CN217542868U - Laser-induced desorption-plasma emission spectroscopy system - Google Patents
Laser-induced desorption-plasma emission spectroscopy system Download PDFInfo
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Abstract
The utility model relates to a laser-induced desorption-plasma emission spectroscopy system belongs to elemental analysis technical field. The utility model comprises a sample introducing device, a low-temperature plasma atomization/excitation device, a laser induced desorption device, a spectrum measurement and data processing device, wherein the sample introducing device consists of a tabletting sample, an insulating carrier and a bidirectional transmission platform; the excitation device comprises an annular electrode, a quartz tube, a gas path joint, a gas flow controller and an alternating current high-voltage power supply; the laser induced desorption device comprises a laser generator, a laser transmission optical fiber and a focusing lens; the spectral measurement data processing device comprises a collimating lens, an optical fiber, a CCD detector and a host utility model; the analyzer is suitable for rapid detection of heavy metals, sulfur and halogen in solid and liquid samples, can realize real-time online detection, and can meet the requirements of element analyzers with low energy consumption and high sensitivity.
Description
Technical Field
The utility model relates to a laser-induced desorption-plasma emission spectroscopy system belongs to elemental analysis technical field.
Background
The samples of soil, crops, food, medicines and the like are characterized by complex components and low contents of heavy metal elements or effective sulfur and halogen, so that the sensitivity and the matrix interference resistance are the primary conditions for selecting the determination method for determining the samples. The spectroscopic methods based on graphite furnace atomic absorption spectrometry, inductively coupled plasma emission spectrometry, atomic fluorescence spectrophotometry, etc. have higher sensitivity for detecting heavy metals, sulfur and halogen, but need to pass through complicated sample pretreatment methods, such as: dilution, extraction, digestion, ashing, purification, redissolution and the like are carried out to improve the repeatability and accuracy of the detection. The complicated sample pretreatment method increases the analysis time, and causes unnecessary environmental pollution and detection errors due to the use of a large amount of extraction solvent and incomplete digestion steps. In addition, the traditional analytical instrument mostly needs a strict vacuum environment, and the instrument and equipment are large in size, so that the requirements of high-throughput and multi-batch real-time field analysis cannot be met.
In recent years, atmospheric pressure spectroscopic analysis techniques based on Dielectric Barrier Discharge (DBD) have attracted more and more attention due to their low energy consumption, strong excitation capability, high sensitivity and simple analytical operation methods. The DBD-based atomic/molecular emission spectroscopy is mainly used for analyzing gas and liquid samples at present, and because the DBD plasma temperature is low, usually room temperature, and cannot directly desorb the analyte in the tablet sample, it is difficult to be used for analyzing the tablet sample. Meanwhile, when a DBD spectroscopy is used for detecting gaseous and liquid samples, the samples to be detected are usually directly introduced into a gas path of the DBD, so that discharge instability is easily caused, even discharge property is changed, the stability of detection signals is affected, and the detection sensitivity is reduced.
SUMMERY OF THE UTILITY MODEL
Based on various restrictions of the existing elemental spectrum analysis method, the utility model aims to provide a laser-induced desorption-plasma emission spectroscopy system to develop it into the analytical instrument that is applicable to the rapid detection of heavy metal, sulfur and halogen in solid and liquid samples, so as to satisfy the strong demand of people to the portable elemental analyzer that can realize real-time online detection, can satisfy low energy consumption, high sensitivity again.
Laser-induced desorption-plasma emission spectroscopy system, including following part:
the sample introducing device comprises a tabletting sample, an insulating carrier and a bidirectional transmission platform; the tabletting sample is a tabletting formed by mixing the sample to be detected and a matrix material or directly powdering the sample to be detected and then processing, the tabletting sample is placed on the bidirectional transmission platform through an insulating carrier, and the tabletting sample moves along the X axis and the Y axis under the driving of the bidirectional transmission platform;
the excitation device comprises a quartz tube, a gas flow controller, an annular electrode and an alternating current high-voltage power supply; the quartz tube is vertically positioned above the tabletting sample, the quartz tube is connected with the gas flow controller through a gas circuit joint, the annular electrode is connected with the alternating-current high-voltage power supply, and the plasma torch is converged on the surface of the tabletting sample at a certain flow rate under the control of the gas flow controller;
the laser-induced desorption device comprises a focusing lens and a laser generator; the focusing lens is obliquely arranged above the tabletting sample, the focusing lens is connected with the laser generator through an optical fiber, and the laser is converged on the surface of the tabletting sample at a certain power and a certain incidence angle under the control of the laser generator;
the spectral measurement data processing device comprises a collimating lens and a CCD detector, wherein the collimating lens is arranged on one side of a tablet sample in parallel, the collimating lens is connected with the CCD detector through an optical fiber, and the collimating lens is aligned with the surface of the sample to transmit collected spectral optical information to the CCD detector.
Preferably, the tabletting samples are compressed into circular slices with uniform thickness and diameter by a tabletting machine, and the positions of the tabletting samples are adjusted along the x axis and the y axis by a bidirectional transmission platform.
Preferably, the matrix material of the tabletting sample is a mixture of one or more of microcrystalline cellulose, graphite and paraffin.
Preferably, the plasma is introduced into the inlet of the quartz tube through the gas path joint, and two groups of annular electrodes are arranged side by side along the outer wall of the outlet of the quartz tube; the plasma initiates dielectric barrier discharge under the action of the electrified annular electrode to generate a directional flow plasma torch.
Preferably, the plasma is converged on the surface of the tablet sample under the action of a ring-shaped electrode with current and voltage changes.
Preferably, the plasma is a gas excited by dielectric barrier discharge with a flow rate of 0.5-1.2L/min.
Preferably, the focal length of the focusing lens is 5cm, the incident included angle range is 30-90 degrees, and the laser spot of the focusing lens and the plasma torch are converged at the same point.
Preferably, the collimating lens is aligned with and placed in the same plane as the sample surface.
The utility model discloses the beneficial effect of system is: (1) The occupied space is small, the weight is light, and the volume of the traditional spectrum analysis instrument is mostly more than 1m 3 The weight of the instrument is mostly over 100kg; the system volume of the utility model is about 0.07m 3 The mass is about 10kg, and the portable type portable electric water heater has the characteristic of portability;
(2) The power consumed by the system of the utility model is 50-500W, and compared with the power of 1000W of the traditional ICP-AES, the energy consumption is greatly reduced;
(3) The system of the utility model has no vacuum condition limitation and can be operated under the normal pressure environment.
Drawings
Fig. 1 is a schematic diagram of the system of the present invention.
Fig. 2 is a schematic structural diagram of the excitation device of the present invention.
In the figure: 1. a quartz tube; 2. a ring-shaped electrode; 3. a gas circuit joint; 4. a gas flow controller; 5. an alternating current high voltage power supply; 6. a focusing lens; 7. a laser generator; 8. a collimating lens; 9. a CCD detector; 10. a bidirectional transmission platform; 11. an insulating carrier; 12. the samples were pressed into tablets.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1:
this embodiment 1 is after making liquid and solid sample preforming sample 12, adopts the utility model provides a laser-induced desorption-low temperature plasma atomic/molecular emission spectrometry detects the system architecture characteristic of the element that awaits measuring in the sample. The system structure of the laser-induced desorption-low-temperature plasma atomic/molecular emission spectrometry is shown in fig. 1 and 2, and comprises a sample introducing device, a low-temperature plasma atomization/excitation device, a laser-induced desorption device and a spectrum measurement and data processing device.
The sample introducing device is composed of a pressed sample 12, an insulating carrier 11 and a bidirectional transmission platform 10. The pressed sample 12 is placed directly on the insulating carrier 11 and the relative position of the sample to the plasma torch and laser is controlled by the bi-directional transfer platform 10.
The excitation device comprises an annular electrode 2, a quartz tube 1, a gas path joint 3, a gas flow controller 4 and an alternating current high-voltage power supply 5. The quartz tube 1 is connected with a gas flow controller 4 through a gas path joint 3, and the flow rate of the plasma gas in the quartz tube 1 is regulated by the gas flow controller 4. In the working state of the instrument, an alternating current high-voltage power supply 5 supplies power to a ring-shaped electrode 2 wound outside the tube wall of a quartz tube 1 to trigger dielectric barrier discharge and generate a plasma torch.
The laser induced desorption device comprises a laser generator 7, a laser transmission optical fiber and a focusing lens 6. The laser output by the laser generator 7 is converged on the surface of the pressed sample 12 with the plasma torch after being collected by the transmission optical fiber transmission and the focusing lens 6.
The spectral measurement data processing device comprises a collimating lens 8, an optical fiber, a CCD detector 9 and a host. Optical signals generated by low-temperature plasma excitation are collected by the collimating lens 8, transmitted by the optical fiber and detected by the CCD detector 9, and then transmitted to the host for data analysis, and data analysis software used by the host is commercially available spectrasite software.
In the technical scheme, a pair of annular electrodes 2 is wound on the outer wall of the quartz tube 1 at a position 5-10mm away from the end of the outlet tube, and the distance between the two annular electrodes 2 is 10-15mm. Among the annular electrodes 2, the annular electrode 2 close to the outlet end of the quartz tube 1 is grounded, and the annular electrode 2 far away from the outlet end of the quartz tube 1 is provided with bidirectional sine wave high voltage by an alternating current high voltage power supply 5. The gas supply device comprises a gas storage bottle, a gas flow controller 4 and a gas path pipe, wherein the inlet end of the quartz pipe 1 is connected with the gas flow controller 4 through a gas path joint 3 and the gas path pipe, and the gas flow controller 4 is used for adjusting and stabilizing the flow speed of plasma.
In the technical scheme, when the sample to be detected is solid, the sample needs to be pulverized by a pulverizer, and then the sample is made into a wafer with the thickness of 1-3mm and the diameter of 13mm by a tablet press under the pressure of 1.5 MPa. The wafer is placed directly on an insulating carrier 11 in the sample introduction system and the position of the sample is adjusted by a bidirectional transport stage 10 in the x and y axes. The tablet press has no special requirements, and the drug pulverizer and the infrared tablet press are both applicable.
In the technical scheme, when the sample to be detected is liquid, 1-50 mu L of the liquid sample is added into a matrix formed by mixing microcrystalline cellulose, graphite and other materials, and the mixture is air-dried and then is tabletted by a tabletting machine to prepare the sample. The method of preparing the pressed sample was the same as that of the pressed sample 12.
In the above technical solution, the laser generated by the laser source is guided by a laser transmission fiber, and the outlet end of the laser transmission fiber is connected to the focusing lens 6. The focal length of the focusing lens 6 is 5cm, and the incident included angle of the laser emitted by the focusing lens 6 on the surface of the sample is 30-90 degrees.
In the technical scheme, the tip of the plasma torch emitted by the excitation device and the laser are intersected on the surface of the tabletting sample 12, and the plasma torch is perpendicular to the surface of the tabletting sample 12.
In the above technical solution, the collimating lens 8 is aligned to the surface of the sample and placed in the same plane as the surface of the sample, one end of the collimating lens 8 is connected to the signal transmission optical fiber, and the optical signal is transmitted to the CCD detector by the optical fiber.
In order to obtain better technical effect, on the basis of the technical scheme, the utility model discloses still can further take following technical measure. The following technical measures can be taken individually, in combination, or simultaneously.
The dielectric barrier discharge plasma can adopt argon, helium, nitrogen, air and the like. Any plasma which can be excited by dielectric barrier discharge can be used as the working gas of the utility model.
The quartz tube 1 in the excitation device is preferably 10cm long and 2mm in inner diameter.
The output current of the alternating current high-voltage power supply 5 is 0-100mA, the output voltage is 0-10kV, and the output voltage is in a bidirectional sine wave or square wave form. Any high voltage power supply capable of providing the above current and voltage parameters can be used as the power supply in the excitation device of the present invention.
The flow rate of the plasma is controlled by a gas flow controller 4, and the flow rate of the common gas is 0.5-1.2L/min.
The ring electrode 2 material may be any electrically conductive material including, but not limited to, brass, aluminum, stainless steel, silver, platinum, graphite, and alloys thereof.
In the preparation method of the tablet sample 12, the matrix material mixed with the solid or liquid sample may be one or more of microcrystalline cellulose, paraffin, graphite and other materials, or the tablet sample 12 may be directly tableted without using the matrix material.
In the laser induced desorption device, the used laser has any wavelength from ultraviolet light to infrared band (266-2940 nm), and the output form of the laser can be continuous or pulse. In the case of continuous laser, the laser output power is preferably not less than 1W, and in the case of pulsed laser, the single pulse laser output energy is preferably not less than 1mJ.
Any suitable host, such as a laptop, desktop, etc., may be used for the spectral data processing device. The data processing software can adopt commercially available software, such as spectrasite software.
The utility model discloses can extensively apply to the elemental analysis occasion, the quick spectral detection occasion of heavy metal, elemental sulfur, halogen among the in particular to preforming sample 12.
Claims (7)
1. A laser-induced desorption-plasma emission spectroscopy system comprising:
the sample introducing device comprises a tabletting sample (12), an insulating carrier (11) and a bidirectional transmission platform (10); the tabletting sample (12) is a tabletting formed by mixing a sample to be detected and a matrix material or directly powdering the sample to be detected and then processing, the tabletting sample (12) is placed on the bidirectional transmission platform (10) through the insulating carrier (11), and the tabletting sample (12) moves along the X axis and the Y axis under the driving of the bidirectional transmission platform (10);
the excitation device comprises a quartz tube (1), a gas flow controller (4), a ring-shaped electrode (2) and an alternating current high-voltage power supply (5); the quartz tube (1) is vertically positioned above the tabletting sample (12), the quartz tube (1) is connected with a gas flow controller (4) through a gas circuit joint (3), the annular electrode (2) is connected with an alternating current high-voltage power supply (5), and the plasma torch is converged on the surface of the tabletting sample (12) at a certain flow rate under the control of the gas flow controller (4);
the laser-induced desorption device comprises a focusing lens (6) and a laser generator (7); the focusing lens (6) is obliquely arranged above the tabletting sample (12), the focusing lens (6) is connected with the laser generator (7) through an optical fiber, and the laser is converged on the surface of the tabletting sample (12) at a certain power and a certain incidence angle under the control of the laser generator (7);
spectral measurement data processing apparatus, including collimating lens (8) and CCD detector (9), collimating lens (8) parallel arrangement is in preforming sample (12) one side, and collimating lens (8) link to each other through optic fibre and CCD detector (9), and collimating lens (8) aim at the spectral optical information transmission to CCD detector (9) that the sample surface will be gathered.
2. The laser induced desorption-plasma emission spectroscopy system as set forth in claim 1, wherein the tabletted sample (12) is compressed into a circular disk of uniform thickness and diameter by a tablet press, and the position of the tabletted sample (12) is adjusted along x-axis and y-axis by the bi-directional transport platform (10).
3. The laser-induced desorption-plasma emission spectroscopy system as claimed in claim 1, wherein the inlet of the quartz tube (1) is introduced into the plasma through the gas circuit joint (3), and two groups of annular electrodes (2) are arranged side by side along the outer wall of the outlet of the quartz tube (1); the plasma body initiates dielectric barrier discharge under the action of the electrified annular electrode (2) to generate a directional flow plasma torch.
4. The laser induced desorption-plasma emission spectroscopy system of claim 3 wherein the plasma is focused on the surface of the tabletted sample (12) by the annular electrode (2) with varying current and voltage.
5. The laser-induced desorption-plasma emission spectroscopy system of claim 3, wherein the plasma is a gas excited by dielectric barrier discharge at a flow rate of 0.5-1.2L/min.
6. The laser-induced desorption-plasma emission spectroscopy system according to claim 1, wherein the focal length of the focusing lens (6) is 5cm, the included angle of incidence ranges from 30 to 90 degrees, and the laser spot of the focusing lens (6) and the plasma torch both meet at the same point.
7. Laser induced desorption-plasma emission spectroscopy system according to claim 1, wherein the collimator lens (8) is aligned and placed in the same plane as the sample surface.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116990287A (en) * | 2023-08-14 | 2023-11-03 | 元素聚焦(青岛)科技有限公司 | Solid sample spectrum-mass spectrum imaging system and method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116990287A (en) * | 2023-08-14 | 2023-11-03 | 元素聚焦(青岛)科技有限公司 | Solid sample spectrum-mass spectrum imaging system and method |
| CN116990287B (en) * | 2023-08-14 | 2024-05-03 | 元素聚焦(青岛)科技有限公司 | Solid sample spectrum-mass spectrum imaging system and method |
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