CN104655609A - Excitation apparatus and emission spectrometer - Google Patents
Excitation apparatus and emission spectrometer Download PDFInfo
- Publication number
- CN104655609A CN104655609A CN201310589733.9A CN201310589733A CN104655609A CN 104655609 A CN104655609 A CN 104655609A CN 201310589733 A CN201310589733 A CN 201310589733A CN 104655609 A CN104655609 A CN 104655609A
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- liquid
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- capillary channel
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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
-
- 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
- G01N21/69—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 specially adapted for fluids, e.g. molten metal
Abstract
The invention provides an excitation apparatus and an emission spectrometer. The excitation apparatus includes a sample trough used for accommodating a to-be-test liquid, a transparent insulating separating plate and an excitation source. The transparent insulating separating plate is disposed in the sample trough and separates the to-be-test liquid into a first liquid part and a second liquid part. A plurality of capillary passageways are formed in the transparent insulating separating plate and are used for mutually communicating the first liquid part and the second liquid part therethrough. The excitation source includes a high-voltage power supply, and two high-voltage electrodes connected thereto. The two high-voltage electrodes are respectively arranged in the first liquid part and the second liquid part. The high-voltage power supply, when being switched on, can excite the first liquid part and the second liquid part to form a first liquid electrode and a second liquid electrode and generate an emission spectrum. The excitation apparatus is based on the principle of liquid electrodes, is small in size and is high in detection precision.
Description
Technical field
The present invention relates to field of analytic instrument, particularly a kind of excitation apparatus for tenor in tracer liquid and emission spectrometer.
Background technology
Along with developing rapidly of China's economy, the living standard of people there has also been swift and violent raising.Meanwhile, because the exploitation of mankind's heavy metal, smelting, processing and business manufacturing activities are increasing, cause many heavy metals to enter in air, water, soil as lead, mercury, cadmium, chromium etc., cause serious environmental pollution; Especially in water quality with the heavy metal that various chemical state or chemical form exist, will retain, accumulate and move after entered environment or the ecosystem, cause serious harm.
Domestic and international laboratory is very abundant to the detection method of metallic element, such as: ultraviolet can the method such as spectrophotometric method (UV), atomic absorption method (AAS), atomic fluorescence method (AFS), inductively coupled plasma method (ICP), X fluorescence spectrum method (XRF), Inductively coupled plasma-mass spectrometry (ICP-MS), instrument based on these principle designs also emerges in an endless stream, the low and middle-grade A wide selection of colours and designs of various instrument height, apparatus manufacture is employed new technology and is released new instrument repeatedly, greatly meets the testing requirement in laboratory.But along with the development in epoch, testing requirement also extend to scene from laboratory, require also not only to be only " accurately ", extend again " fast ".These new demands require also very high to Instrument Design, and instrument will walk out laboratory, and small-sized or portable, the design based on these classic methods manifests drawback gradually, supports that portable new method becomes the focus of current Instrument Design gradually.
Some producer domestic makes portability instrument in trial, but still is the instrument based on atomic absorption method principle, portable not equal to miniaturization, and the not ideal chose of in-site measurement.The design of external Ye You producer produces portable plasma excitation apparatus and emission spectrometer, battery-powered, can be used for in-site measurement; Measure multiple element, detection limit 0.1ppm ~ 100ppm simultaneously, and simple to operate; But its key issue is that its Detection capability is poor, cannot meets and detect requirement (ppb level) to metal in the water quality such as potable water, industrial waste water, electroplating wastewater in GB, and expensive, therefore its application is restricted.
Electrochemical process is development in recent years a kind of method faster, and it is rely on classical direct current polarography, derives again the method such as oscillographic polarography, anodic stripping voltammetry on this basis.The detectability of electrochemical process is lower, and measurement sensitivity is higher, and metallic element at the scene is just progressively applied in measuring.But the shortcoming of electrochemical process can not be ignored more, Electrode selectivity is not high, easily subsidiary reaction occurs, and reduces current efficiency; Electrode easily forms adsorbed layer and oxide film, and stained electrode makes voltage raise; Electrode in use needs often polishing and affects accuracy and the reliability of test result.
Summary of the invention
One object of the present invention is to overcome current laboratory and on-the-spot tenor pick-up unit volume is large, accuracy of detection is low deficiency, provides the emission spectrometer that a kind of volume is little, accuracy of detection is high;
Another object of the present invention is to provide a kind of excitation apparatus for emission spectrometer of the present invention.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
According to an aspect of the present invention, the invention provides a kind of excitation apparatus, comprise for the sample cell of splendid attire liquid to be detected, transparent insulation dividing plate and excitaton source.Transparent insulation dividing plate is located in described sample cell, and described liquid to be detected is isolated into Part I liquid and Part II liquid, this lamina of septum pellucidum is provided with through capillary channel, and described Part I liquid and Part II liquid are interconnected by this capillary channel; Two high-field electrodes that excitaton source comprises high-voltage power supply and is connected with this high-voltage power supply, described two high-field electrodes are arranged in described Part I liquid and Part II liquid respectively, and described high-voltage power supply can excite described Part I liquid and Part II liquid formation first liquid electrode and second liquid electrode and produce emission spectrum after starting.
According to an embodiment of the invention, described two high-field electrodes are arranged at two open-ended places of described capillary channel respectively.
According to an embodiment of the invention, described high-voltage power supply is direct supply, AC power or the pulse power, and voltage range is 200 ~ 2000 volts.
According to an embodiment of the invention, the diameter of described capillary channel is 0.05mm ~ 0.50mm.
According to an embodiment of the invention, described lamina of septum pellucidum is vertical at described sample cell diapire.
According to an embodiment of the invention, described transparent insulation dividing plate and described sample cell are formed in one structure or separable assembled structure.
According to an embodiment of the invention, described excitation apparatus also comprises direct current enrichment electrode, and this direct current enrichment electrode comprises the negative electrode being arranged on contiguous described capillary channel position and at least one anode be located at away from described cathode site.
According to an embodiment of the invention, described anode is located in described sample cell or to be located at described sample cell outer and press close to the perisporium of described sample cell.
According to an embodiment of the invention, described negative electrode is located in described capillary channel.
According to an embodiment of the invention, the number of described anode is one, and it is located at described liquid upper surface to be detected, and described capillary channel is located at the bottom of described lamina of septum pellucidum.
According to an embodiment of the invention, described negative electrode is located at outside described sample cell, and presses close to the diapire of described sample cell.
According to an embodiment of the invention, the number of described anode is two, is relatively located in described liquid to be detected, and presses close to the perisporium of described sample cell respectively.
According to a further aspect in the invention, the invention provides a kind of emission spectrometer, comprise for generation of the excitation apparatus of metallic ion emission spectrum, for receiving described emission spectrum and this emission spectrum being decomposed into monochromatic monochromator and being used for receiving and processing required monochromatic Signal reception treating apparatus.Wherein said excitation apparatus is excitation apparatus of the present invention.
As shown from the above technical solution, advantage of the present invention and good effect are:
In the present invention, the liquid to be detected in sample cell is isolated into two parts by transparent insulation dividing plate, and this two parts liquid is communicated with by a capillary channel, and sample cell and capillary channel are full of the solution to be detected of conduction.The electrode of excitaton source is inserted respectively in two parts liquid to be detected, high-voltage power supply is applied between two electrodes, under the effect of high-voltage power supply, bubble is produced in capillary channel, solution in capillary channel disconnects and forms gap by bubble, and two parts liquid to be detected forms two liquid electrodes, and these two liquid electrodes produce plasma at gap location, impurity element sputtering in liquid to be detected enters plasma, inspires emission spectrum.Therefore the present invention utilizes liquid electrode principle to detect, and accuracy of detection is high.
And the excitation apparatus in the present invention only comprises sample cell, transparent insulation dividing plate and excitaton source, structure is simple, and volume is little, and undesirable gas is protected, and is convenient for carrying, is convenient to on-site rapid measurement; And low in energy consumption, energy-conserving and environment-protective.
Further, in excitation apparatus of the present invention, be also provided with the direct current enrichment electrode by negative electrode and anodic formation, and the contiguous capillary channel of negative electrode, anode is away from capillary channel.Therefore, in the present invention, before excitation-emission spectrum, the heavy metal ion can first treated in tracer liquid carries out enrichment, according to actual needs, several times can be reached to hundreds of times to the accumulation ability of metallic ion, even higher, significantly improve the concentration of metallic ion in capillary channel, thus increased substantially the Detection capability of metallic ion, and further increased accuracy of detection of the present invention.
By referring to accompanying drawing description of a preferred embodiment, above-mentioned and other objects, features and advantages of the present invention will be more obvious.
Accompanying drawing explanation
Fig. 1 is the structural representation of excitation apparatus first embodiment of the present invention;
Fig. 2 is the principle schematic forming liquid electrode in excitation apparatus first embodiment of the present invention;
Fig. 3 is the structural representation of excitation apparatus second embodiment of the present invention;
Fig. 4 is the structural representation of excitation apparatus of the present invention 3rd embodiment;
Fig. 5 is the schematic diagram of emission spectrometer of the present invention.
Embodiment
Specific embodiments of the invention are described in detail below in conjunction with accompanying drawing.It should be noted that the embodiments described herein is only for illustrating, is not limited to the present invention.
Excitation apparatus embodiment 1
As shown in Figure 1, excitation apparatus first embodiment of the present invention, comprises sample cell 1, transparent insulation dividing plate 2 and excitaton source.
Sample cell 1 is for splendid attire liquid to be detected.This sample cell 1 can be made up of insulating material such as quartz glass etc.The shape of sample cell 1 is not limit, and can be hollow cuboid, the hollow square bodily form, cylindrical shape, etc.Sample cell 1 has diapire 11 and perisporium 12.
Transparent insulation dividing plate 2 is located in sample cell 1, and transparent insulation dividing plate 2 is made up of material that is transparent and insulation, and when the material of sample cell 1 is identical with the material of transparent insulation dividing plate 2 as being quartz glass, then transparent insulation dividing plate 2 and sample cell 1 can be one-body molded.Certain transparent insulation dividing plate 2 also can be an independently structure, is sealingly fastened in sample cell 1 by modes such as bondings.Liquid to be detected in sample cell 1 is isolated into mutually isolated Part I liquid and Part II liquid by transparent insulation dividing plate 2.Transparent insulation dividing plate 2 can be vertical at sample cell 1 centre position, so that the liquid in sample cell 1 is divided into the identical two parts of volume, certainly not as limit.
This lamina of septum pellucidum 2 is provided with the through capillary channel 20 that diameter is 0.10mm, and the diameter of capillary channel 20 is not limited with 0.10mm, and the diameter of usual capillary channel 20 is all feasible within the scope of 0.05mm ~ 0.50mm.Can also change accordingly according to condition in addition, capillary channel 20 is maximum reaches 2.00mm.Part I liquid and Part II liquid are interconnected by this capillary channel 20.
Two high-field electrodes 31 that excitaton source comprises high-voltage power supply 80 and is connected with this high-voltage power supply 80.In this embodiment, high-voltage power supply 80 to be voltage the be AC power of 1200 volts, certainly not as limit, high-voltage power supply also can be direct supply or the pulse power, and voltage range is all feasible within the scope of 200 ~ 2000 volts.Two high-field electrodes 31 are arranged in Part I liquid and Part II liquid respectively, and preferably, two high-field electrodes 31 are arranged at two open-ended places of capillary channel 20 respectively.
In excitation apparatus first embodiment of the present invention, high-voltage power supply 80 can excite Part I liquid and Part II liquid formation first liquid electrode and second liquid electrode and produce emission spectrum after starting.Be described as follows:
As shown in Figure 2, Part I liquid and Part II liquid are interconnected by capillary channel 20, when between Part I liquid and Part II liquid during high-pressure, and Part I liquid and Part II heated liquid and produce bubble.Because the diameter of capillary channel 20 is less, the liquid of capillary channel 20 disconnects by the bubble 100 therefore in capillary channel 20, and then is disconnected the path of Part I liquid and Part II fluid connection.At this moment Part I liquid and Part II liquid just define liquid electrode, and two liquid electrodes produce plasma discharge at bubble 100 place under high-tension electricity effect, thus produce the emission spectrum of metal cation.
Excitation apparatus embodiment 2
As shown in Figure 3, the difference of excitation apparatus second embodiment of the present invention and the first embodiment is only: excitation apparatus also comprises direct current enrichment electrode, therefore has the enrichment function treating metal cation in tracer liquid.
In this excitation apparatus second embodiment, direct current enrichment electrode comprises negative electrode 30 and an anode 40.
It is outer and press close to the diapire 11 of sample cell 1 that negative electrode 30 is located at sample cell 1, and corresponding with lamina of septum pellucidum 2.Now capillary channel 20 can be opened in the position of bottom close to negative electrode 30 of lamina of septum pellucidum 2.
Anode 40 is located in sample cell 1, and is positioned at liquid upper surface to be detected.
When applying DC voltage between negative electrode 30 and anode 40, then the kation in liquid is assembled in negative electrode 30 side, and negative ion is assembled in anode 40 side simultaneously, and such kation can be assembled in capillary channel 20, forms higher ion concentration, realizes the object of enrichment.According to the feature of solution, suitable enrichment times can be selected.Enrichment times is relevant with DC voltage and enrichment time, can from several times to hundreds of times, even higher.Such as, for being the solution of 1ppb containing Cd concentration of element, DC voltage 24 volts, 10 seconds conduction time can reach 5 times of enrichments.Generally, conduction time is longer, and voltage is larger, and accessible enrichment times is higher.
Other structure of this excitation apparatus second embodiment is identical with the first embodiment, repeats no more here.
Excitation apparatus embodiment 3
As shown in Figure 4, the difference of excitation apparatus of the present invention 3rd embodiment and the second embodiment is only:
The number of anode 40 is two, is relatively located in the liquid to be detected of sample cell 1, and presses close to the perisporium 12 of sample cell 1; It is outer and press close to the perisporium 12 of sample cell 1 that two anodes 40 also can be located at sample cell 1.Capillary channel 20 is located in the middle part of lamina of septum pellucidum 2, and corresponds to two anodes 40.Negative electrode 30 is located in capillary channel 20.
In actual use, can also there be various ways the position of negative electrode 30 and anode 40.For strengthening concentration effect, the two as far as possible mutual away from.Ensure that negative electrode 30 is in position, adjacent capillaries road 20, to increase the concentration of metal cation in capillary channel 20 simultaneously.
Other structure of this excitation apparatus the 3rd embodiment is identical with the second embodiment, repeats no more here.
Emission spectrometer
As shown in Figure 5, emission spectrometer of the present invention, excitation apparatus 50, monochromator 60 and Signal reception treating apparatus 70.
Excitation apparatus 50 is excitation apparatus of the present invention, and it can produce metal cation emission spectrum.
Monochromator 60 can receive emission spectrum and this emission spectrum is decomposed into monochromatic light, thus is separated from composite light source by the characteristic spectral line of tested element.The type of monochromator can be plane grating monochromator, concave grating monochromator, also can be echelle grating monochromator.
Signal reception treating apparatus 70 comprises detecting device and Circuits System, and detector type can be photomultiplier, also can be solid state detector.Signal reception treating apparatus 70 can receive the monochromatic light after decomposing, and carries out analyzing and processing with this.
Emission spectrometer application biliquid electrode activated plasma emission spectrum principle of the present invention, the interelectrode high pressure of start liquid, there is plasma discharge in capillary channel inside in liquid electrode, thus produces the emission spectrum of metal cation; Emission spectrum enters into monochromator 60 through after lamina of septum pellucidum 2, then is processed by Signal reception treating apparatus 70, finally draws type and the content of metallic element in liquid to be detected.
Although exemplary embodiment describe the present invention with reference to several, should be appreciated that term used illustrates and exemplary and nonrestrictive term.Spirit or the essence of invention is not departed from because the present invention can specifically implement in a variety of forms, so be to be understood that, above-described embodiment is not limited to any aforesaid details, and explain widely in the spirit and scope that should limit in claim of enclosing, therefore fall into whole change in claim or its equivalent scope and remodeling and all should be claim of enclosing and contained.
Claims (13)
1. an excitation apparatus, is characterized in that, comprising:
Sample cell (1), for splendid attire liquid to be detected;
Transparent insulation dividing plate (2), be located in described sample cell (1), and described liquid to be detected is isolated into Part I liquid and Part II liquid, this lamina of septum pellucidum (2) is provided with through capillary channel (20), and described Part I liquid and Part II liquid are interconnected by this capillary channel (20); And
Excitaton source, two high-field electrodes comprising high-voltage power supply and be connected with this high-voltage power supply, described two high-field electrodes are arranged in described Part I liquid and Part II liquid respectively, and described high-voltage power supply can excite described Part I liquid and Part II liquid formation first liquid electrode and second liquid electrode and produce metal cation emission spectrum after starting.
2. excitation apparatus as claimed in claim 1, it is characterized in that, described two high-field electrodes are arranged at two open-ended places of described capillary channel (20) respectively.
3. excitation apparatus as claimed in claim 1, it is characterized in that, described high-voltage power supply is direct supply, AC power or the pulse power, and voltage range is 200 ~ 2000 volts.
4. excitation apparatus as claimed in claim 1, it is characterized in that, the diameter of described capillary channel (20) is 0.05mm ~ 0.50mm.
5. excitation apparatus as claimed in claim 1, it is characterized in that, described lamina of septum pellucidum (2) is vertical at described sample cell (1) diapire.
6. excitation apparatus as claimed in claim 1, is characterized in that, described transparent insulation dividing plate (2) and described sample cell (1) are formed in one structure or separable assembled structure.
7. the excitation apparatus according to any one of claim 1-6, is characterized in that, described excitation apparatus also comprises direct current enrichment electrode, and this direct current enrichment electrode comprises:
Negative electrode (30), is arranged on contiguous described capillary channel (20) position; And
At least one anode (40), is located at the position away from described negative electrode (30).
8. excitation apparatus as claimed in claim 7, is characterized in that, described anode (40) is located in described sample cell (1) or is located at described sample cell (1) and press close to the perisporium of described sample cell outward.
9. excitation apparatus as claimed in claim 7, it is characterized in that, described negative electrode (30) is located in described capillary channel (20).
10. excitation apparatus as claimed in claim 7, it is characterized in that, the number of described anode (40) is one, and it is located at described liquid upper surface to be detected, and described capillary channel (20) is located at the bottom of described lamina of septum pellucidum (2).
11. excitation apparatus as claimed in claim 9, it is characterized in that, described negative electrode (30) is located at described sample cell (1) outward, and presses close to the diapire of described sample cell (1).
12. excitation apparatus as claimed in claim 7, is characterized in that, the number of described anode (40) is two, is relatively located in described liquid to be detected, and presses close to the perisporium of described sample cell (1) respectively.
13. 1 kinds of emission spectrometers, comprise for generation of the excitation apparatus (50) of metallic ion emission spectrum, for receiving described emission spectrum and this emission spectrum being decomposed into monochromatic monochromator (60) and for receiving and processing required monochromatic Signal reception treating apparatus (70), it is characterized in that, described excitation apparatus (50) is the excitation apparatus according to any one of claim 1-12.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310589733.9A CN104655609A (en) | 2013-11-20 | 2013-11-20 | Excitation apparatus and emission spectrometer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310589733.9A CN104655609A (en) | 2013-11-20 | 2013-11-20 | Excitation apparatus and emission spectrometer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105115959A (en) * | 2015-07-09 | 2015-12-02 | 西北师范大学 | Metal element liquid phase cathode discharge plasma spectrum rapid detection system and detection method thereof |
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| CN105115959B (en) * | 2015-07-09 | 2017-11-07 | 西北师范大学 | The liquid phase cathodic discharge plasma spectrometry rapid detection system and detection method of metallic element |
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Application publication date: 20150527 |