CN108593631B - Method for detecting molecular free radical spectrum by aerosol-assisted laser probe - Google Patents
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Abstract
The invention discloses a method for detecting molecular free radical spectrum by an aerosol-assisted laser probe, which comprises the following steps: atomizing a solution containing metal elements into aerosol, placing the aerosol around a sample to be detected containing non-metal elements, and ablating the sample to be detected by adopting laser to combine the non-metal elements in the sample to be detected with the metal elements in the aerosol to generate free radical molecules; and detecting a fluorescence spectrum signal emitted by the free radical molecule to obtain the type and the content of the non-metal elements in the sample to be detected. The method is simple and reliable, avoids the influence of the matrix spectrum on the spectrum of the nonmetallic element, and improves the detection sensitivity of the laser probe on the nonmetallic element.
Description
Technical Field
The invention belongs to the field of laser plasma emission spectroscopy, and particularly relates to a method for detecting molecular free radical spectroscopy by an aerosol-assisted laser probe.
Background
The laser probe, called laser-induced breakdown spectroscopy (L IBS for short), is an atomic emission spectroscopy analysis technique, the basic principle of which is to ablate plasma on the surface of a sample to be measured by using a pulse laser beam, and to acquire the type and content information of elements contained in the sample by collecting and analyzing the emission spectrum of the plasma.
However, due to the special structure of the non-metal element atoms, the excitation energy required by the electron energy level is high, the characteristic spectral line with strong intensity in the plasma is concentrated in a vacuum ultraviolet region, and is easily absorbed by oxygen when the non-metal element atoms propagate in the air, so that the non-metal element atoms need to be collected under the protection of vacuum or inert gas, and are easily interfered by a matrix spectrum, and high requirements are provided for an optical collection system.
Due to the defects and shortcomings, further improvement and improvement are urgently needed in the field, a simple and reliable method for detecting the content of the nonmetallic elements by using the laser probe is designed, the signal intensity is improved, the influence of a matrix spectrum on a nonmetallic element spectrum can be avoided, and the detection sensitivity of the laser probe on the nonmetallic elements is improved.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a method for detecting a molecular free radical spectrum by an aerosol-assisted laser probe, so that the technical problems that the detection method is complicated and unreliable, the spectrum of a matrix has influence on the spectrum of a non-metallic element, and the detection sensitivity of the laser probe to the non-metallic element is low are solved.
In order to achieve the above object, the present invention provides a method for detecting molecular free radical spectroscopy by an aerosol-assisted laser probe, comprising:
(1) atomizing a solution containing metal elements into aerosol, placing the aerosol around a sample to be detected containing non-metal elements, and ablating the sample to be detected by adopting laser to combine the non-metal elements in the sample to be detected with the metal elements in the aerosol to generate free radical molecules;
(2) and detecting a fluorescence spectrum signal emitted by the free radical molecule to obtain the type and the content of the non-metal elements in the sample to be detected.
Further, the specific implementation manner of the step (1) is as follows:
atomizing a solution containing a metal element into aerosol, placing the aerosol around a sample to be detected containing a nonmetal element, ablating the sample to be detected by adopting laser, heating the sample to be detected and the aerosol to become plasma, atomizing the nonmetal element in the sample to be detected and the metal element in the aerosol to enter the plasma, and combining the nonmetal element atom and the metal element atom in the plasma into a free radical molecule.
Further, the step (2) comprises:
(2-1) the excited radiation or the spontaneous radiation of the radical molecule generates an electron energy level transition, thereby emitting a fluorescence spectrum signal;
and (2-2) detecting a fluorescence spectrum signal emitted by the free radical molecule to obtain the type and content of the non-metal elements in the sample to be detected.
Further, the specific implementation manner of the step (2-1) is as follows:
the plasma is irradiated by laser with the wavelength required by the excited transition of the electrons of the free radical molecules, and when the energy of a single photon irradiated by the laser is equal to the difference between two energy levels in the free radical molecules, the excited transition absorption of the electrons of the lower energy level is generated, the electrons of the upper energy level are transited to the upper energy level, the electrons of the upper energy level are unstable, the spontaneous radiation transition is generated, and the fluorescence spectrum signal is emitted.
Furthermore, the content of the metal element in the solution containing the metal element is higher than that of the nonmetal element in the sample to be detected.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the method utilizes the free radical molecular spectrum combined by the nonmetal elements and the metal elements in the visible waveband to replace the nonmetal atomic spectrum detection in the deep ultraviolet waveband, makes up the defect that the optical acquisition system has low acquisition efficiency in the deep ultraviolet waveband, and improves the detection sensitivity of the nonmetal elements. Because the use of non-metal atomic lines of deep ultraviolet wave bands which are easy to be absorbed by air is avoided, and free radical molecular spectral lines combined by non-metal elements and metal elements of visible light wave bands are used, a light path system does not need to be protected by vacuum or inert gas, and the detection method is simple and reliable.
(2) The method of the invention replaces the non-metal atomic spectrum in the conventional laser probe by detecting the emission spectrum of the free radical molecule combined by the non-metal element and the metal element, represents the content of the non-metal element by detecting the spectrum intensity of the free radical molecule combined by the non-metal element and the metal element, selectively adds the wavelength tunable laser beam to directly irradiate the plasma, only selectively excites the free radical molecule combined by the non-metal element and the metal element in the plasma, hardly influences other spectral lines of the emission spectrum of the plasma, can effectively reduce the interference of the spectral lines of the substrate, reduces the substrate effect, simultaneously enhances the free radical molecule signal combined by the non-metal element and the metal element with high selectivity, and improves the detection sensitivity of the laser probe to the non-metal element. The light path is changed less, the advantage of laser probe detection is not damaged, and the detection of the non-metal elements in a laboratory or an industrial field can be realized.
(3) Compared with a vacuum or inert gas protection method, the method provided by the invention can change the sample more quickly in the detection process, and can realize industrial online and remote analysis. The method utilizes the wavelength tunable laser as a non-metal element spectrum enhancing tool, and has common points with the excitation source of the laser probe, so compared with the existing methods at home and abroad, the method reserves the advantages of remote detection, on-line analysis, indiscriminate solid-liquid gaseous analysis and the like of the laser probe in the atmospheric environment.
Drawings
FIG. 1 is a schematic flow chart of a method for detecting molecular radical spectroscopy by an aerosol-assisted laser probe according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a detection apparatus according to an embodiment of the present invention;
FIG. 3 is a Ca-Cl radical spectrum of a sodium chloride sample provided in example 1 of the present invention;
FIG. 4 is a Ca-F radical spectrum of a sodium fluoride sample provided in example 2 of the present invention;
FIG. 5 is a Ca-F radical spectrum of a sodium fluoride sample provided in example 3 of the present invention;
the same reference numbers will be used throughout the drawings to refer to the same or like elements or structures, wherein:
1 is a fixed wavelength laser; 2 is a wavelength tunable laser; 3 is a grating spectrometer; 4 is an enhanced CCD; 5 is a time sequence generator; 6 is a computer; 7 is an atomization device; 8 is a vent pipe; 9 is a reflector; 10 is a first focusing lens; 11 is a second focusing lens; 12 is a spectrum collecting head; 13 is a transmission optical fiber; 14 is a USB data transmission line; 15 is a synchronizing signal transmission line; sample 16 is shown.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in fig. 1, a method for detecting molecular radical spectroscopy by an aerosol-assisted laser probe includes:
(1) atomizing a solution containing a metal element into aerosol, placing the aerosol around a sample to be detected containing a nonmetal element, ablating the sample to be detected by adopting laser, heating the sample to be detected and the aerosol to become plasma, atomizing the nonmetal element in the sample to be detected and the metal element in the aerosol to enter the plasma, and combining the nonmetal element atom and the metal element atom in the plasma into a free radical molecule.
(2) The plasma is irradiated by laser with the wavelength required by the excited transition of the electrons of the free radical molecules, and when the energy of a single photon irradiated by the laser is equal to the difference between two energy levels in the free radical molecules, the excited transition absorption of the electrons of the lower energy level is generated, the electrons of the upper energy level are transited to the upper energy level, the electrons of the upper energy level are unstable, the spontaneous radiation transition is generated, and the fluorescence spectrum signal is emitted. And detecting a fluorescence spectrum signal emitted by the free radical molecule to obtain the type and the content of the non-metal elements in the sample to be detected.
Furthermore, the content of the metal element in the solution containing the metal element is higher than that of the nonmetal element in the sample to be detected. So as to ensure that enough metal elements in the aerosol enter plasma after being atomized and are combined with non-metal element atoms.
As shown in FIG. 2, a detection device for implementing the method of the present invention comprises a fixed wavelength laser 1, a wavelength tunable laser 2, a grating spectrometer 3, an enhanced CCD4, a timing generator 5, a computer 6, an atomization device 7, a vent pipe 8, a reflector 9, a first focusing lens 10, a second focusing lens 11, a spectrum collection head 12, a transmission fiber 13, a USB data transmission line 14, a synchronization signal transmission line 15 and a sample 16, wherein the timing generator 5 is used for controlling the timing of light emission and spectrum collection of the instrument, trigger signals are provided for the fixed wavelength laser 1, the wavelength tunable laser 2 and the enhanced CCD4 through the synchronization signal transmission line 15, the fixed wavelength laser 1 is used for emitting laser beams for ablating the sample and aerosol, the reflector 9 is arranged in the laser emission direction and is used for reflecting the laser beams to the first focusing lens 10, the sample 16 is arranged in the emergent light direction of the first focusing lens 10, the wavelength tunable laser 2 is used for adjusting and emitting a specific wavelength laser beam which can enable the free radical molecules to be measured to generate energy level transition, the second focusing lens 11 is arranged in the emergent light direction of the specific wavelength laser, used for focusing laser beams on plasma, an atomizing device 7 is used for atomizing a solution configured in advance into aerosol and transferring the aerosol to a plasma region above a sample through a vent pipe 8, an outlet of the vent pipe 8 is arranged close to a laser ablation region so as to improve the aerosol content of the ablation region, a grating spectrometer 3 is connected with a spectrum collecting head 12 through an optical fiber 13, the device is used for imaging the collected plasma emission spectrum on the enhanced CCD4 after light splitting, the enhanced CCD4 is connected with the computer 6 through the USB data transmission line 14, and the spectrum result is used for qualitative and quantitative analysis.
The method for improving the detection sensitivity of the non-metal elements in the laser probe has the following action mechanism:
a laser is adopted to output laser beams to ablate the surface of a sample to be measured, the aerosol on the surface of the sample and close to the surface of the sample is rapidly heated to be changed into plasma, non-metal elements contained in the sample are atomized into non-metal element atoms to enter the plasma, metal elements in the aerosol are atomized to enter the plasma, and the non-metal atoms and the metal element atoms are combined into free radical molecules; selectively adjusting a wavelength tunable laser to a wavelength required by the stimulated transition of electrons of free radical molecules combined by non-metal elements and metal elements, outputting laser and irradiating plasma, wherein when the energy of a single photon of irradiated laser is equal to the difference between two energy levels in the free radical molecules combined by the non-metal elements and the metal elements, the electrons at the lower energy level are absorbed by the stimulated transition and are transitioned to the upper energy level, the electrons at the upper energy level are unstable, the spontaneous radiation transition is generated, and fluorescence is emitted. Collecting and recording emission fluorescence spectra of the free radical molecules combined by the non-metal elements and the metal elements, and performing qualitative or quantitative analysis by using the fact that the spectral intensity of the free radical molecules combined by the non-metal elements and the metal elements is in direct proportion to the content of the non-metal in the sample, so that the sensitivity of the laser probe to the detection of the non-metal elements can be improved.
Example 1
This method will be described in detail with reference to the detection of chlorine in sodium chloride as an example.
The sample was selected as sodium chloride with a chlorine content of 60.68 wt%.
The laser was a Brilliant type laser from Quantel, France, and the spectrometer was a SCT320 type spectrometer from Princeton Instrument. Selecting Ca-C1 free radical A2Π-X2The (0, 0)618.5nm and 621.1nm spectral lines in the ∑ band are observed lines.
(1) Pressing analytically pure sodium chloride powder into a wafer sample with the diameter of 4mm, preparing a calcium bromide solution with the concentration of 1g/ml, atomizing the calcium bromide solution into aerosol by using an ultrasonic atomizer, and spraying the aerosol to the vicinity of the surface of the sodium chloride sample;
(2) turning on a Brilliant laser to output laser, ablating the surface of a sodium chloride sample, generating plasma on the surface of the sodium chloride sample, enabling chlorine in the sodium chloride and metal elements in aerosol to be atomized and enter the plasma, and combining the chlorine atoms and the metal elements into Ca-C1 free radicals;
(3) collection of Ca-Cl radical A2Electron spontaneous radiative transition to X in pi energy band v-0 energy level2∑ the fluorescence signal emitted when the energy band v is 0 energy level is recorded.
As shown in FIG. 3, no weaker 621.1nm spectrum of Ca-Cl radicals was observed without aerosol assistance. A621.1 nm spectrum of Ca-Cl radicals was observed after aerosol assistance with 1g/ml CaBr solution.
In conclusion, the method can obviously detect the spectrum of the nonmetal elements in the laser probe and improve the sensitivity of the laser probe for detecting the chlorine element.
Example 2
This method will be described in detail with reference to the detection of fluorine in sodium fluoride as an example.
The sample is selected to be sodium fluoride, and the content of fluorine element is 45.24%.
The laser is an Ultra50 type laser from Bigsky, USA, and the spectrometer is an SR-500i type spectrometer from Andor. Selecting Ca-F free radical A2Π-X2The (0, 0)606.4nm spectrum in the ∑ band is the observation line.
(1) Pressing analytically pure sodium fluoride powder into a wafer sample with the diameter of 4mm, preparing 4ml of calcium bromide solution with the concentration of 1g/ml, atomizing the calcium bromide solution into aerosol by using an ultrasonic atomizer, and spraying the aerosol to the vicinity of the surface of the sodium fluoride sample;
(2) an Ultra50 laser is turned on to output laser, the surface of a sodium chloride sample is ablated, plasma is generated on the surface of the sodium chloride sample, chlorine in the sodium chloride and metal elements in aerosol are atomized and enter the plasma, and the chlorine atoms and the metal elements are combined into Ca-C1 free radicals;
(3) collection of Ca-F radical A2Electron spontaneous radiative transition to X in pi energy band v-0 energy level2∑ the fluorescence signal emitted when the energy band v is 0 energy level is recorded.
As shown in fig. 4, no weaker 606.4nm spectrum of Ca-F radicals was observed without aerosol assistance. After aerosol-assisted addition of 1g/ml CaBr solution, a spectrum of 606.4nm Ca-F radicals was observed. .
In conclusion, the method can obviously detect the spectrum of the nonmetal elements in the laser probe and improve the sensitivity of the laser probe for detecting the fluorine elements.
Example 3
Calcium bromide solutions with different concentrations are prepared, and the method is described in detail by taking the example of detecting fluorine in sodium fluoride.
The sample is selected to be sodium fluoride, and the content of fluorine element is 45.24%.
The laser is Brilliant type laser from Quantel in France, and the spectrometer is SR-500i type spectrometer from Andor. Selecting Ca-F free radical A2Π-X2The (0, 0)606.4nm spectrum in the ∑ band is the observation line.
(1) Pressing analytically pure sodium fluoride powder into a wafer sample with the diameter of 4mm, preparing 4ml of calcium bromide solution with the concentration of 0.5g/ml and 1g/ml, atomizing the calcium bromide solution into aerosol by using an ultrasonic atomizer, and spraying the aerosol to the position near the surface of the sodium fluoride sample;
(2) opening an Ultra50 laser to output laser, ablating the surface of a sodium chloride sample, generating plasma on the surface of the sodium chloride sample, enabling chlorine in the sodium chloride and metal elements in aerosol to be atomized and enter the plasma, and combining the chlorine atoms and the metal elements into Ca-Cl free radicals;
(3) collection of Ca-F radical A2Electron spontaneous radiative transition to X in pi energy band v-0 energy level2∑ the fluorescence signal emitted when the energy band v is 0 energy level is recorded.
As shown in FIG. 5, a weaker 606.4nm spectrum of Ca-F radicals was observed after aerosol-assist addition of 0.5g/ml CaBr solution. After adding 1g/ml CaBr solution aerosol for assistance, a stronger spectrum of the Ca-F free radical 606.4nm can be observed.
In summary, the metal ion solution is prepared in a concentration as high as possible to ensure that sufficient particles are bonded to the nonmetal elements. The method can obviously detect the spectrum of the non-metal element in the laser probe and improve the sensitivity of the laser probe for detecting the fluorine element.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A method for detecting molecular free radical spectrum by an aerosol-assisted laser probe is characterized by comprising the following steps:
(1) atomizing a solution containing metal elements into aerosol, placing the aerosol around a sample to be detected containing non-metal elements, and ablating the sample to be detected by adopting laser to combine the non-metal elements in the sample to be detected with the metal elements in the aerosol to generate free radical molecules;
(2) detecting a fluorescence spectrum signal emitted by free radical molecules to obtain the type and content of non-metal elements in a sample to be detected;
the content of the metal elements in the solution containing the metal elements is higher than that of the nonmetal elements in the sample to be detected.
2. The method for detecting molecular free radical spectroscopy by using the aerosol-assisted laser probe as claimed in claim 1, wherein the specific implementation manner of the step (1) is as follows:
atomizing a solution containing a metal element into aerosol, placing the aerosol around a sample to be detected containing a nonmetal element, ablating the sample to be detected by adopting laser, heating the sample to be detected and the aerosol to become plasma, atomizing the nonmetal element in the sample to be detected and the metal element in the aerosol to enter the plasma, and combining the nonmetal element atom and the metal element atom in the plasma into a free radical molecule.
3. The method for detecting molecular radical spectroscopy with an aerosol-assisted laser probe as claimed in claim 2, wherein the step (2) comprises:
(2-1) the excited radiation or the spontaneous radiation of the radical molecule generates an electron energy level transition, thereby emitting a fluorescence spectrum signal;
and (2-2) detecting a fluorescence spectrum signal emitted by the free radical molecule to obtain the type and content of the non-metal elements in the sample to be detected.
4. The method for detecting molecular free radical spectroscopy by using the aerosol-assisted laser probe as claimed in claim 3, wherein the specific implementation manner of the step (2-1) is as follows:
the plasma is irradiated by laser with the wavelength required by the excited transition of the electrons of the free radical molecules, and when the energy of a single photon irradiated by the laser is equal to the difference between two energy levels in the free radical molecules, the excited transition absorption of the electrons of the lower energy level is generated, the electrons of the upper energy level are transited to the upper energy level, the electrons of the upper energy level are unstable, the spontaneous radiation transition is generated, and the fluorescence spectrum signal is emitted.
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| CN111948187A (en) * | 2020-09-18 | 2020-11-17 | 南开大学 | Device and method for detecting free radicals |
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