CN104162523A - Removal method for residual oily soil and water vapor in vacuum spectrometer chamber of X-ray fluorescence spectrophotometer - Google Patents
Removal method for residual oily soil and water vapor in vacuum spectrometer chamber of X-ray fluorescence spectrophotometer Download PDFInfo
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- CN104162523A CN104162523A CN201310182736.0A CN201310182736A CN104162523A CN 104162523 A CN104162523 A CN 104162523A CN 201310182736 A CN201310182736 A CN 201310182736A CN 104162523 A CN104162523 A CN 104162523A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/04—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by a combination of operations
Abstract
The invention relates to a removal method for residual oily soil and water vapor in a vacuum spectrometer chamber of an X-ray fluorescence spectrophotometer. The method is carried out after cleaning and wiping visual oily soil and water vapor on the internal surface of the spectrometer chamber of the X-ray fluorescence spectrophotometer, and is characterized by comprising the following steps of: heating and baking the spectrometer chamber to volatilize the residual oily soil and water, putting a molecular sieve in a molecular sieve storage case, allowing the molecular sieve storage case to enter the spectrometer chamber and absorb the volatilized oily soil and the water, purging the oily soil and the water vapor in the spectrometer chamber of the X-ray fluorescence spectrophotometer with a negative pressure pulse gas flow, allowing spectrophotometers to perform vacuum leakage alternately in turn, using the negative pressure pulse purging gas flow for removal, and exhausting oil gas and the water vapor blown away by the negative pressure pulse purging gas flow to thoroughly remove pollutants in the spectrometer chamber. The method removes the oily soil and the water vapor in the spectrometer chamber of the spectrophotometer efficiently and thoroughly, allows analytical test data to be stable, and enables the instruments to run reliably; an operating method is easy to grasp, and a spectrometer system is not damaged during use.
Description
Technical field
The present invention relates to a kind of physics and chemistry checkout gear, specifically about a kind of clean method of X-fluorescence spectrometer.
Background technology
X-fluorescence spectrometer undertake Zhe Jin factory raw material as the product bit test of iron ore and all kinds of auxiliary materials, smelt the furnace charges such as required sintering deposit constituent analysis, carry out the constituent analysis of blast-melted each chemical element, the test of all kinds of finished product sheet material thickness of coating, and bear the test analysis task of sample in a large amount of scientific research projects, therefore X-fluorescence spectrometer is the important physics and chemistry detecting instrument equipment of modern smelter.
X-fluorescence spectrometer beam splitting system complex structure interior shape is irregular, it is many to relate to parts, there is oily water contaminated vapor cleaning difficulty, the low specific aim of operating efficiency is poor, is difficult to thoroughly remove, because the residual existence of greasy dirt steam has had a strong impact on the accuracy of analysis detecting data.Although can carry out routine cleaning to the visual greasy dirt steam of beam splitting system inner surface in the time safeguarding, but after in very long a period of time cannot disintegrate at nook, optical splitter corner greasy dirt, the steam of cleaning of heavy collection can evaporate gradually, contaminated samples causes the abnormal of analysis detecting data, and especially the element chemistry content analysis such as sulphur, phosphorus, silicon is more so influenced.Beam splitting system cleaning oil pollution efficiency is low, speed is slow, and cleaning performance is not thorough.Can not decompose cleaning to the X ray electron-optical system of large-scale precision; owing to lacking systematicness and beam splitting system cleaning oil pollution method targetedly; can not effectively instruct the spot check upkeep operation of X-fluorescence spectrometer beam splitting system; repair time length, weak effect cause the unnecessary loss of time; cause the secondary pollution of light-splitting chamber, increase the effective operation ratio that has reduced instrument operation downtime.
In greasy dirt in light-splitting chamber, the content of the element such as sulphur, phosphorus, silicon is higher, although through conventional cleaning, but remain in residue greasy dirt in light-splitting chamber under the thermal-radiating effect of X ray, evaporate and pollute the testing sample that enters light-splitting chamber, make the light element contents such as sulphur, phosphorus, silicon measure due to the interference of these pollutants inaccurate, as in the time thoroughly not carrying out light-splitting chamber cleaning, measure molten iron sample and miss by a mile.
The X-ray tube of X-fluorescence spectrometer beam splitting system breaks because aging or its mass defect can cause beryllium window, causes that high voltage insulating oil enters beam splitting system, makes spectrometer light-splitting chamber and vacuum pipe internal contamination; In addition, the vavuum pump in vacuum system is after long-term operation, and pumping fluid wherein also can cause diffuse pollution to vacuum light-splitting chamber.Now X-fluorescence spectrometer just cannot normally use, and therefore needs described pollution to remove.The peak power output of X-ray tube is subject to the restriction of anode element fusing point and heat conductivity, and the heat that anode produces carries out cooling with mobile water.Due to cooling water pipe the deteriorated factor such as break, steam unavoidably enters vacuum light-splitting chamber and causes pollution.In order to prevent that above-mentioned fault from causing the pollution of X-fluorescence spectrometer beam splitting system, after just need to the greasy dirt of light-splitting chamber inner surface, steam being carried out routine cleaning and are wiped, also need be in the case of ensureing that the integrality of equipment is not disintegrated, greasy dirt and steam to light-splitting chamber inner surface remnants are efficiently removed rapidly.
The Chinese patent application that is " vacuum line cleaning device and system " in denomination of invention discloses a kind of vacuum line cleaning device and the system introduced for No. CN201020210793.7, and wherein vacuum line cleaning device comprises: at least two channel washers, at least one brush head and draw-gears; Between described channel washer, be flexibly connected with fit structure and form channel washer group; Described brush head is arranged at least one channel washer; Described draw-gear is arranged on the two ends of described channel washer group.Be applicable to the more vacuum pipe in clean curved junction, pull back and forth channel washer to clear up vacuum pipe with draw-gear.This patent application relates to mechanical hardware cleaning apparatus for pipes, does not relate to the removing of oil residues sewage vapour in X-fluorescence spectrometer light-splitting chamber.
The Chinese patent application that is " vacuum line clean-out separator system " in denomination of invention discloses has introduced a kind of vacuum line clean-out separator system for No. CN200780037472.2, it is removed liquid substance and chip and provides the not vacuum containing pollutant to return for get rid of thing from vacuum, utilize cyclone separation liquid and the chip of the circulation rotating that vacuum discharge pipe and input vacuum logistics bring out, make liquid and chip fall bottom and be discharged to collecting chamber, and clean vacuum-flow is guided clean vacuum outlet hole into.This patent application relates to vacuum line clean-out separator system, does not also relate to the removing of oil residues sewage vapour in X-fluorescence spectrometer light-splitting chamber.
Summary of the invention
The object of this invention is to provide a kind of sweep-out method of oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber, can efficiently thoroughly remove rapidly greasy dirt and the steam of X-fluorescence spectrometer vacuum light-splitting chamber inner surface remnants, to avoid causing the pollution of X-fluorescence spectrometer beam splitting system.
The sweep-out method of the oil residues sewage vapour of a kind of X-fluorescence spectrometer vacuum light-splitting chamber of the present invention, visual greasy dirt, the steam of X-fluorescence spectrometer light-splitting chamber inner surface are cleared up wipe after implement, it is characterized in that comprising the following steps: to light-splitting chamber heat baking residual greasy dirt moisture is evaporated; Molecular sieve is inserted to molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber the oily water evaporating is divided and adsorbed; Carry out X-fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam; Make each optical splitter one after the other vacuum leak, remove by pulse negative pressure sweep gas stream; And make to purge by pulse negative pressure oil gas, the steam discharge that air-flow blows away, to complete the thorough removing of light-splitting chamber internal contamination.
Wherein, to light-splitting chamber, the baking of heating is open X ray and maintain heat radiation and the beam splitting system heated at constant temperature of certain power.
Wherein, described molecular sieve Storage Box comprises upper cover and container body, and the profile of described molecular sieve Storage Box meets X-fluorescence optical spectrometer sample system dimension, and the upper and lower surrounding of molecular sieve Storage Box all has pressure relief opening.
Wherein, at the upper cover of described molecular sieve Storage Box, the metal net mask that is less than sieve particle order number is installed.
Wherein, described the oily water evaporating is divided the step of adsorbing to comprise the Storage Box that molecular sieve is housed is sent into X-fluorescence optical spectrometer sample chamber by sample conveyer carry out vacuum and take out in advance, and until vacuum is opened light-splitting chamber optical gate after normal, so that the molecular sieve in Storage Box effectively adsorbs greasy dirt steam and vapour molecule residual in light-splitting chamber.
Wherein, the molecular sieve in Storage Box adsorbs Hou Zaiyouyuan road to greasy dirt steam residual in light-splitting chamber and vapour molecule to be exited, and back and forth completes adsorption operation with this.
Wherein, be equipped with flow leakage mouth and install control magnetic valve additional on the passage of optical splitter, magnetic valve is connected with optical splitter by self-enclosed snap joint; When magnetic valve no power, always in closed condition, make light-splitting chamber keep vacuum; The step of carrying out X-fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam is under the negative pressure state that is maintaining condition of high vacuum degree; In the time carrying out light-splitting chamber pollution cleanup, produce adjustable periodic pulse signal by pulse signal generator and promote amplifying circuit, produce pulse voltage and drive magnetic valve to open and close with certain period frequency, to form the optical splitter vacuum leak of light-splitting chamber, form air pulse with the adjusting control of magnetic valve being opened to the cycle, to form underbalance pulse gas channel, purge air-flow thereby form underbalance pulse.
Wherein, the oil gas, the steam that blow away by pulse negative pressure purging air-flow are to be discharged to vavuum pump outside along vacuum pipe, to complete the removing of light-splitting chamber internal contamination.
Wherein the technical parameter of the sweep-out method of X-fluorescence spectrometer vacuum light-splitting chamber oil residues sewage vapour is arranged to: beam splitting system starts heated at constant temperature function, makes light-splitting chamber keep 35 ± 1 DEG C; X-ray power maintains 600W, keeps the heat radiation in light-splitting chamber; Use is received X-type molecular sieve and is adsorbed; In beam splitting system light-splitting chamber, maintain the vacuum leak amount of 30 ± 2Pa pressure; Magnetic valve on-off action frequency is 0.2～1Hz.
The invention has the beneficial effects as follows: the inventive method removing spectrometer light-splitting chamber interior oil sewage vapour efficiency is high, removing is thorough, use this method needn't the dismounting of spectrometer light-splitting chamber be decomposed and be reinstalled, it is high that activity duration shortens efficiency, especially avoided reinstalling the precision adjustment of the electron-optical system that light-splitting chamber, point optical channel bring, the engineer that this adjustment work mostly is equipment manufacturing can carry out under professional equipment support.The inventive method is applicable to the X-fluorescence spectrometer of different model, applied widely; Method of operating is grasped easy, upper quick-moving, in use, can not cause damage to beam splitting system, and it is stable, reliable that greasy dirt steam is thoroughly removed the elementary analysis test datas such as rear X-fluorescence spectrometer sulphur, phosphorus, silicon.
Brief description of the drawings
Fig. 1 is the flow chart of the sweep-out method of the oil residues sewage vapour of the spectrometer vacuum light-splitting chamber of one embodiment of the invention;
Fig. 2 is that the master of the molecular sieve Storage Box of the anti-function of splashing of the loading molecular sieve that adopts of the inventive method looks half sectional view;
Fig. 3 is the top view of Fig. 2;
Fig. 4 is that molecular sieve Storage Box enters X-fluorescence spectrometer light-splitting chamber and adsorbs greasy dirt, aqueous vapor schematic diagram;
Fig. 5 is that X-fluorescence spectrometer optical splitter replaces underbalance pulse gas flow purging schematic diagram;
Fig. 6 is the schematic diagram that the underbalance pulse air-flow of repacking increase produces control device.
Detailed description of the invention
For above-mentioned purpose of the present invention, feature and advantage can be become apparent, below in conjunction with accompanying drawing, the specific embodiment of the present invention is elaborated.First it should be noted that, the present invention is not limited to following detailed description of the invention, and the spirit that those skilled in the art should embody from following embodiment is understood the present invention, and each technical term can be done the most wide in range understanding based on Spirit Essence of the present invention.In figure, same or analogous member uses the same reference numerals to represent.
Now illustrate by reference to the accompanying drawings the sweep-out method (hereinafter to be referred as sweep-out method) of the oil residues sewage vapour of a kind of X-fluorescence spectrometer vacuum light-splitting chamber of one embodiment of the present of invention.The method visual greasy dirt, the steam of X-fluorescence spectrometer light-splitting chamber inner surface are cleared up wipe after implement, as shown in Figure 1, comprise the following steps:
P1: light-splitting chamber is heated to toast evaporates greasy dirt moisture;
P2: molecular sieve is inserted to molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber and the oily water evaporating is divided adsorb (seeing Fig. 2 to Fig. 4);
P3: from optical splitter vacuum leak mouth, by self-enclosed fast insert-pull joint access Leakage Gas electromagnetic valve pipeline, under the control of outside pulse signal generator and drive circuit, leak regular underbalance pulse purging air-flow light-splitting chamber is carried out to greasy dirt steam purging removing (seeing Fig. 5 and Fig. 6);
P4: make each optical splitter one after the other vacuum leak (making vacuum in light-splitting chamber is 30Pa left and right), remove by pulse negative pressure sweep gas stream;
P5: make the oil gas, the steam that blow away by pulse negative pressure purging air-flow be discharged to vavuum pump outside along vacuum pipe, complete the thorough removing of light-splitting chamber internal contamination.
Now describe above steps in detail in conjunction with Fig. 2 to Fig. 6.
After the visual greasy dirt of X-fluorescence spectrometer light-splitting chamber 6 inner surface, steam are cleared up and are wiped, also have greasy dirt, steam residual, further clear up through above steps.
In P1 step, first, the X-ray tube 7 of unlatching X-fluorescence spectrometer makes X ray maintain certain power and the photosystem of giving a mark is opened heated at constant temperature function, light-splitting chamber 6 is played to baking effect, under thermal-radiating effect, inner residual greasy dirt, the moisture of light-splitting chamber 6 evaporates in time, so that adsorb and purge.
In P2 step, as shown in Figure 4, by the molecular sieve Storage Box 11(that molecular sieve (not shown) is housed as shown in Figure 2,3) sending into X-fluorescence optical spectrometer sample chamber 12 by sample conveyer 13 carries out vacuum and takes out in advance, until open light-splitting chamber optical gate (shutter) 10 after vacuum is normal, the molecular sieve in Storage Box 11 effectively adsorbs greasy dirt steam and vapour molecule residual in light-splitting chamber 6.
In P3 step, carry out X-fluorescence spectrometer light-splitting chamber 6 underbalance pulse gas flow purging greasy dirts, steam, can obtain good oily water with intermittent pulse form during in the interior motion of light-splitting chamber 6 and divide removing effect when purging air-flow.X-fluorescence spectrometer light-splitting chamber 6 is in good sealing form, all maintaining at ordinary times condition of high vacuum degree, for example, below 5Pa, the atmosphere outside of light-splitting chamber 6 has just formed negative pressure state relatively, utilize the gas kinetic energy of this negative pressure, as shown in Figure 5 and Figure 6, on optical splitter 6, leak magnetic valve 21 opens and closes with certain period frequency under pulse signal generator 17 and drive circuit control, people is optical splitter 8 vacuum leaks that cause light-splitting chamber 6, form underbalance pulse and purge air-flow, light-splitting chamber 6 is cleaned and depolluted.
In P4 step, in order to prevent the excessive fault that causes of live load of vavuum pump 14,15, adopt each optical splitter 8 one after the other vacuum leaks, for example making the interior vacuum of light-splitting chamber 6 is 30Pa left and right, form underbalance pulse and purge air-flow, now also to open X ray and heated at constant temperature function keeps certain heat radiation, allow oil gas, the steam brought into play be blown away by air-flow.
In step 5, make the oil gas, the steam that blow away by pulse negative pressure purging air-flow be discharged to vavuum pump 14,15 outsides along vacuum pipe 16, complete the thorough removing of light-splitting chamber 6 internal contaminations.
Wherein, open X ray and maintain certain power (as 30KV, 20mA; Be equivalent to the heat radiation of 600W power) and beam splitting system heated at constant temperature function, play baking effect, under thermal-radiating effect, inner residual greasy dirt, the moisture of light-splitting chamber 6 evaporates in time, adsorbs and purges.
Wherein, in X-fluorescence spectrometer light-splitting chamber 6, oil residues, steam are carried out to Adsorption with molecular sieve, light-splitting chamber 6 is owing to vacuumizing all the time in negative pressure state, molecular sieve enters light-splitting chamber 6 will pass through the variation to vacuum environment by atmosphere, the conversion from vacuum to atmospheric environment again after absorption.This method is put into appropriate molecular sieve the molecular sieve Storage Box 11 of custom-designed metal material.Molecular sieve Storage Box 11 comprises upper cover 2 and container body 3, the profile of described molecular sieve Storage Box 11 meets X-fluorescence optical spectrometer sample system dimension, and pressure relief opening 4,5 is all arranged at molecular sieve Storage Box 11 surroundings and bottom, enter after vacuum environment in Storage Box gas energy quick and stable and discharge and reach internal and external pressure balance, to prevent that molecular sieve from entering after vacuum environment pressure and die-offing to splash and cause secondary pollution everywhere; The metal net mask 1 that is less than sieve particle order number is installed molecular sieve is retrained to the container body 3 of putting into again Storage Box at upper cover 2 simultaneously, when use, Storage Box 11 being sent into X-fluorescence optical spectrometer sample chamber 12 by sample conveyer 13 carries out vacuum and takes out in advance, until open light-splitting chamber optical gate (shutter) 10 after vacuum is normal, molecular sieve in Storage Box 11 effectively adsorbs greasy dirt steam and vapour molecule residual in light-splitting chamber 6, absorption Hou Zaiyouyuan road is exited, and back and forth completes adsorption operation with this.Such method has been avoided manually light-splitting chamber 6 being amplified to gas, opens light-splitting chamber 6 and removes to place molecular sieve and vacuumize, and after absorption, light-splitting chamber 6 amplifies gas and opens light-splitting chamber 6 and take out this tediously long numerous and diverse manual work mode of molecular sieve.
Wherein, after absorption, the residual greasy dirt of light-splitting chamber 6, steam reduce, but not yet thoroughly remove, and use underbalance pulse gas flow purging.Optical splitter passage to X-fluorescence spectrometer beam splitting system carries out appropriate reconstruction, as shown in Figure 6, the underbalance pulse air-flow that repacking increases produces control device, comprise: on optical splitter passage, increase flow leakage control magnetic valve 21, magnetic valve by self-enclosed snap joint be connected tracheae 23, fast interface 24 with leak fast interface 9 with the optical splitter of optical splitter 8 and be connected, when magnetic valve 21 no power always in closed condition, make light-splitting chamber 6 keep good vacuum, in the time carrying out light-splitting chamber pollution cleanup, produce adjustable periodic pulse signal by pulse signal generator 17, remove to promote for example signal amplifier 18 of amplifying circuit, produce pulse voltage and drive magnetic valve 21 by relay 19, because the cycle of magnetic valve 21 opens and closes the vacuum leak that causes state at intermittence, at the interior formation underbalance pulse of optical splitter 6 air-flow, air-flow is by export-oriented light-splitting chamber 6 internal flows of optical splitter 8, purge contaminated light-splitting chamber 6 inner surfaces, taken away by air-flow through purging continuously after stain oil gas and vapour molecule, and pass through vacuum pipe 16 through vavuum pump 14, 15 get rid of, finally reach not dismantle and decompose beam splitting system and the object of clean light-splitting chamber internal contamination.
Wherein, passage 8a, the 8b of each optical splitter 8 of light-splitting chamber 6 alternately blows: because X-fluorescence spectrometer vacuum system intermediate pump exhaust capacity is limited, and when vacuum gauge (being generally Pirani gauge) is worked under low vacuum environment, very easily make its platinum filament burn open circuit, cannot observe light-splitting chamber vacuum state, therefore use passage 8a, the 8b one after the other of each optical splitter 8 to blow, keep light-splitting chamber 6 relative high vacuum environment, alleviate vavuum pump 14,15 live load, prevent that vacuum gauge from damaging under low vacuum environment.
Process of the test: after X-fluorescence spectrometer light-splitting chamber is by greasy dirt, moisture contamination, after the inner preliminary cleaning of light-splitting chamber, use this method thoroughly to remove the residual greasy dirt of light-splitting chamber, steam, use molecular sieve adsorption and negative pressure to purge combined method to residue cleaning, removal.
The sweep-out method technical parameter of greasy dirt steam of the present invention arranges as follows:
1) beam splitting system starts heated at constant temperature function, makes light-splitting chamber keep 35 ± 1 DEG C;
2) x-ray power maintains 600W(30KV, 20mA), keep the heat radiation in light-splitting chamber;
3) use and receive X-type molecular sieve and adsorb;
4) in beam splitting system light-splitting chamber, maintain the vacuum leak amount of 30 ± 2Pa pressure;
5) magnetic valve on-off action frequency is 0.2～1Hz.
The inventive method has the following advantages compared with other technologies:
(1) make the interior generation heat of light-splitting chamber 6 with the heated at constant temperature function of the suitable x-ray power of X-fluorescence spectrometer and beam splitting system, under thermal-radiating baking effect, accelerate the volatilization of oil residues, vapour molecule in light-splitting chamber, for good condition has been created in the application of molecular sieve adsorption and negative pressure purging air-flow.
(2) molecular sieve adsorption: molecular sieve has high strength, Heat stability is good, specific area is large, the advantage that adsorptivity is strong, as sodium X-type molecular sieve (X crystal structure type sodium type) can adsorb oil gas and vapour molecule below cut off diameter 10A, its profile is graininess higher mechanical strength, enter vacuum environment after sieve particle can not break because of sudden changes in pressure; Simultaneously molecular sieve enters after light-splitting chamber 6 under x-ray bombardment along with the rising of temperature can keep the stable of physical and chemical performance.Appropriate molecular sieve is put into custom-designed metal Storage Box 11, molecular sieve Storage Box 11 profiles meet X-fluorescence optical spectrometer sample system dimension and are convenient to carry, in order to prevent that molecular sieve from entering after vacuum environment pressure and die-offing to splash and cause secondary pollution everywhere, the upper and lower surrounding of Storage Box all has pressure relief opening 4,5, enters after vacuum environment in Storage Box gas energy quick and stable and discharges and reach internal and external pressure balance; With the metal net mask 1 that is less than sieve particle order number, molecular sieve is placed to constraint simultaneously and put into again Storage Box 11, when use, molecular sieve Storage Box 11 being sent into X-fluorescence optical spectrometer sample chamber 12 by sample conveyer 13 carries out vacuum and takes out in advance, until open light-splitting chamber shutter 10 after vacuum is normal, the molecular sieve in Storage Box 11 effectively adsorbs greasy dirt steam and vapour molecule residual in light-splitting chamber.
(3) optical splitter 8 negative pressure purge: under normal condition, light-splitting chamber 6 outsides of X-fluorescence spectrometer are atmospheric conditions, and in light-splitting chamber 6, be all the time in vacuum environment, by pipeline 16, light-splitting chamber 6 is carried out to continuous air extraction with vavuum pump 14,15, to keep the having vacuum below 5Pa pressure in light-splitting chamber 6.If suitably cause artificial vacuum leak to utilize the poor formation negative-pressure air-flow of external and internal pressure passage, greasy dirt residual in light-splitting chamber and steam are carried out to continuous flow purging, finally wipe oil and steam are residual.Optical splitter passage to X-fluorescence spectrometer beam splitting system carries out appropriate reconstruction, on optical splitter passage, increase flow leakage mouth and install additional and control magnetic valve 21, while not powering up at ordinary times, magnetic valve is always in closed condition, in the time carrying out light-splitting chamber pollution cleanup, form air pulse by (making light-splitting chamber vacuum people as adjusting to the vacuum of 20～30Pa pressure) taking pulse signal generator 17 and drive circuit by magnetic valve being opened to the adjusting control in cycle, form underbalance pulse gas channel, air-flow is by the export-oriented light-splitting chamber internal flow of optical splitter, purge contaminated light-splitting chamber inner surface, taken away by air-flow through purging continuously after stain oil gas and vapour molecule, and pass through vacuum pipe 16 through vavuum pump 14, 15 get rid of, finally reach not dismantle and decompose beam splitting system and the object of clean light-splitting chamber internal contamination.In sum, the inventive method removing spectrometer light-splitting chamber interior oil sewage vapour efficiency is high, removing is thorough, use this method needn't the dismounting of spectrometer light-splitting chamber be decomposed and be reinstalled, it is high that activity duration shortens efficiency, especially avoided reinstalling the precision adjustment of the electron-optical system that light-splitting chamber, point optical channel bring, the engineer that this adjustment work mostly is equipment manufacturing can carry out under professional equipment support.The inventive method is applicable to the X-fluorescence spectrometer of different model, applied widely; Method of operating is grasped easy, upper quick-moving, in use, can not cause damage to beam splitting system, and it is stable, reliable that greasy dirt steam is thoroughly removed the elementary analysis test datas such as rear X-fluorescence spectrometer sulphur, phosphorus, silicon.
Greasy dirt steam is removed the X-fluorescence spectrometer measurement Contrast on effect (in table one) of front and back, taking the pig iron standard specimen SCRM of standard specimen office of Britain 652/4 on MXF-2300 X-fluorescence spectrometer continuous 10 times measure chemical contents as example (x-ray tube voltage 40KV, tube current 60mA, 40 seconds times of integration):
Table one: X-fluorescence spectrometer contrast table
In sum, by heated at constant temperature, make light-splitting chamber produce heat to utilize heat radiation effect by oil residues sewage vapour volatilization in X-fluorescence spectrometer light-splitting chamber; Utilize molecular sieve Storage Box 11 that molecular sieve is put into light-splitting chamber 6, take out in advance and open light-splitting chamber optical gate 10 by vacuum and adsorb oil residues G&W vapour molecule; In light splitting vacuum system, form suitable vacuum leak amount, form purging air-flow continuous band and walk light-splitting chamber 6, the residual greasy dirt of vacuum pipe 16, steam, and get rid of by vavuum pump 14,15 scavenge ports.In order to keep the relative high vacuum environment of light-splitting chamber, alleviate vavuum pump live load, prevent that vacuum gauge from damaging under low vacuum environment, take each passage to replace Purge methods.
The application example that method of the present invention is now described is as follows.
Before converter, fast separating tests chamber MXF2300 X-fluorescence spectrometer, because X-ray tube mass defect beryllium window breaks, causes that high voltage insulating oil and cooling water enter light-splitting chamber and vacuum line, causes the inner severe contamination of optical splitter and vacuum pipe.To contaminated light-splitting chamber and vacuum pipe inner surface carried out conventional clean and wipe after, after instrument operation along with light-splitting chamber temperature raises, under light-splitting chamber heated at constant temperature function and X ray heat radiation effect, oil residues, steam that heavy collection cannot directly be removed at nook, optical splitter corner evaporate gradually, when contaminated samples causes stokehold molten iron sample to analyze, the light element such as silicon, p and s detects data and occurs unusual fluctuations, cannot meet the analyzing and testing requirement of stokehold.In the case of ensureing that the integrality of equipment is not disintegrated, first adopt molecular sieve adsorption under heat radiation, again 21 element passage optical splitters in light-splitting chamber are carried out to one after the other underbalance pulse gas flow purging method, finally efficiently remove rapidly remaining insulating oil greasy dirt and steam, ensured the X-fluorescence spectrometer stable operation of matter inspection chamber.
The present invention met X-fluorescence spectrometer beam splitting system contaminated after, in the case of ensureing that the integrality of equipment is not disintegrated, do not damage the space geometry position of beam splitting system electro-optical device and X ray light path, efficiently, remove up hill and dale the residual greasy dirt of light-splitting chamber and vacuum pipe, steam, prevent that measured sample from polluting, ensure especially light element data stable, reliable of X-fluorescence spectrometer analysis data.The inventive method wide accommodation, is applicable to, on dissimilar X-fluorescence spectrometer, having a wide range of application value.
Should be understood that those skilled in the art can make various changes or modifications the present invention after having read above-mentioned instruction content of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (9)
1. the sweep-out method of the oil residues sewage vapour of an X-fluorescence spectrometer vacuum light-splitting chamber, visual greasy dirt, the steam of X-fluorescence spectrometer light-splitting chamber inner surface are cleared up wipe after implement, it is characterized in that comprising the following steps: to light-splitting chamber heat baking residual greasy dirt moisture is evaporated; Molecular sieve is inserted to molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber the oily water evaporating is divided and adsorbed; Carry out X-fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam; Make each optical splitter one after the other vacuum leak, remove by pulse negative pressure sweep gas stream; And make to purge by pulse negative pressure oil gas, the steam discharge that air-flow blows away, to complete the thorough removing of light-splitting chamber internal contamination.
2. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 1, is characterized in that, to light-splitting chamber, the baking of heating is open X ray and maintain heat radiation and the beam splitting system heated at constant temperature of required power.
3. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 1, it is characterized in that, described molecular sieve Storage Box comprises upper cover and container body, the profile of described molecular sieve Storage Box meets X-fluorescence optical spectrometer sample system dimension, and the upper and lower surrounding of molecular sieve Storage Box all has pressure relief opening.
4. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 3, is characterized in that, the metal net mask that is less than sieve particle order number is installed at the upper cover of described molecular sieve Storage Box.
5. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 1, it is characterized in that, described the oily water evaporating is divided the step of adsorbing to comprise the Storage Box that molecular sieve is housed is sent into X-fluorescence optical spectrometer sample chamber by sample conveyer carry out vacuum and take out in advance, and until vacuum is opened light-splitting chamber optical gate after normal, so that the molecular sieve in Storage Box effectively adsorbs greasy dirt steam and vapour molecule residual in light-splitting chamber.
6. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 6, it is characterized in that, molecular sieve in Storage Box adsorbs Hou Zaiyouyuan road to greasy dirt steam residual in light-splitting chamber and vapour molecule to be exited, and back and forth completes adsorption operation with this.
7. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 1, it is characterized in that, on the passage of optical splitter, be equipped with flow leakage mouth and install control magnetic valve additional, magnetic valve is connected with optical splitter by self-enclosed snap joint; When magnetic valve no power, always in closed condition, make light-splitting chamber keep vacuum; The step of carrying out X-fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam is under the negative pressure state that is maintaining condition of high vacuum degree; In the time carrying out light-splitting chamber pollution cleanup, produce adjustable periodic pulse signal by pulse signal generator and promote amplifying circuit, produce pulse voltage and drive magnetic valve to open and close with certain period frequency, to form the optical splitter vacuum leak of light-splitting chamber, form air pulse with the adjusting control of magnetic valve being opened to the cycle, to form underbalance pulse gas channel, purge air-flow thereby form underbalance pulse.
8. the sweep-out method of the oil residues sewage vapour of X-fluorescence spectrometer vacuum light-splitting chamber according to claim 1, it is characterized in that, the oil gas, the steam that blow away by pulse negative pressure purging air-flow are to be discharged to vavuum pump outside along vacuum pipe, to complete the removing of light-splitting chamber internal contamination.
9. according to the sweep-out method of the oil residues sewage vapour of the X-fluorescence spectrometer vacuum light-splitting chamber described in any one of claim 1 to 8, it is characterized in that, the technical parameter of the sweep-out method of X-fluorescence spectrometer vacuum light-splitting chamber oil residues sewage vapour is arranged to: beam splitting system starts heated at constant temperature function, makes light-splitting chamber keep 35 ± 1 DEG C; X-ray power maintains 600W, keeps the heat radiation in light-splitting chamber; Use is received X-type molecular sieve and is adsorbed; In beam splitting system light-splitting chamber, maintain the vacuum leak amount of 30 ± 2Pa pressure; Magnetic valve on-off action frequency is 0.2～1Hz.
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