CN109342479A - Monochromatic focusing X-ray light source and the method that Lead in low quantity arsenic is analyzed using the light source - Google Patents
Monochromatic focusing X-ray light source and the method that Lead in low quantity arsenic is analyzed using the light source Download PDFInfo
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- CN109342479A CN109342479A CN201811495391.3A CN201811495391A CN109342479A CN 109342479 A CN109342479 A CN 109342479A CN 201811495391 A CN201811495391 A CN 201811495391A CN 109342479 A CN109342479 A CN 109342479A
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- 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
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- 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
Abstract
The present invention discloses a kind of monochromatic focusing X-ray light source and the method using light source analysis Lead in low quantity arsenic, light source includes ray emission mechanism, preceding light bar, focusing ring and rear light bar, preceding light bar is arranged corresponding to ray emission mechanism, focusing ring is arranged in front of preceding light bar, light bar is arranged in front of focusing ring afterwards, focusing ring inner surface on the inside of focusing ring uses drum organization, and preceding light bar focuses ring inner surface and the coaxial arrangement of rear light bar, and axle center and the central axes of ray emission mechanism coincide.The present invention images X using cydariform condenser and carries out monochromatic, convergence, to form high-intensitive monochromatic light, can detect to low content arsenic element.The X-ray of irradiating sample of the present invention absorbs limit 11.867keV just above the K of arsenic element, can efficiently excite the characteristic X-ray of arsenic element but not excitation lead element, it is entirely avoided the interference of lead element characteristic fluorescence.
Description
Technical field
The present invention discloses a kind of X-ray source and its application, especially a kind of monochromatic focusing X-ray light source and uses the light
The method of source analysis Lead in low quantity arsenic.
Background technique
In social production and people's lives, it is often necessary to analyze, detect harmful element, most common quick detection
Method is x ray fluorescence spectrometry, and used instrument is Xray fluorescence spectrometer.
Xray fluorescence spectrometer (i.e. X-Ray Fluorescence Spectrometer, be often simply called XRF) is used as one
Kind Fast nondestructive evaluation tool, is widely used in harmful element detection field.Its principle is: X-ray fluorescence spectra analytic approach
(X-Ray Fluorescence) is to be allowed to generate fluorescence (secondary using the atom in primary X-ray photons excitation test substance
X-ray) and the method that carries out elemental analysis.When x-ray photon irradiate object when, it may occur that including heat, transmission, scattering,
Interaction including photoelectric effect etc., wherein the fluorescent X-ray in photoelectric effect can be used to do elemental analysis.It please refers to attached
Fig. 1, when the combination that x-ray photon energy is greater than atom inner electron in irradiated object can (Binding Energy, this energy
Also referred to as absorb limit) when, transition occurs after the radiation energy of the inner electron RESONANCE ABSORPTION ray of core, and in internal layer electron orbit
On leave a hole, outer-shell electron in upper state jumps back to the hole of lower state, by superfluous energy in the form of X-ray
It releases, generated X-ray is the x-ray fluorescence spectral line for representing each element feature, and referred to as characteristic X-ray, energy is equal to
The specific electronics interlayer transition energy of the energy level difference of atom inner-shell electron, i.e. atom.
The symbol representation method common first names (Siegbahn) of characteristic X-ray are named according to transition situation, such as to K layers of transition
It is K linear system, including K α (L layers to K layers of transition), K β (being typically M layers to K layers of transition), is L linear system to L layers of transition.Feature
The relative intensity of X-ray spectral line is generally K linear system intensity > L linear system intensity > M linear system intensity, (typical with intensity K α > K β in linear system
K α and K β intensity than being about 15:2), L α > L β (typical L α and L β intensity are than being about 4:3) selects stronger feature in principle
X-ray spectral line performs an analysis.X-ray fluorescence method is to identify element (qualitative) according to the energy of characteristic X-ray, and according to this
Element x-ray fluorescence number of photons carrys out content (quantitative) of the analytical element in object.
While wherein the effect of detector is the characteristic X-ray photon of reception element, the photon of different-energy is distinguished, and
The photon of different-energy is counted, all X-ray detectors all have certain energy resolving power, referred to as energy point
Resolution, can tell the x-ray photon that energy has certain gap, energy resolution usually with the MnK α line at 5.9keV most
Significantly the breadth of spectrum line at half (FWHM) indicates.
In view of analysis object element (its K in analysis object (electric equipment products, mineral, oil plant, metal material etc.)
Linear system or L linear system energy are lower than 50keV), commercial X-ray Fluorescence Spectrometer multiselect more common at present is detected with silicon semiconductor
Device, the energy resolution of such detector it is common be 145eV (1keV=1000eV), it is optimal can be to 125eV, the above resolution ratio number
Value is ideally to obtain in laboratory, to the resolution ratio of different-energy x-ray photon about in above-mentioned value base in practical application
Increase about 50eV~300eV on plinth.Commercial X-ray Fluorescence Spectrometer more common at present selects the light for doing characteristic x-ray fluorescence
Sub- Energy distribution selects spectral line to perform an analysis in 0~50keV energy section, and according to the relative intensity rule of characteristic X-ray spectral line.
Attached drawing 2 and attached drawing 3 are please referred to, some element spectral lines can be encountered in practice and interfere with each other situation: (1), adjacent spectral
Line interference: it is visited if the characteristic x-ray fluorescence photon energy difference that simultaneous certain elements are respectively analyzed in sample is less than
The energy resolution of device is surveyed, then detector cannot be distinguished, i other words currently used commercial X-ray Fluorescence Spectrometer can not be simultaneously
Analyze these elements.Typical example has: lead (Pb), arsenic (As) are existed simultaneously in sample, the L α energy of lead is 10.542keV,
The K α energy of arsenic is 10.532keV, and the two differs about 10eV, is far below detector energy resolution ratio, cannot be by area of detector institute
Point.(2), times peak interference: if the minimum that the time interval that two or more x-ray photons reach detector is less than detector is rung
Time interval is answered, then detector can record the energy supposition of these photons, and then using superimposed energy as judgement feature X
The foundation of ray, resulting phenomenon are commonly referred to as a times peak, wherein 2 times of peaks are the most obvious, 3 times or more times peaks are unobvious, often
It is not considered.Typical example has: lead (Pb), iron (Fe) is existed simultaneously in sample, the K α energy of iron is 6.4keV, 2 times of peak energy
Amount is 12.8keV, differs about 17eV with the L α energy of lead, cannot be distinguished by detector.(3), escape peak interferes: visiting when entering
Survey device x-ray photon energy be higher than detector receive matrix element absorption limit (in common detector matrix element be silicon Si,
When the absorption of K linear system is limited to 1.839), there is certain probability excitation matrix element to generate its characteristic X-ray, due to the original of matrix element
Son is to characteristic x-ray absorption very little itself, so the X-ray generated is just escaped from detector, while generating an additional arteries and veins
Punching, energy is equal to the energy difference of incident photon and matrix element characteristic X-ray (Si K α energy is 1.74keV), through detector
Photoelectric conversion simultaneously shows on spectrogram, referred to as escape peak (evolution peak).Typical example has: iron (Fe) K β escape peak energy is
5.318keV (iron Fe K β energy 7.058keV subtracts silicon Si K α energy 1.74keV), differs with chromium (Cr) K α energy 5.412
94eV cannot be distinguished by detector.
If there is one or more interference, then existing common commercial X-ray Fluorescence Spectrometer is often unable to cope with, most typically
Example are as follows: exist simultaneously lead (Pb), arsenic (As) in sample, belong to the interference of adjacent spectral line, to analyze in such sample at present
Used method is to select the L β (12.626) of lead as characteristic X-ray when lead, avoids the interference of arsenic.And it analyzes arsenic and then selects
The K β (11.726) of arsenic is used as characteristic X-ray.But if arsenic in sample constituent content is low, the K β intensity of arsenic is weak, and is easy
The interference of lead element is received, commercial X-ray Fluorescence Spectrometer there is no effective detection means at present.
Summary of the invention
When for Xray fluorescence spectrometer in the prior art mentioned above, arsenogen cellulose content is low in the sample, detection
The disadvantage of effect difference, the present invention provide a kind of monochromatic focusing X-ray light source and the method using light source analysis Lead in low quantity arsenic,
It uses cydariform condenser to carry out monochromatic, convergence to X-ray, to form high-intensitive monochromatic light, can to low content arsenic element into
Row detection.
The technical solution used to solve the technical problems of the present invention is that: a kind of monochrome focusing X-ray light source, light source include penetrating
Line trigger mechanism, preceding light bar, focusing ring and rear light bar, preceding light bar are arranged corresponding to ray emission mechanism, and focusing ring is arranged preceding
In front of light bar, rear light bar is arranged in front of focusing ring, and the focusing ring inner surface on the inside of focusing ring uses drum organization, preceding light bar,
Ring inner surface and the coaxial arrangement of rear light bar are focused, axle center and the central axes of ray emission mechanism coincide.
A method of Lead in low quantity arsenic being analyzed using such as above-mentioned monochromatic focusing X-ray light source, this method includes following
Step:
Emit at S1, ray tube target center it is monochromatic before ray, it is premenstrual in after light bar, preceding outer light bar limitation, with focusing
The identical angular illumination of lattice plane angle of ring to focus ring inner surface each point；
S2, on the lattice plane for focusing ring inner surface, occur Bragg diffraction, it is monochromatic before ray by monochrome chemical conversion be monochrome
X-ray energy is the homogeneous ray of 11.87keV, focuses on sample surfaces after light bar limitation after；
S3, focused radiation irradiating sample excite the x-ray fluorescence of specific element to be analyzed in sample, are received by a detector
Afterwards by computer disposal, the information such as the content of element are obtained.
The technical scheme adopted by the invention to solve the technical problem further comprises:
The ray emission mechanism includes shell, anode, filament, window and target, and anode is embedded in inside the shell, target
It is fixedly mounted on anode, filament is fixedly mounted inside the shell, and filament is arranged corresponding to target, and window is fixedly mounted on shell
On, window, which uses, there is the material of high transmittance to be made X-ray.
The target to the distance between filament is 10~20mm, and the distance between target to window is 20~40mm.
The preceding light bar includes preceding outer light bar and preceding interior light bar, and preceding outer light bar and preceding interior light bar are not easy to wear using X-ray
Saturating material is made, and preceding interior light bar uses truncated cone-shaped, and bottom area is less than topside area, and preceding interior light bar bottom plane is mounted on window
It is hollow shape inside preceding outer light bar on mouth, boring is in truncated cone-shaped, and preceding outer light bar interior bottom portion area is less than topside area,
Preceding interior light bar bottom plane is mounted on window, and preceding interior light bar is arranged in preceding outer light bar, preceding interior light bar center line and preceding outer light
Hollow center line inside column is overlapped.
The preceding interior light bar base diameter is 13~14.5mm, and the angle between preceding interior light bar lateral surface and center line is
12.3~13.0 °；Hollow base diameter in preceding outer light bar is 18~19mm, the hollow side and center line in preceding outer light bar it
Between angle be 17.51~17.91 °.
The height of the preceding outer light bar is 8~10mm, and the height of preceding interior light bar is 20~24mm.
The focusing ring is made of a bulk crystal, or is spliced using two pieces or more of crystal, focusing ring material
Material is topaz, lithium fluoride, sodium chloride, quartz or artificial plural layers etc. but unlimited, and the interplanar distance of lattice plane is 0.2014 μm.
The focusing ring height is 30~34mm, and the distance between focusing ring bottom to target is 63.5~64.8mm,
Focusing top surface of ring to the distance between sample to be tested focus point is 63.5~64.8mm.
The focusing ring inner surface is John's type, Johnson's type or logatithmic spiral type, when making focusing ring, will first be focused
The inner surface of ring bends to radius 2R, then removes surfacing by radius of curvature of R, focuses each parameter of ring inner surface: R=120
~200mm, 2R=240~400mm, 15.036 ° of incident ray incidence angle θ=, homogeneous X-ray energy is 11.87keV.
The rear light bar includes that interior light bar and rear outer light bar, rear interior light bar and rear outer light bar are not easy to wear using X-ray afterwards
Saturating material is made, it is rear in light bar use truncated cone-shaped, bottom area is greater than topside area, it is rear in light bar lateral surface and center line it
Between angle be 12.3~13.0 °, be hollow shape inside rear outer light bar, boring is in truncated cone-shaped, afterwards outer light bar interior bottom portion
Area is greater than topside area, it is rear in light bar be arranged in rear outer light bar, it is rear in light bar center line with it is hollow inside outer light bar afterwards
Center line be overlapped, the angle between hollow side and center line in rear outer light bar is 17.51~17.91 °, thus it is rear outside
The gap of annular is formed between light bar and rear interior light bar；Or rear light bar uses smallcolumn diaphragm, smallcolumn diaphragm is not easy using X-ray
The material penetrated is made, and smallcolumn diaphragm is a hollow taper type, and inner surface is along the done section of plane for passing through frustum axis
The angle of edge and axis should be greater than θ.
The beneficial effects of the present invention are: the present invention, which images X using cydariform condenser, carries out monochromatic, convergence, to be formed
High-intensitive monochromatic light can detect low content arsenic element.K of the X-ray of irradiating sample of the present invention just above arsenic element
Limit 11.867keV is absorbed, can efficiently excite the characteristic X-ray of arsenic element but not excitation lead element, it is entirely avoided lead element
The interference of characteristic fluorescence.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Detailed description of the invention
Fig. 1 is the interaction schematic diagram of X-ray and substance.
Fig. 2 is that x-ray fluorescence generates schematic diagram.
Fig. 3 is the overhaul flow chart of commercial energy dispersion type Xray fluorescence spectrometer.
Fig. 4 is that Bragg's equation reflects schematic diagram.
Fig. 5 is one the schematic diagram of the section structure of the embodiment of the present invention.
Fig. 6 is two the schematic diagram of the section structure of the embodiment of the present invention.
Fig. 7 is focusing ring structural schematic diagram of the present invention.
Fig. 8 is the A partial enlargement structural representation of Fig. 7.
In figure, 1- shell, 2- anode, 3- filament, 4- window, 5- target, 6- target center, the central axes 7-, outer light before 8-
Column, interior light bar before 9-, ray before 10- is monochromatic, 11- focusing ring, 12- focus ring inner surface, interior light bar after 13-, outer light after 14-
Column, ray after 15- is monochromatic, 16- sample, 17- sample surfaces focus point, 18- detector, 19- smallcolumn diaphragm, 20- focus point,
Normal of the 21- perpendicular to lattice plane, the lattice plane that 22- was bent, plane of crystal 23- ground as radius of curvature using R.
Specific embodiment
The present embodiment is the preferred embodiment for the present invention, other its all principles and basic structure are identical or close as the present embodiment
As, within that scope of the present invention.
Incorporated by reference to referring to attached drawing 5, to attached drawing 8, it mainly includes penetrating that the present invention, which is mainly a kind of monochromatic focusing X-ray light source,
Line trigger mechanism, preceding light bar, focusing ring 11 and rear light bar, preceding light bar are arranged corresponding to ray emission mechanism, and focusing ring 11 is arranged
In front of preceding light bar, rear light bar setting uses cydariform knot in 11 front of focusing ring, the focusing ring inner surface 12 of 11 inside of focusing ring
Structure, preceding light bar focus ring inner surface 12 and the coaxial arrangement of rear light bar, and axle center and the central axes 7 of ray emission mechanism coincide.
In the present embodiment, ray emission mechanism is mainly ray tube, and ray tube includes shell 1, anode 2, filament 3, window 4
With target 5, anode 2 is inlaid in shell 1, and target 5 is fixedly mounted on anode 2, and filament 3 is fixedly mounted in shell 1, and lamp
Silk 3 corresponds to target 5 and is arranged, and window 4 is fixedly mounted on shell 1, and window 4 is using the material to X-ray with high transmittance
It is made, X-ray can be made to penetrate, project, in the present embodiment, thin window, mylar, glass made of beryllium Be element is can be used in window 4
The materials such as glass are made, and filament 3 is arranged corresponding to window 4, i.e. filament 3, the center line of window 4 and target 5 and ray emission mechanism
Central axes 7 coincide.It is the vacuum of condition of high vacuum degree in ray tube, vacuum degree can reach 133.322 × 10-6~133.322
×10-7Pa, the effect of ray tube are transmitting X-ray, and X-ray is by being the center of circle, diameter about 0.010mm~2mm with target center 6
Circle (the being not limited to circle) field emission of (unlimited), and have the injection of window 4.In the present embodiment, target 5 is between filament 3
Distance is 10~20mm, and the distance between preferred target 5 to filament 3 is 16.5mm, and the distance between target 5 to window 4 is
20~40mm, the distance between preferred target 5 to window 4 are 29mm.
In the present embodiment, according to the difference of working method, mainly there are several types of modes for X-ray tube:
(1) the first high pressure mode: 3 one end of filament ground connection, ray tube anode 2 plus positive high voltage；
(2) another high pressure mode: filament 3 plus negative high voltage, ray tube anode 2 are grounded；
(3) the third high pressure mode: filament 3 plus negative high voltage, ray tube anode 2 plus positive high voltage.
The purpose of above high pressure mode is generation high voltage electric field, and the thermal electron for generating filament is moved to target 5, from
And target 5 is excited to generate X-ray.
In the present embodiment, preceding light bar includes preceding outer light bar 8 and preceding interior light bar 9, and preceding outer light bar 8 and preceding interior light bar 9 are penetrated using X
The material that line is not easy to penetrate is made, generally lead, copper, steel etc. but unlimited, preceding outer light bar 8 and preceding 9 material of interior light bar in the present embodiment
Material is lead.In the present embodiment, preceding interior light bar 9 uses truncated cone-shaped, and bottom area is less than topside area, preceding interior 9 bottom plane of light bar
It being mounted on window 4, preceding interior 9 base diameter of light bar is 13~14.5mm, and interior 9 base diameter of light bar is 13.07mm before preferred,
Angle between preceding 9 lateral surface of interior light bar and center line is 12.3~13.0 °, interior 9 lateral surface of light bar and center line before preferred
Between angle be 12.7 °；It is hollow shape inside preceding outer light bar 8 in the present embodiment, boring is in truncated cone-shaped, preceding outer light bar 8
Interior bottom portion area is less than topside area, and preceding interior 9 bottom plane of light bar is mounted on window 4, and preceding interior light bar 9 is arranged in preceding outer light
In column 8, preceding interior 9 center line of light bar is overlapped with the hollow center line inside preceding outer light bar 8, in the present embodiment, in preceding outer light bar 8
Hollow base diameter be 18~19mm, it is preferred before hollow base diameter in outer light bar 8 be 18.52mm, in preceding outer light bar 8
Hollow side and center line between angle be 17.51~17.91 °, it is preferred before hollow side in outer light bar 8 and center
Angle between line is 17.71 °, to form the gap of annular between preceding outer light bar 8 and preceding interior light bar 9.
Preceding interior light bar 9 and preceding outer light bar 8, which limit the ray emitted from target center 6, is radiated at 11 inner surface of focusing ring,
Preceding interior light bar 9 can highly be higher than preceding outer light bar 8, so that preceding interior light bar edge blocks preceding outer 9 inner wall of light bar to sample surfaces completely
The scattered x-ray of focus.In the present embodiment, the height of preceding outer light bar 8 is 8~10mm, and the height of preferred preceding outer light bar 8 is
10mm, the height of preceding interior light bar 9 are 20~24mm, and the height of interior light bar 9 is 22mm before preferred.X-ray is by with target center 6
For the center of circle, circle (being not limited to circle) field emission of diameter about 0.010mm~2mm (unlimited), after window 4, by preceding interior
Light bar 9, preceding outer light bar 8 are limited within the scope of a hollow cone, and are irradiated to 11 inner wall of focusing ring, this part ray is known as single
Ray before color, it is monochromatic before ray include various energy X-ray, be " polychrome " X-ray.
The effect of focusing ring 11 is to make the ray for being irradiated to its inner surface that diffraction monochromatization occur using Bragg's equation,
And focus on sample surfaces focus point.In the present embodiment, ring inner surface 12 is focused inside focusing ring 11, focuses ring inner surface 12
In cydariform, i.e., its rounded distribution, middle position are relatively large in diameter, and both ends diameter is smaller, and a bulk crystal can be used in focusing ring 11
It is made, can also be spliced using two pieces or more of crystal (similar to the oak barrel structure of dress grape wine).The present embodiment
In, 11 height of focusing ring is 30~34mm, and preferred 11 height of focusing ring is 32mm, and 11 bottom of focusing ring is between target 5
Distance is 63.5~64.8mm, and the distance between preferred 11 bottom of focusing ring to target 5 is 64.17mm, 11 top surface of focusing ring
It is 63.5~64.8mm to the distance between sample focus point 17, preferred 11 top surface of focusing ring is between sample focus point 17
Distance is 64.17mm.
In the present embodiment, focusing ring 11 is made of crystal, and crystal can will be regarded as to the parallel atomic plane structure for being d by spacing
At each parallel atomic plane is known as lattice plane.11 material of focusing ring can be topaz, lithium fluoride, sodium chloride, quartz, artificial more
Layer film etc. but unlimited uses lithium fluoride (LiF) in the present embodiment, and the plane of reflection is (200), and crystal is lithium fluoride, being of LiF
Formula, (200) are which plane of reflection is polished when being description production crystal, and the interplanar distance of the lattice plane d is 0.2014 μm.Cloth
Glug law expression formula is as follows:
2dsin θ=n λ
In above formula, d is the spacing of lattice plane, and λ is incident ray wavelength, and θ is that incident ray, emergent ray and lattice are flat
The angle in face, n are integer.
When meeting above formula, emergent ray is equal with the wavelength of incident ray, such as penetrates incidence using light bar, slit device
Line is all incident on lattice plane with the angle θ, and emergent ray is only obtained at the angle θ, and the available X equal with incident ray wavelength is penetrated
Line achievees the effect that ray monochromatization.
Focusing ring inner surface 12 can be about writing brush type, Johnson's type or logatithmic spiral type but unlimited, using about in the present embodiment
The inferior type of writing brush.When making focusing ring 11, the inner surface of focusing ring 11 is first bent into radius 2R, there is curvature in lattice plane at this time,
Referred to as lattice plane；Again using R as radius of curvature removal surfacing, in the present embodiment, minimizing technology is using grinding.The present embodiment institute
The focusing ring 11 used has the cylindrical shape of axial curvature for inner wall, other schemes can also be combined into non-annularity focalizer by multi-disc.This
Each parameter of ring inner surface: R=120~200, preferred R=160mm, 2R=240~400mm, preferred 2R is focused in embodiment
=320mm, θ=15.036 °.Homogeneous X-ray energy is 11.87keV in the present embodiment.
In the present embodiment, there are two types of structure types for rear light bar:
Embodiment one: please referring to attached drawing 5, and in the present embodiment, rear light bar includes light bar 13 and rear outer light bar 14 in rear, rear interior
Light bar 13 and rear outer light bar 14 are made of the material that X-ray is not easy to penetrate, generally lead, copper, steel etc. but unlimited, the present embodiment
In be lead.In the present embodiment, interior light bar 13 uses truncated cone-shaped afterwards, and bottom area is greater than topside area, 13 lateral surface of rear interior light bar
Angle between center line is 12.3~13.0 °, and the angle after preferred between interior 13 lateral surface of light bar and center line is
12.7°；It is hollow shape inside rear outer light bar 14 in the present embodiment, boring is in truncated cone-shaped, rear outer 14 interior bottom portion face of light bar
Product is greater than topside area, it is rear in light bar 13 be arranged in rear outer light bar 14, it is rear in inside 13 center line of light bar and rear outer light bar 14
Hollow center line be overlapped, in the present embodiment, the angle between hollow side and center line in rear outer light bar 14 is 17.51
~17.91 °, preferably the angle between the hollow side and center line in rear outer light bar 14 is 17.71 °, thus in rear outer light
The gap of annular is formed between column 14 and rear interior light bar 13.X-ray after monochrome is limited to one by interior light bar 13, rear outer light bar 14 afterwards
Determine angle, and block the scattered x-ray of focusing ring inner wall generation, reduces its irradiating sample surface.In the present embodiment, rear light bar exists
It is used in focusing application.
Embodiment two: please referring to attached drawing 6, and in the present embodiment, rear light bar uses smallcolumn diaphragm 19, and smallcolumn diaphragm 19 uses X
The material that ray is not easy to penetrate is made, generally lead, copper, steel etc. but unlimited, is lead in the present embodiment.Smallcolumn diaphragm 19 is
Heart taper type, inner surface should be greater than θ along the edge in the done section of plane and the angle of axis for passing through frustum axis.Aperture light
Column 19 uses in orifice type application.
Ray after monochrome is limited to certain angle by rear light bar, and blocks the scattered x-ray of focusing ring inner wall generation,
Reduce the focusing ring inner wall scattered x-ray on irradiating sample surface.
The present invention protects a kind of method using above-mentioned monochromatic focusing X-ray light source analysis Lead in low quantity arsenic simultaneously, including
Following step:
Emit at S1, ray tube target center 6 it is monochromatic before ray, it is premenstrual in after light bar 9, preceding outer light bar 8 limit, with it is poly-
The identical angular illumination of lattice plane angle of burnt ring 11 to focus 12 each point of ring inner surface；
S2, on the lattice plane for focusing ring inner surface 12, occur Bragg diffraction, it is monochromatic before ray by monochrome chemical conversion be single
Color X-ray energy is the homogeneous ray of 11.87keV, focuses on sample surfaces after light bar limitation after.
S3, focused radiation irradiating sample excite the x-ray fluorescence of specific element to be analyzed in sample, the i.e. spy of the element
It levies X-ray and obtains the information such as the content of element by computer disposal after being received by a detector.
In the present embodiment, since the rear light bar form of use is different, focus version is also different:
Embodiment one, the rear light bar using focusing structure, monochromatic treated X-ray warp later in light bar 13 and after outside
After the blocking of light bar 14, ray focusing is concentrated on a little, is conducive to detect the zonule on small area sample or sample.
In the present embodiment, target center 6 to 11 lower surface of focusing ring distance is 63.5~64.8mm, preferred target center
6 arrive 11 lower surface of focusing ring apart from being 64.17mm, and 11 height of focusing ring is 30~34mm, and preferred 11 height of focusing ring is
32mm, 11 upper surface of focusing ring to focus point distance be 63.5~64.8mm, preferred 11 upper surface of focusing ring to focus point away from
From for 64.17mm.
Embodiment two, the rear light bar using orifice type structure, in focal spot one smallcolumn diaphragm 19 of placement, focusing ring
In 12 emergent ray of surface, the ray that the ray for being only θ with lattice plane angle can be emitted by smallcolumn diaphragm 19, other angles,
That is the scattered x-ray of focusing ring inner wall generation, is blocked by smallcolumn diaphragm 19, will not be irradiated to sample surfaces.Orifice type application can
More completely avoid 11 inner wall scattered rays irradiating sample of focusing ring.Orifice type application can one, irradiating sample surface annular region.
In the present embodiment, target center 6, preceding interior light bar 9, preceding outer light bar 8, focusing ring 11, rear light bar, sample surfaces are focused
Point is arranged around central axes 7, but central axes 7 and 2 surface of anode are not necessarily vertical, and central axes 7 are not necessarily hung down with 16 surface of sample
Directly, 18 window center vertical line of detector and the angle on 16 surface of sample are changeable.
In above-described embodiment, focusing and two kinds of concrete application forms of orifice type are given, when implementation, without being limited thereto two
Kind, other application form can be selected according to the actual situation.
Providing in above-described embodiment is the analysis side that Lead in low quantity arsenic is carried out using the monochromatic focusing X-ray light source of the present invention
Method, when it is implemented, monochromatic focusing X-ray light source in the present invention can also by adjusting light channel structure to different-energy ray into
Row monochrome focuses, and has similar the case where interfering with each other element with analysis, such as at the same time containing cobalt (K α energy 6.94keV, K suction
Receive limit 7.112keV), survey cobalt element etc. in the sample of erbium (L α energy 6.949keV, L absorb limit 8.358keV), it is only necessary to adjustment is poly-
Burnt 3 structure of ring and preceding light bar structure and rear light bar structure, can be obtained the homogeneous X-ray of the specific wavelength of needs.
The present invention selects X camera shooting using cydariform condenser, converges, so that high-intensitive monochromatic light is formed, it can be to low
Content arsenic element is detected.The X-ray of irradiating sample of the present invention absorbs limit 11.867keV just above the K of arsenic element, can be high
The characteristic X-ray but not excitation lead element of effect excitation arsenic element, it is entirely avoided the interference of lead element characteristic fluorescence.
Claims (11)
1. a kind of monochrome focusing X-ray light source, it is characterized in that: the light source includes ray emission mechanism, preceding light bar, focusing ring
With rear light bar, preceding light bar is arranged corresponding to ray emission mechanism, and focusing ring is arranged in front of preceding light bar, and rear light bar setting is focusing
In front of ring, the focusing ring inner surface on the inside of focusing ring uses drum organization, and preceding light bar, focusing ring inner surface and rear light bar are coaxially set
It sets, axle center and the central axes of ray emission mechanism coincide.
2. monochrome focusing X-ray light source according to claim 1, it is characterized in that: the ray emission mechanism includes outer
Shell, anode, filament, window and target, anode are embedded in inside the shell, and target is fixedly mounted on anode, and filament is fixedly mounted on
In shell, and filament is arranged corresponding to target, and window is fixedly mounted on the shell, and window, which is used, has high transmittance to X-ray
Material be made.
3. monochrome focusing X-ray light source according to claim 2, it is characterized in that: the target between filament away from
From for 10~20mm, the distance between target to window is 20~40mm.
4. monochrome focusing X-ray light source according to claim 1, it is characterized in that: the preceding light bar includes preceding outer light bar
With preceding interior light bar, preceding outer light bar and preceding interior light bar are made of the material that X-ray is not easy to penetrate, and preceding interior light bar uses truncated cone-shaped,
Bottom area is less than topside area, and preceding interior light bar bottom plane is mounted on window, is hollow shape inside preceding outer light bar, internal empty
The heart is in truncated cone-shaped, and preceding outer light bar interior bottom portion area is less than topside area, and preceding interior light bar bottom plane is mounted on window, preceding interior
Light bar is arranged in preceding outer light bar, and preceding interior light bar center line is overlapped with the hollow center line inside preceding outer light bar.
5. monochrome focusing X-ray light source according to claim 4, it is characterized in that: the preceding interior light bar base diameter is
13~14.5mm, the angle between preceding interior light bar lateral surface and center line is 12.3~13.0 °；Hollow base in preceding outer light bar
Diameter is 18~19mm, and the angle between hollow side and center line in preceding outer light bar is 17.51~17.91 °.
6. monochrome focusing X-ray light source according to claim 4, it is characterized in that: the height of the preceding outer light bar be 8~
10mm, the height of preceding interior light bar are 20~24mm.
7. monochrome focusing X-ray light source according to claim 1, it is characterized in that: the focusing ring is brilliant using a monolith
System is at or being spliced using two pieces or more of crystal, focusings ring material is topaz, lithium fluoride, sodium chloride, quartz or manually
Plural layers etc. but unlimited, the interplanar distance of lattice plane are 0.2014 μm.
8. monochrome focusing X-ray light source according to claim 2, it is characterized in that: the focusing ring height be 30~
34mm, the distance between focusing ring bottom to target be 63.5~64.8mm, focus top surface of ring to sample to be tested focus point it
Between distance be 63.5~64.8mm.
9. monochrome focusing X-ray light source according to claim 1, it is characterized in that: the focusing ring inner surface is John
The inner surface of focusing ring when making focusing ring, is first bent to radius 2R by type, Johnson's type or logatithmic spiral type, then with R is song
Rate radius removes surfacing, and focus each parameter of ring inner surface: R=120~200mm, 2R=240~400mm, incident ray enter
Firing angle θ=15.036 °, homogeneous X-ray energy are 11.87keV.
10. monochrome focusing X-ray light source according to claim 1, it is characterized in that: the rear light bar includes light bar in rear
With rear outer light bar, rear interior light bar and rear outer light bar are made of the material that X-ray is not easy to penetrate, and rear interior light bar uses truncated cone-shaped,
Bottom area is greater than topside area, and the angle between rear interior light bar lateral surface and center line is 12.3~13.0 °, in rear outer light bar
Portion is hollow shape, and boring is in truncated cone-shaped, and rear outer light bar interior bottom portion area is greater than topside area, and rear interior light bar is arranged rear
In outer light bar, rear interior light bar center line is overlapped with the hollow center line inside rear outer light bar, the hollow side in rear outer light bar
Angle between center line is 17.51~17.91 °, to form the gap of annular between rear outer light bar and rear interior light bar；
Or rear light bar uses smallcolumn diaphragm, smallcolumn diaphragm is made of the material that X-ray is not easy to penetrate, and smallcolumn diaphragm is a hollow cone
Platform shape, inner surface should be greater than θ along the edge in the done section of plane and the angle of axis for passing through frustum axis.
11. a kind of monochromatic focusing X-ray light source using as described in any one of claims 1 to 10 analyzes Lead in low quantity arsenic
Method, it is characterized in that: the method includes the following steps:
Emit at S1, ray tube target center it is monochromatic before ray, it is premenstrual in after light bar, preceding outer light bar limitation, with focusing ring
The identical angular illumination of lattice plane angle to focus ring inner surface each point；
S2, on the lattice plane for focusing ring inner surface, occur Bragg diffraction, it is monochromatic before ray by monochrome chemical conversion be that monochrome X is penetrated
Heat input is the homogeneous ray of 11.87keV, focuses on sample surfaces after light bar limitation after；
S3, focused radiation irradiating sample, excite sample in specific element to be analyzed x-ray fluorescence, after being received by a detector by
Computer disposal obtains the information such as the content of element.
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| CN201811013196.2A CN108872282A (en) | 2018-08-31 | 2018-08-31 | Monochromatic focusing X-ray light source and the method that Lead in low quantity arsenic is analyzed using the light source |
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| CN201811495391.3A Pending CN109342479A (en) | 2018-08-31 | 2018-12-07 | Monochromatic focusing X-ray light source and the method that Lead in low quantity arsenic is analyzed using the light source |
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| US3898455A (en) * | 1973-11-12 | 1975-08-05 | Jr Thomas C Furnas | X-ray monochromatic and focusing system |
| CN1155659A (en) * | 1996-01-05 | 1997-07-30 | 松下电器产业株式会社 | Curved diffraction surface type graphite crystal X-ray monochrometer and manufacturing method therefor |
| CN101356589A (en) * | 2005-08-01 | 2009-01-28 | 纽约州立大学研究基金会 | X-ray imaging systems employing point-focusing, curved monochromating optics |
| CN101553881A (en) * | 2006-10-24 | 2009-10-07 | 塞莫尼根分析技术有限责任公司 | Two-stage X-ray concentrator |
| CN204789414U (en) * | 2015-06-29 | 2015-11-18 | 中国建材检验认证集团股份有限公司 | Provocative energy dispersion type X ray fluorescence appearance of single wavelength ray |
| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
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2018
- 2018-08-31 CN CN201811013196.2A patent/CN108872282A/en active Pending
- 2018-12-07 CN CN201811495391.3A patent/CN109342479A/en active Pending
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|---|---|---|---|---|
| US3898455A (en) * | 1973-11-12 | 1975-08-05 | Jr Thomas C Furnas | X-ray monochromatic and focusing system |
| CN1155659A (en) * | 1996-01-05 | 1997-07-30 | 松下电器产业株式会社 | Curved diffraction surface type graphite crystal X-ray monochrometer and manufacturing method therefor |
| CN101356589A (en) * | 2005-08-01 | 2009-01-28 | 纽约州立大学研究基金会 | X-ray imaging systems employing point-focusing, curved monochromating optics |
| CN101553881A (en) * | 2006-10-24 | 2009-10-07 | 塞莫尼根分析技术有限责任公司 | Two-stage X-ray concentrator |
| CN204789414U (en) * | 2015-06-29 | 2015-11-18 | 中国建材检验认证集团股份有限公司 | Provocative energy dispersion type X ray fluorescence appearance of single wavelength ray |
| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
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