CN112630208A - Sample introduction system for atomic spectrum or mass spectrum - Google Patents
Sample introduction system for atomic spectrum or mass spectrum Download PDFInfo
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- CN112630208A CN112630208A CN201910953713.2A CN201910953713A CN112630208A CN 112630208 A CN112630208 A CN 112630208A CN 201910953713 A CN201910953713 A CN 201910953713A CN 112630208 A CN112630208 A CN 112630208A
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- 230000005284 excitation Effects 0.000 claims abstract description 22
- 238000001593 atomic mass spectrometry Methods 0.000 claims abstract description 16
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 16
- 229910052721 tungsten Inorganic materials 0.000 claims description 16
- 239000010937 tungsten Substances 0.000 claims description 16
- 239000002274 desiccant Substances 0.000 claims description 15
- 230000002572 peristaltic effect Effects 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
本发明的目的在于提供一种用于原子光谱或质谱的进样系统，能够有效去除试样中水分和基质，提高原子光谱仪、质谱仪激发单元的激发能力和稳定性，从而提高原子光谱仪、质谱仪的分析性能。包括：液体阴极辉光放电蒸气发生装置；与所述液体阴极辉光放电蒸气发生装置相连的气液分离器；与所述气液分离器相连的干燥装置；为所述液体阴极辉光放电蒸气发生装置提供电能的电源系统。
The purpose of the present invention is to provide a sample introduction system for atomic spectroscopy or mass spectrometry, which can effectively remove moisture and matrix in the sample, improve the excitation capability and stability of the excitation unit of the atomic spectrometer and mass spectrometer, and thereby improve the atomic spectrometer and mass spectrometer. analytical performance of the instrument. Including: a liquid cathode glow discharge vapor generating device; a gas-liquid separator connected with the liquid cathode glow discharge vapor generating device; a drying device connected with the gas-liquid separator; for the liquid cathode glow discharge vapor A power supply system that provides electrical energy to the generating device.
Description
Technical Field
The invention belongs to the field of atomic spectrum and mass spectrum analysis, relates to the technical field of sample introduction of atomic spectrum and mass spectrum, and more particularly relates to a sample introduction system of atomic spectrum and mass spectrum, which can be applied to the field of atomic spectrum and mass spectrum.
Background
With the development of heavy industry, heavy metal pollution is increasingly serious. For heavy metal micro trace analysis, an atomic spectrometer and a mass spectrometer are widely applied due to the advantages of low detection limit, high sensitivity, simultaneous multi-element analysis, simple operation and the like. However, for the liquid sample injection, atomization efficiency is not high, matrix interference is large, detection limit of some elements (such as mercury) is high, and sensitivity is poor. Therefore, it is desirable to improve the analysis sensitivity and stability of atomic spectrometers and mass spectrometers by using a sample injection system that reduces matrix interference and improves atomization efficiency and sample injection efficiency.
At present, the sampling devices for sampling liquid samples of atomic spectrometers and mass spectrometers generate hydride, are subjected to electrothermal evaporation and the like, can separate elements to be detected from solution matrixes, and reduce the energy consumption of the matrixes to an excitation unit, but the sampling systems have higher cost and operation cost, and do not have good sensitization effect on some elements (such as mercury), so that the application of the sampling devices is limited.
Therefore, in order to improve the sensitivity of the atomic spectrometer and the mass spectrometer to meet the requirement of environmental detection, a sample introduction system which is low in cost, simple to operate and convenient to combine with the atomic spectrometer and the mass spectrometer is required to be developed, and the sample introduction system can effectively remove moisture and matrix in a sample and improve the analysis performance of the atomic spectrometer and the mass spectrometer.
Disclosure of Invention
In view of this, the present invention provides a sample injection system for atomic spectroscopy or mass spectrometry, which can effectively remove moisture and matrix in a sample, and improve the excitation capability and stability of an excitation unit of an atomic spectrometer and a mass spectrometer, thereby improving the analysis performance of the atomic spectrometer and the mass spectrometer.
The invention relates to a sample introduction system for atomic spectroscopy or mass spectrometry, which comprises:
a liquid cathode glow discharge vapor generating device;
the gas-liquid separator is connected with the liquid cathode glow discharge steam generating device;
the drying device is connected with the gas-liquid separator;
and the power supply system is used for providing electric energy for the liquid cathode glow discharge vapor generating device.
Further, a conventional SCGD (liquid cathode glow discharge spectrometer) is a glow discharge at atmospheric pressure, and is connected to a detector as an excitation source. In the application, the SCGD is improved to be used as a steam generating device and is used together with an ICP-OES (inductively coupled plasma atomic emission spectrometer) so as to optimize a sample injection system of the ICP-OES, and therefore the sensitivity of the ICP-OES is improved. Because ICP-OES does not allow air to enter, SCGD needs a quartz cover to separate glow discharge from outside air, so that generated element vapor is conveyed to a detection system along with carrier gas, air interference is avoided, and pollution of glow discharge products to the surrounding environment is reduced. The quartz material meets the requirement of high temperature resistance, and the quartz cover is transparent, so that the discharge condition can be observed.
Further, in the present invention, the liquid cathode glow discharge vapor generation device is a device for forming atomic or molecular vapor by atomizing an element to be measured in a solution with microplasma generated by liquid cathode glow discharge, and includes: quartz cover, last mouthful of stopper, lower mouthful of stopper, glass capillary, peristaltic pump, row's of waste pipe, negative pole graphite rod and positive pole tungsten rod, quartz cover possesses carrier gas entry, carrier gas export and graphite rod inserted hole, positive pole tungsten rod inserts from last mouthful of stopper center, lower mouthful of stopper possesses two holes, inserts respectively the glass capillary with arrange the waste pipe, the graphite rod inserted hole is embedded negative pole graphite rod, negative pole graphite rod one end possesses a radial aperture, and the vertical through is crossed in the hole the glass capillary, the peristaltic pump to glass capillary transportation sample solution, and the transportation waste liquid in the row's of waste pipe.
Preferably, the anode tungsten rod and the glass capillary are coaxial, so that ignition is smooth, and a loop is realized by the fact that the anode tungsten rod is contacted with the solution through the highest liquid level when the anode tungsten rod and the glass capillary are ignited. Meanwhile, the effective volume of glow discharge can be limited, so that the discharge is more stable.
Preferably, after most of condensed water is removed by the vapor generated by the liquid cathode glow discharge vapor generation device through the gas-liquid separator, the vapor concentration of the element to be detected is increased through the drying device, and the vapor is conveyed to an excitation and detection unit of an atomic spectrometer or a mass spectrometer by carrier gas.
According to the invention, aerosol generated by the liquid cathode glow discharge steam generating device can sequentially enter the atomic spectrometer and the mass spectrometer through the gas-liquid separator and the drying device for further excitation, so that the condensation loss in a pipeline is reduced, the influence of moisture in steam on the energy consumption and stability of an excitation unit is reduced, the steam concentration of an element to be detected is improved, and the detection sensitivity is improved.
In the present invention, the carrier gas pipes of the atomic spectrometer and the mass spectrometer may be connected to the liquid cathode glow discharge vapor generation device, and the carrier gas of the atomic spectrometer and the mass spectrometer may be used as the carrier gas of the vapor generated by the liquid cathode glow discharge vapor generation device. Preferably, the carrier gas is introduced from the carrier gas inlet of the quartz cover, the flow rate of the carrier gas can be directly controlled by computer software of an atomic spectrometer or a mass spectrometer, a gas flowmeter is not needed, and the operation is simpler.
In the invention, the gas-liquid separator comprises a container, a waste discharge pipe, an air inlet pipe and an air outlet pipe, the air inlet pipe is connected with the liquid cathode glow discharge steam generating device, the air outlet pipe is connected with the drying device, and the peristaltic pump transports the condensate in the waste discharge pipe. The beneficial effects are as follows: most of condensed water can be removed by using the gas-liquid separator, the concentration of element steam is improved, the energy loss of the excitation unit is reduced, and the stability of the excitation unit is also improved. Most of condensed water in the element steam is removed through a gas-liquid separator, and part of steam is removed through a drying device. The two cannot be reversed in order, otherwise the drying device would be rendered inoperative by absorption of large quantities of water vapor. The gas-liquid separator continuously operates because condensed water is discharged in time.
Preferably the container top has two holes, insert respectively the intake pipe with the outlet duct, the intake pipe with the carrier gas outlet of quartz capsule links to each other, the outlet duct mouth of pipe height is higher than the intake pipe mouth of pipe height, container lateral wall or bottom have a hole, insert waste pipe, waste pipe mouth of pipe height is less than the intake pipe mouth of pipe height, the peristaltic pump transportation condensate in the waste pipe of arranging. The beneficial effects are as follows: the intake pipe mouth of pipe height is lower, and trachea length is longer, the vapor condensation of being convenient for, and the outlet duct mouth of pipe height is higher, and trachea length is shorter, is convenient for give vent to anger. The height of the pipe orifice of the waste discharge pipe determines the liquid level height of the waste liquid, the pipe orifices of the two gas pipes cannot be below the liquid level, otherwise, gas transportation is not smooth, and the effect of removing condensed water cannot be achieved.
According to the invention, the drying device may include a transparent container, a drying agent, and an air outlet pipe, the air outlet pipe is connected to the excitation unit of the atomic spectrometer or the mass spectrometer, and the drying agent is contained in the transparent container. The transparent container can observe the use condition of the drying agent in real time.
The drying agent is filled in the transparent container, two holes are formed in the top of the container and are respectively inserted into the air outlet pipe of the drying device and the air outlet pipe of the gas-liquid separator, the height of the pipe orifice of the air outlet pipe of the drying device is higher than that of the pipe orifice of the air outlet pipe of the gas-liquid separator, and the upper surface of the drying agent is lower than that of the pipe orifice of the air outlet pipe of the gas-liquid separator.
The height of the mouth of the air inlet pipe of the drying device is lower, so that the drying device is beneficial to more fully drying air, but the air inlet pipe does not extend below the surface of the drying agent as far as possible, because if the analysis time is too long, more moisture is absorbed by the drying agent, and much condensed water exists. The drying device can absorb the steam which is not condensed in the gas-liquid separator, thereby further improving the steam concentration and the excitation efficiency of the excitation unit.
In the invention, the main body of the quartz cover is a quartz tube with the height of 75-78 mm, the inner diameter of 26-30 mm and the wall thickness of 1.5-2 mm; the carrier gas inlet, the carrier gas outlet and the graphite rod insertion opening are respectively thin quartz tubes with the inner diameters of 2-4 mm, 4-5 mm and 5-6 mm, and are respectively fired at the position 5-7 mm away from the bottom, 54-58 mm and 17-19 mm away from the bottom of the main body.
According to the invention, the device is very small and convenient to be used together with an atomic spectrometer or a mass spectrometer.
In the present invention, the power supply system may be a dc power supply for supplying electric energy to the liquid cathode glow discharge vapor device. The direct current power supply applies high voltage to the two electrodes, micro-plasma is formed between the two electrodes, elements to be detected in the solution undergo desolvation in the micro-plasma, and are combined with secondary electrons after coulomb explosion to form gaseous atoms, and the gaseous atoms enter an atomic spectrometer or a mass spectrometer along with carrier gas for excitation and analysis. The sample is converted into a gaseous form and is introduced into an excitation unit of an atomic spectrometer or a mass spectrometer, so that the sample injection efficiency is higher.
In the invention, the air inlet pipe and the air outlet pipe of the gas-liquid separator and the air outlet pipe of the drying device are respectively air pipes with the lengths of 15-20 mm, 10-15 mm and 20-40 mm.
According to the invention, the gas inlet pipe and the gas outlet pipe of the gas-liquid separator and the gas outlet pipe of the drying device are used for connecting the liquid cathode glow discharge steam generating device and an atomic spectrometer or a mass spectrometer to transmit samples, the shorter the gas pipe length is, the less the sample is lost on a transmission path, and meanwhile, the phenomenon that gas flow is blocked due to condensation of water vapor in the gas pipe is reduced.
According to the invention, the samples and the waste liquid in the sample introduction pipeline and the waste discharge pipe of the liquid cathode glow discharge steam generating device and the waste discharge pipe of the gas-liquid separator are respectively introduced and discharged by the same peristaltic pump, so that the space is reduced, and the operation is simple.
Drawings
FIG. 1 is a schematic diagram of an overall structure of a sample injection system for atomic spectroscopy or mass spectrometry according to an embodiment of the present invention;
reference numerals:
1-carrier gas inlet 2-quartz cover 3-upper opening plug 4-lower opening plug 5-anode tungsten rod 6-graphite rod insertion opening 7-graphite electrode (cathode graphite rod) 8-cathode glass capillary 9-waste discharge pipe 10-carrier gas outlet 11-lead 12-current limiting resistor 13-power supply 14-container 15-gas inlet pipe 16 of gas-liquid separator, gas outlet pipe 17 of gas-liquid separator, peristaltic pump 18-waste liquid 19-sample solution 20-waste liquid 21-transparent container 22-drying agent 23-gas outlet pipe of drying device.
Detailed Description
The present invention is further described below in conjunction with the following embodiments and the accompanying drawings, it being understood that the drawings and the following embodiments are illustrative of the invention only and are not limiting thereof.
Fig. 1 is a schematic overall structure diagram of a sample injection system for atomic spectroscopy or mass spectrometry according to an embodiment of the present invention. As shown in fig. 1, the sample injection system for atomic spectroscopy and mass spectrometry according to the present embodiment includes: a liquid cathode glow discharge vapor generating device; a gas-liquid separator; a drying device; and a power supply system for providing electrical energy to the liquid cathode glow discharge vapor generating device.
As shown in fig. 1, in the sample injection system for atomic spectroscopy or mass spectrometry of the present embodiment, the liquid cathode glow discharge vapor generation device includes a quartz cover 2, an upper port plug 3, a lower port plug 4, a cathode glass capillary 8, a peristaltic pump 17, a waste discharge pipe 9, a graphite electrode 7 (i.e., a cathode graphite rod), and an anode tungsten rod 5. The liquid cathode glow discharge vapor generation device also comprises a sample introduction pipeline which is not shown, preferably a sample introduction pipeline with an air bag, so that the liquid level of the solution reaches the maximum height by extruding the air bag, and the rapid ignition is realized.
Preferably, in the liquid cathode glow discharge vapor generator of the present embodiment, the main body of the quartz cover 2 is a quartz tube having a height of 75 to 78 mm, an inner diameter of 26 to 30 mm and a wall thickness of 1.5 to 2 mm, and the carrier gas inlet 1, the carrier gas outlet 10 and the graphite rod insertion port 6 are thin quartz tubes having inner diameters of 2 to 4 mm, 4 to 5 mm and 5 to 6 mm, respectively, and are fired at a distance of 5 to 7 mm from the bottom, 54 to 58 mm and 17 to 19 mm from the bottom of the main body.
As also shown in fig. 1, a dc power supply supplies power to the liquid cathode glow discharge vapor generation device to discharge and atomize the entering sample, thereby forming elemental vapor. For example, a high voltage power supply 13 shown in fig. 1, and a current limiting resistor 12 of, for example, 1.25 k Ω is connected in series in the liquid cathode glow discharge vapor generation device, so as to greatly reduce the probability of transition from glow discharge to arc discharge and improve the stability of glow discharge.
Preferably, a high voltage power supply capable of providing a DC high voltage of 0-1500V can be used.
With the help of the above, the lead wire led out from the positive electrode of the high-voltage power supply is connected with the anode tungsten rod 5, and the lead wire led out from the negative electrode is connected with the graphite electrode 7 through the current-limiting resistor 12. The graphite electrode 7 is horizontally inserted into the graphite rod insertion port 6 and fixed to one side of the quartz cover 2. The cathode glass capillary tube 8 vertically penetrates through the graphite electrode 7 with the hole and the high-temperature-resistant lower opening plug 4 and is located 2-4 mm, preferably 3 mm, right below the anode tungsten rod 5. The upper end pipe orifice of the cathode glass capillary 8 is 2-4 mm higher than the graphite electrode, and preferably 3 mm. The coaxial design of the anode tungsten rod 5 and the cathode glass capillary tube 8 ensures that the liquid cathode glow discharge steam generating device has higher integration level, improves the energy density of liquid cathode glow discharge, and further improves the atomization efficiency and the steam generation efficiency.
Preferably, the upper and lower port plugs 3 and 4 may be machined from a high temperature resistant, acid resistant, corrosion resistant insulator material such as polytetrafluoroethylene; the diameter of the anode tungsten rod 5 can be 1.5-3 mm, and preferably 2.5 mm.
As shown in fig. 1, in the sample injection system for atomic spectroscopy or mass spectrometry of the present embodiment, the gas-liquid separator includes a container 14, an inlet pipe 15, an outlet pipe 16, and a waste discharge pipe not shown.
Preferably, the container 14 is made of a high temperature resistant material, the top of the container 14 is provided with two holes into which the gas inlet pipe 15 and the gas outlet pipe 16 are respectively inserted, the gas inlet pipe 15 is connected with the carrier gas outlet 10 of the quartz cover 2, the height of the pipe orifice of the gas inlet pipe 15 is lower than that of the pipe orifice of the gas outlet pipe 16, the side wall of the container 14 is provided with one hole into which the waste discharge pipe is inserted, the height of the pipe orifice of the waste discharge pipe is lower than that of the pipe orifice of the gas inlet pipe 15, and.
As shown in fig. 1, in the sample injection system for atomic spectroscopy or mass spectrometry according to the present embodiment, the drying device includes a transparent container 21, a drying agent 22, and an air outlet pipe 23.
Preferably, the transparent container 21 is filled with the drying agent 22, the top of the transparent container 21 is provided with two holes, the two holes are respectively inserted into the air outlet pipe 23 of the drying device and the air outlet pipe 16 of the gas-liquid separator, the air outlet pipe 23 of the drying device is connected with the excitation unit of the atomic spectrometer or the mass spectrometer, the height of the opening of the air outlet pipe 23 of the drying device is higher than that of the opening of the air outlet pipe 16 of the gas-liquid separator, and the upper surface of the drying agent 22 is lower. The transparent container 21 is transparent, so that the use condition of the drying agent can be observed in real time and replaced in time.
Wherein, the drying agent is a solid substance which has no adsorption effect on the element vapor to be detected.
In addition, the carrier gas outlet 10 of the liquid cathode glow discharge vapor generation device of the embodiment is connected with a gas-liquid separator through an air inlet pipe 15, the gas-liquid separator is connected with a drying device through an air outlet pipe 16, the drying device is connected with an excitation unit of an atomic spectrometer and a mass spectrometer through an air outlet pipe 23, and the air inlet pipe 15 and the air outlet pipe 16 of the gas-liquid separator and the air outlet pipe 23 of the drying device can be respectively silica gel hoses with the lengths of 15-20 mm, 10-15 mm and 20-40 mm.
By means of the method, vapor generated by liquid cathode glow discharge can rapidly enter an atomic spectrometer or a mass spectrometer for further excitation and analysis, and condensation loss in a pipeline is reduced. The gas-liquid separator and the drying device improve the concentration of the element steam to be detected and reduce the interference of moisture on the excitation unit of the atomic spectrometer or the mass spectrometer.
Preferably, the sample injection system for atomic spectroscopy or mass spectrometry in the present embodiment uses the carrier gas of the atomic spectrometer or mass spectrometer itself as the discharge medium of the liquid cathode glow discharge and the sample transport carrier gas. The carrier gas pipe of the atomic spectrometer or mass spectrometer is connected with the carrier gas inlet 1 of the quartz cover 2.
By means of the method, the flow rate of the carrier gas can be directly controlled by computer software of the atomic spectrometer or the mass spectrometer, an additional gas flowmeter is not needed, occupied space is reduced, and the operation is simpler.
In addition, the ignition of the experimental device requires a certain concentration of acid as the electrolyte solution. The sample solution is acid with a certain concentration as a medium. The sample solution 19 is introduced into the cathode glass capillary 8 through a sample inlet pipe by a peristaltic pump 17, and the waste liquid 18 in the quartz cover 2 is led out through a waste discharge pipe 9 by the same peristaltic pump 17.
Wherein the dielectric acid can be one of inorganic acids such as nitric acid, hydrochloric acid, sulfuric acid and the like with the pH value of 0.8-1.2. During the experiment, the rotating speed of the peristaltic pump 17 can be adjusted to enable the flow rate of the sample to be 2000-4000 mu L/min, and the sample solution can continuously overflow from the top end of the cathode glass capillary tube 8 of the liquid cathode glow discharge steam generating device.
The top end of the cathode glass capillary tube 8 is kept 3 mm away from the bottom end of the anode tungsten rod 5, and the sample solution overflowing from the top end of the cathode glass capillary tube 8 is contacted with the graphite electrode 7, thereby forming a glow discharge loop. After applying high voltage to the two electrodes, glow discharge microplasma is generated between the two electrodes.
Taking an inductively coupled plasma atomic emission spectrometer as an example, an operation flow example of the present invention is as follows:
1) the atomizer of the inductively coupled plasma atomic emission spectrometer is disassembled, and the sample injection system is installed, so that the sealing of each interface is ensured to be airtight. And stably igniting the ICP-OES for more than 20 min.
2) The gas path control column of the ICP-OES computer software was used to set the atomization gas flow rate at 0 mL/min.
3) The flow rate of the peristaltic pump 17 is adjusted to enable the sample solution 19 to continuously overflow from the top end of the cathode glass capillary 8; and (3) taking the sample solution 19 as a cathode and a metal tungsten rod as an anode, applying high voltage to the two electrodes to generate stable liquid cathode glow discharge micro-plasma, and carrying out atomization on elements to be detected in the solution in a glow discharge area to form atomic vapor.
4) In the stage of applying high pressure in the step 3), the air bag of the sample injection pipeline is slightly pressed, so that the liquid level of the sample solution 19 reaches the highest level and is in contact with the anode tungsten rod 5, thereby realizing a loop and generating glow discharge. The air bag is slowly loosened, and the discharge stably exists.
5) The sample flow rate was set at 2000-.
6) The flow rate of the atomizing gas is adjusted to a certain specific value within 150 mL/min-700 mL/min by utilizing the gas circuit control of ICP-OES computer software. The specific regulation mode is to slowly increase the flow rate of the atomizing gas to a set value so as to ensure the stable ignition of the liquid cathode glow discharge steam generating device.
7) And editing the method by using operating software of ICP-OES, wherein the atomizing airflow rate in the method is the same as the flow rate set by the gas circuit control, selecting the first three spectral lines of the element to be detected, storing, clicking the analysis and the operation to obtain the corresponding spectrogram and the signal intensity of the element to be detected in the sample.
8) And taking the corresponding dielectric acid as a blank solution, and obtaining the difference between the signal intensity and the signal intensity of the sample, namely the net signal intensity of the element to be detected in the sample.
As the present invention may be embodied in several forms without departing from the spirit of essential characteristics thereof, the present embodiments are therefore illustrative and not restrictive, since the scope of the invention is defined by the appended claims rather than by the description herein, and all changes that fall within metes and bounds of the claims, or equivalence of such metes and bounds thereof are therefore intended to be embraced by the appended claims.
Claims (7)
1. A sample introduction system for atomic spectroscopy or mass spectrometry, comprising:
a liquid cathode glow discharge vapor generating device;
the gas-liquid separator is connected with the liquid cathode glow discharge steam generating device;
the drying device is connected with the gas-liquid separator;
and the power supply system is used for providing electric energy for the liquid cathode glow discharge vapor generating device.
2. The sample introduction system for atomic spectroscopy or mass spectrometry according to claim 1, wherein the liquid cathode glow discharge vapor generation device is a device for atomizing an element to be measured in a solution into atomic or molecular vapor by using microplasma generated by liquid cathode glow discharge, and comprises: the device comprises a quartz cover, an upper opening plug, a lower opening plug, a glass capillary tube, a peristaltic pump, a waste discharge tube, a cathode graphite rod and an anode tungsten rod, wherein the glass capillary tube is vertically inserted into the cathode graphite rod and keeps the glass capillary tube coaxial with the anode tungsten rod, and the peristaltic pump transports electrolyte solution to the glass capillary tube and transports waste liquid in the waste discharge tube.
3. The sample introduction system for atomic spectroscopy or mass spectrometry according to claim 1, wherein the vapor generated by the liquid cathode glow discharge vapor generation device passes through the gas-liquid separator to remove most of condensed water, then passes through the drying device to increase the vapor concentration of the element to be detected, and is transported to the excitation and detection unit of the atomic spectrometer or mass spectrometer by the carrier gas.
4. The sample introduction system for atomic spectroscopy or mass spectrometry as claimed in claim 1, wherein a carrier gas pipe of an atomic spectrometer or mass spectrometer is connected with the liquid cathode glow discharge vapor generation device, and a carrier gas of the atomic spectrometer or mass spectrometer is used as a carrier gas of vapor generated by the liquid cathode glow discharge vapor generation device.
5. The sampling system for atomic spectrum or mass spectrum of claim 1, wherein the gas-liquid separator comprises a container, a waste discharge pipe, an air inlet pipe and an air outlet pipe, the air inlet pipe is connected with the liquid cathode glow discharge vapor generation device, the air outlet pipe is connected with a drying device, and the peristaltic pump transports the condensate in the waste discharge pipe.
6. The sample introduction system for atomic spectroscopy or mass spectrometry according to claim 1, wherein the drying device comprises a transparent container, a drying agent and an air outlet pipe, the air outlet pipe is connected with an excitation unit of an atomic spectrometer or a mass spectrometer, and the drying agent is filled in the transparent container.
7. The sample introduction system for atomic spectroscopy or mass spectrometry of claim 1, wherein the power supply system is a dc power supply that provides electrical power to the liquid cathode glow discharge vapor generation device.
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