CN103278519B - A kind of online sulfur-bearing analytical equipment - Google Patents
A kind of online sulfur-bearing analytical equipment Download PDFInfo
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- CN103278519B CN103278519B CN201310181369.2A CN201310181369A CN103278519B CN 103278519 B CN103278519 B CN 103278519B CN 201310181369 A CN201310181369 A CN 201310181369A CN 103278519 B CN103278519 B CN 103278519B
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Abstract
The invention discloses a kind of online sulfur-bearing analytical equipment, comprise measuring channel, X-ray signal generator, detector, pressure transducer, protection cavity and control module; Protection cavity is fixedly connected with measuring channel; X-ray signal generator, detector, pressure transducer are all inlaid on protection cavity; Measuring channel is 120 ~ 170 degree of bend pipes, and the duct wall of bending outer arc is provided with detection window; X-ray signal generator and detector are at the homonymy of detection window; Control module is arranged on the outside of protection cavity, and it is connected with pressure transducer with detector respectively.The present invention directly tests, without the need to tracing steam sample in pipeline; Adopt the SDD detector of Novel belt thermoelectric cooling, without the need to heat eliminating medium; Sealing flame proof, purges explosion-proof without the need to malleation; Device is contactless with sample in measuring process, has an impact hardly to fluids within pipes state, under high condensation point crude oil sample, high flow condition, still can keep high accuracy.
Description
Technical field
The present invention relates to a kind of analytical instrument, particularly relate to a kind of online sulfur-bearing analytical equipment.
Background technology
At present, international community has become environmental protection emphasis to the restriction management and control of sulfur content in petrochemicals especially oils product (as gasoline, diesel oil, lubrication wet goods).As containing too high sulphur in fuel oil, easily with the air generation oxidation reaction be dissolved in oil, reduce the stability of fuel oil.In oil fuel process, sulphur also can reduce the conversion of toxic discharge, causes engine fuel system to corrode.In addition, the sulphuric dioxide also severe contamination physical environment of combustion of sulfur generation.As can be seen here, Sulfur content in Fuel Oil content of controlling well is very important, and various countries are also all improving petrol and diesel oil oil product standard and accelerating oil product upgrade job.Sulfur content is an important index in crude oil and products thereof, is also must the strict index controlled in petroleum products and conversion of exhaust gas thereof.Sulfur content on-line monitoring is all significant to improving petroleum refining process and improving oil quality.
The object of Sulfur Analysis monitoring comprises three aspects: the gas of crude oil and product oil, sulfur recovery process, industrial smoke and air.The method that sulphur detects has following several usually: 1. coulometric titration (US2008250846A1) 2. lead acetate method 3. oscilloscopic polarography 4. chemoluminescence method 5. ultraviolet fluorescence method 6.X ray fluorescence (US4577338).Wherein, Coulomb equation, lead acetate method, chemoluminescence method and ultraviolet fluorescence method all need to transform element sulphur in sample, are equipped with electrolytic solution, reaction chamber, acetic acid. g., lead tape, ozone, ultraviolet light etc. and carry out quantitatively to transformation substance, thus determine sulfur content.Oscilloscopic polarography is that the dissufion current that the redox reaction utilizing measured matter on electrode produces is analyzed, and needs electrolyte in process.The operation of above method is comparatively complicated tediously long, and often relates to the step that pyroreaction, burning, hydrogenation etc. be unfavorable for petrochemical complex production scene anti-explosion safety.
X-ray fluorescence method (X-ray Fluorescence Spectrometer is called for short XRF) is a kind of non-contacting non-destructive measuring method, and directly measure sample, the sample measured does not change.Comparatively speaking, other method needs and the step such as oxygen, ozone or hydrogen reaction, burning, sample transmission, dilution, and flow process is complicated, causes the many factors of measuring error.XRF method and testing tool thereof are due to simple and reliable, and disturbing factor is little, easy to operate, and detection limit is very low, and (theory can reach 10
-15gram), become in petrochemical iy produced process a kind of main oil product elemental analysis method used.X-ray fluorescence method is as a kind of material composition characterization method of maturation, be applied in multiple industry field, it can measure multiple element composition in oil product, can detect the light element that magnesium sulphur is such, can detect again the heavy element as iron, cobalt, nickel, plumbous even uranium.
The off-line static test equipment of current XRF is a lot, all there are the XRF analysis device (JP1214748A of independent brand in domestic and international Duo Jia experimental analysis equipment manufacturers, CN201020675273, CN200920068390, US2004213373A1), but the manufacturer that successfully can make the online element sulphur analyser that petrochemicals are produced and detected is also few, mainly contain the SLFA-2800 of Japanese Horiba(hole field in the market), DKK-TOA, U.S. XOS(Sindie Online and TurnKey series), Hach (SAC-200 and HSAC-2000) company.These online equipment are in measuring process, and are all the analytic units over long distances sample in pipeline being incorporated into equipment, Configuration Control Unit controls power supply, X source and detector, each valve.For ensureing sample flow, need configuration low pressure vapours companion heat; For each unit and entirety reach requirement of explosion proof, need to consume gas and carry out malleation purging; Meanwhile, for ensureing that detector normally works, logical chilled water or refrigerating gas is needed.Multichannel unit be connected with pipeline make overall volume and weight large.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, provides a kind of nothing companion heat, without the need to heat eliminating medium, gas positive pressure purges, take up space little online sulfur-bearing analytical equipment without the need to consuming.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of online sulfur-bearing analytical equipment, described device comprises measuring channel, X-ray signal generator, detector, pressure transducer, protection cavity and control module; Described protection cavity is fixedly connected with measuring channel; Described X-ray signal generator, detector, pressure transducer are all inlaid on protection cavity; Described measuring channel, for being 120 ~ 170 degree of bend pipes, the duct wall of bending outer arc is provided with detection window; Described detection window is the small perforate of crooked pipeline side tangent plane; Described X-ray signal generator and detector are at the homonymy of detection window; Described control module is arranged on the outside of protection cavity, and it is connected with pressure transducer with detector respectively.
Wherein measuring channel angle is too little, pipe bending get Tai Gao, and during process window, accuracy requirement is too high; Angle is too large, and machined surface is oversize, causes working (machining) efficiency obviously to decline, and is convenient to make within the scope of 120 ~ 170 degree.
Control module is control circuit board, and connection signal generator controls its switch, monitors its running parameter; Bonding pressure sensor gathers its monitor signal and by digital output modul sample introduction valve, also can connect other purposes sensor in addition and gather the parameters such as humiture, control other device, transmit different systems signal etc.It and computer direct connect in succession, and operating personnel can each unit of Monitoring and Controlling by control panel.
Pressure transducer Real-Time Monitoring protection cavity internal pressure is with proterctive equipment safety, and when window is revealed, when pressure exceeds standard, the feedback signal of sensor can cut off sample introduction valve to ensure safety by control module.
Further, above-mentioned online sulfur-bearing analytical equipment, described detection window is circular hole, and circular hole is of a size of mm rank, and its diameter is less than 5mm.
Further, above-mentioned online sulfur-bearing analytical equipment, described detection window is elliptical aperture, and elliptical aperture is of a size of mm rank, and elliptical aperture major axis is 4 ~ 5mm, and minor axis is 2 ~ 4mm.
Because the less compressive resistance in aperture is higher, in order to meet pipeline compressive resistance, major and minor axis size can not more than 5mm.Consider X-ray signal focal spot size simultaneously, can not do too small, so general size is in mm rank.
Further, above-mentioned online sulfur-bearing analytical equipment, described elliptical aperture major axis is 4.5mm, and minor axis is 2mm.
Further, above-mentioned online sulfur-bearing analytical equipment, the material of described detection window is the polyurethane film that 20 ~ 100um is thick.
Further, above-mentioned online sulfur-bearing analytical equipment, the material of described detection window is the polyurethane film that 50um is thick.
Further, above-mentioned online sulfur-bearing analytical equipment, described X-ray signal generator is X-ray tube.
Further, above-mentioned online sulfur-bearing analytical equipment, described detector is silicon drifting detector.
The products such as in this device, X-ray signal generator can select KEWEI200G, Amptek Mini-X, Moxtek Magnum X-ray Source; The available model of pressure transducer is a lot, as long as monitoring pressure difference all can adopt in principle at MPa rank, this device of sensor that size is suitable.The force value that device is collected by control circuit board detected pressures sensor, when exceeding secure threshold, control panel provides switch order, by the sample introduction valve closing of testing conduit front end, thus ensures device security.
Adopt X-ray tube as sender unit, after power-off, just no longer there is harmfulness.
Further, above-mentioned online sulfur-bearing analytical equipment, described protection cavity inner surface is provided with sheet lead; The junction of described protection cavity and X-ray signal generator, detector, pressure transducer is provided with mechanical sealing member.
Mechanical sealing member is the gland fixing with trip bolt comprising O type circle, phenyl tetrafluoride pad, is used for X signal source, detector, pressure transducer sealing to be fixed on effect protection cavity reaching shielding leakproof.
Sheet lead is utilized to carry out radiation protection to ray channel.
Further, above-mentioned online sulfur-bearing analytical equipment, described measuring channel, X-ray signal generator, detector, pressure transducer, protection cavity and control module are all in a flameproof cabinet.
Described anti-explosion box body material uses stainless steel usually, and internal components is connected with outside by explosion-proof wiring hole.
Device of the present invention adopts sample measuring channel to bend, carry out small perforate (mm rank) mode to pipeline outer arc to measure, small size window design both ensure that compressive resistance, achieved again on-line checkingi truly, entered other device without the need to introduction pipe inner sample.Select X source and the high-performance novel SDD detector of function i ntegration, compact, tightly depend on detection cavity and the control module of pipeline integrated design explosion-proof leakage-proof, single unit system concision and compact and safe and reliable.System completely instant on-line checkingi pipe interior flowing sample, no longer needs to be equipped with tracing steam and ensures mobility to sample heating; Integrated configuration design can realize the design of mechanical seal flame proof, and radiation protection, anti-leak cavity and sensing, control module are all built in flameproof cabinet, and undesirable gas malleation purges explosion-proof.
Apparatus design of the present invention for directly to test sample in pipeline, without the need to accompanying heat steam; Adopting the SDD detector of Novel belt thermoelectric cooling, be suitable for 0 ~ 50 DEG C of environment temperature, cooling without the need to additionally leading to heat eliminating medium.The design of sealing flame proof, purges explosion-proof without the need to malleation; Without the need to sample changeover and pre-service, without heating arrangement, do not consume gas.And adopting control and the data processing software of autonomous Design, measuring process can adopt single-point, continuous, interval various ways, and automatic record after setting, without the need to human attendance.And remote transmitting device can be adopted to carry out Long-distance Control, data acquisition and sample demarcation etc. at master-control room to pick-up unit.Device is contactless with sample in measuring process, has an impact hardly to fluids within pipes state, under high condensation point crude oil sample, high flow condition, still can keep high accuracy.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for instructions, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the structural representation of a kind of online sulfur-bearing analytical equipment of the present invention;
Fig. 2 is the structural representation of the detection window of a kind of online sulfur-bearing analytical equipment of the present invention;
Fig. 3 is the partial enlarged drawing of the detection window of a kind of online sulfur-bearing analytical equipment of the present invention.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1
As Figure 1-3, a kind of online sulfur-bearing analytical equipment, comprises measuring channel 5, X-ray signal generator 1, detector 2, pressure transducer 3, protection cavity 4 and control module.
Protection cavity 4 is fixedly connected with measuring channel 5, and X-ray signal generator 1, detector 2, pressure transducer 3 are all inlaid on protection cavity 4.
Measuring channel 5, for being 120 ~ 170 degree of bend pipes, the duct wall of bending outer arc is provided with detection window 6.Detection window is the small perforate of crooked pipeline side tangent plane.
X-ray signal generator 1 and detector 2 are at the homonymy of detecting window 6 mouthfuls, and control module is arranged on the outside in protection chamber 4, and it is connected with pressure transducer 3 with detector 2 respectively.
Detection window is circular hole, and circular hole is of a size of mm rank, and its diameter is less than 5mm.
Detection window also can be elliptical aperture, and circular hole is of a size of mm rank, and elliptical aperture major axis is 4 ~ 5mm, and minor axis is 2 ~ 4mm.
The material of detection window is the polyurethane film that 20 ~ 100um is thick.
Preferably, X-ray signal generator 1 is X-ray tube.
Preferably, detector 2 is silicon drifting detector.
Preferably, protection cavity inner surface is provided with sheet lead 8, and protection cavity 4 is provided with mechanical sealing member 7 with the junction of X-ray signal generator 1, detector 2, pressure transducer 3.
Preferably, measuring channel 5, X-ray signal generator 1, detector 2, pressure transducer 3, protection cavity 4 and control module are all in a flameproof cabinet.
In the present embodiment, measuring channel is designed in 150 degree bend pipes, and the polyurethane film of employing 50um makes window material, the elliptical aperture major axis 4.5mm of detection window 6, minor axis 2mm, withstand voltagely reaches 4MPa.
Principle of work of the present invention: test sample flows through detection window 6 through measuring channel 5, by outlet return to former pipeline.Detection window 6 becomes an elliptical aperture to be formed by being tangentially machined to duct wall to the pipeline outer arc of measuring channel naturally.X-ray signal generator 1 launches energy 3 ~ 50KeV, the X-ray beam of diameter 1 ~ 2mm, and through window 6 excited sample, in sample, element sulphur sends that energy is respectively 2.31, the K of 2.468KeV
α, K
βdeng fluorescent x ray, received by silicon drifting detector 2, become element sulphur fluorogram through Treatment Analysis and export (can occur the characteristic fluorescence spectrum of multiple element in experiment) simultaneously, the intensity (i.e. integral area) of element sulphur characteristic peak is directly proportional to element sulphur concentration in sample.By demarcating and calculate the photoluminescence spectrum intensity of element sulphur, the sulphur concentration in sample can be drawn.
Embodiment 2
In the present embodiment, in the present embodiment, measuring channel is designed in 120 degree bend pipes, and the polyurethane film of employing 20um makes window material, elliptical aperture major axis 4mm, minor axis 2mm, withstand voltagely reaches 4MPa.
Other guide is identical with enforcement 1.
Embodiment 3
In the present embodiment, in the present embodiment, measuring channel is designed in 170 degree bend pipes, and the polyurethane film of employing 100um makes window material, elliptical aperture major axis 5mm, minor axis 2.5mm, withstand voltagely reaches 3MPa.
Other guide is identical with enforcement 1.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. an online sulfur-bearing analytical equipment, is characterized in that: described device comprises measuring channel, X-ray signal generator, detector, pressure transducer, protection cavity and control module; Described protection cavity is fixedly connected with measuring channel; Described X-ray signal generator, detector, pressure transducer are all inlaid on protection cavity; Described measuring channel, for being 120 ~ 170 degree of bend pipes, the duct wall of bending outer arc is provided with detection window; Described detection window is the small perforate of crooked pipeline side tangent plane; Described X-ray signal generator and detector are at the homonymy of detection window; Described control module is arranged on the outside of protection cavity, it is connected with pressure transducer with detector respectively, described detector is silicon drifting detector, and described measuring channel, X-ray signal generator, detector, pressure transducer, protection cavity and control module are all in a flameproof cabinet.
2. online sulfur-bearing analytical equipment according to claim 1, is characterized in that: described detection window is circular hole, and circular hole is of a size of mm rank, and its diameter is less than 5mm.
3. online sulfur-bearing analytical equipment according to claim 1, it is characterized in that: described detection window is elliptical aperture, and elliptical aperture is of a size of mm rank, elliptical aperture major axis is 4 ~ 5mm, and minor axis is 2 ~ 4mm.
4. online sulfur-bearing analytical equipment according to claim 3, it is characterized in that: described elliptical aperture major axis is 4.5mm, minor axis is 2mm.
5. the online sulfur-bearing analytical equipment according to claim 1,2,3 or 4, is characterized in that: the material of described detection window is the polyurethane film that 20 ~ 100um is thick.
6. online sulfur-bearing analytical equipment according to claim 5, is characterized in that: the material of described detection window is the polyurethane film that 50um is thick.
7. the online sulfur-bearing analytical equipment according to claim 1,2,3 or 4, is characterized in that: described X-ray signal generator is X-ray tube.
8. online sulfur-bearing analytical equipment according to claim 1, is characterized in that: described protection cavity inner surface is provided with sheet lead; The junction of described protection cavity and X-ray signal generator, detector, pressure transducer is provided with mechanical sealing member.
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| CN201310181369.2A CN103278519B (en) | 2013-05-16 | 2013-05-16 | A kind of online sulfur-bearing analytical equipment |
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| CN201310181369.2A CN103278519B (en) | 2013-05-16 | 2013-05-16 | A kind of online sulfur-bearing analytical equipment |
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| CN103278519A CN103278519A (en) | 2013-09-04 |
| CN103278519B true CN103278519B (en) | 2015-09-30 |
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| CN103837559B (en) * | 2014-02-26 | 2016-04-27 | 南京航空航天大学 | The quick sulphur meter of many target scans formula |
| CN107607569A (en) * | 2017-09-30 | 2018-01-19 | 陈勇 | Online analysis of total sulfur equipment |
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| FR2741155B1 (en) * | 1995-11-15 | 1997-12-05 | Commissariat Energie Atomique | APPARATUS FOR ANALYZING A FLUORESCENCE X SOLUTION |
| US8625737B2 (en) * | 2010-02-09 | 2014-01-07 | X-Ray Optical Systems, Inc. | Sample module with sample stream supported and spaced from window, for X-ray analysis system |
| US9057685B2 (en) * | 2011-08-15 | 2015-06-16 | X-Ray Optical Systems, Inc. | Sample viscosity and flow control for heavy samples, and X-ray analysis applications thereof |
| CN203275325U (en) * | 2013-05-16 | 2013-11-06 | 北京乾达源科技有限公司 | Online sulfur content analysis device |
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