EP1530714A1 - Analyse par fluorescence x a l'aide d'un guide d'ondes relie a la source et au detecteur - Google Patents

Analyse par fluorescence x a l'aide d'un guide d'ondes relie a la source et au detecteur

Info

Publication number
EP1530714A1
EP1530714A1 EP03763588A EP03763588A EP1530714A1 EP 1530714 A1 EP1530714 A1 EP 1530714A1 EP 03763588 A EP03763588 A EP 03763588A EP 03763588 A EP03763588 A EP 03763588A EP 1530714 A1 EP1530714 A1 EP 1530714A1
Authority
EP
European Patent Office
Prior art keywords
ray
substance
conductor
radiation
source
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP03763588A
Other languages
German (de)
English (en)
Inventor
Elisabeth Katz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of EP1530714A1 publication Critical patent/EP1530714A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/06—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diffraction, refraction or reflection, e.g. monochromators
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076—X-ray fluorescence

Definitions

  • the invention relates to a device for performing an online element analysis according to the preamble of claim 1.
  • X-ray fluorescence is a measurement method frequently used in science and industry by means of which the proportion of certain elements in a sample can be measured.
  • the sample is irradiated with X-rays in order to excite certain electronic transitions of the elements of interest.
  • 0 is mostly the K ⁇ transition.
  • the recombination of the excited transitions takes place in some cases with radiation, the energy quanta emitted here having a characteristic value for this element.
  • the energy of the emitted photon is generally between 1 and 30 keV. At the lower end of this energy range in particular, the emitted soft X-rays have only a very short range in solids or air, so that there are considerable measurement problems, particularly in industrial applications.
  • the present invention relates to a device in which X-ray fluorescence measurement is used in an online method.
  • a substance flow belonging to a running process is guided past a measuring station, this measuring station being at least one X-ray source and at least one X-ray fluorescence detector.
  • Such devices have numerous industrial applications, for example in online analysis with regard to coal used in an industrial process, for example to measure the proportion of ash or sulfur or also proportions of other special elements. Other applications include the steel industry. Here, for example, the proportion of certain elements in a still hot slag stream is measured.
  • a central problem of the present measurement technology is that especially the ⁇ -quanta at the low-energy end of the energy spectrum of interest are difficult to detect due to their short range in air.
  • offline laboratory measurements in which there is sufficient time to prepare the sample accordingly, and in which the samples are introduced into corresponding measuring devices with precisely adjustable geometries, the measurement problems can be solved comparatively easily.
  • applications of interest in which, in a "factory situation", a substance stream flowing past is measured, the surface geometry of which, at least in some applications, changes at least slightly over time, the situation is much more difficult.
  • PCT / US99 / 20867 deals with the problem of arranging an X-ray source and an X-ray fluorescence detector in relation to a transport device for an online element analysis. It is proposed there to arrange the X-ray fluorescence detector as close as possible to the substance to be measured flowing past, in particular at a distance of less than 5 cm. Since the X-ray emission is essentially isotropic, the intensity of the X-ray fluorescence radiation naturally decreases proportionally 1 / r 2 . The absorption in the air is not even taken into account here. Accordingly, it is of course fundamentally correct that the arrangement of the detector close to the sample maximizes the measurable signal. In the However, there are considerable difficulties in implementing the proposal made in PCT / US99 / 20867, at least in some applications:
  • the X-ray source and the X-ray fluorescence detector are arranged on the same side of the sample.
  • This solution is also generally preferred in terms of the power required and the wavelength of the X-ray source. Since both the X-ray source and the X-ray fluorescence detector naturally have a certain spatial dimension, the close arrangement of the X-ray fluorescence detector to the substance to be measured generally makes it necessary to radiate the radiation coming from the X-ray source relatively flat onto the substance being conveyed past or the substance flowing past, as is the case with this is shown, for example, in FIG.
  • Another major problem with the arrangement of the X-ray fluorescence detector close to the substance to be measured is that no substance can be measured at temperatures above about 100 degrees.
  • Special, cooled semiconductor elements are used as X-ray fluorescence detectors, which become blind in the vicinity of strong heat sources.
  • the fluorescent radiation emitted by the substance is no longer fed directly to the X-ray fluorescence detector, but is first coupled into at least one first X-ray conductor and fed via it to the X-ray fluorescence detector.
  • Suitable X-ray conductors are known in the art and consist, for example, of at least one hollow tube, usually in the form of a thin, hollow glass capillary, in the interior of which the X-rays propagate through total reflection. Due to the fact that the X-ray conductors can be made correspondingly thin, completely different geometries are possible compared to the prior art, in particular it is possible to arrange the end of the X-ray conductor close to the surface of the substance to be measured and yet the exciting X-ray radiation almost perpendicular to the substance to shine on.
  • the X-ray fluorescence detector itself can be arranged relatively far away from the substance flowing past, which is particularly advantageous when relatively hot substances are to be measured whose heat radiation must be protected by the X-ray fluorescence detector. Since the known light guides can also be made curved, it is in particular also possible to arrange a heat shield between the conveyor belt and the X-ray fluorescence detector. According to claim 2, the stimulating X-ray radiation is guided over an X-ray conductor, which further facilitates the adjustment of the device and increases the tolerance to changing conditions.
  • the X-ray conductors used consist of the glass capillaries already mentioned. These are known in the art. So far, such X-ray conductors have been used for spatially resolving X-ray emission measurements. For the use proposed here, these glass capillaries have the particular advantage that they have a heat resistance of several hundred degrees Celsius and can therefore be guided very close to the substance to be measured even if it has high temperatures.
  • the hollow tubes / glass capillaries are preferably filled with hydrogen or helium, helium being preferred from a handling point of view.
  • helium being preferred from a handling point of view.
  • the X-ray conductors are preferably combined into a bundle, which has considerable advantages with regard to handling and adjustment and also with regard to overall sensitivity.
  • Laser distance sensors are particularly suitable for this and such a laser distance sensor is preferably coupled to an optical fiber. According to claim 18, this light guide is coupled to at least one of the existing X-ray guides, so that the distance measurements have no location or time offset compared to the X-ray measurement. The overall accuracy of the measurement can thus be increased considerably.
  • an X-ray half lens in the beam path of the X-ray source before the X-ray light occurs on the substance to be measured for parallelizing the X-radiation.
  • FIG. 1 shows a schematic representation of a first embodiment of the invention
  • Converging lens is arranged
  • FIG. 3 shows a schematic illustration of a second embodiment of the invention
  • FIG. 4 shows an X-ray fluorescence detector with connected X-ray conductor in a schematic illustration
  • FIG. 5 shows an alternative embodiment to that shown in FIG.
  • FIG. 6 shows a schematic illustration of an X-ray fluorescence detector and an X-ray source to which an X-ray conductor is connected, which unite to form a bundle
  • FIG. 7 is a partial view from FIG.
  • Figure 8 A bundle of X-ray conductors in cross section in a schematic
  • FIG. 9 shows a further embodiment of a bundle of X-ray conductors in cross section
  • FIG. 10 shows an alternative embodiment to that shown in FIG. 7,
  • FIG. 11 shows an embodiment as shown in FIG. 6, which furthermore has a light guide connected to a laser distance measuring device
  • FIG. 12 shows a schematic illustration of a measuring device according to the prior art
  • FIG. 13 an X-ray source with an X-ray conductor and a wavelength filter
  • FIG. 14a a device with flat X-ray radiation
  • 14b shows a plan view of the device shown in FIG. 14a along the line of sight AA
  • FIG. 15 A device in which polarized X-rays are irradiated onto the substance.
  • Figure 16 A movable measuring arrangement
  • a first embodiment of the invention is shown schematically in FIG.
  • a stream of the substance S to be examined is conveyed past a measuring station on a conveyor belt 51.
  • a leveling edge 53 is arranged upstream of the measuring station in order to obtain as flat a surface as possible of the substance to be measured at the measuring station.
  • the measuring station of this exemplary embodiment consists of an X-ray tube 10, an X-ray fluorescence detector 20 and a first X-ray conductor connected to the radiation inlet of the X-ray fluorescence detector, which is designed in the form of a first glass capillary 30.
  • Such x-ray conducting glass capillaries are available on the market.
  • the exciting X-ray radiation ( ⁇ A ) coming from the X-ray tube 10 is radiated onto the substance surface and generates characteristic excitation states of the elements present in it.
  • the recombination of the excited states takes place partly radiant, whereby in the applications of interest here the K ⁇ -, with heavy elements the L ⁇ - transition is often observed.
  • the radiation emission ( ⁇ E ) is usually isotropic, which means that the radiation intensity decreases with 1 / r 2 without taking air absorption into account.
  • the front end 30a of the first glass capillary is arranged as close as possible to the surface of the substance flow.
  • corresponding glass capillaries 30 can be made relatively thin, this is also possible without colliding with the x-ray tube 10 or its beam path.
  • the X-ray that has entered it spreads out gene radiation from total reflection on the walls, so that only an absorption-related loss of intensity occurs.
  • the X-ray fluorescence detector 20 can be arranged relatively far away from the surface of the substance S to be measured. The problem of minimizing absorption within the glass capillary will be discussed in more detail later.
  • Figure 2 shows an improved embodiment of the embodiment shown in Figure 1.
  • an X-ray half lens 12 is arranged between the X-ray tube 10 and the surface of the substance S to be measured, which leads to a parallelization of the incident X-rays.
  • this has the advantage that the intensity on the area of interest of the substance can be increased while the power of the X-ray tube remains the same.
  • the parallelization of the radiation means that the intensity on the surface of the substance remains constant even if the substance has a has an uneven surface. This improves the reproducibility of the measurement results.
  • FIG. 3 shows a second embodiment of the invention.
  • a substance stream here in particular hot slag, slides down on a chute 55. Part of the slag is continuously removed via an opening in this chute 55 and the turntable 56 and fed to the measuring station.
  • the substance lying on the turntable is leveled over a leveling edge, but the corresponding leveling edge is not here in the plane of the drawing and is therefore not shown.
  • the corresponding substance is returned to the main flow in the chute 55 via a scraper, also not shown.
  • the turntable is located within a shielding housing 58, in which, in the present exemplary embodiment, relatively high temperatures also prevail due to the high temperatures of the slag to be measured. For this reason, both the X-ray tube 10 and the X-ray fluorescence detector 20 as well as all components of the evaluation electronics are arranged outside the shielding housing 58.
  • the coupling and decoupling of the X-ray radiation occurs here in each case via X-ray conductors, namely here through the first glass capillary 30 and the second glass capillary 40. It should be emphasized here that instead of a first glass capillary it is generally also possible to use bundles of first glass capillaries. The same applies to the second glass capillaries.
  • a part of the X-ray radiation generated by the X-ray tube 10 reaches the second glass capillary 40, in which it spreads essentially without loss.
  • a portion of the fluorescence radiation generated by the substance to be measured reaches the first glass capillary 30 and from there into the X-ray fluorescence detector 20, where it is measured.
  • the X-ray fluorescence detectors used generally contain a semiconductor element, here for example an Si pin semiconductor element 25. Such semiconductor elements can generally only work at relatively low temperatures and become blind when the heat is too great.
  • a heat shield 59 is arranged between the shielding housing 58 and the X-ray fluorescence detector 20.
  • This heat shield 59 can work reflectively and / or absorptively and, for example, consist of a heat-insulating material, or can also be actively, for example cooled by water cooling. Because the glass capillaries used here as X-ray conductors can also be curved without losing their X-ray conductivity, it is possible to completely remove the X-ray fluorescence detector 20 from the line of sight of the substance to be measured.
  • FIG. 4 shows the structure of an X-ray fluorescence detector with a connected first glass capillary in somewhat larger detail, albeit schematically.
  • the measurement of low-energy X-ray fluorescence radiation in particular less than 2 keV, is problematic since a very strong absorption occurs in air.
  • the first glass capillary 30 with a light gas, in particular Helium to fill.
  • a semiconductor element for example an Si pin semiconductor element 25 is seated inside the housing 22 and is preferably cooled via a Peltier cooler 26.
  • a power supply and signal line 27 connects the semiconductor element to the control and evaluation electronics.
  • the first glass capillary 30 has a thin window 30b at its front end 30a, for example in the form of a berillium foil.
  • This window also serves to prevent the ingress of dirt particles that could reduce or destroy the X-ray conductivity of the first glass capillary 30.
  • the berillium foil used as a window must be relatively thin.
  • FIG. 5 shows an alternative embodiment to FIG. 4.
  • the interior of the glass capillary 30 and the interior of the housing 22 form a common gas space.
  • a window that closes the first glass capillary 30 has been dispensed with, and the entire arrangement is constantly flushed with helium.
  • the housing 22 is connected to a helium source 28.
  • This arrangement has the advantage that there is no need for a relatively sensitive window.
  • the helium flowing through the arrangement also prevents dirt particles from entering the glass capillary.
  • the glass capillaries used here as X-ray conductors can be bent to a certain degree without losing their X-ray conductivity.
  • the glass capillaries used can be combined into bundles, as shown in FIG. 6.
  • X-ray tube 10 and X-ray fluorescence detector 20 can be spatially separated, however, the end sections of the two glass capillaries 30 and 40 can lie close to one another and extend parallel, see also FIG. 7. This enables a very precisely defined geometry to be generated and, in particular, the measurement is compared to a changing height of the flowing substance, which The presence of coarse-grained substances is in principle unavoidable, relatively insensitive, since both the direction of radiation and the emission of the X-rays are almost perpendicular.
  • FIG. 8 shows a cross section through such a bundle in which the glass capillaries are arranged in a matrix.
  • FIG. 9 shows an exemplary embodiment in which a second glass capillary 40 is surrounded by a plurality of first glass capillaries 30. This arrangement also serves to collect as many of the emitted gamma quanta as possible and to feed them to the X-ray fluorescence detector.
  • Transport belts and turntables occur as transport devices in the illustrated exemplary embodiments. However, it is clear that other transport devices are also possible, for example channels or tubes when measuring liquid substances.
  • FIG. 13 shows a first possibility for reducing the background.
  • a wavelength filter 42 is arranged in the beam path of the exciting X-rays. This wavelength filter 42 is selected such that it essentially only transmits X-rays whose energy is greater than or equal to the lowest desired excitation energy.
  • the wavelength filter 42 also serves as the termination of the second glass capillary 40, the other end of which is connected to the X-ray tube 10.
  • one or more monochromators can also be used.
  • FIGS. 14a and 14b show an alternative or additional possibility of how the measurement background can be reduced.
  • the exciting X-ray radiation is radiated onto the substance at a flat angle ⁇
  • the first glass capillary 30, which captures part of the fluorescence radiation is essentially at the same angle ⁇ to the sample surface and extends parallel to the radiation axis of the exciting X-rays, here parallel to the second glass capillary 40.
  • This arrangement also makes this arrangement relatively insensitive to fluctuations in the height of the substance surface.
  • the scattering of non-absorbed X-rays occurs essentially in the forward direction, so that only a very small part of these can reach the first glass capillary 30. Since the fluorescence is essentially isotropic, the signal to be measured is not reduced, but the background is considerably reduced.
  • the exciting X-ray radiation is polarized by means of a polarizer 44 before it hits the substance surface and is irradiated onto the substance to be examined at the Brewster angle ⁇ B.
  • the proportion of scattered X-rays can be significantly reduced again, see Figure 15.
  • FIG. 16 shows one possibility of how the device according to the invention can be designed very flexibly while maintaining high precision.
  • the X-ray tube 10, the X-ray fluorescence detector 20 and corresponding X-ray conductors, here first glass capillary 30 and second glass capillary 40 are arranged on a carriage 70 which can be moved at least one dimension, so that the ideal position in relation to the substance surface can be set as required without having to a complex adjustment of the X-ray conductors to each other is necessary.
  • pivotability in a vertical plane can also be provided.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

L'invention concerne un dispositif permettant d'effectuer une analyse d'éléments en ligne, sur une substance (S) acheminée ou s'écoulant devant un poste de mesure. Ledit dispositif présente un dispositif de transport pour la substance à mesurer, un poste de mesure avec une source de rayons X (10) et un détecteur de fluorescence X (20) avec une entrée de rayonnements. Afin d'améliorer la tolérance par rapport à des réglages défectueux et à une hauteur variable de la surface des échantillons, au moins un premier guide de rayons X (30) s'étend en direction du sens de transport (51), à partir de l'entrée des rayonnements du détecteur de fluorescence X. les rayonnement émis par la source sont également dirigés en direction de la substance par l'intermédiaire d'un guide de rayons X. L'utilisation de capillaires en verre fins permet d'injecter ou de sortir les rayonnements de manière parallèle et à proximité du point voulu.
EP03763588A 2002-07-10 2003-07-03 Analyse par fluorescence x a l'aide d'un guide d'ondes relie a la source et au detecteur Withdrawn EP1530714A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10230990 2002-07-10
DE10230990A DE10230990A1 (de) 2002-07-10 2002-07-10 Vorrichtung zur Durchführung einer Online-Elementanalyse
PCT/DE2003/002224 WO2004008128A1 (fr) 2002-07-10 2003-07-03 Analyse par fluorescence x a l'aide d'un guide d'ondes relie a la source et au detecteur

Publications (1)

Publication Number Publication Date
EP1530714A1 true EP1530714A1 (fr) 2005-05-18

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EP03763588A Withdrawn EP1530714A1 (fr) 2002-07-10 2003-07-03 Analyse par fluorescence x a l'aide d'un guide d'ondes relie a la source et au detecteur

Country Status (7)

Country Link
US (1) US7313220B2 (fr)
EP (1) EP1530714A1 (fr)
AU (1) AU2003257381B2 (fr)
CA (1) CA2491140A1 (fr)
DE (3) DE10230990A1 (fr)
WO (1) WO2004008128A1 (fr)
ZA (1) ZA200410294B (fr)

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US7020238B1 (en) 2005-01-31 2006-03-28 Oxford Instruments Analytical Oy Adapter and analyzer device for performing X-ray fluorescence analysis on hot surfaces
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Also Published As

Publication number Publication date
DE20309010U1 (de) 2003-08-28
US7313220B2 (en) 2007-12-25
DE10393419D2 (de) 2005-06-09
DE10230990A1 (de) 2004-02-05
WO2004008128A1 (fr) 2004-01-22
ZA200410294B (en) 2005-10-17
AU2003257381B2 (en) 2009-01-22
AU2003257381A1 (en) 2004-02-02
CA2491140A1 (fr) 2004-01-22
US20050232391A1 (en) 2005-10-20

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