CN102095713A - Online detection system of element content of industrial solid powder - Google Patents
Online detection system of element content of industrial solid powder Download PDFInfo
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- CN102095713A CN102095713A CN 201110062072 CN201110062072A CN102095713A CN 102095713 A CN102095713 A CN 102095713A CN 201110062072 CN201110062072 CN 201110062072 CN 201110062072 A CN201110062072 A CN 201110062072A CN 102095713 A CN102095713 A CN 102095713A
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Abstract
The invention relates to the technical field of industrial automatic measurement, and provides an online detection system of element content of industrial solid powder, aiming at solving the problems that the commonly used detection method cannot meet the requirement on fast and real-time online detection of contents of multiple elements in industrial solid powder, and the LIPS (Laser Induced Plasma Spectroscopy) technology is not applied to online detection of contents of elements in industrial solid powder successfully. The online detection system of element content of industrial solid powder comprises a sampling channel, a measurement room, an LIPS detector, a correction device, a sample discharging channel and a working gas generator for supplying gas for the whole detection system, and realizes application of the LIPS technology in online detection of elements in industrial solid powder by a reasonable and compact structure. Proved by experiments, the detection system provided by the invention can detect multiple elements in the industrial solid powder online rapidly in real time so as to guide workers to adjust the production condition in time to improve the production efficiency.
Description
Technical field
The present invention relates to industrial automatic measurement technology field, be specially a kind of industrial solid powder constituent content on-line detecting system.
Background technology
Industrial quantitative test to element in the pressed powder at present generally adopts chemical analysis, x ray fluorescence spectrometry and gamma-rays analytic approach to analyze.Yet chemical analysis complex procedures and length consuming time can't ensure the ageing of industrial On-line Control; X ray fluorescence spectrometry must dispose special sample making apparatus, and the detection elements kind is limited; The shortcoming of gamma-rays analytic approach is that testing result is subjected to the influence of high atomic number element (for example iron) content fluctuation bigger, the costing an arm and a leg of radioactive source, and its maintenance and daily nursing difficulty are also higher, and human body and surrounding enviroment are had radiation hazard.This shows that current various detection meanss are difficult to satisfy industrially carries out the requirement of quick online detection to the pressed powder constituent content, development has become the task of top priority based on the on-line detecting system of new technology.
Laser induced plasma spectrum (LIPS) technology, this is a kind of brand-new material element analytical technology, its principle be with a branch of high energy pulse laser focusing to sample, make the sample surfaces formation plasma of ablating rapidly, accurately know properties of samples and each constituent content by measuring this plasma fluorescence spectrum.LIPS is a kind of contactless real-time detection technique, and this technology also can be carried out long-range non-cpntact measurement except that having advantages such as accuracy of detection height, highly sensitive, speed is fast, multielement is measured simultaneously, be particularly suitable for being applied in the rugged surroundings.Therefore, this technology can be used as the optimal selection of industrial solid powder constituent content being carried out online detection, thereby the guiding work personnel in time adjust production status, to enhance productivity.Yet this technology does not also have relevant report in the successful Application of the online context of detection of industrial solid powder constituent content at present.
Summary of the invention
The present invention for solve detection means commonly used be difficult to satisfy to multiple constituent content in the industrial solid powder carry out requirement that quick real-time online detects and at present the LIPS technology also do not have the problem of successful Application in the online context of detection of industrial solid powder constituent content, a kind of industrial solid powder constituent content on-line detecting system based on the LIPS technology is provided.
The present invention is achieved by the following technical solutions: a kind of industrial solid powder constituent content on-line detecting system, the LIPS pick-up unit that comprises sampling channel, the measuring chamber that is connected with sampling channel, is connected with connecting pipe with measuring chamber, the means for correcting that is connected with sampling channel by ejector, the sample output passage that is connected with measuring chamber with sampling channel and the working gas generation device that working gas is provided for whole detection system; Described sampling channel comprises sampling conduit, ejector, automatically controlled T-valve, whirlwind powder collector, following tube cell, logical powder duct under the sampling conduit, on connect ejector, the lower channel of automatically controlled T-valve and ejector with connecting tube be connected, right passage is connected with connecting tube with the input port of whirlwind powder collector, the delivery outlet of whirlwind powder collector is connected with measuring chamber by tube cell down; Described measuring chamber top is connected with following tube cell, and the bottom is connected with sample output passage, and a side is connected with the LIPS pick-up unit with connecting pipe, and the connecting pipe two ends between described measuring chamber and the LIPS pick-up unit are provided with left window eyeglass and right window eyeglass; Described means for correcting is connected with the left passage of automatically controlled T-valve by ejector; Described sample output passage is made of gas exhaust duct and ejector, and the upper end of gas exhaust duct is connected with the exhausr port of whirlwind powder collector, the lower end communicates logical powder channel under the ejector with the connecting tube of ejector and measuring chamber bottom; The outlet of described working gas generation device (or air supply opening) by connecting tube respectively with the ejector that is connected with means for correcting, down the ejector in tube cell, measuring chamber, the sampling channel, the ejector in the sample output passage connect, wherein the outlet of working gas generation device with and the ejector that is connected of means for correcting between connecting tube on solenoid valve is housed, and on the connecting tube between the ejector in following tube cell, measuring chamber, the sample output passage valve is housed respectively, and on the connecting tube between the ejector in the sampling channel motorized valve is housed.
On the following tube cell that described sampling channel is connected with measuring chamber Vib. is housed, deposits at tube wall, cause line clogging to prevent powder.
On the connecting pipe between described measuring chamber and the LIPS pick-up unit solenoid valve and pressure transducer are housed; generally solenoid valve is in open state; light path can be passed through smoothly; when the measuring chamber internal pressure is elevated to a certain degree; high pressure breaks through the left window eyeglass; this moment, pressure transducer detected pressure signal; turn-off solenoid valve immediately (when specifically implementing; by the detected pressure signal of pressure transducer solenoid valve is turn-offed control; be that those skilled in the art realize easily; for example; the detected pressure signal of pressure transducer is transferred to the controller of a known configurations; when controller has been judged pressure signal; export a control signal and realize shutoff) solenoid valve; prevent that right window eyeglass from continuing to be destroyed by high pressure, and then cause the severe contamination of background gas, so solenoid valve and pressure transducer can play the effect of self-protection under emergency the LIPS pick-up unit.
Described working gas generation device comprises the well heater that is used for heated air, and working gas is heated to more than 100 ℃, prevents the water vapor condensation in pipeline in background gas and the working gas, causes the accumulation of powder and the obstruction of pipeline.
The outlet of described working gas generation device with and the ejector that is connected of means for correcting between connecting tube on the solenoid valve installed, its effect is: provide working gas by gauge tap for the ejector that is connected with means for correcting.
The valve of installing on the connecting tube between the outlet of described working gas generation device and the following tube cell, its effect is: constantly give down and charge into working gas with dilution background gas concentration in the tube cell, prevent that the elemental composition in the background gas from causing larger interference to the measured value of the element to be measured in the powder.
The valve of installing on the outlet of described working gas generation device and the connecting tube between the measuring chamber, its effect is: supply with working gas to the measuring chamber top and distribute with the air-flow that improves measuring chamber inside, thereby formation eddy current, make in the powdered sample whereabouts to be positioned at all the time on the laser focus point, reduce the pollution of powder simultaneously the left window eyeglass.
The valve of installing on the outlet of described working gas generation device and the connecting tube between the ejector in the sample output passage, its effect is: this ejector that is controlled to be by switch provides working gas.
The motorized valve of installing on the outlet of described working gas generation device and the connecting tube between the ejector in the sampling channel, its effect is: when the LIPS pick-up unit detects signal weaker, manually or automatically transfer the aperture (how realizing that automatic adjusting also is that those skilled in the art realize easily) of big motorized valve, increase acquisition rate by the flow that increases working gas, to guarantee to have enough LIPS signal intensities to powder.
During detection, at first the powder in the powder channel is sampled by sampling conduit, powder of being gathered and background gas are by after with pressurized air being the controlled ejector of working gas, flow, pass through automatically controlled T-valve again (at this moment, the left passage of automatically controlled T-valve turn-offs, right passage is open-minded with lower channel) enter and carry out the gas powder in the whirlwind powder collector and separate, break away from the background gas powder away from the gas exhaust duct of whirlwind powder collector top, under the suction of the ejector of sample output passage, sent back to powder channel through sample output passage; Isolated powders is in whirlwind powder collector bottom, by following tube cell, enter measuring chamber under the effect of Vib., by the LIPS pick-up unit composition of powdered sample is carried out express-analysis, these powdered samples are sent back to powder channel under the effect of the ejector of sample output passage simultaneously.The LIPS pick-up unit uses pulsed laser as excitaton source, connecting pipe and the window eyeglass at two ends thereof of output laser pulse between measuring chamber and LIPS pick-up unit focuses on powdered sample surface in the measuring chamber, focusing on position formation plasma, the partial radiation spectrum of this plasma imports spectrometer into, the fluorescence spectrum of spectrometer article on plasma body detects, institute's photometry spectrum data draw the measured value of constituent content to be measured in the powdered sample by the data processing of microcomputer.The known standard powdered sample of constituent content to be measured is housed in the means for correcting, is used for this on-line detecting system is carried out regular calibration.Timing, the lower channel of automatically controlled T-valve turn-offs, left side passage and right passage are open-minded, and solenoid valve is open-minded, under the suction of ejector, standard model is inhaled into the whirlwind powder collector with working gas, after the separation of gas powder, standard model enters measuring chamber, after detecting through the LIPS pick-up unit, sent back in the powder channel under the effect of the ejector of sample output passage, the LIPS pick-up unit is proofreaied and correct the analysis software calibration equation according to testing result.The working gas generation device then provides required working gas for this on-line detecting system.
Compared with prior art, the present invention is reasonable with it, compact structure realizes that the LIPS technology is in industrial application to the online context of detection of pressed powder constituent content, through evidence, detection system of the present invention can be carried out quick real-time online to the industrial solid powder especially flying dust multiple element of (claiming flyash again) (comprising silicon, iron, aluminium, calcium, magnesium, sodium, potassium, sulphur and various trace elements etc.) and be detected, thereby the guiding work personnel in time adjust production status, to enhance productivity.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the structural representation of measuring chamber among the present invention and LIPS pick-up unit.
1-sampling conduit among the figure; The 2-working gas; The 3-ejector; The automatically controlled T-valve of 4-; 5-whirlwind powder collector; The 6-gas exhaust duct; The 7-ejector; Tube cell under the 8-; The 9-Vib.; The 10-measuring chamber; The 11-LIPS pick-up unit; The 12-means for correcting; The 13-solenoid valve; The 14-ejector; 15-left window eyeglass; The right window eyeglass of 16-; The 17-solenoid valve; The 18-pressure transducer; The 19-air compressor; The 20-reduction valve; The 21-tensimeter; The 22-well heater; The 23-motorized valve; The 24-valve; The 25-valve; The 26-function signal generator; The 27-spectrometer; The 28-laser instrument; The vertical convex lens of 29-; The 30-plasma; The last plane mirror of 31-; 32-lower plane catoptron; The horizontal convex lens of 33-; 34-total silicon optical fiber; The 35-USB data line; The 36-microcomputer; The 37-valve.
Embodiment
As shown in drawings, a kind of industrial solid powder constituent content on-line detecting system, the measuring chamber 10 that comprise sampling channel, is connected, the LIPS pick-up unit 11 that is connected with connecting pipe with measuring chamber 10, the means for correcting 12 that is connected with sampling channel by ejector 14, the sample output passage that is connected with measuring chamber 10 with sampling channel and the working gas generation device that working gas 2 is provided for whole detection system with sampling channel; Described sampling channel comprises sampling conduit 1, ejector 3, automatically controlled T-valve 4, whirlwind powder collector 5, following tube cell 8,1 time logical powder duct of sampling conduit, on connect ejector 3, the lower channel of automatically controlled T-valve 4 and ejector 3 with connecting tube be connected, right passage is connected with connecting tube with the input port of whirlwind powder collector 5, the delivery outlet of whirlwind powder collector 5 is connected with measuring chamber 10 by tube cell 8 down; Described measuring chamber 10 tops are connected with following tube cell 8, and the bottom is connected with sample output passage, and a side is connected with LIPS pick-up unit 11 with connecting pipe, and the connecting pipe two ends between described measuring chamber and the LIPS pick-up unit are provided with left window eyeglass 15 and right window eyeglass 16; Described means for correcting 12 is connected with the left passage of automatically controlled T-valve 4 by ejector 14; Described sample output passage is made of gas exhaust duct 6 and ejector 7, and gas exhaust duct 6 upper ends are connected with the exhausr port of whirlwind powder collector 5, the lower end communicates 7 times logical powder channels of ejector with the connecting tube of ejector 7 and measuring chamber 10 bottoms; The outlet of described working gas generation device (or air supply opening) by connecting tube respectively with the ejector 14 that is connected with means for correcting 12, following tube cell 8, measuring chamber 10, ejector 3 in the sampling channel, ejector 7 in the sample output passage connects, wherein the outlet of working gas generation device with and the ejector 14 that is connected of means for correcting 12 between connecting tube on solenoid valve 13 is housed, with following tube cell 8, measuring chamber 10, on the connecting tube between the ejector 7 in the sample output passage valve 24 is housed respectively, valve 25, valve 37, and motorized valve 23 is housed on the connecting tube between the ejector in the sampling channel 3.
On described sampling channel and the following tube cell that measuring chamber 10 is connected Vib. 9 is housed, deposits at tube wall, cause line clogging to prevent powder.
Described working gas generation device comprises the well heater 22 that is used for heated air, and working gas 2 is heated to more than 100 ℃, prevents the water vapor condensation in pipeline in background gas and the working gas 2, causes the accumulation of powder and the obstruction of pipeline.
The outlet of described working gas generation device with and the ejector 14 that is connected of means for correcting 12 between connecting tube on the solenoid valve 13 installed, its effect is: provide working gas 2 by gauge tap for the ejector 14 that is connected with means for correcting 12.
The valve of installing on the connecting tube between the outlet of described working gas generation device and the following tube cell 8 24, its effect is: constantly give down and charge into working gas 2 with dilution background gas concentration in the tube cell 8, prevent that the elemental composition in the background gas from causing larger interference to the measured value of the element to be measured in the powder.
The valve of installing on the connecting tube between the outlet of described working gas generation device and the measuring chamber 10 25, its effect is: supply with working gas 2 to measuring chamber 10 tops and distribute with the air-flow that improves measuring chamber 10 inside, thereby formation eddy current, make in the powdered sample whereabouts to be positioned at all the time on the laser focus point, reduce the pollution of powder simultaneously left window eyeglass 15.
The valve of installing on the outlet of described working gas generation device and the connecting tube between the ejector in the sample output passage 7 37, its effect is: this ejector 7 that is controlled to be by switch provides working gas 2.
The motorized valve of installing on the outlet of described working gas generation device and the connecting tube between the ejector in the sampling channel 3 23, its effect is: when LIPS pick-up unit 11 detects signal weaker, manually or automatically transfer the aperture of big motorized valve 23, increase acquisition rate by the flow that increases working gas 2, to guarantee to have enough LIPS signal intensities to powder.
During detection, at first sample by the powder in 1 pair of powder channel of sampling conduit, powder of being gathered and background gas are by after with pressurized air being the controlled ejector 3 of working gas 2, flow, pass through automatically controlled T-valve 4(more at this moment, the left passage of automatically controlled T-valve 4 turn-offs, right passage is open-minded with lower channel) enter and carry out the gas powder in the whirlwind powder collector 5 and separate, break away from the background gas powder away from the gas exhaust duct 6 of whirlwind powder collector 5 tops, under the suction of the ejector 7 of sample output passage, sent back to powder channel through sample output passage; Isolated powders is in whirlwind powder collector 5 bottoms, by following tube cell 8, under the effect of Vib. 9, enter measuring chamber 10, composition by 11 pairs of powdered samples of LIPS pick-up unit carries out express-analysis, and these powdered samples are sent back to powder channel under the effect of the ejector 7 of sample output passage simultaneously.The LIPS pick-up unit can draw the measured value of constituent content to be measured in the powdered sample fast through check and analysis.The known standard powdered sample of constituent content to be measured is housed in the means for correcting 12, is used for this on-line detecting system is carried out regular calibration (for example 4-5 week once).Timing, the lower channel of automatically controlled T-valve 4 turn-offs, left side passage and right passage are open-minded, and solenoid valve 13 is open-minded, under the suction of ejector 14, standard model is inhaled into whirlwind powder collector 5 with working gas 2, after the separation of gas powder, standard model enters measuring chamber 10, after detecting through LIPS pick-up unit 11, sent back in the powder channel under the effect of the ejector 7 of sample output passage, LIPS pick-up unit 11 is proofreaied and correct the analysis software calibration equation according to testing result.The working gas generation device provides required working gas 2 for this on-line detecting system.
The LIPS pick-up unit of realizing the online testing goal of above-mentioned industrial solid powder constituent content is existing ripe known products.Described LIPS pick-up unit 11 is usually by function signal generator 26, spectrometer 27, laser instrument 28 and microcomputer 36 constitute, the signal output part of function signal generator 26 is connected with the signal input part of spectrometer 27, the signal output part of spectrometer 27 is connected with the signal input part of laser instrument 28, the laser of laser instrument 28 send mouthful and the spectra collection mouth of spectrometer 27 between be respectively equipped with emitting light path and input path, emitting light path comprise be arranged in the LIPS pick-up unit 11 with laser send mouth over against vertical convex lens 29 and aforesaid two be vertically installed between LIPS pick-up unit 11 and the measuring chamber 10 the connecting pipe two ends and with the left window eyeglass 15 and the right window eyeglass 16 of vertical convex lens 29 deads in line, input path comprises being arranged at makes incident light spectrum converge to the last plane mirror 31 of total silicon optical fiber in the LIPS pick-up unit 11, lower plane catoptron 32, horizontal convex lens 33, wherein go up plane mirror 31 and lower plane catoptron 32 be set in parallel in the LIPS pick-up unit 11 and minute surface and vertical window over against being 45 °, horizontal convex lens 33 are arranged at and are positioned at two plane mirrors below in the LIPS pick-up unit, and the data output end of spectrometer 27 is connected with the data input pin of microcomputer 36 by usb data line 35.
During detection, function signal generator 26 triggers spectrometer 27 with the TTL square-wave signal of characteristic frequency; Spectrometer 27 is the rising edge of each the TTL square-wave signal time zero as this time measurement, and responds a same frequency spike pulse signal triggering laser instrument 28; After the shoot laser of laser instrument 28 converges through vertical convex lens 29, incide the powdered sample surface through right window eyeglass 16 and left window eyeglass 15 respectively, focusing on position formation plasma 30, after the reflection of the partial radiation light of this plasma 30 through last plane mirror 31 and lower plane catoptron 32, converge to total silicon optical fiber 34 by horizontal convex lens 33 again, import spectrometer 27 into by total silicon optical fiber 34; Spectrometer 27 according to preset delay time and integral time the article on plasma body fluorescence spectrum (220nm-700nm) detect, institute's photometry spectrum data reach microcomputer 36 by usb data line 35 and carry out data processing, draw the measured value of constituent content to be measured in the powdered sample.
Described function signal generator 26, spectrometer 27, laser instrument 28 and microcomputer 36 are existing product, and described spectrometer 27 adopts vacuum ultraviolet spectrometer, and laser instrument 28 adopts the Nd:YAG laser instrument.
The working gas generation device is existing mature technology, is that one of ordinary skill in the art realize easily.In this embodiment, the working gas generation device also comprises air compressor 19, dispose the pressure that reduction valve 20 and tensimeter 21(are used for monitoring gas simultaneously), its workflow is: at first compressed by 19 pairs of working gass of air compressor, then after reduction valve 20 decompressions, enter well heater 22, working gas 2 is heated to more than 100 ℃, supply with whole detection system by each pipeline.
Claims (6)
1. industrial solid powder constituent content on-line detecting system is characterized in that: the measuring chamber that comprise sampling channel, is connected with sampling channel (10), the LIPS pick-up unit (11) that is connected with connecting pipe with measuring chamber (10), the means for correcting (12) that is connected with sampling channel by ejector (14), the sample output passage that is connected with measuring chamber (10) with sampling channel and the working gas generation device that working gas (2) is provided for whole detection system; Described sampling channel comprises sampling conduit (1), ejector (3), automatically controlled T-valve (4), whirlwind powder collector (5), following tube cell (8), sampling conduit (1) down logical powder duct, on connect ejector (3), the lower channel of automatically controlled T-valve (4) and ejector (3) with connecting tube be connected, right passage is connected with connecting tube with the input port of whirlwind powder collector (5), the delivery outlet of whirlwind powder collector (5) is connected with measuring chamber (10) by tube cell (8) down; Described measuring chamber (10) top is connected with following tube cell (8), the bottom is connected with sample output passage, one side is connected with LIPS pick-up unit (11) with connecting pipe, and the connecting pipe two ends between described measuring chamber and the LIPS pick-up unit are provided with left window eyeglass 15 and right window eyeglass 16; Described means for correcting (12) is connected with the left passage of automatically controlled T-valve (4) by ejector (14); Described sample output passage is made of gas exhaust duct (6) and ejector (7), gas exhaust duct (6) upper end is connected with the exhausr port of whirlwind powder collector (5), the lower end communicates with the connecting tube of ejector (7) and measuring chamber (10) bottom, and ejector (7) is logical powder channel down; The outlet of described working gas generation device by connecting tube respectively with the ejector (14) that is connected with means for correcting (12), following tube cell (8), measuring chamber (10), ejector in the sampling channel (3), ejector in the sample output passage (7) connects, wherein the outlet of working gas generation device with and the ejector (14) that is connected of means for correcting (12) between connecting tube on solenoid valve (13) is housed, respectively with following tube cell (8), measuring chamber (10), valve (24) is housed on the connecting tube between the ejector in the sample output passage (7), valve (25), valve (37), and motorized valve (23) is housed on the connecting tube between the ejector in the sampling channel (3).
2. industrial solid powder constituent content on-line detecting system according to claim 1 is characterized in that: on described sampling channel and the following tube cell (8) that measuring chamber (10) is connected Vib. (9) is housed.
3. industrial solid powder constituent content on-line detecting system according to claim 1 and 2 is characterized in that: solenoid valve (17) and pressure transducer (18) are housed on the connecting pipe of described measuring chamber (10) and LIPS pick-up unit (11).
4. industrial solid powder constituent content on-line detecting system according to claim 1 and 2 is characterized in that: described working gas generation device comprises the well heater (22) that is used for heating work gas.
5. industrial solid powder constituent content on-line detecting system according to claim 3 is characterized in that: described working gas generation device comprises the well heater (22) that is used for heating work gas.
6. industrial solid powder constituent content on-line detecting system according to claim 4, it is characterized in that: described working gas generation device also comprises air compressor (19), disposes reduction valve (20) and tensimeter (21) simultaneously.
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CN104363689B (en) * | 2014-11-18 | 2017-02-08 | 聚光科技(杭州)股份有限公司 | Analysis power source and mineral powder analysis device and method |
CN105241851A (en) * | 2015-09-25 | 2016-01-13 | 清华大学 | Solid powder online detection apparatus based on laser-induced breakdown spectroscopy technology |
CN105136752A (en) * | 2015-09-25 | 2015-12-09 | 清华大学 | Online powder detecting device and measuring method based on laser-induced breakdown spectroscopy |
CN105136752B (en) * | 2015-09-25 | 2018-04-10 | 清华大学 | Online powder detection means and its measuring method based on LIBS |
CN105445240A (en) * | 2016-01-11 | 2016-03-30 | 中国神华能源股份有限公司 | Monitoring system of process of producing aluminum oxide through coal ash |
CN105731076A (en) * | 2016-03-23 | 2016-07-06 | 郭家彤 | Pneumatic conveying pipeline for gas-solid two-phase flow |
CN107664590A (en) * | 2017-11-01 | 2018-02-06 | 江苏啸峰环保科技股份有限公司 | Flue particulate matter isokinetic sampling and Constant Current Control System and its preprocess method based on jet modulation |
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CN109521002A (en) * | 2018-11-29 | 2019-03-26 | 华南理工大学 | A kind of fuel characteristic measurement method of solid fuel particle stream |
CN109521002B (en) * | 2018-11-29 | 2021-05-14 | 华南理工大学 | Fuel characteristic measuring method for solid fuel particle flow |
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