CN104162523B - The sweep-out method of the oil residues sewage vapour of X fluorescence spectrometer vacuum light-splitting chamber - Google Patents
The sweep-out method of the oil residues sewage vapour of X fluorescence spectrometer vacuum light-splitting chamber Download PDFInfo
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- CN104162523B CN104162523B CN201310182736.0A CN201310182736A CN104162523B CN 104162523 B CN104162523 B CN 104162523B CN 201310182736 A CN201310182736 A CN 201310182736A CN 104162523 B CN104162523 B CN 104162523B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
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Abstract
The present invention is a kind of sweep-out method of oil residues sewage vapour of X fluorescence spectrometer vacuum light-splitting chamber, implement after carrying out cleaning erasing at the visual greasy dirt to X fluorescence spectrometer light-splitting chamber inner surface, steam, it is characterized in that comprising the following steps: heating to toast to light-splitting chamber makes the greasy dirt moisture remained evaporate; Molecular sieve is inserted molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber and the oily water evaporated is divided adsorb; 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, removed by pulsating negative pressure sweep gas stream; And make by pulsating negative pressure purge air-flow blow away oil gas, steam discharge, to complete the thorough removing of light-splitting chamber internal contamination.The inventive method removing spectrometer light-splitting chamber interior oil sewage vapour efficiency is high, removing is thorough, and analyzing test data is stablized, reliable; Method of operating is grasped easily, can not cause damage in using to beam splitting system.
Description
Technical field
The present invention relates to a kind of Physico-chemical tests device, specifically about a kind of clean method of X fluorescence spectrometer.
Background technology
X fluorescence spectrometer be responsible for into factory's raw material as iron ore and all kinds of auxiliary material product bit test, smelt needed for the furnace charge such as 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 project, therefore X fluorescence spectrometer is the important Physico-chemical tests instrument and 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, and the existence remained due to greasy dirt steam has had a strong impact on the accuracy of analysis detecting data.Although routine cleaning can be carried out to the visual greasy dirt steam of beam splitting system inner surface when safeguarding, greasy dirt, the steam of the cleaning but the collection that sinks within a period of time very long afterwards cannot disintegrate at nook, optical splitter corner can evaporate gradually, contaminated samples causes the exception 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 slow, and cleaning performance is not thorough.Decomposition cleaning can not be carried out to the X-ray electron-optical system of large-scale precision; owing to lacking systematicness and beam splitting system cleaning oil pollution method targetedly; effectively can not 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 reducing instrument downtime and run.
In greasy dirt in light-splitting chamber, the content of the element such as sulphur, phosphorus, silicon is higher, although through conventional cleaning, but the residue greasy dirt remained in light-splitting chamber is under the thermal-radiating effect of X-ray, evaporate and pollute the testing sample entering light-splitting chamber, it is inaccurate that interference due to these pollutants makes the light element contents such as sulphur, phosphorus, silicon measure, as when thoroughly not carrying out light-splitting chamber cleaning, measuring molten iron sample and missing by a mile.
The X-ray tube of X fluorescence spectrometer beam splitting system can cause beryllium window to break due to aging or its mass defect, causes high voltage insulating oil to enter beam splitting system, makes spectrometer light-splitting chamber and vacuum pipe internal contamination; In addition, the vavuum pump in vacuum system is after longtime running, 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 to remove described pollution.The peak power output of X-ray tube is subject to the restriction of anode element fusing point and heat conductivity, and the water of the heat flowing that anode produces cools.Deterioration due to cooling water pipe such as to be broken at the factor, and steam unavoidably enters vacuum light-splitting chamber and causes pollution.In order to the pollution preventing above-mentioned fault from causing X fluorescence spectrometer beam splitting system, after just needing the greasy dirt to light-splitting chamber inner surface, steam to carry out routine cleaning erasing, also need when ensureing that the integrality of equipment is not disintegrated, the greasy dirt of light-splitting chamber inner surface remnants and steam are efficiently removed rapidly.
Disclose No. CN201020210793.7 in the denomination of invention Chinese patent application that is " vacuum line cleaning device and system " and describe a kind of vacuum line cleaning device and system, wherein vacuum line cleaning device comprises: at least two channel washers, at least one brush head and draw-gears; Be flexibly connected with fit structure between described channel washer and formed 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 vacuum pipe that clean curved junction is more, pull channel washer to clear up vacuum pipe back and forth 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.
Disclose No. CN200780037472.2 in the denomination of invention Chinese patent application that is " vacuum line clean-out separator system " and describe a kind of vacuum line clean-out separator system, it does not return containing the vacuum of pollutant for getting rid of in thing from vacuum to remove liquid substance and chip and provide, the cyclone separation liquid of the circulation rotating utilizing Vacuum exhaust line to bring out with input vacuum stream and chip, make liquid and chip fall bottom and be discharged to collecting chamber, and clean vacuum-flow guides clean vacuum outlet port 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, efficiently thoroughly can remove greasy dirt and the steam of X fluorescence spectrometer vacuum light-splitting chamber inner surface remnants rapidly, to avoid the pollution causing 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, implement after carrying out cleaning erasing at the visual greasy dirt to X fluorescence spectrometer light-splitting chamber inner surface, steam, it is characterized in that comprising the following steps: heating to toast to light-splitting chamber makes the greasy dirt moisture remained evaporate; Molecular sieve is inserted molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber and the oily water evaporated is divided adsorb; 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, removed by pulsating negative pressure sweep gas stream; And make by pulsating negative pressure purge air-flow blow away oil gas, steam discharge, to complete the thorough removing of light-splitting chamber internal contamination.
Wherein, be open X-ray and maintain heat radiation and the beam splitting system heated at constant temperature of certain power to light-splitting chamber baking of heating.
Wherein, described molecular sieve Storage Box comprises upper cover and container body, and the profile of described molecular sieve Storage Box meets X fluorescence spectrometer sample system size, 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 being less than sieve particle order number is installed.
Wherein, the described oily water to evaporating divides the step of adsorbing to comprise the Storage Box that molecular sieve is housed is sent into X fluorescence spectrometer sample room by sample conveyer and carries out vacuum and take out in advance, and until vacuum normal after open light-splitting chamber optical gate, to make the molecular sieve in Storage Box, greasy dirt steam residual in light-splitting chamber and vapour molecule are effectively adsorbed.
Wherein, the molecular sieve in Storage Box carries out absorption 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, the passage of optical splitter is equipped with flow leakage mouth and installs Controlling solenoid valve additional, magnetic valve is connected with optical splitter by self-enclosed snap joint; Be in closed condition during magnetic valve no power always, make light-splitting chamber keep vacuum; Carrying out the step of X fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam, is under the negative pressure state that maintain condition of high vacuum degree; When 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 with certain period frequency opening and closing, to form the optical splitter vacuum leak of light-splitting chamber, air pulse is formed with regulable control magnetic valve being opened to the cycle, to form underbalance pulse gas channel, thus form underbalance pulse purging air-flow.
Wherein, the oil gas blown away by pulsating negative pressure purging air-flow, steam are discharged to outside vavuum pump 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; The vacuum leak amount of 30 ± 2Pa pressure is maintained in beam splitting system light-splitting chamber; 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, this method is used to decompose the dismounting of spectrometer light-splitting chamber and to reinstall, it is high that activity duration shortens efficiency, the precision adjustment of the electron-optical system of specifically avoid and reinstall light-splitting chamber, dividing optical channel to 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, can not cause damage in using to beam splitting system, and greasy dirt steam is thoroughly removed the elementary analysis test datas such as rear X fluorescence spectrometer sulphur, phosphorus, silicon and stablized, reliable.
Accompanying drawing explanation
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 splashguard function of the loading molecular sieve that the inventive method adopts 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 carries out absorption 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 of the underbalance pulse air-flow generation control device that repacking increases.
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 to understand the present invention, and each technical term can do the most wide in range understanding based on Spirit Essence of the present invention.In figure, same or analogous component uses the same reference numerals to represent.
Now illustrate the sweep-out method (hereinafter referred to 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 by reference to the accompanying drawings.The method is implemented after carrying out cleaning erasing at the visual greasy dirt to X fluorescence spectrometer light-splitting chamber inner surface, steam, as shown in Figure 1, comprises the following steps:
P1: greasy dirt moisture is evaporated to light-splitting chamber baking of heating;
P2: molecular sieve is inserted molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber and the oily water evaporated is divided adsorb (see 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 and purge air-flow and greasy dirt steam is carried out to light-splitting chamber purge and remove (see Fig. 5 and Fig. 6);
P4: make each optical splitter one after the other vacuum leak (making vacuum in light-splitting chamber be about 30Pa), removed by pulsating negative pressure sweep gas stream;
P5: make to purge by pulsating negative pressure oil gas, the steam that air-flow blows away and be discharged to outside vavuum pump along vacuum pipe, complete the thorough removing of light-splitting chamber internal contamination.
Existing composition graphs 2 to Fig. 6 describes above steps in detail.
After cleaning erasing is carried out to the visual greasy dirt of X fluorescence spectrometer light-splitting chamber 6 inner surface, steam, also have greasy dirt, steam to remain, clear up further through above steps.
In P1 step, first, the X-ray tube 7 of unlatching X fluorescence spectrometer makes X-ray maintain certain power and photosystem of giving a mark opens heated at constant temperature function, baking effect is played to light-splitting chamber 6, under thermal-radiating effect, the greasy dirt of light-splitting chamber 6 internal residual, moisture evaporate, in time so that carry out adsorbing and purging.
In P2 step, as shown in Figure 4, the molecular sieve Storage Box 11(of molecular sieve (not shown) will be housed as shown in Figure 2,3) send into X fluorescence spectrometer sample room 12 by sample conveyer 13 and carry out vacuum and take 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 residual in light-splitting chamber 6 and vapour molecule.
In P3 step, carry out X fluorescence spectrometer light-splitting chamber 6 underbalance pulse gas flow purging greasy dirt, steam, good oily water can be obtained when purging air-flow and moving in light-splitting chamber 6 with intermittent pulse form and divide elimination effect.X fluorescence spectrometer light-splitting chamber 6 is in good sealing form, all maintain condition of high vacuum degree at ordinary times, such as below 5Pa, the atmosphere outside of relative light-splitting chamber 6 just defines negative pressure state, utilize the gas kinetic energy of this negative pressure, as shown in Figure 5 and Figure 6, optical splitter 6 leaks magnetic valve 21 under pulse signal generator 17 and drive circuit control with certain period frequency opening and closing, people is optical splitter 8 vacuum leak causing light-splitting chamber 6, form underbalance pulse and purge air-flow, cleaning is carried out to light-splitting chamber 6 and depollutes.
In P4 step, in order to prevent, the live load of vavuum pump 14,15 is excessive causes fault, adopt each optical splitter 8 one after the other vacuum leak, vacuum in light-splitting chamber 6 is such as made to be about 30Pa, 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 steps of 5, make to purge by pulsating negative pressure oil gas, the steam that air-flow blows away and be discharged to outside vavuum pump 14,15 along vacuum pipe 16, complete the thorough removing of light-splitting chamber 6 internal contamination.
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, the greasy dirt of light-splitting chamber 6 internal residual, moisture evaporate in time, carry out adsorbing and purging.
Wherein, in X fluorescence spectrometer light-splitting chamber 6, Adsorption is carried out to oil residues, steam with molecular sieve, light-splitting chamber 6 is in negative pressure state all the time owing to vacuumizing, molecular sieve enters light-splitting chamber 6 and will pass through by the change of air to vacuum environment, the conversion after absorption again from vacuum to atmospheric environment.The molecular sieve Storage Box 11 of custom-designed metal material put into by appropriate molecular sieve by this method.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 spectrometer sample system size, and pressure relief opening 4,5 is all arranged at molecular sieve Storage Box 11 surrounding and bottom, after entering vacuum environment, in Storage Box, gas energy quick and stable is discharged and is reached internal and external pressure balance, and after entering vacuum environment to prevent molecular sieve, pressure splashes of die-offing causes secondary pollution; Be provided with at upper cover 2 be simultaneously less than sieve particle order number metal net mask 1 to put into the container body 3 of Storage Box again to molecular sieve constraint, during use, Storage Box 11 is sent into X fluorescence spectrometer sample room 12 by sample conveyer 13 to carry out vacuum and take 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 residual in light-splitting chamber 6 and vapour molecule, absorption Hou Zaiyouyuan road is exited, and back and forth completes adsorption operation with this.Such method avoids manually amplifies gas to light-splitting chamber 6, opens light-splitting chamber 6 and goes 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, light-splitting chamber 6 remains greasy dirt, steam reduces, but not yet thoroughly removes, and uses underbalance pulse gas flow purging.Appropriate reconstruction is carried out to the optical splitter passage of X fluorescence spectrometer beam splitting system, as shown in Figure 6, the underbalance pulse air-flow that repacking increases produces control device, comprise: on optical splitter passage, increase flow leakage Controlling solenoid 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, be in closed condition during magnetic valve 21 no power always, make the vacuum that light-splitting chamber 6 keeps good, when carrying out light-splitting chamber pollution cleanup, adjustable periodic pulse signal is produced by pulse signal generator 17, go to promote amplifying circuit such as signal amplifier 18, produce pulse voltage and drive magnetic valve 21 by relay 19, cycle opening and closing due to magnetic valve 21 causes the vacuum leak of intermittent condition, underbalance pulse air-flow is formed in optical splitter 6, air-flow is by the internal flow of optical splitter 8 export-oriented light-splitting chamber 6, purge contaminated light-splitting chamber 6 inner surface, through purging after stain oil gas and vapour molecule are taken away by air-flow continuously, and by vacuum pipe 16 through vavuum pump 14, 15 get rid of, finally reach the object do not dismantled and decompose beam splitting system and clean light-splitting chamber internal contamination.
Wherein, passage 8a, 8b of each optical splitter 8 of light-splitting chamber 6 alternately blow: because X fluorescence spectrometer vacuum system intermediate pump exhaust capacity is limited, and vacuum gauge (being generally Pirani gauge) when working under low vacuum environment, its platinum filament is very easily made to burn open circuit, light-splitting chamber vacuum state cannot be observed, therefore passage 8a, 8b one after the other of each optical splitter 8 is used to blow, keep light-splitting chamber 6 high vacuum environment relatively, alleviate the live load of vavuum pump 14,15, prevent 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 that this method remains greasy dirt to light-splitting chamber, steam is thoroughly removed, to residue cleaning, remove and use molecular sieve adsorption and negative pressure to purge combined method.
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) the vacuum leak amount of 30 ± 2Pa pressure is maintained in beam splitting system light-splitting chamber;
5) magnetic valve on-off action frequency is 0.2 ~ 1Hz.
The inventive method has the following advantages compared with other technologies:
(1) make to produce heat in 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 in light-splitting chamber, vapour molecule, the application purging air-flow for molecular sieve adsorption and negative pressure creates good condition.
(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 form) can adsorb oil gas and the vapour molecule of below cut off diameter 10A, its profile is that graininess has higher mechanical strength, and after entering vacuum environment, sieve particle can not break because pressure changes suddenly; After simultaneously molecular sieve enters 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 profile meets X fluorescence spectrometer sample system size and is convenient to conveying, after entering vacuum environment to prevent molecular sieve, pressure splashes of die-offing causes secondary pollution, the upper and lower surrounding of Storage Box all has pressure relief opening 4,5, and after entering vacuum environment, in Storage Box, the discharge of gas energy quick and stable reaches internal and external pressure balance; Place constraint with the metal net mask 1 pair of molecular sieve being less than sieve particle order number simultaneously and put into Storage Box 11 again, during use, molecular sieve Storage Box 11 is sent into X fluorescence spectrometer sample room 12 by sample conveyer 13 to carry out vacuum and take 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 residual in light-splitting chamber and vapour molecule.
(3) optical splitter 8 negative pressure purges: under normal condition, light-splitting chamber 6 outside of X fluorescence spectrometer is atmospheric condition, and be in vacuum environment all the time in light-splitting chamber 6, namely continuous air extraction is carried out with vavuum pump 14,15 by pipeline 16 pairs of light-splitting chambers 6, to keep the vacuum having below 5Pa pressure in light-splitting chamber 6.If suitably cause artificial vacuum leak to utilize external and internal pressure difference to form negative-pressure air-flow passage, continuous flow purging is carried out to greasy dirt residual in light-splitting chamber and steam, can finally wipe oil and steam remain.Appropriate reconstruction is carried out to the optical splitter passage of X fluorescence spectrometer beam splitting system, optical splitter passage increases flow leakage mouth and installs Controlling solenoid valve 21 additional, when not powering up at ordinary times, magnetic valve is in closed condition always, when carrying out light-splitting chamber pollution cleanup, air pulse is formed by (making light-splitting chamber vacuum people be the vacuum adjusting to 20 ~ 30Pa pressure) by regulable control magnetic valve being opened to the cycle with pulse signal generator 17 and drive circuit, namely underbalance pulse gas channel is formed, air-flow is by the export-oriented light-splitting chamber internal flow of optical splitter, purge contaminated light-splitting chamber inner surface, through purging after stain oil gas and vapour molecule are taken away by air-flow continuously, and by vacuum pipe 16 through vavuum pump 14, 15 get rid of, finally reach the object do not dismantled and decompose beam splitting system and 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, this method is used to decompose the dismounting of spectrometer light-splitting chamber and to reinstall, it is high that activity duration shortens efficiency, the precision adjustment of the electron-optical system of specifically avoid and reinstall light-splitting chamber, dividing optical channel to 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, can not cause damage in using to beam splitting system, and greasy dirt steam is thoroughly removed the elementary analysis test datas such as rear X fluorescence spectrometer sulphur, phosphorus, silicon and stablized, reliable.
Greasy dirt steam removes X fluorescence spectrometer measurement effect contrast (see table one) of front and back, on MXF-2300X XRF, chemical content (x-ray tube voltage 40KV is measured continuous 10 times for standard specimen office of Britain pig iron standard specimen SCRM652/4, tube current 60mA, 40 seconds times of integration):
Table one: X fluorescence spectrometer contrast table
In sum, by heated at constant temperature, light-splitting chamber is made to 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, taken out and open light-splitting chamber optical gate 10 by vacuum in advance and carry out adsorbing residual oil gas and 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 got rid of by vavuum pump 14,15 scavenge port.In order to keep the relative high vacuum environment of light-splitting chamber, alleviating the live load of vavuum pump, preventing vacuum gauge from damaging under low vacuum environment, taking each passage to replace Purge methods.
Now illustrate that an application example of method of the present invention is as follows.
Before converter, fast separating tests room MXF2300X XRF breaks because of X-ray tube mass defect beryllium window, causes high voltage insulating oil and cooling water to enter light-splitting chamber and vacuum line, causes optical splitter and the inner severe contamination of vacuum pipe.After conventional clean and erasing is carried out to contaminated light-splitting chamber and vacuum pipe inner surface, along with light-splitting chamber temperature raises after instrument runs, under light-splitting chamber heated at constant temperature function and X-ray heat radiation effect, heavy oil residues, the steam that cannot directly remove at nook, optical splitter corner of collecting evaporates gradually, when contaminated samples causes stokehold molten iron sample to analyze there are unusual fluctuations in the light element detection such as silicon, p and s data, cannot meet the analysis testing requirement of stokehold.When the integrality of the equipment of guarantee is not disintegrated, first molecular sieve adsorption under employing heat radiation, again one after the other underbalance pulse gas flow purging method is carried out to 21 element passage optical splitters in light-splitting chamber, finally efficiently remove remaining insulating oil greasy dirt and steam rapidly, ensure that the X fluorescence spectrometer stable operation of matter inspection room.
Present invention accomplishes X fluorescence spectrometer beam splitting system contaminated after, when the integrality of the equipment of guarantee is not disintegrated, do not damage the space geometry position of beam splitting system electro-optical device and X-ray light path, efficiently, removing light-splitting chamber and vacuum pipe remain greasy dirt, steam up hill and dale, prevent measured sample from polluting, ensure that X fluorescence spectrometer analyzes the stable, reliable of data especially light element data.The inventive method wide accommodation, is applicable to, in 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, and these equivalent form of values fall within the application's appended claims limited range equally after having read above-mentioned instruction content of the present invention.
Claims (9)
1. the sweep-out method of the oil residues sewage vapour of an X fluorescence spectrometer vacuum light-splitting chamber, implement after carrying out cleaning erasing at the visual greasy dirt to X fluorescence spectrometer light-splitting chamber inner surface, steam, it is characterized in that comprising the following steps: heating to toast to light-splitting chamber makes the greasy dirt moisture remained evaporate; Molecular sieve is inserted molecular sieve Storage Box and make molecular sieve Storage Box enter light-splitting chamber and the oily water evaporated is divided adsorb; 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, removed by pulsating negative pressure sweep gas stream; And make by pulsating negative pressure purge air-flow blow away oil gas, steam discharge, 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, heating to toast to light-splitting chamber is unlatching X-ray and the heat radiation and the beam splitting system heated at constant temperature that maintain 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 spectrometer sample system size, 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, is provided with at the upper cover of described molecular sieve Storage Box the metal net mask being less than sieve particle order number.
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, the described oily water to evaporating divides the step of adsorbing to comprise the Storage Box that molecular sieve is housed is sent into X fluorescence spectrometer sample room by sample conveyer and carries out vacuum and take out in advance, and until vacuum normal after open light-splitting chamber optical gate, to make the molecular sieve in Storage Box, greasy dirt steam residual in light-splitting chamber and vapour molecule are effectively adsorbed.
6. the sweep-out method of the oil residues sewage vapour of X fluorescence spectrometer vacuum light-splitting chamber according to claim 5, it is characterized in that, molecular sieve in Storage Box carries out absorption 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, the passage of optical splitter is equipped with flow leakage mouth and installs Controlling solenoid valve additional, magnetic valve is connected with optical splitter by self-enclosed snap joint; Be in closed condition during magnetic valve no power always, make light-splitting chamber keep vacuum; Carrying out the step of X fluorescence spectrometer light-splitting chamber underbalance pulse gas flow purging greasy dirt, steam, is under the negative pressure state that maintain condition of high vacuum degree; When 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 with certain period frequency opening and closing, to form the optical splitter vacuum leak of light-splitting chamber, air pulse is formed with regulable control magnetic valve being opened to the cycle, to form underbalance pulse gas channel, thus form underbalance pulse purging air-flow.
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 blown away by pulsating negative pressure purging air-flow, steam are discharged to outside vavuum pump along vacuum pipe, to complete the removing of light-splitting chamber internal contamination.
9. the sweep-out method of the oil residues sewage vapour of the X fluorescence spectrometer vacuum light-splitting chamber according to 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; The vacuum leak amount of 30 ± 2Pa pressure is maintained in beam splitting system light-splitting chamber; Magnetic valve on-off action frequency is 0.2 ~ 1Hz.
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| US6667475B1 (en) * | 2003-01-08 | 2003-12-23 | Applied Materials, Inc. | Method and apparatus for cleaning an analytical instrument while operating the analytical instrument |
| CN101501817A (en) * | 2006-05-24 | 2009-08-05 | 阿尔卡特朗讯 | Method and device for removing pollution from a confined environment |
| CN102426164A (en) * | 2011-08-22 | 2012-04-25 | 东南大学 | Method for collecting and detecting material decomposition product or material transformation product under strong laser irradiation |
| CN202547998U (en) * | 2012-03-28 | 2012-11-21 | 上海北裕分析仪器有限公司 | Dehydration device for gaseous molecular absorption spectrometer |
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| US6667475B1 (en) * | 2003-01-08 | 2003-12-23 | Applied Materials, Inc. | Method and apparatus for cleaning an analytical instrument while operating the analytical instrument |
| CN101501817A (en) * | 2006-05-24 | 2009-08-05 | 阿尔卡特朗讯 | Method and device for removing pollution from a confined environment |
| CN102426164A (en) * | 2011-08-22 | 2012-04-25 | 东南大学 | Method for collecting and detecting material decomposition product or material transformation product under strong laser irradiation |
| CN202547998U (en) * | 2012-03-28 | 2012-11-21 | 上海北裕分析仪器有限公司 | Dehydration device for gaseous molecular absorption spectrometer |
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