CN111103265A - Atomizer for atomic fluorescence analysis and atomic fluorescence instrument - Google Patents
Atomizer for atomic fluorescence analysis and atomic fluorescence instrument Download PDFInfo
- Publication number
- CN111103265A CN111103265A CN201811269964.0A CN201811269964A CN111103265A CN 111103265 A CN111103265 A CN 111103265A CN 201811269964 A CN201811269964 A CN 201811269964A CN 111103265 A CN111103265 A CN 111103265A
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- furnace
- ceramic
- atomizer
- atomic fluorescence
- fluorescence analysis
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- 238000012921 fluorescence analysis Methods 0.000 title claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 51
- 239000010453 quartz Substances 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000007769 metal material Substances 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 8
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- 239000012774 insulation material Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 150000004678 hydrides Chemical class 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000010425 asbestos Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052895 riebeckite Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/645—Specially adapted constructive features of fluorimeters
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Optics & Photonics (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to an atomizer for atomic fluorescence analysis, which comprises a furnace body support, a furnace core, a quartz furnace sleeved in the furnace core, a furnace body outer cover sleeved outside the furnace core, a ceramic cover plate, electric furnace wires and other parts, wherein the furnace core and the furnace body outer cover are made of insulating and heat-resistant non-metallic materials, the parts are clamped or fixed without being fixed by screws, and can be integrally disassembled and maintained without cooling after stopping working.
Description
Technical Field
The invention belongs to the field of analytical chemistry, relates to an atomic fluorescence analysis device and parts thereof, and particularly relates to improvement of an atomizer in the atomic fluorescence analysis device.
Background art scene
Atomic fluorescence analysis has been widely used for the determination of trace amounts of As, Sb, Bi, Hg, Se, and the like. The basic principle is that ions of an element to be detected in an acidic medium (usually hydrochloric acid) react with a strong reducing agent (usually potassium borohydride or sodium borohydride) to be reduced into gaseous hydride or atoms, and a large amount of hydrogen is generated. The hydride molecules are dissociated into ground state atoms in the high-temperature hydrogen flame and excited to a high energy state by radiation of a specific frequency of an excitation light source, and the excited state atoms emit fluorescence of a characteristic wavelength in the form of light radiation in the de-excitation process due to extreme instability of the high energy level. The fluorescence intensity is correlated with the concentration of the element to be detected, and the concentration of the element to be detected is obtained by measuring the fluorescence signal of the element to be detected by a detector (usually a photomultiplier).
The atomic fluorescence analysis device (also called atomic fluorescence instrument, atomic fluorescence photometer and atomic fluorescence spectrometer) designed according to the principle mainly comprises a transfusion system, a steam generation system (or called reactor), an atomizer, an excitation light source and a detection system. The test solution and the reducing agent are conveyed through the liquid conveying system and are carried by carrier liquid (also called carrier liquid) to be fed into the reactor to carry out chemical reaction, and the generated gaseous hydride molecules and hydrogen enter the atomizer under the carrying of the carrier gas (usually argon).
The atomization of hydride relies on the high temperature of the hydrogen flame, and the atomization process is performed with reference to an atomizer. The atomizer comprises a furnace body, a quartz furnace arranged in the furnace body, furnace wires at the opening of the quartz furnace tube and other conventional parts, and the parts are mostly fastened by using screws, so that the disassembly, the assembly and the maintenance are inconvenient; the existing furnace body is made of metal materials, the furnace body is always in a high-temperature state due to continuous hydrogen flame in detection, the high temperature of the furnace body not only causes the temperature of the whole working environment of the instrument to rise to influence the service life, but also causes baseline drift to influence the detection seriously due to the temperature rise of the working environment; in addition, in the existing atomizer, the thick asbestos pad is needed to support the furnace wire at the opening of the quartz furnace tube, so that the furnace wire at the opening of the quartz furnace tube can be ensured to ignite hydrogen according to the heat of the furnace wire, and the asbestos pad is easy to pulverize and scatter everywhere and is a carcinogen, thereby influencing the use of users.
Disclosure of Invention
The present invention aims to provide a novel atomizer for atomic fluorescence analysis, which effectively solves the above problems.
The atomizer for atomic fluorescence analysis comprises a furnace body support, a furnace core, a quartz furnace sleeved in the furnace core, a furnace body outer cover sleeved outside the furnace core, a ceramic cover plate, an electric furnace wire and other parts, wherein the furnace core and the furnace body outer cover are made of insulating heat-resistant non-metallic materials, and the parts are clamped or fixed without screws.
The atomic fluorescence analysis uses the atomizer, and furnace body dustcoat upper end establishes two at least draw-in grooves, and the buckle is established to ceramic cover board side counterpoint, and buckle and draw-in groove lock are with furnace body dustcoat upper end and ceramic cover board joint.
The electric furnace wire is inserted between the ceramic cover plate and the quartz furnace pipe orifice.
And a ceramic heat insulation layer is arranged between the ceramic cover plate and the top end face of the furnace core, and the ceramic heat insulation layer supports and positions the electric furnace wire at the pipe orifice of the quartz furnace.
The ceramic heat insulation layer is filled among the ceramic cover plate, the top end face of the furnace core and the outer wall of the opening of the quartz furnace in a conformal manner, and the ceramic heat insulation layer is made of one or a plurality of heat insulation materials such as ceramic sheets, ceramic fibers and mica sheets.
The atomizer for atomic fluorescence analysis is characterized in that an inner groove is formed in the upper portion of a furnace core, and the bottom of a ceramic heat insulation layer is filled in the inner groove. The ceramic heat insulation layer can be formed by stacking ceramic fiber ropes, mica sheets or ceramic sheets and ceramic fiber ropes in sequence, and the ceramic fiber ropes on one side are filled in the inner grooves.
Specifically, the atomizer for atomic fluorescence analysis is characterized in that a groove body (51) and a step (53) are arranged at the upper part of a furnace body support, and two slotted holes (52) are formed in the side wall of the groove body; the lower part of the furnace core is provided with a bulge (11) which is embedded in the groove body; the inner pipe joint and the outer pipe joint at the lower part of the quartz furnace are clamped in the slotted holes and extend out to the side surface; the quartz furnace is sleeved in the furnace core cavity, and a pipe orifice (33) of the quartz furnace extends upwards out of the top end surface of the furnace core; the furnace body outer cover is sleeved on the periphery of the furnace core, and the bottom (21) of the furnace body outer cover abuts against and is seated on a step (53) of the furnace body support.
The atomic fluorescence analysis device formed by assembling the atomizer with the existing transfusion system, the reactor, the excitation light source and the detector also belongs to the invention.
By adopting the scheme, the novel atomizer has the advantages that the furnace body is made of the non-metal material which has excellent heat dissipation performance and is completely insulated, the atomizer can be maintained without cooling after stopping working, and the phenomenon of baseline drift is overcome because the temperature of the furnace body is not too high in the working process; all the components are assembled in a matching way, and the mounting does not need to be fastened by screws, so that the whole body can be disassembled, assembled and maintained; the opening of the quartz furnace adopts heat insulation materials such as mica, ceramic and the like, and carcinogenic asbestos is eliminated. The invention integrally improves the quality of the atomizer.
The invention is described in detail below with reference to the figures and examples.
Drawings
FIG. 1 is a schematic diagram of the overall appearance of the atomizer of the present invention;
FIG. 2 is a schematic diagram of the atomizer sub-assembly of the present invention;
FIG. 3 is a schematic cross-sectional view of the atomizer of the present invention;
FIG. 4 is a data screenshot of the detection limit and reproducibility of Hg determination using an atomic fluorescence instrument equipped with the atomizer of the present invention.
Detailed Description
The invention discloses a novel atomizer. The structure of which is shown in fig. 1-3, comprising: the furnace comprises a furnace core 1, a quartz furnace 3 sleeved in the furnace core 1, a furnace body outer cover 2 sleeved outside the furnace core 1, a ceramic cover plate 4 clamped with the upper end of the furnace body outer cover, an electric furnace wire 7 embedded between the ceramic cover plate 4 and the pipe orifice of the quartz furnace 3, and ceramic heat insulation layers 61, 62 and 63 filled between the ceramic cover plate 4 and the top end face of the furnace core 1, wherein the furnace body parts are formed by the above components, and a furnace body support 5 is arranged at the bottom of the furnace body and used for supporting the furnace body. Here:
the quartz furnace 3 is a commercially available product, and is a sleeve composed of a central tube (inner tube) and an outer tube which are separated from each other, and the inner tube and the outer tube are connected with hydride and hydrogen (carried by carrier gas) generated by the reactor and shielding gas through an inner tube joint 31 and an outer tube joint 32, respectively.
The furnace core 1 is integrally an I-shaped cavity member, the quartz furnace 3 is sleeved in the cavity, a pipe orifice 33 of the quartz furnace extends upwards out of the top end surface 13 of the furnace core 1, the shape and the size of a lower bulge 11 of the furnace core 1 are matched with those of an upper groove body 51 of the furnace body support 5, and the bulge 11 is embedded in the groove body 51. The upper part of the furnace core 1 can be provided with an inner groove 12 for accommodating the ceramic heat insulation layer 6.
Two slotted holes 52 are opened on the side wall of the upper groove body 51 of the furnace body support 5, and the inner pipe joint 31 and the outer pipe joint 32 of the quartz furnace 3 extend to the side surface through the slotted holes 52.
The furnace body outer cover 2 is cylindrical and is sleeved on the periphery of the furnace core 1, the bottom 21 of the furnace body outer cover is abutted against a step 53 of a furnace body support, and the upper part of the furnace body outer cover is provided with at least two clamping grooves 22 which are clamped and buckled with a buckle 42 arranged on the side edge of the ceramic cover plate 4.
The electric furnace wire 7 is sleeved on the inner side surface of the ceramic cover plate 4, and is supported and fixed on the periphery of the pipe orifice 33 of the quartz furnace 3 through a ceramic heat insulation layer 61-63 filled between the ceramic cover plate 4 and the top end surface of the furnace core 1. The shape of the ceramic heat insulation layers 61-63 changes along with the shape of the filled gaps, the materials can be one or a combination of a plurality of heat insulation materials such as ceramic sheets, ceramic fibers, mica sheets and the like, and as shown in figure 3, three heat insulation materials 61, 62 and 63 are selected.
The above components are assembled in such a way that: the upper part of the quartz furnace 3 is sleeved into the inner cavity of the furnace core 1 from bottom to top, the bottoms of the furnace core 1 and the quartz furnace 3 are sleeved into an upper groove body 51 of a furnace body support, and an inner pipe joint 31 and an outer pipe joint 32 of the quartz furnace 3 are clamped into a slotted hole 52; the ceramic cover plate 4 with the electric furnace wires 7 is clamped at the upper end of the furnace body outer cover 2, the space from the upper end of the furnace core 1 to the pipe orifice of the quartz furnace 2 is filled with ceramic heat-insulating layers 61-63, and finally the furnace body outer cover 2 is sleeved outside the furnace core 1 and is seated on the step 53 of the furnace body support 5. The atomizer is assembled in this way, and structures such as clamping grooves are used for fixing parts in the assembly process, and screws are not needed.
In the atomizer, the furnace core 1 and the furnace body outer cover 2 are both made of insulating and heat-resistant non-metallic materials, and metal materials are not used.
The atomizer of the invention is assembled with the existing transfusion system, reactor, excitation light source and detector, etc., to form the novel atomic fluorescence analysis device of the invention.
The novel atomic fluorescence analysis device is used for atomic fluorescence analysis, can be successfully used for measuring As, Hg, Se, Pb and Cd in various samples, wherein the detection limit and reproducibility data of the measured mercury are listed As figure 4, which shows that the instrument has good detection stability and overcomes the problem of baseline drift caused by the temperature rise of the original atomic fluorescence instrument.
Claims (9)
1. An atomizer for atomic fluorescence analysis comprises a furnace body support, a furnace core, a quartz furnace sleeved in the furnace core, a furnace body outer cover sleeved outside the furnace core, a ceramic cover plate, an electric furnace wire and other parts, and is characterized in that the furnace core and the furnace body outer cover are made of insulating and heat-resistant non-metallic materials, and the parts are clamped or fixed without screws.
2. An atomizer for atomic fluorescence analysis according to claim 1, characterized in that the furnace body dustcoat upper end is equipped with at least two draw-in grooves, the ceramic cover plate side is counterpointed and is equipped with the buckle, buckle and draw-in groove lock with furnace body dustcoat upper end and ceramic cover plate joint.
3. An atomizer for atomic fluorescence analysis according to claim 2, characterized in that said electric furnace wire is inserted between the ceramic cover plate and the quartz furnace nozzle.
4. An atomizer for atomic fluorescence analysis according to claim 3, characterized in that a ceramic thermal insulating layer is provided between the ceramic cover plate and the top end face of the furnace core, and the ceramic thermal insulating layer supports and positions the electric furnace wire at the nozzle of the quartz furnace.
5. An atomizer for atomic fluorescence analysis according to claim 4, characterized in that said ceramic thermal insulation layer is filled between the ceramic cover plate, the top end face of the furnace core and the outer wall of the opening of the quartz furnace, and the ceramic thermal insulation layer is made of one or more thermal insulation materials such as ceramic sheet, ceramic fiber and mica sheet.
6. An atomizer for atomic fluorescence analysis according to claim 5, characterized in that the upper portion of the furnace core is provided with an inner groove (12), and the bottom of said ceramic thermal insulating layer is filled in the inner groove.
7. An atomizer according to claim 6, wherein ceramic fiber rope, mica sheet or ceramic sheet, ceramic fiber rope are stacked in turn to form said ceramic thermal insulation layer.
8. A atomizer for atomic fluorescence analysis according to any one of claims 1 to 7, characterized in that the upper part of the furnace body support is provided with a tank (51) and a step (53), and the side wall of the tank is provided with two slotted holes (52); the lower part of the furnace core is provided with a bulge (11) which is embedded in the groove body; the inner pipe joint and the outer pipe joint at the lower part of the quartz furnace are clamped in the slotted holes and extend out to the side surface; the quartz furnace is sleeved in the furnace core cavity, and a pipe orifice (33) of the quartz furnace extends upwards out of the top end surface of the furnace core; the furnace body outer cover is sleeved on the periphery of the furnace core, and the bottom (21) of the furnace body outer cover abuts against and is seated on a step (53) of the furnace body support.
9. An atomic fluorescence analysis device, comprising the atomizer according to any one of claims 1 to 8, and an existing transfusion system, a reactor, an excitation light source, and a detector.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811269964.0A CN111103265A (en) | 2018-10-29 | 2018-10-29 | Atomizer for atomic fluorescence analysis and atomic fluorescence instrument |
| PCT/CN2019/113966 WO2020088444A1 (en) | 2018-10-29 | 2019-10-29 | Atomizer for analytical instrument |
| PH12021550914A PH12021550914A1 (en) | 2018-10-29 | 2021-04-22 | Atomizer for analytical instrument |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811269964.0A CN111103265A (en) | 2018-10-29 | 2018-10-29 | Atomizer for atomic fluorescence analysis and atomic fluorescence instrument |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111103265A true CN111103265A (en) | 2020-05-05 |
Family
ID=70419957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811269964.0A Pending CN111103265A (en) | 2018-10-29 | 2018-10-29 | Atomizer for atomic fluorescence analysis and atomic fluorescence instrument |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111103265A (en) |
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Application publication date: 20200505 |