CN1054486A - Oil radiation spectrum analyzer with microwave plasma - Google Patents
Oil radiation spectrum analyzer with microwave plasma Download PDFInfo
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- CN1054486A CN1054486A CN 90107023 CN90107023A CN1054486A CN 1054486 A CN1054486 A CN 1054486A CN 90107023 CN90107023 CN 90107023 CN 90107023 A CN90107023 A CN 90107023A CN 1054486 A CN1054486 A CN 1054486A
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- microwave plasma
- emission spectroscopy
- atomic emission
- plasma atomic
- resonator cavity
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Abstract
The invention belongs to field of measuring technique, is that a kind of microwave plasma atomic emission spectroscopy method of utilizing is measured TRACE ELEMENTS ANALYSIS instrument in the oil plant.Mainly by microwave generator, resonator cavity, monochromator, condenser, photomultiplier, registering instrument or MICROCOMPUTER PROCESSING partly wait composition.Adopt the ultrasonic atomizatio sample introduction, go by heating-water condensation-concentrated sulphuric acid molten, with microwave generator and the resonator cavity daughter torches such as generation that are coupled.The daughter emission spectrum that waits according to oil plant is measured the content of element.The present invention has that the detection elements scope is wide, and the range of linearity is wide, precision height, characteristics such as detection limit is low, and is easy to operate.
Description
The invention belongs to field of measuring technique, is a kind of analytical instrument of utilizing the plasma emission spectroscopy measurement constituent content wherein of oil plant.
Existing emission spectrometric analyzer, employing electric arc that has and spark are applicable to conductor and pressed powder sample analysis as excitation source, and the preparation of standard specimen is very time-consuming, and excite limited in one's abilityly, and stability of light source is poor.Inductively coupled plasma emission spectrography is measured content of elements in the oil plant, be to use high-frequency electrical energy, plasma torch by the resulting similar flame in appearance of inductive coupling is an excitation source, its analytic sample has higher sensitivity and precision, but cost of equipment and operation cost are higher.
The microwave plasma atomic emission spectroscopy method can use helium and argon gas as working gas, has the very strong ability that excites, can measure the nearly all element that comprises halogen, but since its sample bear can be low, also be provided with the proximate analysis instrument that utilizes the microwave plasma atomic emission spectroscopy method at present.
The purpose of this invention is to provide a kind of microwave plasma atomic emission spectroscopy that utilizes, measure the analytical instrument of micronutrient levels in the oil plant, it is simple in structure, and is easy to operate, the accuracy of detection height, and sensing range is wide.
The present invention mainly adopts the ultrasonic atomizatio sample introduction, goes molten method by heating-water condensation-concentrated sulphuric acid, improves the ability to bear of gas ions torch to sample.Produce stable plasma torch with microwave generator and resonator cavity coupling.With monochromator or spectrograph beam split,, data are gathered and handled with registering instrument or microcomputer through behind the photomultiplier.
Fig. 1 is a synoptic diagram of the present invention.1,2 are carrier gas valve, 3 spray chambers, 4 well heaters, 5 ultrasonic atomizers, 6 condensers, 7 concentrated sulphuric acid absorption cells, 8 resonator cavitys, 9 condensers, 10 monochromators, 11 photomultipliers among the figure.
Fig. 2 is light path system figure of the present invention.12 is entrance slit among the figure, 13 spherical mirrors, 14 plane gratings, 15 beam-splitters, 16 catoptrons, 17 exit slits.
Fig. 3 is a circuit block diagram of the present invention.
Fig. 4 is an operation room of the present invention.
The present invention is mainly by the microwave plasma atomic emission spectroscopy part, resonator cavity 8, monochromator 10, condenser 9, photomultiplier 11, compositions such as registering instrument or microsystem.Microwave plasma atomic emission spectroscopy partly has, carrier gas valve 1,2, spray chamber 3, well heater 4, ultrasonic atomizer 5, condenser 6, concentrated sulphuric acid absorption cell 7 etc.Monochromator 10 is by entrance slit 12, spherical mirror 13, plane grating 14, beam-splitter 15, catoptron 16, exit slit 17 compositions such as grade.
The course of work of the present invention is as follows.
As shown in Figure 1, before the working sample, bearing carrier gas valve 1 is opened carrier gas valve 2, makes carrier gas (argon gas) directly enter the discharge tube that is arranged in resonator cavity 8.Under the effect of microwave energy, light and in discharge tube, to form and to keep a stable plasma flare through high-frequency igniter.During working sample, sample solution is added in the spray chamber, through the ultrasonic atomizatio effect, sample segment solution forms gasoloid, introduces in the plasma through carrier gas (argon gas), and is evaporated there, atomization, excites and ionization.In order to keep plasma flare, should remove the moisture content that contains in the gasoloid as far as possible neatly not by cancellation.Therefore, adopted the dissolving system that has concentrated sulphuric acid absorption cell 7.Go molten process to be: the aqueous aerosol that contains moisture content is heated through well heater 4, make that moisture content becomes water vapour in the sample, then, 6 condensations are stayed in the condenser 6 aerocolloidal most of water vapor condensing water droplet through condenser, and remaining moisture content further absorbs through concentrated sulphuric acid absorption cell 7 again to be removed.So just can under the condition of low power microwave energy, make plasma not by cancellation.The dry gas colloidal sol of sample then is evaporated in plasma, atomization is launched various characteristic radiations with exciting, contained elementary composition difference in the sample, the wavelength components of emission is also different, and the wavelength of the elemental characteristic radiation of surveying is known, therefore, by adjusting the intensity that monochromator 10 just can record the characteristic radiation that each element sends.This intensity be with sample in each element concentration dependent, radiation intensity is big more, the concentration of contained this element is big more in the sample.This light intensity is transformed into the correspondent voltage signal through photomultiplier 11, is noted by registering instrument or microsystem, just can measure the concentration of contained this element in the sample.
The performance of the ultrasonic atomizer 5 in the microwave plasma atomic emission spectroscopy part, directly influence forms the aerocolloidal concentration of sample in spray chamber, and then influences the sample size that enters plasma, and nature can influence the size that transmits.The power of ultrasonic atomizer is big more, and aerosol concentration is just big more, and it is also just big more to transmit.The present invention has selected for use high-power switch tube as the vibration of ultrasonic atomizer 5 and power tube and preferred circuit and component parameters; Adopt axial flow blower to the power tube enhance heat; Select large-sized transducing sheet for use.
The present invention has a usefulness blind nut 19 fixed end caps 18 at an end of resonator cavity 8 in housing 20.And discharge tube 29 passes from the end cap center.Because the existence of end cap 18 has reduced the microwave radiation in the chamber.Coupling piece 24 is fixed with the gap of tuning pipe 28, makes the performance of resonator cavity more stable like this.Quartz discharge tube 29 leads directly in cavity, is fit to emission spectrographic analysis.Insulator 6 uses polytetrafluoroethylmaterial material, and the reflective power of resonator cavity 8 is reduced, and easily lights.Secondly cavity is made with aluminium alloy, makes its weight saving, making and easy to operate, cheap.
Structure of the present invention as shown in Figure 4.General structure is the post plank frame.Open the upper right side wicket, the inside is an operation room.Resonator cavity 8 can upper and lower within the specific limits, forward and backward adjustment in operation room, and 9 in condenser moves before and after can be on slideway, guarantees that light beam focuses on the entrance slit.
Light path system of the present invention as shown in Figure 2.Incide the natural light or the polychromatic light of grating monochromator, through projecting behind the entrance slit 12 on the spherical mirror 13, entrance slit 12 is on the focal plane of spherical mirror 13, and therefore, the light beam after spherical mirror 13 reflections is a parallel beam.Parallel beam is divided into the parallel beam of different wave length after plane grating 14 beam split, invest another spherical mirror 13 with different angle of diffraction, and spherical mirror 13 plays photographic lens, so parallel beam will be in catoptron 16 reflection back imaging on its focal plane.Thereby obtain resemble (spectrum line) of a series of entrance slit.Exit slit 17 is on the focal plane of another spherical mirror 13.According to exit slit 17 opens wide sizes, allow the very narrow a part of light beam in wavelength interval to penetrate.When grating rotates in the direction of the clock, can obtain the monochromatic beam (spectrum line) of the very high different wave length of spectral purity at exit slit 17 places.
Circuits System of the present invention as shown in Figure 3.The signal of photomultiplier 11 outputs, amplification strengthens its voltage signal through amplifier, outputs to A/D and is converted to digital quantity, is handled by the single card microcomputer follow procedure again, prints the result.
The invention solves a plasma torch difficult problem low to the sample ability to bear. And have that the detection elements scope is wide, accuracy of detection is higher, detection limit is lower, detects linear wide ranges, and volume is little, and is easy to operate, make and operating cost low, to advantages such as environment for use are less demanding.
The present invention adopts microcomputer to carry out data acquisition and processing (DAP), and test result can numeral show and printout.
The present invention has versatility widely, is applicable to that aviation, railway, boats and ships, power station, precision optical machinery, commodity inspection, environmental protection, geology, metallurgy, medical department carry out quantitative test to trace element.
Claims (5)
1, a kind of microwave plasma atomic emission spectroscopy analyser is characterized in that by the microwave plasma atomic emission spectroscopy part resonator cavity 8, condenser 9, monochromator 10, photomultiplier 11, compositions such as registering instrument or microprocessor system, described microwave plasma atomic emission spectroscopy partly has carrier gas valve 1 and 2, spray chamber 3, well heater 4, ultrasonic atomizer 5, condenser 6, concentrated sulphuric acid absorption cell 8 etc.
2, microwave plasma atomic emission spectroscopy analyser according to claim 1, an end that it is characterized in that the housing in the resonator cavity 8, have an end cap 18 usefulness blind nuts to fix, coupling piece 24 is fixed with the gap of resonatron 28, and quartz discharge tube 29 leads directly in cavity.
3, microwave plasma atomic emission spectroscopy analyser according to claim 1 is characterized in that the plasma emissioning light of sample converts electric signal to by photomultiplier 11, converts digital quantity to A/D after amplifying, and carries out MICROCOMPUTER PROCESSING.
4, microwave plasma atomic emission spectroscopy instrument according to claim 1 is characterized in that resonator cavity 8 in operation room, can upper and lower, forward and backward adjustment.
5, microwave plasma atomic emission spectroscopy analyser according to claim 1, it is characterized in that condenser 9 can the slideway in operation room on before and after move.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107023 CN1018864B (en) | 1990-08-17 | 1990-08-17 | Oil radiation spectrum analyzer with microwave plasma |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107023 CN1018864B (en) | 1990-08-17 | 1990-08-17 | Oil radiation spectrum analyzer with microwave plasma |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1054486A true CN1054486A (en) | 1991-09-11 |
| CN1018864B CN1018864B (en) | 1992-10-28 |
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ID=4880372
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90107023 Expired CN1018864B (en) | 1990-08-17 | 1990-08-17 | Oil radiation spectrum analyzer with microwave plasma |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1018864B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648640B (en) * | 2004-01-15 | 2010-05-05 | 松下电器产业株式会社 | Ingredient analysis method and ingredient analysis apparatus |
| CN103945631A (en) * | 2014-04-06 | 2014-07-23 | 浙江大学 | Improved microwave plasma torch device and application |
| CN105938097A (en) * | 2016-04-15 | 2016-09-14 | 成都以太航空保障工程技术有限责任公司 | Multi-element oil liquid analysis system based on CCD polychromator |
| CN109297951A (en) * | 2018-08-29 | 2019-02-01 | 上海化工研究院有限公司 | The high effect forced nebulization sampling system of Pneumatic constant pressure type for special spectrum analysis |
-
1990
- 1990-08-17 CN CN 90107023 patent/CN1018864B/en not_active Expired
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1648640B (en) * | 2004-01-15 | 2010-05-05 | 松下电器产业株式会社 | Ingredient analysis method and ingredient analysis apparatus |
| CN103945631A (en) * | 2014-04-06 | 2014-07-23 | 浙江大学 | Improved microwave plasma torch device and application |
| CN103945631B (en) * | 2014-04-06 | 2016-04-13 | 浙江大学 | A kind of microwave plasma torch device of improvement and application |
| CN105938097A (en) * | 2016-04-15 | 2016-09-14 | 成都以太航空保障工程技术有限责任公司 | Multi-element oil liquid analysis system based on CCD polychromator |
| CN109297951A (en) * | 2018-08-29 | 2019-02-01 | 上海化工研究院有限公司 | The high effect forced nebulization sampling system of Pneumatic constant pressure type for special spectrum analysis |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1018864B (en) | 1992-10-28 |
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