4.108mg/L, and people like Heijongshan use filter paper as a substrate to enrich a liquid sample for detection, wherein the detection limit of Pb reaches 3.87 mg/L.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing a LIBS liquid detection sample based on chelating resin.
The invention is realized by the following technical scheme:
a method for preparing a LIBS liquid assay sample based on a chelating resin, comprising the steps of:
(1) putting a preset amount of chelate resin into a glass tube, sealing one side of the glass tube by using a filter screen, and connecting one side of the glass tube with a peristaltic pump tube;
(2) under the drive of the peristaltic pump, a solution to be detected containing metal elements passes through a glass tube placed with chelate resin at a preset flow rate under the drive of the peristaltic pump, so that the solution to be detected is fully contacted with the chelate resin, and metal ions contained in the solution to be detected are enriched and adsorbed on the chelate resin;
(3) after a half volume of solution to be measured is introduced into the glass tube, the peristaltic pump is suspended, and the glass tube is reversely placed in a pipeline of the peristaltic pump so as to be adsorbed more uniformly;
(4) continuously introducing the solution to be detected until the solution to be detected is completely introduced into the glass tube;
(5) taking out the chelating resin from the glass tube, drying, and if the chelating resin is placed in a watch glass, putting the watch glass in a drying box for drying;
(6) the dried chelate resin was removed and ground and tableted to produce LIBS liquid test samples. Tabletting the milled powder under the action of a tabletting machine if the milling is carried out in a mortar, thereby preparing the required LIBS liquid test sample;
(7) and (3) realizing trace analysis of the heavy metal in the water body by adopting a laser-induced breakdown spectroscopy technology.
The chelating resin is fully contacted with the solution to be detected by utilizing the super-strong binding force of the chelating resin and metal ions so as to enable the metal ions contained in the solution to be detected to be enriched and adsorbed on the chelating resin, thereby converting the liquid to be detected into a solid for LIBS detection. The chelating resin has strong adsorbability to metal ions because functional atoms on the chelating resin can perform a coordination reaction with the metal ions to form a stable structure similar to a small-molecule chelate, and in addition, the chelating resin is used as a polymer matrix and does not contain metal elements, so that other heavy metals do not interfere with measurement during LIBS analysis.
In the technical scheme, the glass tube is vertically placed in the sample feeding process, the inner diameter of the glass tube is 3-20mm, and the length of the glass tube is 5-20 cm.
In the technical scheme, the sampling amount of the chelating resin is 0.5-10 g.
In the technical scheme, in the step (2), the step (3) and the step (4), the flow rate of the peristaltic pump is set to be 1-30 mL/min.
In the above technical scheme, in the step (5), the temperature of the drying box is selected to be 30-50 ℃.
In the above technical scheme, in the step (6), the pressure of the tablet press is set to be 5-20MPa, and the tablet pressing time is set to be 1-5 min.
The invention has the advantages and beneficial effects that:
the chelating resin is introduced into the LIBS liquid detection field for the first time, and the chelating resin is fully contacted with the solution to be detected by utilizing the super-strong binding force of the chelating resin and metal ions so that the metal ions contained in the solution to be detected are enriched and adsorbed on the chelating resin, so that the liquid to be detected is converted into a solid for LIBS detection, and the problems of liquid sputtering, liquid level fluctuation, laser quenching and the like in the process of detecting the liquid by the LIBS are well solved.
In addition, because functional atoms on the chelating resin can perform a coordination reaction with metal ions to form a stable structure similar to a micromolecular chelate, the chelating resin has very strong adsorbability to the metal ions, the solution is fully contacted with the chelating resin by a mode of introducing the solution to be detected by a peristaltic pump, and correspondingly, the adsorption efficiency of the chelating resin to the heavy metal ions in the solution is also greatly improved. Meanwhile, the glass tube is kept vertically in the sample introduction process all the time, and the solution to be detected with half volume is turned around after being introduced into the glass tube, so that the adsorption is more uniform.
Compared with other existing schemes of converting liquid to be detected into solid and then carrying out LIBS detection, the method provided by the invention has better enrichment effect, and the detection sensitivity and precision are further improved, so that the method is particularly suitable for application occasions such as industrial sewage treatment and heavy metal element trace analysis of liquid.
In addition, the chelating resin is used as a polymer matrix and does not contain metal elements, so that other heavy metal elements do not interfere with measurement during LIBS analysis, and a good detection effect can be obtained. Compared with other existing schemes of converting liquid to be detected into solid and then performing LIBS detection, the method provided by the invention has better enrichment effect, the sample is hardly interfered by other heavy metal elements, and the detection sensitivity and precision are further improved.
The chelate resin is low in price and easy to obtain, instruments used by the sample preparation device are common laboratory instruments such as a peristaltic pump, a beaker, a glass tube and a watch glass, the experimental operation is simple and convenient, and the sample manufacturing cost is low.
Drawings
FIG. 1 is a flow chart of a method for preparing a LIBS liquid detection sample based on a chelating resin according to the present invention;
FIG. 2 is an exemplary diagram illustrating a system component for implementing the process shown in FIG. 1, wherein the devices or components employed are arranged in accordance with the teachings of the present invention;
FIG. 3 is a schematic diagram of the structure of the LIBS detection device;
FIG. 4 is a spectrum of chelating resin before and after adsorbing copper element;
FIG. 5 is a plot of flow rate versus achievable spectral line intensity for a sample under test during preparation of a LIBS liquid test sample in accordance with the method of the present invention;
FIG. 6 is a calibration curve obtained for copper with respect to a test sample using LIBS;
the same reference numbers will be used throughout the drawings to refer to the same or like elements, wherein:
1-a peristaltic pump; 2-peristaltic pump tubing; 3-a first beaker; 4-liquid to be measured; 5, a glass tube; 6-chelating resin; 7, a filter screen; 8-second beaker; 9-waste liquid; 10-watch glass; 11-chelate resin after completion of adsorption; 14-Nd is YAG laser; 15-a reflector; 16-a focusing lens; 17-plasma; 18-a sample to be tested; 19-a two-dimensional moving platform; 20-a light-collecting lens; 21-an optical fiber coupler; 22-an optical fiber; 23-a spectrometer; 24-ICCD; 25-a computer; 26-controller.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
The functional atoms on the chelating resin can generate coordination reaction with metal ions to form a stable structure similar to a micromolecular chelate, so that the chelating resin has very strong adsorbability to the metal ions. According to the invention, the chelating resin is introduced into the LIBS liquid detection field for the first time by utilizing the super-strong binding force of the chelating resin and the metal ions, and the metal ions contained in the solution to be detected are enriched and adsorbed on the chelating resin, so that the liquid to be detected is converted into a solid to carry out LIBS detection. In addition, the chelating resin is used as a polymer matrix and does not contain metal elements, so that other heavy metal elements do not interfere with measurement during LIBS analysis, and a good detection effect can be obtained, so that the chelating resin is particularly suitable for application occasions such as industrial sewage treatment and liquid heavy metal element trace analysis.
FIG. 1 is a flow chart of a chelating resin-based method for preparing LIBS liquid assay samples constructed in accordance with the present invention; FIG. 2 is a diagram that schematically illustrates a system component for performing the process shown in FIG. 1. As shown in fig. 1 and 2, the process mainly includes the following processing steps:
first, an appropriate amount of chelate resin was weighed and poured into a glass tube. More specifically, a glass tube 5 is placed vertically and one side is connected to a peristaltic pump tube 2, and after pouring chelate resin 6 (having a weight of, for example, 0.9g) into the glass tube 5 (having an inner diameter of 4mm and a length of 10cm) from the other side, the side is sealed with a filter 7.
Then, the solution to be measured was slowly passed through a glass tube containing a chelate resin. More specifically, liquid 4 to be measured (sample volume 60mL) is taken and poured into a first beaker 3, the liquid 4 to be measured is slowly introduced into a glass tube 5 through a peristaltic pump tube 2, the flow rate of the peristaltic pump is set to be 3mL/min, heavy metal ions in the solution 4 to be measured are enriched and adsorbed on chelate resin 6 in the process, and the obtained waste liquid 9 flows out to a second beaker 8 from one side of the glass tube 5, which is wrapped by a filter screen 7; the peristaltic pump 1 is suspended after 30mL of liquid 4 to be detected is introduced into the glass tube 5, the glass tube 5 is turned around, namely the glass tube 5 is taken down, the filter screen is wrapped on the tube opening on one side which is originally connected with the peristaltic pump tube 2, the filter screen is taken down from the tube opening on one side which is originally wrapped by the filter screen 7 and then connected with the peristaltic pump tube 2, and then the rest liquid 4 to be detected is continuously introduced.
Finally, after the liquid 4 to be measured is completely introduced into the glass tube 5, the chelate resin 11 having completed the adsorption is taken out and dried, and then ground and tabletted. More specifically, the chelate resin 11 after completion of adsorption was taken out of the glass tube 5 and transferred to a petri dish 10, and then placed in a drying oven, dried at a temperature of 30 ℃ to 40 ℃, and the dried chelate resin was put in a mortar for grinding and then tabletted, with the pressure of the tabletting machine set to 10MPa and the tabletting time set to 2min, thereby preparing the desired LIBS liquid test sample.
FIG. 3 shows a schematic structural diagram of a device for subsequent LIBS detection according to the sample preparation method of the present invention. In the detection process, high-energy laser emitted by a Nd-YAG laser 14 is reflected by a reflector 15, focused on a sample 18 on a two-dimensional electric displacement platform 19 controlled by a controller 26 by a focusing lens 16 with the focal length of 100mm, and excites the sample to generate high-temperature plasma 17, light emitted by the high-temperature plasma 17 is Coupled into an optical fiber 22 through an optical fiber coupler 21 by a light receiving lens 20, the collected light is transmitted to a spectrometer 23 through the optical fiber 22, the spectrometer 23 spreads the composite light into monochromatic light, an enhanced Charge Coupled Device (ICCD) 24 amplifies the signal and performs photoelectric conversion, finally, a collected characteristic spectrogram is displayed on a computer terminal 25, and the spectral data is used for subsequent analysis of the LIBS technology.
The test sample preparation process and subsequent analysis of the present invention will be described in more detail with reference to specific examples.
Example 1
Taking a liquid to be detected containing heavy metal element copper (Cu) as an example, firstly weighing a proper amount of chemical reagent copper sulfate pentahydrate and mixing the chemical reagent copper sulfate pentahydrate with deionized water to prepare a mother solution with the concentration of 1000mg/L, and then diluting the mother solution step by step into a standard solution required by an experiment, wherein the concentrations of the prepared standard solutions are respectively 0.5mg/L, 2mg/L, 3mg/L, 4mg/L and 5 mg/L.
Weighing 0.9g of chelating resin, pouring the chelating resin into a glass tube, weighing 60mL of standard solution by using a measuring cylinder to serve as solution to be detected, adjusting the flow rate of a peristaltic pump to be 3mL/min, and then carrying out operations such as adsorption, drying, grinding, tabletting and the like according to the steps of the invention to prepare a series of required test samples, wherein the liquid to be detected is converted into a solid state.
And then, spectrum collection is carried out on a series of prepared test samples by using the detection device shown in fig. 3, wherein an Ultra 100 lamp pump compact Nd: YAG pulse laser of Quantel company is selected as the Nd: YAG laser 14, the laser wavelength is 1064nm, the pulse width is 5.82ns, the repetition frequency is 20Hz and the laser energy is 100mJ, and the pulse laser vertically focuses on the sample 18 to be tested after passing through the reflector 1 and the focusing lens 16 in sequence. The radiation light of plasma 17 generated by laser breakdown of a sample to be measured is coupled into an optical fiber 22 through an optical fiber coupler 21 by a light receiving lens 20, then transmitted to a spectrometer 23, subjected to photoelectric conversion by ICCD24, and finally displayed on a computer terminal 25 to obtain a characteristic spectrogram.
The chelating resin absorbed copper shown in figure 4 can be obtained by analyzing the acquired spectrograms of hair characteristics and experimental data
The spectrograms before and after the element and the relation graph of the flow rate of the sample to be measured and the obtained spectral line intensity shown in figure 5. As can be seen from fig. 4, the chelating resin matrix itself does not interfere with the spectral line of copper element, and there is no interference measurement of other heavy metal elements during LIBS analysis, and in addition, it can be seen that the spectral line of Cu i 324.7nm has higher intensity than other characteristic spectral lines, so that this spectral line is selected as the characteristic spectral line in the subsequent analysis of the experiment. Fig. 5 shows the relationship between the flow rate and the spectral line intensity of the sample to be measured, and it can be seen that the spectral line intensity gradually decreases with the increase of the flow rate, but considering that the liquid to be measured needs a longer time to pass through the glass tube if the flow rate decreases, the sample passing time is as short as possible while the higher spectral line intensity is obtained as possible, and the flow rate of the liquid to be measured is selected to be 3mL/min in the experiment for subsequent experiments.
Through comparative testing and analysis, in order to obtain higher spectral intensity and signal-to-back ratio at the same time, the acquisition parameters of the experiment are preferably set as follows: the laser pulse energy is 70mJ, the detection delay is 3 mus, and the gate width is 3 mus. Fig. 4 is a calibration curve of the copper element obtained by using LIBS on the test sample, and it can be seen that the linear fitting degree of the copper element is 0.995, and the detection limit of the copper element under the method is 0.027mg/L, which indicates that the sample preparation method can establish the linear relationship between the spectral line intensity and the concentration of the element to be detected, and the quantitative analysis on the heavy metal in the water body is feasible.
In summary, the sample preparation method provided by the invention not only can reduce the conversion of the liquid to be detected into the solid state under the conditions of simple operation method and low operation cost so as to fully exert the advantages of the LIBS technology in the aspect of solid detection, but also can obtain higher adsorption effect and lower detection limit due to the fact that the chelating resin has very strong adsorbability to metal ions and the heavy metal elements in the liquid to be detected can be fully adsorbed by the chelating resin in a peristaltic pump sample injection mode. The trace detection of the heavy metal in the water body by the sample preparation method provided by the invention has wide application prospect.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (6)
1. A method for preparing a LIBS liquid detection sample based on chelating resin is characterized by comprising the following steps:
(1) putting a preset amount of chelate resin into a glass tube, sealing one side of the glass tube by using a filter screen, and connecting one side of the glass tube with a peristaltic pump tube;
(2) the solution to be detected containing the metal element passes through the glass tube with the chelating resin at a preset flow rate under the driving of the peristaltic pump, and the solution to be detected is fully contacted with the chelating resin, so that metal ions contained in the solution to be detected are enriched and adsorbed on the chelating resin;
(3) after a half volume of solution to be measured is introduced into the glass tube, the peristaltic pump is suspended, and the glass tube is reversely placed in a pipeline of the peristaltic pump so as to be adsorbed more uniformly;
(4) continuously introducing the solution to be detected until the solution to be detected is completely introduced into the glass tube;
(5) taking out the chelating resin from the glass tube and drying;
(6) taking out the dried chelating resin, grinding, tabletting and preparing a LIBS liquid test sample;
(7) and analyzing the prepared sample by adopting a laser-induced breakdown spectroscopy system to obtain the content analysis of the metal elements in the water body.
2. The method for preparing LIBS liquid detection sample based on chelating resin as claimed in claim 1, wherein: the glass tube is vertically placed in the sample injection process, the inner diameter of the glass tube is 3-20mm, and the length of the glass tube is 5-20 cm.
3. The method for preparing LIBS liquid detection sample based on chelating resin as claimed in claim 1, wherein: and (3) enriching the metal elements in the water body by using chelate resin, wherein the sampling amount of the chelate resin is 0.5-10 g.
4. The method for preparing LIBS liquid detection sample based on chelating resin as claimed in claim 1, wherein: in the step (2), the step (3) and the step (4), the flow rate of the peristaltic pump is set to be 1-30 mL/min.
5. The method for preparing LIBS liquid detection sample based on chelating resin as claimed in claim 1, wherein: in the step (5), the drying temperature is selected to be 30-50 ℃.
6. The method for preparing LIBS liquid detection sample based on chelating resin as claimed in claim 1, wherein: in the step (6), the pressure intensity of the tablet press is set to be 5-20MPa, and the tablet pressing time is set to be 1-5 min.
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| CN114324491A (en) * | 2022-03-10 | 2022-04-12 | 深圳市检验检疫科学研究院 | Equipment and method for detecting heavy metal content by applying amino chelate resin |
| CN117805085A (en) * | 2024-02-29 | 2024-04-02 | 北京市农林科学院智能装备技术研究中心 | Method for measuring concentration of trace heavy metal ions in liquid |
| CN117805085B (en) * | 2024-02-29 | 2024-06-07 | 北京市农林科学院智能装备技术研究中心 | Method for measuring concentration of trace heavy metal ions in liquid |
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