WO2003102574B1 - Method and apparatus for analysis of elements in bulk substance - Google Patents

Method and apparatus for analysis of elements in bulk substance

Info

Publication number
WO2003102574B1
WO2003102574B1 PCT/US2003/016702 US0316702W WO03102574B1 WO 2003102574 B1 WO2003102574 B1 WO 2003102574B1 US 0316702 W US0316702 W US 0316702W WO 03102574 B1 WO03102574 B1 WO 03102574B1
Authority
WO
WIPO (PCT)
Prior art keywords
sample
analyzer
source
data
detector
Prior art date
Application number
PCT/US2003/016702
Other languages
French (fr)
Other versions
WO2003102574A1 (en
Inventor
Clinton L Lingren
David B Cook
James F Miller
Stephen J Foster
Original Assignee
Sabia Inc
Clinton L Lingren
David B Cook
James F Miller
Stephen J Foster
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 Sabia Inc, Clinton L Lingren, David B Cook, James F Miller, Stephen J Foster filed Critical Sabia Inc
Priority to AU2003234658A priority Critical patent/AU2003234658A1/en
Publication of WO2003102574A1 publication Critical patent/WO2003102574A1/en
Publication of WO2003102574B1 publication Critical patent/WO2003102574B1/en

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T3/00—Measuring neutron radiation
    • G01T3/06—Measuring neutron radiation with scintillation detectors
    • 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
    • G01N23/221—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 activation analysis
    • G01N23/222—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 activation analysis using neutron activation analysis [NAA]
    • 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
    • G01N23/225—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 using electron or ion
    • G01N23/2255—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 using electron or ion using incident ion beams, e.g. proton beams
    • 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
    • G01N2223/074—Investigating materials by wave or particle radiation secondary emission activation analysis
    • G01N2223/0745—Investigating materials by wave or particle radiation secondary emission activation analysis neutron-gamma activation analysis

Abstract

A substance analyzer (110) utilizing Prompt Gamma Neutron Activation Analysis for identifying characteristics of a substance and method of manufacturing the same are disclosed. The analyzer (110) is small enough to be portable and to allow its use in many applications where current analyzers cannot be utilized. The analyzer (110) uses a neutron radiation source (120) and a gamma-ray detector (140) to activate the sample material (130) and detect the prompt gamma rays emitted by the sample material (130). A novel housing for such an analyzer and method for making the housing are also described. Novel methods of operating such an analyzer including via a communications network are also disclosed. Also disclosed are data analysis methods that improve the accuracy and sensitivity of the results of such material analysis.

Claims

[received by the International Bureau on 09 January 2004 (09.01.04); remaining claims unchanged (11 pages)] original claims 25, 48 and 51 amended ;
24. The substance analyzer of Claim 22, wherein the neutron absorbing material comprises at least one substance selected from the group consisting of: boron, indium, cadmium, gadolinium, hafnium, samarium, europium, dysprosium, rhodium, erbium, thulium, iridium, platinum, or gold.
25. A material analyzer for detecting the elemental composition of a bulk material comprising: a radioactive source adapted to emit neutrons; a sample volume having an open entrance end and an open exit end and adapted to convey a flow of cement clinker; a first composition of material adapted to moderate, shield and reflect radiation emitted by the source, wherein the cement clinker absorbs neutrons emitted by the source and then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the at least one gamma ray; and a housing comprising an outer container and an inner container, said housing adapted to contain the source, the detector, the sample volume, the flow of cement clinker and the first composition of material, wherein the flow of cement clinker enters the sample volume via the entrance end and exits the sample volume via the open exit end.
26. The material analyzer of Claim 25, wherein the generally cylindrical sample volume is a pipe extending substantially longitudinally through the analyzer.
27. The material analyzer of Claim 26, wherein the material being analyzed is a flow of geological survey materials.
28. The material analyzer of Claim 26, wherein the material analyzed is a flow of mining tailings.
29. The material analyzer of Claim 26, wherein the pipe is made of Acrylonitrile-Butadiene-Styrene.
30. The material analyzer of Claim 26, wherein the pipe is made of iron.
31. The material analyzer of Claim 27, wherein at least a portion of the pipe extending through the active region of measurement is made of reactor-grade zirconium.
32. A material analyzer for detecting the elemental composition of a coal slurry comprising: a source of neutrons;
-33- a sample volume having an open entrance end and an open exit end adapted to convey a flow of the coal slurry; a composition of material adapted to moderate, shield and reflect neutrons emitted by the source, wherein neutrons emitted by the source are absorbed by the coal slurry, which then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the at least one gamma ray emitted by the coal slurry; and a housing having an entrance side and an exit side and that is adapted to contain the source, the detector, the sample volume, the flow of the coal slurry and the composition of material, wherein the sample volume extends within the housing from the entrance to the exit, wherein the coal slurry enters the sample volume via the entrance end and exits the sample volume via the exit end, and wherein the housing comprises an outer container and an inner container.
33. The material analyzer of Claim 32, wherein the sample volume is generally rectangular.
34. The material analyzer of Claim 32, wherein the outer container is a first commercial storage drum.
35. The material analyzer of Claim 34, wherein the inner container is a second commercial storage drum that is smaller than the first commercial storage drum.
36. The material analyzer of Claim 35, wherein the inner container is made of polyethylene.
37. The material analyzer of Claim 35, wherein a gap is formed between the inner container and outer container, and wherein the gap contains shielding material.
38. A gamma radiation detector for detection of gamma rays emitted by bulk material to be analyzed in a material analyzer that detects the elemental composition of the bulk material, comprising: a scintillation crystal adapted to emit a photon upon interaction of the gamma rays to be detected with an electron of the crystal; a photon detector having an excitation energy and adapted to develop electrical signals in response to photons emitted by the scintillation crystal, wherein the excitation energy is reduced to a relatively low level to minimize heat generated by the detector; and
-34- insulation adapted to surround and contain the crystal and the photon detector, and adapted to prevent the transfer of heat energy between either of the bulk material and the environment and the photon detector.
39. A radiation source holder for use in a substance analyzer, comprising: a generally elongated holder body having a source end and a locking end; a plurality of receptacles in the holder body, said receptacles located proximate to the source end, wherein each of the plurality of receptacles is adapted to receive a radioactive source and wherein each of the plurality of receptacles is positioned adjacent to the others of said receptacles; and a locking mechanism engaged with the locking end of the holder body.
40. The radiation source holder of Claim 38, comprising at least two receptacles.
41. A system for analyzing bulk substances, comprising: a memory adapted to store digital information; a bulk substance analyzer adapted to develop electrical signals corresponding to a material sample being analyzed; a converter adapted to convert the electrical signals from the analyzer into digital information; and a processor adapted to store the digital information to and retrieve the digital information from the memory, wherein the processor is further adapted to process the digital information, and wherein the memory and processor are adapted to store unprocessed raw data for subsequent retrieval and processing.
42. The system of Claim 41, wherein the converter is an analog to digital converter.
43. The system of Claim 41, wherein the converter also includes a digital-to- analog converter.
44. The system of Claim 41, further comprising: a parallel processor adapted to coordinate with the processor to perform algorithms; an input/output module adapted to coordinate and control a flow of information into the computer and further adapted to control a flow of information out of the computer; an input mechanism adapted to provide information and instructions to the computer; a power supply adapted to provide electrical energy to the computer and to a nuclear bulk materials analyzer; and an output module adapted to receive an output signal from the input/output module.
45. The system of Claim 44, wherein the output module comprises a monitor.
46. The system of Claim 44, wherein the output module comprises a web server.
47. A substance analyzer for identifying characteristics of a sample of a substance, comprising: a source of neutrons; a sample volume adapted to contain the sample of the substance; a first composition of material adapted to moderate, shield and reflect any neutrons emitted by the at least one source, wherein neutrons emitted by the at least one source are absorbed by the sample, and wherein the sample then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the at least one gamma ray emitted by the sample; a housing adapted to contain the source, the detector, the sample volume, the sample and the composition of material; and a load cell adapted to develop an electrical signal corresponding to a mass of the sample contained in the sample volume.
48. A substance analyzer for identifying characteristics of a sample of a substance, comprising: a source of neutrons; a sample volume adapted to contain the sample of the substance; a composition of material adapted to moderate, shield and reflect any neutron radiation emitted by the source, wherein neutrons emitted by the source are absorbed by the sample, and wherein the sample then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the at least one emitted gamma ray;
-36- a housing having a generally longitudfhal axιs~and~adapted to contain the source, the detector, the sample volume, the sample and the composition of material; and an elevator adapted to displace the sample in the sample volume generally parallel to the longitudinal axis of the housing.
49. A substance analyzer for identifying characteristics of a sample of a substance, comprising: a source of neutrons; a sample volume adapted to contain the sample of the substance; a composition of material adapted to moderate, shield and reflect any neutron radiation emitted by the source, wherein neutrons emitted by the source are absorbed by the sample, and wherein the sample then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the emitted at least one gamma ray; a generally cylindrical housing adapted to contain the source, the detector, the sample volume, the sample and the composition of material; and a rotator, adapted to rotate the sample in the sample volume.
50. A sample holder for use in a nuclear substance analyzer that identifies the characteristics of a substance, the sample holder comprising a generally tubular container having a closed end and an open end, wherein the container is made of pipe having an outer diameter and an inner diameter.
51. A system for three-dimensional surveying of a concentration of various elements in the earth, comprising: a portable material analyzer adapted to analyze the concentration of elements; a drill adapted to extract a plurality of material samples from the earth; means for correlating material analyses to a respective drill depth of each of the plurality of material samples by performing at least one of the acts of recording drill depth associated with each sample, and determining bit height corresponding to the removal location of the associated sample.
52. The system of Claim 51, wherein the correlating means is a drill depth gage.
-37-
53. The system , of Claim 51, wherein the system further comprises a geographical map adapted to correlate a drill location of each of the plurality samples with a geographical location, and wherein each of the plurality of samples are analyzed to produce a data set representing the concentration of the elements in each of the samples.
54. A portable substance analyzer for identifying the characteristics of a sample of a substance, comprising: a source of neutrons; a sample volume adapted to contain the sample of the substance; a composition of material adapted to moderate, shield and reflect any neutron radiation emitted by the source, wherein neutrons emitted by the source are absorbed by the sample, and wherein the sample then emits at least one gamma ray; a gamma radiation detector adapted to develop electrical signals in response to detection of the at least one emitted gamma ray; and a generally cylindrical housing adapted to contain the source, the detector, the sample volume, the sample and the composition of material, wherein the housing is generally less than 50 inches tall and generally less than 40 inches in diameter.
55. A system for operating a substance analyzer, comprising: a sample analyzer adapted to determine an elemental composition of a bulk substance sample; a computer adapted to process data received from the sample analyzer; a communications network; a plurality of workstations adapted to communicate via the communications network; and a communications server that is responsive to commands from the computer and the workstations, wherein the communications server is adapted to control a plurality of network resources.
56. A method of analyzing bulk substances in real-time, comprising: forming a sample volume with a pipe; inserting a sample of substance into the sample volume; placing a neutron source adjacent to the pipe;
. -38- . placing a gamma radiation detector adjacent to the pipe at a location along the pipe that generally corresponds to a location of the radioactive source; housing the sample volume, the sample, the radiation source and the radiation detector in a container; and analyzing a set of data developed by the radiation detector.
57. The method of Claim 56, wherein the pipe is standard ABS pipe.
58. The method of Claim 56, wherein the pipe is standard iron pipe.
59. A method of manufacturing a housing for a real-time nuclear element analyzer comprising: forming an inner surface with an inner container having a first diameter; forming an outer surface with an outer container having a second diameter that is larger than the first diameter; and depositing a pourable housing material into a space formed between the inner surface and the outer surface.
60. A method of removing pulse pileup from a data spectrum collected from a material analyzer, comprising: selecting a spectrum of collected data to be analyzed; determining a count rate for the selected spectrum of data; calculating a theoretical spectrum of data from the count rate by: assuming the selected spectrum of data was unpiled data; identifying average pileup values from reference sources for that count rate; and piling up the selected spectrum to a theoretical piled up spectrum of data using the identified values; subtracting the selected spectrum of data from the theoretical piled up spectrum of data to estimate a theoretical pileup; and subtracting the theoretical pileup from the selected spectrum of collected data.
61. A method of adjusting a gain and an offset from a selected spectrum of data representing the composition of materials in a material sample, comprising: selecting a spectrum of data to be analyzed; finding recognizable peaks in the selected spectrum of data; and
-39- applying least squares fit to the selected spectrum of data to define gain and offset correction factors for the measured peaks.
62. The method of Claim 61, wherein a step of filtering data to remove any extraneous data points is performed after selecting a spectrum of data.
63. The method of Claim 61 , further comprising: resampling the selected spectrum of data using the gain and offset correction factors to derive a resampled spectrum of data; performing multiple linear regression on the resampled spectrum of data to determine a polynomial equation having coefficients; and applying a calibration polynomial to the polynomial equation to develop a set of analysis results.
64. A method of finding a plurality of recognizable data peaks in the analysis of a spectrum of data from a real-time substance analyzer, comprising: determining the instantaneous first derivative over the entire data spectrum to develop a set of derivative results; taking an average of the set of derivative results; selecting and applying a scale factor to the derivative results to develop a scaled spectrum of data; and locating a plurality of peaks by comparing the scaled spectrum of data to the average of the derivative results to develop a peak count.
65. The method of Claim 64, wherein a step of smoothing the set of derivative results to develop a set of smoothed results is performed after the step of determining the instantaneous first derivative over the entire data spectrum.
66. The method of Claim 64, further comprising determining whether the peak count falls within a predetermined range, wherein if the peak count is not within the predetermined range, then the selecting and locating steps are repeated until the peak count is within the predetermined range such that a recognizable energy peak can be located.
67. A method of stabilizing the performance of a neutron activation material analyzer used to produce a spectrum of data, comprising: insulating a detector against heat transfer; and
-40- lowering an amount of heat genei tted in the "detector, wherein said' lowering is accomplished by reducing an excitation energy in the detector and by using low energy consuming electronic components.
68. A method of analyzing the elemental composition of a bulk material sample in a static sample analyzer, comprising: generating a signal representing gamma radiation emitted from the sample; measuring the weight of the sample being analyzed; and generating a signal representing the mass of the sample being analyzed.
69. A method of analyzing the elemental composition of a bulk material sample in a bulk material analyzer, comprising: generating a signal representing gamma radiation emitted from the sample; and rotating the sample in the analyzer during an analysis period.
70. A method of analyzing the elemental composition of a bulk material sample in a bulk material analyzer, comprising: generating a signal representing gamma radiation emitted from the sample; and elevating a sample in the analyzer during an analysis period.
71. A method of surveying the elemental composition of a portion of the earth, comprising: drilling a hole in the surface of the earth from which a material sample is extracted; determining a geographical position of the hole; determining a depth from which the sample was extracted; analyzing one or more characteristics of the sample using a portable material analyzer located substantially near the drill site; and correlating a set of analysis data with the depth and geographical position of the sample.
72. The method of Claim 71, wherein the survey is performed in real-time as the analyzing step is performed substantially at the time the sample is taken.
73. A method of manufacturing a sample container for use in a bulk material static sample analyzer, comprising: cutting a length of standard pipe having a top end and a bottom end; and
-41- attaching a bottom to the bottom end of the length of pipe.
74. A method of operating a bulk material analyzer with a communication network, comprising: connecting the analyzer to a computer adapted to operate the analyzer and receive and store data from the analyzer; connecting the computer to a communication network; and connecting a plurality of remote units to the communication network, wherein the remote units are capable of transmitting a plurality of command signals to the computer via the communication network and the server, to operate the analyzer.
75. A method of operating a bulk material analyzer with a communication network, comprising: activating the analyzer to analyze a sample of material contained in the analyzer; retrieving raw data from the analyzer; storing the raw data; selecting a portion of the stored raw data to be analyzed; determining offset and gain correction factors from the selected portion of data; determining at least one characteristic of the sample of material from the spectrum of data; and outputting the at least one characteristic, wherein the activating and outputting steps are performed over a communications network.
76. The method of Claim 75, wherein the communications network comprises the Internet and wherein the activating and outputting steps are actuated by signals transmitted over the Internet using a remote workstation.
77. A bulk material analyzer for analyzing material carried on a conveyor having first and second sides, wherein the analyzer comprises at least one neutron radiation source located on the first side and at least one detector located on the first side.
78. A bulk material analyzer for analyzing material carried on a conveyor having first and second sides, the analyzer comprising: at least one source located on one of the first and second sides of the conveyor and adapted to emit neutrons;
-42- a composition ot material adapted to moderate, shield and reflect the neutrons, wherein said neutrons emitted by the source are absorbed by the bulk material, and wherein the bulk material then emits at least one gamma ray; and a gamma radiation detector located on one of the first and second sides of the conveyor and adapted to develop electrical signals in response to detection of the at least one emitted gamma ray, wherein the at least one source and the detector are both located on the same side of the conveyor.
79. The analyzer of Claim 78, wherein the conveyor is a conveyor belt system.
80. The analyzer of Claim 78, wherein the conveyor is a conveying tube.
81. The analyzer of Claim 78, wherein the at least one source is located in a separate structure from the detector.
82. The analyzer of Claim 78, wherein the first side is below the conveyor and the second side is above the conveyor.
83. The analyzer of Claim 78, further comprising at least two sources.
84. The analyzer of Claim 78, wherein the at least one source is housed in a first structure, and wherein the detector is housed in a second structure.
85. The analyzer of Claim 78, wherein the composition of material further comprises a reflector material adapted to direct the neutrons onto the material being analyzed.
86. The analyzer of Claim 78, further comprising a pivot adapted to rotate the detector.
87. The analyzer of Claim 81, further comprising a pivot adapted to rotate a detector housing about an axis.
88. A material analyzing system for analyzing a bulk material, comprising: an on-line bulk material analyzer; and a sampling mechanism for directing a flow of the bulk material through the on-line bulk material analyzer.
-43-
PCT/US2003/016702 2002-06-03 2003-05-27 Method and apparatus for analysis of elements in bulk substance WO2003102574A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003234658A AU2003234658A1 (en) 2002-06-03 2003-05-27 Method and apparatus for analysis of elements in bulk substance

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US38592602P 2002-06-03 2002-06-03
US60/385,926 2002-06-03
US10/222,726 US7152002B2 (en) 2002-06-03 2002-08-16 Method and apparatus for analysis of elements in bulk substance
US10/222,726 2002-08-16

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WO2003102574B1 true WO2003102574B1 (en) 2004-03-04

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AU2003234658A1 (en) 2003-12-19
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US7778783B2 (en) 2010-08-17
US20030225531A1 (en) 2003-12-04
US20070095157A1 (en) 2007-05-03

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