CN101349662B - Portable metallic element analyzer - Google Patents

Portable metallic element analyzer Download PDF

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Publication number
CN101349662B
CN101349662B CN2008100132236A CN200810013223A CN101349662B CN 101349662 B CN101349662 B CN 101349662B CN 2008100132236 A CN2008100132236 A CN 2008100132236A CN 200810013223 A CN200810013223 A CN 200810013223A CN 101349662 B CN101349662 B CN 101349662B
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ray
shutter body
ray shutter
radioactive source
scallop hole
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CN2008100132236A
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CN101349662A (en
Inventor
张伟
龚亚林
侯朝勤
尹毅强
卢元利
尹德有
尚庆敏
刘辉
周洪军
赵晶
李岩峰
于海明
蒋宝庆
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Dandong Dongfang Measurement and Control Technology Co Ltd
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Dandong Dongfang Measurement and Control Technology Co Ltd
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Abstract

The invention relates to a portable metallic element analyzer, which analyzes the composing components and the relative contents thereof of various metallic elements in ores through character X-ray spectrums which are triggered out from various metallic elements by a computer according to the Moseley's law, and obtains metallic elements which are contained in ores and the contents of various metallic elements. A radioactive source and a detector conserve the final character X-ray spectrums through shielding a collimator and processing by multi-channel pulsed signals, and the final character X-ray spectrum is transmitted to a notebook computer through a USB interface immediately or after a period, and the species and the content of metallic elements which are contained in ores are finally got through spectrum deconvolution software to analyze the shape of the spectrum. The portable metallic element analyzer can directly measure ores in fields, which is convenient to carry and use, and the accuracy is high.

Description

A kind of portable metallic element analyzer
Technical field
The present invention relates to a kind of metallic element analysis device, relate to a kind of X-ray analysis measuring instrument specifically.
Technical background
The field of non-ferrous metal industry mine locating at present, mining generally all are that the scout samples in the open air on the spot, take back the laboratory then and carry out fragmentation, grinding, screening, carry out chemical analysis then.By the constituent content data of sample ore and the distribution of sampling spot, determine mineral ore, perhaps whether decision is worth exploitation.But when sampling, the constituent content of this place's ore that can't know for sure can only be judged by experience, and the result has caused the low ore of a lot of useful element content by acquisition process, causes waste, has also delayed the time.
And present existing hand-held x-ray fluorescence analyzer, the content that is primarily aimed at several element-specific (mostly being Cd, Cr, Pb, Hg, Br) is analyzed, and can not analyze containing which unknown element in the ore.And the excitaton source that is adopted is X-ray tube, needs the operating voltage of several ten thousand volts when work, brings certain danger for the hand-held person, and increased power consumption, reduced the service time under the no external power supply condition.The detector that is adopted also mostly is proportional counter tube in addition, and energy resolution is not high, and the Measurement and analysis precision is low.
Summary of the invention
At above problem, the invention provides a kind of easy to carryly, can directly analyze metallic element in the ore, have the ore metallic element analysis pick-up unit of high energy resolution.
The technical solution adopted in the present invention is: a kind of portable metallic element analyzer: USB interface (8) is housed being shaped on the handle housing (9) of handle, measure button (7), shielding collimator (3) is equipped with in the bottom in housing, ray shutter body (4) is housed in shielding collimator (3), shielding collimator (3) inwall is shaped on scallop hole (31), have a scallop hole (41) in the inner of ray shutter body (4), radioactive source (1) is installed in ray shutter body (4) top, at shielding collimator (3) opposite side detector (2) is housed, in radioactive source (1) one side battery (6) is housed, in detector (2) one sides circuit board (5) is housed, battery (6) output terminal connects the power input of circuit board (5), the power output end of circuit board (5) connects detector (2), the signal output part of detector (2) connects the signal input part of circuit board (5), and the signal output part of circuit board (5) connects computing machine (10) by USB output interface (8).
A kind of portable metallic element analyzer of the present invention is square to be certain linear according to the energy of the characteristic X-ray of different elements and this Atom of Elements, by detecting the energy of the characteristic X-ray that each element is inspired in the ore, tell and contain which element kind; By the intensity of this elemental characteristic X ray, analyze the content of this element.
Radioactive source and detector are fixed in the radiation collimation shield assembly according to certain relative position, and the angle that guarantees the two is less than 60 degree.The radiation collimation shield is made of heavy metal lead, can well block effect to ray.
The radiation collimation shield fixedly is being equipped with a ray shutter body before the source positions, the ray shutter body can be twitched, and have a scallop hole in the inner, after the ray shutter body is outwards twitched, scallop hole is over against radioactive source, and ray can become the covering of the fan radiation, and the ray shutter body of extracting out triggers the total power switch of instrument simultaneously, the detector power supply begins to start, and begins detector is freezed.Inwardly twitch to reference position when the ray shutter body, fan shape hole is removed radioactive source, and ray can't give off instrument, and general supply is closed.
The radiation collimation shield assembly has a scallop hole in the detector front.In the purpose of radioactive source and detector front scalloping, be to be measured to certain area respectively for the analyte that makes the detector below.In scallop hole, cover one deck light metal separation layer, lead is sheltered from, can avoid lead in the radiation collimation shield assembly to be subjected to rays excite and send characteristic X-ray and influence instrument measurement.
In the bottom of instrument, the plastics system back up pad of a hollow is housed, guarantee that relative radioactive source of analyte and position of detector are certain when measuring.
During measurement, the ray shutter body is outwards twitched, trigger the instrument general supply, again instrument is positioned on the object being measured stably, the perhaps hand-held outside surface of instrument being close to measured object.This moment, the x radiation x that sends of radioactive source was to measured object, inspired the feature X fluorescence of various elements in the object, and was detected device and receives.Treat in stable condition after, press the measurement button in instrument handle the place ahead, instrument begins to measure.
Measure beginning, the detector signal treatment circuit is started working, the signal of detector output is handled, the pulse signal that the ray energy that formation amplitude and detector receive is proportional, and the paired pulses amplitude is differentiated identification, the total quantity of same magnitude pulse is accumulated in together, and finally forming a transverse axis is that pulse height (corresponding energy), the longitudinal axis are the collection of illustrative plates of pulse number.
Timing circuit by gauge internal picks up counting, and after Measuring Time reaches default time span, measures and finishes.The collection of illustrative plates that instrument will finally acquire is stored in the storage unit in the circuit.Immediately or after a period of time be transferred to notebook computer by USB interface, come collection of illustrative plates is carried out analyzing and processing by the executive routine of pre-installing in the notebook computer again.
Determine by location, road, extrapolate the energy of character pair X fluorescent x ray,, determine to contain in the measured object which element according to the energy of feature X fluorescence and the corresponding relation of different elements to each peak position in the collection of illustrative plates.
Determine the content H of this element according to following experimental formula by peak area:
H=∑(Ai·S i)+B·S 0+C
S wherein iI characteristic X-ray peak area for this element; S 0Be radioactive source ray scattering peak area.Ai, B, C are undetermined coefficient.Determining of these coefficients can be demarcated by the measurement to the simulation print of corresponding element different proportioning.
Concrete scaling method is: by the measurement to difference simulation print, note the content of corresponding certain element and i characteristic X-ray peak area S of this element iAnd radioactive source ray scattering peak area S 0, by the nonlinear fitting method of routine, undetermined coefficient Ai, the B, the C that obtain in the formula get final product.
To the corresponding relation of location, peak position road and energy in the collection of illustrative plates, can judge by following calibration mode:
Measurement by to A, two kinds of known different elements of B can obtain individual features peak position road location N respectively AAnd N B, the characteristic X-ray ENERGY E of their respectively corresponding A, B element A, E BThen the corresponding relation of location, road N and ENERGY E can be determined according to following formula:
E = E A - E B N A - N B × N + E A N B - E B N A N B - N A
Characteristics of the present invention are simple in structure, and easy operating is easy to carry, and use powered battery, can preserve the collection of illustrative plates that measures, and wait to return back input computer and handle, or be transferred to analyzing and processing in the notebook computer at any time, are particularly suitable for open-air the use.
The present invention mainly is applicable to the open-air mine locating of non-ferrous metal, also can be used in stockpile, the ore storage bin composition and constituent content analysis to ore, breeze.
Description of drawings:
Fig. 1 is a structural representation of the present invention
Fig. 2 is that the ray shutter body of the A-A view among Fig. 1 is twitched the effect synoptic diagram
Among the figure: 1 radioactive source, 2 detectors, 3 shielding collimators, 4 ray shutter bodies, 5 circuit boards, 6 batteries, 7 measure button, 8USB output interface, 9 handle housings, 10 computing machines, 31 shielding collimator scallop holes, 41 ray shutter body scallop holes, 42 separation layers.
Embodiment:
Specify structure of the present invention and using method in conjunction with the accompanying drawings.Structure is seen Fig. 1.
Measure button 7 being shaped on to be equipped with on the handle housing 9, at handle housing 9 rears USB output interface 8 is housed, USB output interface 8 connects computing machine 10, bottom in housing, shielding collimator 3 is housed, in shielding collimator 3, have scallop hole 31, shielding collimator 3 is made shield by heavy metal, on shielding collimator scallop hole 31 inwalls, be covered with the thick aluminium matter of 2mm separation layer, the purpose of scalloping be make ray that radioactive source 1 sends can irradiation to the certain area of measured object, in be sidelong an aluminium lamination purpose be measurement to be brought influence for characteristic X-ray that the lead that reduces in the shielding collimator 3 is inspired.Fixedly radioactive source 1 and detector 2 in shielding collimator 3, the ray that 3 pairs of radioactive sources 1 of shielding collimator send carries out shielding protection, ray can only be propagated in certain spatial dimension, detector 2 is protected, the ray that radioactive source 1 is sent can not shine directly on the detector 2, and the various characteristic X-rays that send after having only measured object to be stimulated just can be detected device 2 and receive.Excitaton source adopts the isotope radioactive source, need not power supply, is fit to field work; Detector adopts the Si-PIN detector of high-performance, electricity refrigeration, can have higher energy resolution by the electricity refrigeration under the normal temperature state.
Ray shutter body 4 is housed in shielding collimator 3, and the installation site is below radioactive source 1.Have ray shutter body scallop hole 41 in the inner of ray shutter body 4, ray shutter body 4 is made shield by heavy metal, on the scallop hole inwall, be covered with the separation layer 42 of light metal, ray shutter body 4 is made by lead, the separation layer 42 of scallop hole inwall is the thick aluminum hull of 2mm, and its effect is identical with the effect of scallop hole in the shielding collimator 3.
Ray shutter body 4 can be twitched in shielding collimator 3, sees Fig. 2.After ray shutter body 4 is outwards twitched, trigger battery main switch, the power supply of detector 2 and cryogenic temperature pick-up unit are started working; Simultaneously the aperture of scallop hole is tiny rectifies radioactive source 1, makes that ray that radioactive source 1 sends can be according to the covering of the fan of scallop hole to external radiation.After ray shutter body 4 inwardly inserted, power switch was closed, and instrument quits work; Scallop hole is removed radioactive source 1, and radioactive source 1 is shielded fully, radiationless leaking outside.
Circuit board 5 is installed in the handle housing 9 according to shown position with battery 6, battery 6 output terminals connect the power input of circuit board 5, the power output end of circuit board 5 connects detector 2, the signal output part of detector 2 connects the signal input part of circuit board 5, and the signal output part of circuit board 5 connects computing machine 10 by USB output interface 8.Conventional power circuit, temperature sensing circuit, timer, pulse shaping amplification circuit, pulse height discriminator circuit, counter, memory module are housed on the circuit board.For detector provides working power, detects temperature in the detector, the Measuring Time timing, the signal of detector output is amplified the amplitude of shaping, identification pulse and is accumulated to corresponding address, preserves data.Immediately connect by USB output interface 8, perhaps connect with common desk-top computer after a period of time, by the application software in the computer collection of illustrative plates of preserving is accessed, and carry out analyzing and processing with notebook computer.
When detecting use, ray shutter body 4 outwards to be extracted out, master switch is opened, and detector power supply and refrigeration and temperature detection part are started working; Instrument is fixedly put steady or hand-held, and the lower surface and the measured object of instrument are close to; Treat in stable condition after, press and measure button 7, measure beginning, signal processing circuit is started working; Timing circuit by gauge internal picks up counting, and after Measuring Time reaches default time span, measures and finishes, and the collection of illustrative plates that the storage unit in the circuit will finally obtain is stored.
By the location, road of each peak position in the collection of illustrative plates is determined, extrapolate the energy of character pair X fluorescent x ray, which kind of element what determine correspondence according to the energy of characteristic X-ray is.To the corresponding relation of location, peak position road and energy in the collection of illustrative plates, can judge by following calibration mode:
Measurement by to A, two kinds of known different elements of B can obtain individual features peak position road location N respectively AAnd N B, the characteristic X-ray ENERGY E of their respectively corresponding A, B element A, E BThen the corresponding relation of location, road N and ENERGY E can be determined according to following formula:
E = E A - E B N A - N B × N + E A N B - E B N A N B - N A
Determine the content H of this element according to following experimental formula by the respective peaks area:
H=∑(Ai·S i)+B·S 0+C
S wherein iI characteristic X-ray peak area for this element; S 0Be radioactive source ray scattering peak area.Ai, B, C are undetermined coefficient.
And suitably select suitable excitation ray energy, and can be the principal ingredient of ore of the same race be more not analyzed, improve accuracy of detection.
Application example:
Molybdenum ore generally all association metallic elements such as iron, copper, lead, tungsten are arranged, some even content are more taller than molybdenum.Therefore when the ground observation of molybdenum ore, not only to pay close attention to the height of molybdenum content in the ore, also to know and also contain which available metallic element in the ore in addition, and their content, so that correctly carry out qualitative to the character of ore, determine mineral ore, to have given play to the maximum economic benefit of ore.
The energy of the characteristic X-ray of these metallic elements following (unit K eV):
Element term The symbol of element Atomic number K α energy K β energy L α energy L β energy The L gamma energy
Molybdenum Mo 42 17.478 19.607 ? ? ?
Iron Fe 26 6.403 7.057 ? ? ?
Copper Cu 29 8.047 8.904 ? ? ?
Plumbous Pb 82 ? ? 10.549 12.611 14.762
Tungsten W 74 ? ? 8.396 9.670 11.283
Therefore select 0.25mm stainless steel window, 1.85 * 10 9Bq's 241The Am radioactive source has the higher launching efficiency of above elemental characteristic X ray.And the half life period reach 458 years, so the influence to measurement result that radioactive source self decay is brought can be ignored.
And the content of molybdenum can be according to formula
H Molybdenum=A1S K α molybdenum+ A2S K β molybdenum+ BS 0+ C
Try to achieve.S wherein K α molybdenumFor the K α of molybdenum is the characteristic X-ray peak area, S K β molybdenumFor the K β of molybdenum is the characteristic X-ray peak area, S 0For 241The scattering peak area of Am.A1, A2, B, C are the formula coefficient, can pass through the measurement result for the simulation print of equivalent different Cu grade, try to achieve through nonlinear regression and fitting.By measurement that one group of molybdenum ore is experimentized, can obtain relevant parameters:
A1=0.019816?A2=0.026924?B=0.067624?C=—1.22169
Similarly, Qian content can be according to formula
H Plumbous=A1S L α lead+ A2S L β lead+ A3S L γ lead+ BS 0+ C
Try to achieve.S in the formula L α leadFor the L α of lead is the characteristic X-ray peak area, S L β leadFor the L β of lead is the characteristic X-ray peak area, S L γ leadFor the L γ of lead is the characteristic X-ray peak area, S 0For 241The scattering peak area of Am.A1, A2, A3, B, C are undetermined coefficient.

Claims (3)

1. portable metallic element analyzer, it is characterized in that: USB interface (8) is housed being shaped on the handle housing (9) of handle, measure button (7), shielding collimator (3) is equipped with in the bottom in housing, in shielding collimator (3) one sides ray shutter body (4) is housed, opposite side is equipped with Si-PIN detector (2), shielding collimator (3) inwall is shaped on shielding collimator scallop hole (31), the shielding collimator scallop hole is below the Si-PIN detector, in ray shutter body (4), have a ray shutter body scallop hole (41) that runs through whole ray shutter body, isotope radioactive source (1) is installed in ray shutter body (4) top, after ray shutter body (4) is outwards twitched, the aperture of ray shutter body scallop hole is tiny rectifies isotope radioactive source (1), make ray that isotope radioactive source (1) sends according to the covering of the fan of ray shutter body scallop hole to external radiation, after ray shutter body (4) inwardly inserts, ray shutter body scallop hole is removed isotope radioactive source (1), isotope radioactive source (1) is shielded fully, in isotope radioactive source (1) one side battery (6) is housed, in Si-PIN detector (2) one sides circuit board (5) is housed, the power input of battery (6) output terminal connecting circuit plate (5), the power output end of circuit board (5) connects Si-PIN detector (2), the signal input part of the signal output part connecting circuit plate (5) of Si-PIN detector (2), the signal output part of circuit board (5) connects computing machine (10) by USB output interface (8).
2. according to claim 1 portable metallic element analyzer, it is characterized in that: said shielding collimator is made shield by heavy metal, is covered with the separation layer of light metal on shielding collimator scallop hole inwall.
3. according to claim 1 portable metallic element analyzer, it is characterized in that: said ray shutter body (4) is made shield by heavy metal, is covered with the separation layer of light metal on ray shutter body scallop hole inwall.
CN2008100132236A 2008-09-17 2008-09-17 Portable metallic element analyzer Expired - Fee Related CN101349662B (en)

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Publication number Priority date Publication date Assignee Title
CN103592323A (en) * 2013-11-15 2014-02-19 株洲硬质合金集团有限公司 Method for analyzing and detecting solid solubility of tungsten in cemented carbide binding phase
CN104267056A (en) * 2014-10-15 2015-01-07 苏州工业职业技术学院 X-ray fluorescence tester for testing heavy metal pollution of soil
CN106990122A (en) * 2017-05-11 2017-07-28 北京中矿东方矿业有限公司 A kind of qualitative automatic identifier of tenor of ore
CN107884425A (en) * 2017-12-26 2018-04-06 同方威视技术股份有限公司 System and method for mineral products constituent analysis
CN109596653A (en) * 2018-12-25 2019-04-09 贵州大学 A kind of ensaying device of mining industry

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