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WO2009082373A1 - Analyseur de fluorescence x portable - Google Patents

Analyseur de fluorescence x portable Download PDF

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Publication number
WO2009082373A1
WO2009082373A1 PCT/US2007/026250 US2007026250W WO2009082373A1 WO 2009082373 A1 WO2009082373 A1 WO 2009082373A1 US 2007026250 W US2007026250 W US 2007026250W WO 2009082373 A1 WO2009082373 A1 WO 2009082373A1
Authority
WO
WIPO (PCT)
Prior art keywords
hand
analyzer
held
xrf analyzer
vacuum
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.)
Ceased
Application number
PCT/US2007/026250
Other languages
English (en)
Inventor
Bridget Tannian
Brad Hubbard-Nelson
Alfred Oleru
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.)
Olympus Scientific Solutions Americas Corp
Original Assignee
Innov X Systems Inc
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 Innov X Systems Inc filed Critical Innov X Systems Inc
Priority to PCT/US2007/026250 priority Critical patent/WO2009082373A1/fr
Publication of WO2009082373A1 publication Critical patent/WO2009082373A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • 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
    • 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
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/301—Accessories, mechanical or electrical features portable apparatus

Definitions

  • This invention relates generally to hand-held x-ray fluorescence (XRF) analyzers and more particularly, to an improved hand-held XRF analyzer that provides a desired condition of a controlled volume about and the x-ray source and the detector to improve sensitivity of the analyzer and which alerts the operator if the desired condition has been compromised.
  • XRF x-ray fluorescence
  • Hand-held XRF analyzers are used to detect elements present in a sample.
  • a typical hand-held XRF analyzer includes an x-ray source for directing x-rays to the sample and a detector responsive to the x-rays emitted from the sample.
  • An analyzer processes the output signals produced by the detector and divides the energy levels of the detected x-ray photons into several energy subranges by counts of the number of x-ray photons detected to produce a graph depicting the x-ray spectrum of the sample.
  • Hand-held XRF analyzers are known. See, e.g., the applicants' co-pending applications, U.S. Patent Application Serial No. 11/582,038 filed October 17, 2006 entitled “XRF System with Novel Sample Bottle”, and U.S. Patent Application Serial No. 11/585,367 filed October 24, 2006 entitled “Fuel Analysis System", by one or more common inventors hereof and all of the same assignee, incorporated by reference herein. See also U.S. Patent Nos. 6,501,825; 6,909,770; 6,477,227; and 6,850,592, all of which are incorporated by reference herein.
  • hand-held XRF analyzer an operator can detect whether certain elements are present in sample for use in such applications as, inter alia, security and law enforcement, environmental applications, artistic and historic works, biomedical and pharmaceutical applications, process chemistry, and the like.
  • Another key use of hand-held XRP analyzers is to detect elements listed by the European Union Directive Restriction on the Use of Certain Hazardous Substances (RoHs). This Directive restricts the use of certain hazardous substances, such as lead (P b ), mercury (H g ), cadmium (Ca), chromium (C 1 -) and Bromine (B 1 -), and the like, in manufactured electrical and electronic equipment.
  • conventional hand-held XRF analyzers are limited to providing a vacuum or a purge condition, but not both, in a chamber containing the analyzer components.
  • Conventional hand-held XRF analyzers also typically employ a large chamber which increases the time required to create the vacuum or purge condition. The large volume also requires the operator of the analyzer to carry a pump that continuously maintains the desired vacuum or purge condition.
  • U.S. patent No. 6,909,770 to Schramm et al. relies on a vacuum chamber attachment mounted to the end of a portable XRF analyzer.
  • the sample to be analyzed is placed inside the chamber and the entire volume is evacuated.
  • This approach has the disadvantage of requiring a sample to be removed and placed into the chamber rather than allowing samples to be tested in-situ.
  • the design also requires a larger volume for the vacuum, thus requiring a larger pump which reduces the overall portability of the XRF analyzer.
  • the XRF analyzer as disclosed by Sipila, et al. utilizes a removable gas-filled chamber placed inside the volume about the x-ray source, the sample and the detector.
  • the chamber is filled with an appropriate gas, e.g., helium, and hermetically sealed.
  • the chamber is locked into place and used for a period of time.
  • the drop-in chamber is intended to be field replaceable by the end-user.
  • the analyzer as disclosed by Sipila does not offer a way to replenish the purge gas. The chamber must be removed, purged, and replaced.
  • the conventional hand-held XRF analyzers discussed above are not designed to provide either a vacuum or purge condition as needed and cannot determine if the vacuum or purge condition is being maintained while the analyzer is in operation.
  • the vacuum chamber is integrated with the various components of the analyzer, if the chamber or any of the components fail while the analyzer in operation, the components cannot easily be serviced by the operator in the field.
  • Such a design also prevents the components of the analyzer from being easily upgraded.
  • an improved hand-held XRF analyzer which quickly and easily provides either a vacuum or a predetermined purge condition in a controlled volume about the x-ray source and the detector in order to detect lower atomic number elements and which alerts the operator if the vacuum or the purge condition has been compromised and is serviceable and upgradeable in the field by skilled service engineers is effected with an x-ray source for emitting x-rays through a window to a source.
  • a detector behind the window is responsive to the x-rays radiated from the sample.
  • a controlled volume about the x- ray source and the detector is maintained in either a vacuum or purge condition for a predetermined amount of time to increase the sensitivity of the analyzer.
  • a processor responsive to the detector analyzes the spectrum of emitted x-rays to detect the low atomic number elements and is responsive to a pressure sensor that detects a pressure change inside the controlled volume.
  • the processor is programmed to detect if the vacuum or predetermined purge condition has been compromised.
  • This invention features a hand-held XRF analyzer including an x-ray source for emitting x-rays through a window to a sample.
  • a detector behind the window is responsive to x-rays irradiated by the sample.
  • a controlled volume about the x-ray source and the detector is maintained in a vacuum or a predetermined purge condition for a predetermined amount of time for increasing the sensitivity of the analyzer.
  • a processor is responsive to the detector for analyzes the spectrum of irradiated x-rays and responsive to a pressure sensor for detecting a pressure change inside the controlled volume. The processor is configured to detect if the vacuum or the predetermined purge condition has been compromised.
  • the processor may be configured to detect a predetermined threshold intensity of argon in the controlled volume and provide an output signal indicating the predetermined purge condition has been compromised.
  • the processor may provide an output signal when the pressure of the controlled volume changes indicating the vacuum has been compromised.
  • the vacuum may be maintained for at least 2 hours.
  • the predetermined purge condition may be maintained for at least 2 hours.
  • the hand-held XRF analyzer may include a display responsive to the output signal for displaying an indication that the purge condition has been compromised.
  • the hand-held XRF analyzer may include a display responsive to the output signal for displaying an indication that the vacuum has been compromised.
  • the hand-held XRF analyzer may include a vacuum pump for creating the vacuum in the controlled volume.
  • the hand-held XRF analyzer may include a purge subsystem for supplying a purge gas to the controlled volume for creating the predetermined purge condition in the controlled volume.
  • the purge gas may be helium.
  • the controlled volume may be created in a housing.
  • the housing may be disposed between a top plate and a bottom plate.
  • the housing may be removable.
  • the housing may have a low volume.
  • the hand-held XRF analyzer may include a removable window plate for housing the window.
  • the window may be made of polyimide film or Kapton.
  • the hand-held XRF analyzer may include an 0-ring disposed between the housing and the x-ray source and an 0-ring disposed between the detector and the housing for maintaining the vacuum or the predetermined purge condition for the predetermined amount of time.
  • the processor may be programmed to detect the presence of one or more elements in the sample having low atomic numbers.
  • the one or more elements may include elements having an atomic number in the range of about 11 to 17.
  • the processor may be configured to adjust the vacuum pump to ensure the vacuum is being properly maintained.
  • the processor may be configured to adjust the purge subsystem to ensure the predetermined purge condition is being properly maintained.
  • This invention also features a hand-held XRF analyzer including an x-ray source for emitting x-rays through a window to a sample.
  • a detector behind the window is responsive to x-rays irradiated by the sample.
  • a controlled volume about the x-ray source and the detector is maintained in a vacuum for a predetermined amount of time for increasing the sensitivity of the analyzer.
  • a processor is responsive to the detector for analyzing the spectrum of irradiated x-rays and is responsive to a pressure sensor for detecting a pressure change inside the controlled volume.
  • the processor is configured to detect if the vacuum has been compromised. hi one embodiment, the processor may provide an output signal when the pressure of the controlled volume changes indicating the vacuum has been compromised.
  • the vacuum may be maintained for at least 2 hours.
  • the hand-held XRF analyzer may include a display responsive to the output signal for displaying an indication that the vacuum has been compromised.
  • the hand-held XRF analyzer may include a vacuum pump coupled for creating the vacuum in the controlled volume.
  • the controlled volume may be created in a housing.
  • the housing may be disposed between a top plate and a bottom plate.
  • the housing may be removable.
  • the housing may have a low volume.
  • the hand-held XRF analyzer may include a removable window plate for housing the window.
  • the window may be made of polyimide film or of Kapton.
  • the hand-held XRF analyzer may include an 0-ring disposed between the housing and the x-ray source and an O-ring disposed between the detector and the housing for maintaining the vacuum for the predetermined amount of time in the housing.
  • the processor may be programmed to detect the presence of one or more elements in the sample having low atomic numbers.
  • One or more elements may include elements having an atomic number in the range of about 11 to 17.
  • the processor may be configured to adjust the vacuum pump to ensure the vacuum is being properly maintained.
  • This invention further features a hand-held XRF analyzer including an x-ray source for emitting x-rays through a window to a sample.
  • a detector behind the window is responsive to x-rays irradiated by the sample.
  • a controlled volume about the x-ray source and the detector is maintained in a predetermined purge condition for a predetermined amount of time for increasing the sensitivity of the analyzer.
  • a processor is responsive to the detector for analyzing the spectrum of irradiated x-rays and configured to detect if the predetermined purge condition has been compromised.
  • the processor may be configured to detect a predetermined threshold intensity of argon in the controlled volume and provide an output signal indicating the predetermined purge condition has been compromised.
  • the predetermined purge condition may be maintained for at least 2 hours.
  • the hand-held XRF analyzer may include a display responsive to the output signal for displaying the indication that the purge condition has been compromised.
  • the handheld XRF analyzer may include a purge subsystem for supplying a purge gas into the controlled volume for creating the predetermined purge condition in the controlled volume.
  • the purge gas may be helium.
  • the controlled volume may be created in a housing.
  • the housing may be disposed between a top plate and a bottom plate.
  • the housing may be removable.
  • the housing may have a low volume.
  • the hand-held XRF analyzer may include a removable window plate for housing the window.
  • the window may be made of polyimide film or Kapton.
  • the hand-held XRF analyzer may include an 0-ring disposed between the housing and the x-ray source and an O- ring disposed between the detector and the housing for maintaining the predetermined purge condition for the predetermined amount of time in the housing.
  • the processor may be programmed to detect the presence of one or more elements in the sample having low atomic numbers.
  • the one or more elements may include elements having an atomic number in the range of about 11 to 17.
  • the processor may be configured to adjust the purge subsystem to ensure the predetermined purge condition is being properly maintained.
  • This invention also features a hand-held XRF analyzer including an x-ray source for emitting x-rays through a window to a sample.
  • a detector behind the window is responsive to x-rays irradiated by the sample.
  • a controlled volume about the x-ray source and the detector is maintained in a vacuum or a predetermined purge condition for a predetermined amount of time for increasing the sensitivity of the analyzer.
  • a vacuum pump provides the vacuum in the controlled volume.
  • a purge subsystem supplies a purge gas into the controlled volume to provide the predetermined purge condition in the controlled volume.
  • a processor is responsive to the detector for analyzing the spectrum of irradiated x-rays and responsive to a pressure sensor for detecting a pressure change inside the controlled volume. The processor is programmed to detect if the vacuum or predetermined purge condition has been compromised.
  • This invention also features a method of detecting if a predetermined condition of a controlled volume of a hand-held XRF analyzer is being properly maintained including establishing a controlled volume about an x-ray source and a detector, maintaining the controlled volume in a vacuum or a predetermined purge condition for a predetermined amount of time, detecting if the vacuum or the predetermined purge condition has been compromised.
  • the method includes the step of detecting a predetermined threshold intensity of argon in the controlled volume to determine if the predetermined purge condition has been compromised.
  • the method may include the step of detecting a pressure change in the controlled volume to determine if the vacuum has been compromised.
  • Fig. 1 is simplified three-dimensional view of one embodiment of the handheld XRF analyzer of this invention
  • Fig. 2 is three-dimensional schematic diagram showing the further detail the components of the hand-held XRF analyzer shown in Fig. 1;
  • Fig. 3 is a graph of an example spectrum generated by the hand-held XRF analyzer shown in Figs. 1 and 2 depicting the detection of argon present in the controlled volume about the x-ray source and detector;
  • Fig. 4 is another three-dimensional schematic diagram showing the components of the hand-held XRF analyzer shown in Figs. 1 and 2.
  • hand-held XRF analyzer 10, Fig. 1 of this invention includes x-ray source 12, e.g., an x-ray tube, for emitting x-rays through window 14 to sample 16.
  • Detector 18 behind window 14 is responsive to x-rays radiated by sample 16.
  • Controlled volume 20 about x-ray source 12 and detector 18 is maintained in either a vacuum or predetermined purge condition for a predetermined amount of time, e.g., at least 2 hours, discussed in further detail below.
  • the vacuum or purge condition in controlled volume 20 increases the sensitivity of analyzer 10 to detect, inter alia, elements having lower atomic numbers, such as those elements between sodium (Na, atomic number 11) and chlorine (Cl, atomic number 17).
  • controlled volume 20 is created in housing 21, Fig. 2, where like parts have been given like numbers.
  • the vacuum in housing 21 is typically created with pump 22, Fig. 1 by hose 24 connected to valve 25 coupled to vacuum tube 54, Fig. 2 which is attached to vacuum fitting 23 on housing 21.
  • Pump 22 is typically attached for about 10 seconds to create the vacuum and then removed when analyzer 10 is used for testing.
  • the predetermined purge condition, e.g., a helium purge, in controlled volume 20 in housing 21 is typically created by flushing controlled volume 20 with helium using gas source 28, Fig. 1, e.g., a tank of compressed helium, coupled to hose 24' connected to vacuum attachment 25.
  • Controlled volume 20 is typically flushed for about 10 seconds to refresh the purge gas. Then, gas source 28 of compressed gas is removed when the analyzer is used for testing. Vacuum attachment 25 is coupled to gas tube 56, Fig. 2 which is attached to gas inlet 40 connected to housing 21.
  • the desired vacuum or purge condition in controlled volume 20 is preferably maintained for at least 2 hours to provide hand-held XRF analyzer 10 with the ability to more accurately analyze and test for elements having lower atomic numbers before refreshing the vacuum or re- purging with purge gas.
  • Maintaining controlled volume 20 at the vacuum or purge condition for at least 2 hours eliminates the need for an operator to carry a pump, e.g., pump 22, Fig. 1, to maintain the desired vacuum or the need for the operator to carry a tank of compressed gas, e.g., gas source 28, to maintain a desired purge condition.
  • a pump e.g., pump 22, Fig. 1
  • a tank of compressed gas e.g., gas source 28
  • Processor 30, Fig. 1 is responsive to detector 18 by line 19 and analyzes the spectrum of irradiated x-rays from sample 16. Processor 30 is also responsive to pressure sensor 27 inside controlled volume 20. Processor 30 is programmed to detect if the desired vacuum or purge condition in control volume 20 has been compromised.
  • processor 30 measures a predetermined threshold intensity of argon in controlled volume 20.
  • processor 30 senses an argon intensity in excess of the threshold intensity, processor 30 provides an error message by line 33 to display 32 which indicates the desired purge condition in controlled volume has been compromised.
  • Argon is a naturally occurring element in the ambient atmosphere.
  • hand-held XRF analyzer 10 quickly alerts an operator of a compromised purge condition. Once aware of the compromised purge condition, the operator can re-establish the desired purge condition using gas source 28 or have XRF analyzer repaired by skilled service engineers.
  • detecting the presence of argon in the controlled volume is used to determine if the predetermined purge condition has been compromised, this is not a necessary limitation of this invention, as other elements and substances known by those skilled in the art may be utilized to determine if the predetermined purge condition in the controlled volume has been compromised.
  • Fig. 3 shows an example of a spectrum that is typically generated by Processor 30 and shows the detection of an argon peak, e.g., an argon peak 70 in controlled volume 20 that indicates the purge condition has been compromised.
  • Peak 71 shows at a point when the helium purge has worsened such that the argon concentration is about 20 percent higher than the threshold intensity.
  • pressure sensor 27 When a vacuum is created in controlled volume 20, Fig. 1 , pressure sensor 27, is used to measure the pressure inside controlled volume 20. Processor 30 responds to a pressure change provided by pressure sensor 27 and provides an error signal by line 33 to display 32 that alerts the operator that the vacuum has been compromised.
  • housing 21, Figs. 2 and 4 is connected to x-ray source 12 with O-ring 36 disposed there between.
  • detector 18 is connected to housing 21 with O-ring 38 disposed there between.
  • Face plate 42 with window 14 e.g., a window made of polyimide film, e.g., Kapton, or similar type material, is attached to housing 21 using O-ring 44. Exterior plate 46 attaches to window plate 42 via screws 48. Bottom cover 50 and top cover 52 are disposed over the components described above.
  • housing 21 is designed to be removed only by skilled service engineers. This prevents untrained operators from removing housing 21 and potentially damaging detector 18, x-ray source 12, and the complex electronics associated therewith, which can have an adverse impact on calibration and quality of the measurement of analyzer 10.
  • housing 21 has a volume of about 0.05 cubic inches which is significantly smaller the volume of conventional hand-held XRF analyzers. This provides the ability for analyzer 10 to quickly create the desired vacuum or purge condition for controlled volume 20 inside housing 21, e.g., in less than about 10 seconds. The small volume of controlled volume 20 in housing 21 also holds the desired vacuum or purge conditions longer, thus further eliminating the need for the operator to carry a pump while in operation.
  • an error message may be provided by processor 30, Fig. 1 by line 31 to pump 22 or gas source 28 that is used in feedback to maintain the vacuum or predetermined purge condition in controlled volume 20.

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  • Physics & Mathematics (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 porte sur un analyseur de fluorescence X portable comprenant une source de rayons X pour émettre des rayons X, à travers une fenêtre, vers un échantillon. Un détecteur placé derrière la fenêtre est sensible aux rayons X irradiés par l'échantillon. Un volume contrôlé autour de la source de rayons X et du détecteur est maintenu dans un vide ou dans un état de purge prédéterminé pendant une durée prédéterminée pour améliorer la sensibilité de l'analyseur. Un processeur communique avec le détecteur pour analyser le spectre des rayons X irradiés et communique avec un capteur de pression pour détecter un changement de pression à l'intérieur du volume contrôlé. Le processeur est configuré pour détecter si le vide ou l'état de purge prédéterminé a été compromis.
PCT/US2007/026250 2007-12-21 2007-12-21 Analyseur de fluorescence x portable Ceased WO2009082373A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/US2007/026250 WO2009082373A1 (fr) 2007-12-21 2007-12-21 Analyseur de fluorescence x portable

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2007/026250 WO2009082373A1 (fr) 2007-12-21 2007-12-21 Analyseur de fluorescence x portable

Publications (1)

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WO2009082373A1 true WO2009082373A1 (fr) 2009-07-02

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PCT/US2007/026250 Ceased WO2009082373A1 (fr) 2007-12-21 2007-12-21 Analyseur de fluorescence x portable

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2572569A (en) * 2018-04-03 2019-10-09 Mineral Explor Network Finland Ltd Nugget effect grade assessment
EP4563989A1 (fr) * 2023-11-29 2025-06-04 Bruker Nano GmbH Analyseur xrf à fluorescence x portatif et procédé d'analyse élémentaire avec un analyseur xrf portatif

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5563929A (en) * 1994-02-18 1996-10-08 The Electric Power Research Institute On-line monitor for particulate analyte in a moving liquid
US20030053589A1 (en) * 2001-09-18 2003-03-20 Akihiro Ikeshita Sample preprocessing system for a fluorescent X-ray analysis and X-ray fluorescence spectrometric system using the same
US20060262900A1 (en) * 2005-05-20 2006-11-23 Oxford Instruments Analytical Oy Measurement apparatus and method for determining the material composition of a sample by combined X-ray fluorescence analysis and laser-induced breakdown spectroscopy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5563929A (en) * 1994-02-18 1996-10-08 The Electric Power Research Institute On-line monitor for particulate analyte in a moving liquid
US20030053589A1 (en) * 2001-09-18 2003-03-20 Akihiro Ikeshita Sample preprocessing system for a fluorescent X-ray analysis and X-ray fluorescence spectrometric system using the same
US20060262900A1 (en) * 2005-05-20 2006-11-23 Oxford Instruments Analytical Oy Measurement apparatus and method for determining the material composition of a sample by combined X-ray fluorescence analysis and laser-induced breakdown spectroscopy

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2572569A (en) * 2018-04-03 2019-10-09 Mineral Explor Network Finland Ltd Nugget effect grade assessment
GB2572569B (en) * 2018-04-03 2022-04-13 Mineral Explor Network Finland Ltd Nugget effect grade assessment
EP4563989A1 (fr) * 2023-11-29 2025-06-04 Bruker Nano GmbH Analyseur xrf à fluorescence x portatif et procédé d'analyse élémentaire avec un analyseur xrf portatif

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