Hydride generation-atmospheric pressure glow discharge atomic spectrum device
阅读说明:本技术 一种氢化物发生-大气压辉光放电原子光谱装置 (Hydride generation-atmospheric pressure glow discharge atomic spectrum device ) 是由 汪正 彭晓旭 于 2018-08-01 设计创作,主要内容包括:一种氢化物发生-大气压辉光放电原子光谱装置,该装置包括:T型三通阀;设置在所述T型三通阀上的大气压辉光放电发生区;向所述大气压辉光放电发生区输入载气以及待分析样品并与所述T型三通阀连通的氢化物发生区;设置在所述T型三通阀上,用于对所述大气压辉光放电发生区进行冷却的冷却系统;接收所述大气压辉光放电发生区产生的原子发射光谱信号的检测系统;为所述大气压辉光放电发生区放电提供电能的电源系统。本发明进一步简化了大气压辉光放电激发源装置的结构,并提高了装置的集成度。(A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device, the device comprising: a T-shaped three-way valve; an atmospheric glow discharge generation region arranged on the T-shaped three-way valve; a hydride generating area which inputs carrier gas and a sample to be analyzed to the atmospheric pressure glow discharge generating area and is communicated with the T-shaped three-way valve; the cooling system is arranged on the T-shaped three-way valve and is used for cooling the atmospheric glow discharge generating area; a detection system for receiving the atomic emission spectrum signal generated by the atmospheric pressure glow discharge generation area; and the power supply system is used for providing electric energy for the discharge of the atmospheric pressure glow discharge generation area. The invention further simplifies the structure of the atmospheric glow discharge excitation source device and improves the integration level of the device.)
1. A hydride generation-atmospheric pressure glow discharge atomic spectrum device is characterized in that,
the device includes:
a T-shaped three-way valve;
an atmospheric glow discharge generation region arranged on the T-shaped three-way valve;
a hydride generating area which inputs carrier gas and a sample to be analyzed to the atmospheric pressure glow discharge generating area and is communicated with the T-shaped three-way valve;
the cooling system is arranged on the T-shaped three-way valve and is used for cooling the atmospheric glow discharge generating area;
a detection system for receiving the atomic emission spectrum signal generated by the atmospheric pressure glow discharge generation area;
and the power supply system is used for providing electric energy for the discharge of the atmospheric pressure glow discharge generation area.
2. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the atmospheric pressure glow discharge generation area comprises a first high-temperature-resistant quartz tube, a second high-temperature-resistant quartz tube with the size different from that of the first high-temperature-resistant quartz tube, a hollow electrode and a hollow counter electrode.
3. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 2,
in the atmospheric pressure glow discharge generation area, the hollow electrode is embedded in a first high-temperature-resistant quartz tube with matched size, and the outer wall of the hollow electrode is attached to the inner wall of the first high-temperature-resistant quartz tube.
4. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 2,
the atmospheric pressure glow discharge generation area is embedded with the hollow electrode by adopting a second high-temperature-resistant quartz tube, the first high-temperature-resistant quartz tube and the hollow counter electrode are fixed into a whole, and the hollow electrode and the hollow counter electrode are coaxial.
5. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the hydride generating area adopts inert gas as a discharge medium of atmospheric pressure glow discharge and a sample transmission carrier gas.
6. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the T-shaped three-way valve adopts a PTFE pipe with adaptive size to fix the atmospheric pressure glow discharge generation area on the T-shaped three-way valve.
7. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the cooling system is used for cooling by introducing cooling air between the high-temperature-resistant quartz tube arranged at the outer side of one end of the T-shaped three-way valve and the first high-temperature-resistant quartz tube embedded with the hollow electrode.
8. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the hydride generation zone comprises: peristaltic pump, sample transmission silicone tube, T type reaction piece, gas-liquid separator, gas flowmeter, drier.
9. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
and in the atmospheric pressure glow discharge generation area, the hollow electrode is directly contacted with the hollow counter electrode through connecting a current stabilizing resistor with the resistance value of 2.5-12 k omega in series to trigger and generate atmospheric pressure glow discharge micro plasma.
10. A hydride generation-atmospheric pressure glow discharge atomic spectroscopy device according to claim 1,
the detection system is characterized in that an optical fiber probe of a micro spectrometer is axially arranged along the atmospheric pressure glow discharge generation area, and an ultraviolet fused quartz plane window is arranged between the atmospheric pressure glow discharge generation area and the optical fiber probe.
Technical Field
The invention belongs to the field of atomic spectrum analysis, relates to the technical field of atomic emission spectrum excitation sources, and more particularly relates to a hydride generation-atmospheric pressure glow discharge atomic spectrum device which can be applied to the field of atomic emission spectrum.
Background
With the rapid development of national economic construction and social life, the problems of heavy metal pollution in the environment, heavy metal residue in food and the like are increasingly prominent, and a new challenge is provided for the current analysis and test technology. Today, the most common detection method for micro, trace metal element analysis is mainly atomic spectroscopy/mass spectrometry. Based on the characteristics of high sensitivity, wide linear range and the like, the method becomes an irreplaceable basic analytical instrument in a plurality of fields such as environment, chemical engineering, biology and the like. However, these instruments are bulky, power intensive, require inert gases, even hazardous gases, and are expensive, which limits the miniaturization and portable development of the instrument and makes it difficult to use for on-site analysis and monitoring. The atmospheric pressure glow discharge micro-plasma is plasma with the size limited to millimeter level or even lower, has the characteristics of operation under atmospheric pressure, small volume, low power consumption, stability of spectral measurement and the like, and is easy to realize miniaturization and field analysis. Therefore, the research work of developing the atomic emission spectrum excitation source based on the atmospheric pressure glow discharge micro-plasma has important significance for the portable development of atomic spectrum instruments.
The existing atmospheric pressure glow discharge device applied to an excitation source of an atomic emission spectrum has low detection sensitivity on partial heavy metal elements (such as arsenic, lead, germanium and the like) and high detection limit, and cannot meet the requirement of micro-trace analysis. According to the methods for separating and pre-enriching some elements, such as hydride generation and the like, target elements in a sample are pre-enriched and then excited by using an atomic emission spectrum excitation source, so that the interference of a matrix is effectively reduced, and the selectivity and detection sensitivity of element analysis and the like are improved. Meanwhile, because different elements excite different concentrated positions in the atmospheric pressure glow discharge, when the atomic emission spectroscopy is applied, the optical radiation signals of specific positions in an atmospheric pressure glow discharge generation area need to be selectively collected aiming at the different elements, so that the complexity of element analysis is increased to a certain extent, and the detection stability and sensitivity of the signals are influenced.
In conclusion, according to the excitation characteristic of the atmospheric pressure glow discharge to elements, the atmospheric pressure glow discharge is improved, the structure of the atmospheric pressure glow discharge excitation source device is further simplified, the excitation intensity of different elements is improved under low power consumption, meanwhile, the sensitivity of signal acquisition is improved through the acquisition mode of the atmospheric pressure glow discharge light radiation signals, and the realization that the portable low-power-consumption micro-plasma device can be used for carrying out high-sensitivity and high-selectivity analysis on the elements is a key problem to be solved urgently in the field at present.
Disclosure of Invention
In view of the above, according to the characteristics of atomic emission spectroscopy, the technical problems to be solved by the present invention are to optimally design an atmospheric pressure glow discharge microplasma device, simplify the structure of the whole device, improve the integration level of the whole structure design, and improve the sensitivity of signal detection when the atmospheric pressure glow discharge microplasma device is applied to atomic emission spectroscopy by improving the discharge energy density of the atmospheric pressure glow discharge microplasma device and improving the acquisition mode of atomic emission spectroscopy signals.
In order to achieve the above object, the present invention provides the following technical solutions:
a hydride generation-atmospheric pressure glow discharge atomic spectroscopy device, the device comprising: a T-shaped three-way valve;
an atmospheric glow discharge generation region arranged on the T-shaped three-way valve;
a hydride generating area which inputs carrier gas and a sample to be analyzed to the atmospheric pressure glow discharge generating area and is communicated with the T-shaped three-way valve;
the cooling system is arranged on the T-shaped three-way valve and is used for cooling the atmospheric glow discharge generating area;
a detection system for receiving the atomic emission spectrum signal generated by the atmospheric pressure glow discharge generation area;
and the power supply system is used for providing electric energy for the discharge of the atmospheric pressure glow discharge generation area.
Preferably, the T-shaped three-way valve is a stainless steel T-shaped three-way valve.
The invention further simplifies the structure of the atmospheric glow discharge excitation source device and improves the integration level of the device.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the atmospheric pressure glow discharge generation region includes a first high temperature-resistant quartz tube, a second high temperature-resistant quartz tube having a different size from the first high temperature-resistant quartz tube, a hollow electrode, and a hollow counter electrode. Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, in the atmospheric pressure glow discharge generation region, the hollow electrode is embedded in a first high temperature resistant quartz tube with a matched size, and the outer wall of the hollow electrode is attached to the inner wall of the high temperature resistant quartz tube. More preferably, the inner diameter of the first high-temperature resistant quartz tube is 1.4-1.8 mm, and the outer diameter is 2.8-3.2 mm.
In the invention, the hollow electrode is embedded in the first high-temperature-resistant quartz tube with the adaptive size, so that the effective volume of glow discharge is limited, and the discharge energy density is improved. Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the atmospheric pressure glow discharge generation region adopts a second high temperature resistant quartz tube to fix the first high temperature resistant quartz tube embedded with the hollow electrode and the hollow counter electrode into a whole, and keeps the hollow electrode and the hollow counter electrode coaxial. More preferably, the inner diameter of the second high-temperature resistant quartz tube is 2.8-3.2 mm, and the outer diameter is 3.8-4.2 mm.
By means of the design of the atmospheric pressure glow discharge generating area, the high integration level of the atmospheric pressure glow discharge area is ensured, and the hollow electrode and the hollow counter electrode are coaxial, so that the spectral signal is allowed to be acquired along the axial direction of the atmospheric pressure glow discharge generating area.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectroscopy device, the hydride generation region uses an inert gas (He or Ar) as a discharge medium of the atmospheric pressure glow discharge and a sample transport carrier gas.
By means of this, on the one hand, for transporting the products of the hydride generation zone to the atmospheric pressure glow discharge generation zone; and on the other hand, a certain medium foundation is provided for triggering and maintaining the atmospheric pressure glow discharge micro-plasma.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the T-shaped three-way valve adopts a PTFE (polytetrafluoroethylene, for short, for poly tetra fluoro ethylene) tube with a suitable size to fix the atmospheric pressure glow discharge generation region on the T-shaped three-way valve.
By means of the method, the integration level of the whole device is improved to a certain extent.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the cooling system is configured to cool the substrate by introducing a cooling gas between an outer high temperature-resistant quartz tube installed at one end of the T-shaped three-way valve and a high temperature-resistant quartz tube having a hollow electrode embedded therein.
By virtue of this, the cooling system ensures that the hollow electrode and the hollow counter electrode are not excessively worn under high intensity discharge in the present invention.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the hydride generation region includes a peristaltic pump, a sample transmission silicone tube, a T-shaped reaction block, a gas-liquid separator, a gas flow meter, and a drying agent.
By virtue of this, the hydride generation region of the present invention can extract and separate out effective analytical components. The gas flowmeter ensures that the carrier gas carrying the sample can stably enter the atmospheric pressure glow discharge generation area through the drying agent, and improves the stability of the atmospheric pressure glow discharge micro-plasma.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the carrier gas carries the gas sample generated in the gas-liquid separator into the atmospheric pressure glow discharge generation region through the desiccant at a suitable carrier gas flow rate by the gas flow meter.
With the help of the method, the drying agent absorbs and removes liquid components in effective analysis components generated by hydride reaction, and the stability of the atmospheric pressure glow discharge micro-plasma is improved.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the atmospheric pressure glow discharge generation region is connected in series with a current stabilizing resistor with a resistance value of approximately 2.5 to 12 k Ω, and the hollow electrode is directly contacted with the hollow counter electrode to trigger generation of the atmospheric pressure glow discharge microplasma.
By means of the resistance, the current-stabilizing resistor avoids the phenomenon that the arc is converted into the electric arc in the process of generating the atmospheric pressure glow discharge micro-plasma by the contact triggering of the hollow electrode and the hollow counter electrode, and meanwhile, the stability of the atmospheric pressure glow discharge micro-plasma is improved.
Preferably, in the hydride generation-atmospheric pressure glow discharge atomic spectrum device, the detection system is configured such that the optical fiber probe of the micro spectrometer is axially disposed along the atmospheric pressure glow discharge generation region, and the ultraviolet fused quartz planar window is disposed between the atmospheric pressure glow discharge generation region and the optical fiber probe.
According to the invention, the spectral signal acquisition is carried out along the axial direction of the atmospheric pressure glow discharge generation area, so that on one hand, the sensitivity of optical signal acquisition is improved, and meanwhile, the influence of optical signal fluctuation on the signal acquisition stability is avoided to a certain extent. The portable low-power excitation source device is used for carrying out high-sensitivity and high-selectivity analysis on elements.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a hydride generation-atmospheric glow discharge atomic spectroscopy device according to an embodiment of the present invention;
FIG. 2 is an atomic emission spectrum of Se element by a hydride generation-atmospheric glow discharge atomic spectrum device according to an embodiment of the present invention;
reference numerals:
1-reducing agent 2-sample solution 3-peristaltic pump 4-sample transmission silicone tube 5-T type quartz reaction block 6-gas flowmeter 7-gas-liquid separator 8-desiccant 9-hollow electrode 10-PTFE tube 11-stainless steel T type three-way valve 12-first high temperature resistant quartz tube 13-second high temperature resistant quartz tube 14-outer side high temperature resistant quartz tube 15-hollow counter electrode 16-ultraviolet fused quartz plane window 17-optical fiber probe 18-micro spectrometer 19-high voltage power supply 20-constant current resistance 21-copper wire 22-computer.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which embodiments of the invention are shown and described, and which are to be considered illustrative of the invention only, and not restrictive.
As shown in fig. 1, an atomic spectrum device for hydride generation-atmospheric glow discharge provided by an embodiment of the present invention includes: a stainless steel T-shaped three-
In this embodiment, as shown in fig. 1, the hollow electrode 9 having an inner diameter and an outer diameter of 1.1 mm and 1.6 mm respectively in the atmospheric glow discharge generation region is embedded in the first high temperature
In this embodiment, the hydride generation zone serves as a carrier gas/sample introduction port for the atmospheric pressure glow discharge generation zone. The rotation speed of the peristaltic pump 3 is set to be 0.4-1.0 mL/min, a reducing
Preferably, the carrier gas selected by the hydride generation area can be inert gas Ar or He gas, and the atmospheric pressure glow discharge generated by taking the He gas as a medium is columnar, so that the analyte can be effectively excited.
In the embodiment, a
Preferably, the high
In this embodiment, the
In this embodiment, the working process of the hydride generation-atmospheric pressure glow discharge atomic spectrum device is as follows: the reducing
In conclusion, the hydride generation-atmospheric pressure glow discharge atomic spectrum device structure provided by the embodiment is further simplified, and meanwhile, the integration level of the whole device is improved. The first high temperature
Fig. 2 is an atomic emission spectrum of Se element by the hydride generation-atmospheric glow discharge atomic spectrum device according to one embodiment of the present invention. The reducing
The invention introduces a cooling system to reduce the rapid loss of the hollow electrode 9 and the
In summary, the hydride generation-atmospheric pressure glow discharge atomic spectrum device provided by the invention comprises a stainless steel T-shaped three-way valve, a hydride generation area, a high temperature resistant quartz tube with a matched size, an atmospheric pressure glow discharge generation area and a signal acquisition system. The stainless steel T-shaped three-way valve is used for fixing the atmospheric pressure glow discharge generation area and each part element of the cooling system. The hydride generating area and the atmospheric pressure glow discharge generating area work in a matching way, and the input of carrier gas provides a medium basis for the generation of the atmospheric pressure glow discharge. In the signal detection system, the optical fiber probe couples the optical radiation generated by the atmospheric pressure glow discharge generation area to the micro spectrometer to detect and amplify the signal. When the hydride generation-atmospheric pressure glow discharge atomic spectrum device works, glow discharge micro-plasma generated in an atmospheric pressure glow discharge generation area is bound in a high-temperature-resistant quartz tube with a matched size. Under high intensity discharge, the cooling system can cool the hollow electrode and the hollow counter electrode. In the signal detection system, an atmospheric glow discharge generation area and a micro spectrometer optical fiber probe are horizontally and coaxially arranged for signal acquisition, and an ultraviolet fused quartz plane window is arranged between the atmospheric glow discharge generation area and the optical fiber probe.
The present invention may be embodied in several forms without departing from the spirit of the essential characteristics thereof, and the present invention is therefore to be considered in all respects as illustrative and not restrictive. For example, in the above embodiment, the T-shaped three-way valve is made of stainless steel T-shaped three-
Since the scope of the invention is defined by the claims rather than the specification, and all changes that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
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