Examples disclosed herein relate generally to devices and methods for use in diffusion pumps. More particularly, certain embodiments disclosed herein relate to devices that may be used in an oil diffusion pump for use in a mass spectrometer.
Simple baffles are often inefficient in use of space for funneling gas into an oil diffusion pump and blocking oil vapor from exiting the pump. Common designs are comprised of offset, overlapping plates or surfaces, or chevron slots to achieve optical density. Further, many existing baffles rely on a cooled volume with an optically dense path of exit for oil vapor and aerosol. Such designs often require significant space, assembly, and cost.
In accordance with a first aspect, an oil diffusion pump comprising a jet assembly, a heating element, a chamber and a baffle is provided. In certain examples, the baffle may be a non-cooled baffle that is fluidically coupled to the chamber and comprises a plurality of apertures, wherein at least one of the plurality of apertures comprises a convergent portion and a divergent portion.
In some examples, the baffle may be constructed and arranged with a symmetric number of apertures about a central axis of the baffle. In other examples, the baffle may be constructed and arranged with asymmetric number of apertures about a central axis of the baffle. In additional examples, the oil diffusion pump may further comprise an additional pump fluidically coupled to the diffusion pump. In certain examples, the baffle may further comprise a circumferential ridge. In other examples, the baffle may comprise at least two concentric cones and the apertures may be positioned between the at least two concentric cones. In some examples, the baffle may further comprise at least one rib configured to connect the at least two concentric cones.
In accordance with another aspect, an oil diffusion pump comprising a jet assembly, a heating element, a chamber and a non-cooled baffle fluidically coupled to the chamber and comprising at least two concentric cones is disclosed. In some examples, the baffle may comprise two to five concentric cones. In other examples, the pump may further comprise an additional pump fluidically coupled to the oil diffusion pump. In some examples, the baffle may comprise a circumferential ridge. In certain examples, the baffle may include an aperture positioned between the at least two concentric cones.
In accordance with an additional aspect, a mass spectrometer comprising a mass analyzer, a detector fluidically coupled to the mass analyzer, and an oil diffusion pump fluidically coupled to the mass analyzer and the detector is provided. In certain examples, the oil diffusion pump of the mass spectrometer comprises a jet assembly comprising a plurality of nozzles, a heating element, a chamber configured to receive an oil and coupled to the heating element and the jet assembly, and a non-cooled baffle fluidically coupled to the chamber and comprising a plurality of apertures, wherein at least one of the plurality of apertures comprises a convergent portion and a divergent portion.
In certain examples, the baffle of the mass spectrometer includes at least two concentric cones and apertures are positioned between the at least two concentric cones. In some examples, the baffle may comprise at least one rib connecting the concentric cones. In certain examples, the mass spectrometer further comprises a sample introduction device fluidically coupled to the mass analyzer. In other examples, the mass spectrometer further comprises a gas chromatography system fluidically coupled to the sample introduction device. In additional examples, the oil diffusion pump may be mounted proximate to the mass analyzer of the mass spectrometer.
In accordance with another aspect, a mass spectrometer comprising a mass analyzer, a detector fluidically coupled to the mass analyzer, and an oil diffusion pump fluidically coupled to the mass analyzer and the detector is disclosed. In certain examples, the oil diffusion pump comprises a jet assembly comprising a plurality of nozzles, a heating element, a chamber configured to receive an oil and coupled to the heating element and the jet assembly, and a non-cooled baffle fluidically coupled to the chamber and comprising at least two concentric cones. In some examples, the baffle may include an aperture positioned between the at least two concentric cones. In certain examples, the baffle may further comprise at least one rib configured to connect the concentric cones. In some examples, the mass spectrometer may further comprise a sample introduction device fluidically coupled to the mass analyzer. In other examples, the mass spectrometer may further comprise a gas chromatography system fluidically coupled to the sample introduction device. In certain examples, the oil diffusion pump may be mounted proximate to the mass analyzer of the mass spectrometer
In accordance with an additional aspect, a method of configuring a mass spectrometer is provided. In certain examples, the method comprises mounting an oil diffusion pump proximate to a sample introduction device, and configuring the oil diffusion pump with a non-cooled baffle including at least one aperture comprising a convergent portion and a divergent portion, wherein the baffle is constructed and arranged to retard loss of oil vapor from the oil diffusion pump. In some examples, the method may further comprise configuring the baffle with a plurality of apertures, wherein each aperture comprises a convergent portion and a divergent portion.
In accordance with another aspect, a method of configuring a mass spectrometer comprising mounting an oil diffusion pump proximate to a sample introduction device, and configuring the oil diffusion pump with a non-cooled baffle comprising at least two concentric cones, wherein the baffle is constructed and arranged to retard loss of oil vapor from the oil diffusion pump is disclosed. In some examples, the method may further comprise configuring the baffle with at least one aperture positioned between the concentric cones.
Additional aspects, examples, embodiments and features will be recognized by the person of ordinary skill in the art, given the benefit of the instant specification.
Certain embodiments are described in more detail below with reference to the figures in which:
Unless otherwise clear from the context, the use of the terms “top” and “bottom” is arbitrary and for illustrative purposes only, and the devices disclosed herein may be used in any orientation. In addition, certain dimension, features, components and the like may have been enlarged, distorted or otherwise shown in a non-proportional or non-conventional manner to facilitate a better understanding of the technology disclosed herein.
Certain features, aspects and examples of the technology disclosed herein provide significant advantages over existing systems including, but not limited to, improved gas flow, prevention of flow of oil particles into an instrument, improved detection limits and the like. Certain embodiments of the baffles disclosed herein may be used in a variety of systems having an oil diffusion pump, for example, an oil diffusion pump coupled to a mass spectrometer. Examples of the baffles disclosed herein may be constructed and arranged for use in any oil diffusion pump and provides for gas conductance more easily in one direction than the other. Certain embodiments of the baffles may also significantly reduce, and in some embodiments, prevent flow of oil vapor and particles in one direction. Some examples disclosed herein are directed to a non-cooled baffle. As used herein, “non-cooled baffle” refers to a baffle without active heat removal, e.g., through the use of a cooling fluid. In embodiments where the baffle is a non-cooled baffle, the baffle may have smaller dimensions than a cooled baffle, may decrease the mean free path and increase the likelihood of collisions of gas atoms and molecules with oil vapor and aerosol, may rest on the vacuum chamber without touching the mouth of the pump so heat is not transferred directly by conduction and may provide other advantages such as, for example, be optically dense to prevent a direct path (line of sight) for oil to pass through, provide a suitable surface area for oil vapor to condense, provide suitable surfaces for oil aerosols or particulates to collide and stick, provide a suitable geometry for oil to collect, drip and return to the diffusion pump
In accordance with certain examples, the baffles disclosed herein may be used in an oil diffusion pump. A simplified schematic of an oil diffusion pump that includes a baffle is shown in
In accordance with certain examples, the non-cooled baffle 150 may be constructed and arranged to prevent oil vapor from entering the device or chamber coupled to the fluid inlets 170 and 172, as discussed further below. By including a baffle in certain embodiments of an oil pump, the oil pump may be mounted proximate to a sample introduction device or sample inlet without allowing the oil to enter the detector or analyzer, e.g., the pump may be mounted within a few inches or directly fluidically coupled without any intervening devices. Such advantage may be particularly useful in mass spectrometry to reduce the overall footprint of the instrument. Also, by mounting the diffusion pump closer to the sample introduction device, enhanced fluidic coupling may be achieved to provide better fluid coupling between the pump and the device to which it is attached. This configuration may provide for increased removal of gases that may interfere with detection of species by an instrument and/or may reduce the rate of contamination of the instrument. Additional advantages of using the baffles disclosed herein will be recognized by the person of ordinary skill in the art, given the benefit of this disclosure.
In accordance with certain example, a non-cooled baffle comprising at least two concentric cones is disclosed. Concentric cones have an advantage of concentrating the fluids, e.g., gases, entering the pump. This concentrating effect increases the likelihood of entering molecules colliding with oil vapor traveling upstream. The effect also retards oil back-streaming through the baffle. Concentric cones also provide an efficient use of space which may reduce the overall size of the baffle. The concentric cones may include reversing angles and ribs to hold the cones together. This design may increase efficiency for gas conduction (low restriction and optimized use of space) into an oil diffusion pump. Embodiments of the baffle may be configured with converging surfaces to provide a funneling effect and diverging surfaces to provide a de-funneling effect. The design further increases the effectiveness for blocking and condensing oil vapor and aerosols exiting the oil diffusion pump. Because of the one piece design, the baffle may be produced from a single piece of, for example, metal, although other suitable materials can be used, and the baffle can be easily installed, removed, and cleaned. The desired baffle geometry may be achieved by lathe turning and milling and may be inherently stiff and stable due to the selected materials.
In certain examples, a schematic of a non-cooled baffle comprising concentric cones is shown in
In certain examples, the number of apertures in the baffle may vary and are typically determined by the number of concentric cones that are present. The shape and geometry of the apertures may also be based, at least in part, on the shape and type of concentric cones used. Referring to
In accordance with certain examples, the exact cross-sectional shape of the apertures may vary and different designs may increase fluid flow into pump while reducing the likelihood of oil vapor escaping from the pump. The person of ordinary skill in the art, given the benefit of this disclosure, will recognize that any desired cross-sectional aperture shape may be used so long as a pressure differential is created and no substantial amounts of oil vapor exit the pump. In certain examples, the aperture may include a plurality of convergent and divergent portions as shown in the aperture 405 of
In accordance with certain examples, the baffles disclosed herein may be designed such that the apertures are arranged symmetrically about a central axis (
In accordance with certain examples, the cooled baffles disclosed herein may include an inlet and an outlet for circulating a cooling fluid within the baffle. Cooling of the baffle may be desirable, for example, to condense oil vapor on the baffle surface to prevent the oil vapor from back-streaming. In some examples, the cooling fluid may be water, water including an additive, e.g., salts, ethylene glycol, etc., to raise the boiling point of the water, or some other fluid whose vaporization temperature is above the operating temperature of the diffusion pump. In some examples, the temperature of the cooling fluid may be selected such that the oil vapor condenses but the fluid entering into the pump from the fluid inlets does not condense to any substantial degree. Condensation of the gas may result in contamination of the pump oil and/or poor pump performance requiring frequent changing of the pump oil.
In accordance with certain examples, the exact dimensions of the baffles disclosed herein may vary depending in the size of the pump, pump housing, desired flow rate, desired vacuum and the like. In some examples, the baffle is generally circular (when viewed from the top or bottom) and has a diameter of about 3-6 inches, more particularly about 3-5 inches, e.g., about 4 inches. In certain examples, the top-to-bottom thickness of the baffle may be about 0.25 to about 2 inches, more particularly about 0.5 inches to about 1.5 inches, e.g., about 0.75 inches. In embodiments where the baffle is cooled, it may be desirable to increase the overall dimensions to provide inlets and/or outlets for a cooling fluid.
In accordance with certain examples, the exact material used to produce the baffles may vary, and the selected material may be any material that can withstand the high temperatures and pressures in the pump housing without any substantial adverse affects on pump performance. In some examples, the baffle may include a metal, a high temperature polymer or combinations thereof. In certain examples, the materials used in the baffle desirably do not substantially out gas or release any particulate or gaseous matter that may adversely affect a device to which the pump is providing a vacuum, e.g., to a mass spectrometer, electron microscope, semi-conductor processing equipment, etc. In some examples, the baffle may be made from stainless steel or other generally inert materials to retard or reduce corrosion in the baffle.
In accordance with certain examples, the baffles disclosed herein may include one or more indicia that assist in mounting of the baffle into the pump. Such indicia may include arrows, text, or structural features. For example, a circumferential ridge may be included such that the baffle may only be mounted correctly in one orientation in the pump. Circumferential grooves that are parallel to the central axis of the baffle may be included such that the grooves mate with a mounting member in the pump. Such grooves may be angled suitably to assist in mounting of the baffle into the pump, e.g., the grooves may be angled such that the baffle only mounts in a single orientation in the pump.
In accordance with certain examples, the baffles disclosed herein may include shapes other than concentric cones. In particular, certain embodiments may include apertures with convergent and divergent portions that have been machined or drilled into a solid metal disk. Other embodiments include apertures that have been etched into or otherwise produced from a body. Some examples include joining of two or more pieces or portions together to provide a unitary body having a desired shape and/or desired aperture spacing and arrangement. Additional configurations for producing baffles suitable for use in a diffusion pump will be readily selected by the person of ordinary skill in the art, given the benefit of this disclosure.
In certain examples, the diffusion pumps disclosed herein may be coupled to one or more additional pumps, e.g., mechanical pumps, fore pumps, turbomolecular pumps and the like. For example, a simple mechanical pump may be used to remove the bulk of the gas from the vacuum chamber of the diffusion pump. The diffusion pump may be operative to provide further gas removal to lower the pressure, which results in pulling of a vacuum. Suitable pumps include, but are not limited to, rotary pumps, oil-less (dry) pumps, scroll pumps, molecular drag pumps, diaphragm pumps and the like. Additional suitable pumps will be readily selected by the person of ordinary skill in the art, given the benefit of this disclosure.
In accordance with certain examples, the baffles disclosed herein may include one or more overlapping plates or surfaces, or chevron slots to achieve optical density, in addition to the concentric cones or other geometric structures used in the baffle. Such plates and chevrons may provide for further tuning of the fluid flow into the pump and the further retarding of oil vapor exiting the pump.
In accordance with certain examples, the oil diffusion pumps disclosed herein that include a baffle, e.g., a cooled or non-cooled baffle, may provide a vacuum down to a pressure of about 1×10−6 Torr to about 4×10−7 Torr or lower. In embodiments where the oil diffusion pump is used in a mass spectrometer, the oil diffusion pump may provide a vacuum at a pressure of about 3×10−5 Torr to about 1×10−5 Torr or lower. Additional suitable pressures are possible using the oil diffusion pumps disclosed herein.
In accordance with certain examples, the baffles disclosed herein may be used in an oil diffusion pump coupled to a mass spectrometer. A schematic of a mass spectrometer (MS) is shown in
In accordance with certain examples, the mass analyzer 730 may take numerous forms depending generally on the sample nature, desired resolution, etc. and illustrative mass analyzers are listed below. The detector 740 may be any suitable detection device that may be used with existing mass spectrometers, e.g., electron multipliers, photomultipliers, Faraday cups, coated photographic plates, ion traps, scintillation detectors, etc., and other suitable devices that will be selected by the person of ordinary skill in the art, given the benefit of this disclosure. The processor 750 typically includes a microprocessor and/or computer and suitable software for analysis of samples introduced into the MS 700. One or more databases may be accessed by the processor 750 for determination of the chemical identity of species introduced into MS 700. Other suitable additional devices known in the art may also be used with the MS 700 including, but not limited to, autosamplers, such as those used with TurboMatrix models commercially available from PerkinElmer, Inc. (Waltham, Mass.).
In accordance with certain examples, the mass analyzer of MS 700 may take numerous forms depending on the desired resolution and the nature of the introduced sample. In certain examples, the mass analyzer may be a scanning mass analyzer, a magnetic sector analyzer (e.g., for use in single and double-focusing MS devices), a quadrupole mass analyzer, an ion trap analyzer (e.g., cyclotrons, quadrupole ions traps), time-of-flight analyzers (e.g., matrix-assisted laser desorbed ionization time of flight analyzers), and other suitable mass analyzers that may separate species with different mass-to-charge ratios.
In accordance with certain other examples, the ion source may include a device to implement ionization methods commonly used in mass spectroscopy. For example, electron impact sources may be assembled to ionize species prior to entry of ions into the mass analyzer. In other examples, chemical ionization sources may be used to ionize species prior to entry of ions into the mass analyzer. In yet other examples, field ionization sources may be used to ionize species prior to entry of ions into the mass analyzer. In still other examples, desorption sources such as, for example, those sources configured for fast atom bombardment, field desorption, laser desorption, plasma desorption, thermal desorption, electrohydrodynamic ionization/desorption, etc. may be used. In yet other examples, thermospray ionization sources may be used. It will be within the ability of the person of ordinary skill in the art, given the benefit of this disclosure, to select suitable devices for ionization for use with the devices disclosed herein.
In accordance with certain examples, the MS may be coupled to a chromatography system, such as a gas chromatograph. A gas chromatograph generally includes a sample introduction device, an oven comprising a chromatography column, and one or more fluid flow paths connecting the sample introduction device and the chromatography column. The gas chromatograph is operative to separate species and pass those separated species to the MS for detection. In other examples, the MS may be coupled to a liquid chromatograph or a supercritical fluid chromatograph. Additional suitable devices for coupling to a MS will be readily selected by the person of ordinary skill in the art, given the benefit of this disclosure.
In accordance with certain examples, the MS may be coupled to another MS. The second MS may include a diffusion pump similar to the pump described herein or may include a turbomolecular pump or other suitable type of pump. The use of a diffusion pump in an MS system greatly reduces the overall cost. The second MS system with a turbomolecular pump may be configured as a second stage that can receive high flow rates, e.g., 250 L/second or more. The combination of a first stage having a diffusion pump and a second stage having a turbomolecular pump may reduce the overall system cost while providing for high overall flow rates. It will be recognized by the person of ordinary skill in the art, given the benefit of this disclosure, that the first and second stages may be inverted with the first MS stage including a turbomolecular pump and the second MS stage including a diffusion pump. In such configurations, it may be desirable to vent a portion of the gas stream to reduce the flow rate to an acceptable level for the second MS stage.
In accordance with certain examples, the pumps and MS systems disclosed herein are generally configured to be controlled using software that implements one or more algorithms. Suitable software is commercially available, for example, from PerkinElmer, Inc. (Waltham, Mass.) and includes the TurboMass™ GC/MS software available for use with the Clarus® 600 Mass Spectrometers. It will be within the ability of the person of ordinary skill in the art, given the benefit of this disclosure, to select other suitable algorithms for use with the devices disclosed herein.
In accordance with certain examples, the sensitivity of mass spectrometers coupled to an oil diffusion pump as disclosed herein depends, at least in part, on the species to be detected, the type of detector used, etc. Using photomultipliers, it may be possible to detect, for example, about 1 picogram of octafluoronaphthalene at a signal-to-noise ratio of 30:1. It is a significant advantage that such low detection limits may be achieved by mass spectrometers including low cost oil diffusion pumps that include a baffle as described herein.
In accordance with certain examples, the devices disclosed herein may be used to provide a vacuum to optical instruments. For example, vacuum circular dichroism, vacuum ultraviolet, X-ray spectroscopy or other optical techniques where oxygen or air may absorb the light use a vacuum to purge the sample chamber of any air or oxygen. The oil diffusion pumps disclosed herein may be used in such analytical devices to provide a vacuum for measurement of optical absorption, optical emission, or both, at low cost and without any substantial contamination from back-streaming.
In accordance with certain examples, the baffles disclosed herein may be used in an oil diffusion pump coupled to an electron microscope. In certain examples, the electron microscope comprises an electron beam or electron source, a sample holder, one or more condensers, an objective, and a collector screen. In a transmission electron microscope, electrons are generated as a cathode is heated by application of a current. The electrons travel toward a high voltage at the anode. The acceleration voltage is typically between 50 and 150 kV. The higher the voltage difference, the shorter are the electron waves, which increases the resolution of the microscope. The accelerated electron beams passes through an aperture at the bottom of the anode. The microscope typically includes a lens-system that consists of electronic coils generating an electromagnetic field. The electron beam is first focused by a condenser, and the passes through the sample where some of the electrons are deflected. The degree of deflection depends on the mass-to-charge ratio of the object. The greater the mass of the atoms, the greater is the degree of deflection. For atoms with low atomic numbers, it may be desirable to treat the sample with contrast enhancing chemicals (heavy metals) to get at least some contrast. After passing the sample, the scattered electrons are collected by an objective, and an image is formed. This image may be processed, digitally enhanced or enlarged using a second lens. The formed image may be viewed, for example, using a fluorescent screen or photographic material. The oil diffusion pumps disclosed herein may be coupled to the transmission microscope to provide a vacuum within the microscope.
In accordance with certain examples, the baffles disclosed herein may be used in an oil diffusion pump coupled to semiconductor processing devices and systems. Such devices include, but are not limited to, vapor deposition devices, e.g., vacuum deposition, physical vapor deposition, sputtering devices and the like. For example, the oil diffusion pump may be used to deposit thin film devices or to deposit protective or barrier coatings to prevent corrosion or to withstand harsh environments. In other examples, the oil diffusion pump may be used to provide a lowered pressure in a vacuum deposition chamber. For example, a material to be evaporated may be placed in the chamber. An electron beam may be incident on the material in the chamber, and the resulting heating from the electron beam evaporates the material. A substrate may be positioned within the chamber to receive the evaporated material. The distance between the substrate and the material may be adjusted using mechanical devices, such as a manipulator. The evaporated material may be deposited by condensation on the substrate, e.g., in the case of certain refractories such as alumina, zirconia, titania, etc., or the evaporated material may be carried by a reactive gas to the substrate. Co-evaporization processes may also be used. Additional vapor deposition processes and device suitable for use with the oil diffusion pumps disclosed herein will be readily selected by the person of ordinary skill in the art, given the benefit of this disclosure.
In certain examples, the oil diffusion pump may be used in other devices. For example, the oil diffusion pump may be used with devices and methods designed for crystal growth, such as molecular beam epitaxy. The oil diffusion pump may be used in freeze-drying apparatus. The oil diffusion pump may be used in electron microprobes. The oil diffusion pump may be used in other systems and devices where a vacuum is desirable.
In certain examples, additional features such as valves, cold traps and the like may be used with the oil diffusion pumps disclosed herein. The exact type of oil used in the oil diffusion pumps may vary and suitable oils include, but are not limited to, silicone based oils, Santovac® pump oils, Inland™ pump oils, Modoc™ pump oils and other suitable types of pump oils. The conditions used to operate the pump may be selected, at least in part, on the type of oil used, the desired pressure, the type of heating element and the like.
In accordance with certain examples, a method of retarding oil vapor loss in an oil diffusion pump is provided. In some examples, the method comprising configuring the pump with a baffle constructed and arranged with a plurality of apertures, with at least one of the apertures including a convergent portion and a divergent portion. In some examples, the baffle may be configured such that each aperture includes a convergent and a divergent portion.
In accordance with certain examples, a method of configuring a mass spectrometer is provided. In some examples, the method comprises mounting an oil diffusion pump proximate to a sample introduction device. As discussed above, the term proximate refers to mounting of the diffusion pump next to or adjacent to the sample introduction device. Existing diffusion pumps typically are not mounted proximate to the sample introduction device as the back-streaming of oil vapor interferes with the analysis. The method may further comprise configuring the oil diffusion pump with a baffle including at least one aperture comprising a convergent portion and a divergent portion. In some examples, the baffle may be constructed and arranged to retard loss of oil vapor from the oil diffusion pump.
Certain specific examples are described below to illustrate further the novel technology described herein.
An oil diffusion pump was assembled as follows: An oil diffusion pump (Model No. EO50/60 from Edwards was modified by removing the heat shield and inserting a non-cooled symmetric, conical converging/diverging baffle into the pump mouth from above and within the vacuum chamber. The baffle was machined from a piece of an aluminum bar or plate. The baffle profile was made by turning with a lathe. The converging/diverging apertures were created by milling. The dimensions of the baffle were 3.9 inches in diameter and 0.66 inches thick. The baffle was held in place by gravity. A schematic of the assembled diffusion pump is shown in
Testing of the oil diffusion pump of Example 1 was performed using a mass spectrometer (MS) coupled to a gas chromatograph (GC). The diffusion pump met the 1 picogram octafluoronaphthalene (OFN) 100:1 signal-to-noise standard when allowed to pump for a sufficient period of time, in a clean MS. A vacuum pressure of about 4×10−5 Torr was achieved for nominal operating conditions (GC column flow of 1 mL/min). No apparent oil background was present following 3-4 weeks of normal operation with samples. The pump tolerated up to 3-4 mL/min of carrier gas pressure-pulse when using splitless injections.
When introducing elements of the examples disclosed herein, the articles “a,” “an,” “the” and “said” are intended to mean that there are one or more of the elements. The terms “comprising,” “including” and “having” are intended to be open-ended and mean that there may be additional elements other than the listed elements. It will be recognized by the person of ordinary skill in the art, given the benefit of this disclosure, that various components of the examples may be interchanged or substituted with various components in other examples.
Although certain aspects, examples and embodiments have been described above, it will be recognized by the person of ordinary skill in the art, given the benefit of this disclosure, that additions, substitutions, modifications, and alterations of the disclosed illustrative aspects, examples and embodiments are possible.
This application claims priority to U.S. Provisional Application No. 60/823,569 filed on Aug. 25, 2006, the entire disclosure of which is hereby incorporated herein by reference for all purposes.
Number | Date | Country | |
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60823569 | Aug 2006 | US |