CN102184834A - Hollow cathode lamp and atomic absorption spectrometer manufactured by hollow cathode lamp - Google Patents

Hollow cathode lamp and atomic absorption spectrometer manufactured by hollow cathode lamp Download PDF

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Publication number
CN102184834A
CN102184834A CN2011100997952A CN201110099795A CN102184834A CN 102184834 A CN102184834 A CN 102184834A CN 2011100997952 A CN2011100997952 A CN 2011100997952A CN 201110099795 A CN201110099795 A CN 201110099795A CN 102184834 A CN102184834 A CN 102184834A
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hollow cathode
cathode lamp
hollow
atomic absorption
concave mirror
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CN102184834B (en
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张榕
谭雪飞
秦伟
刘娜
陈琳
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Qiqihar Medical University
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Qiqihar Medical University
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Abstract

The invention discloses a hollow cathode lamp and an atomic absorption spectrometer manufactured by the hollow cathode lamp. The hollow cathode lamp comprises a plurality of hollow cathode lamp filaments, wherein each hollow cathode lamp filament is made of alloy; the hollow cathode lamp filaments on the hollow cathode lamp are made of different kinds of alloy, and each alloy contains multiple elements; the plurality of hollow cathode lamp filaments are arranged on the same optical principal axis equidistantly; and a plurality of hollow anode rings are inserted among the plurality of hollow cathode lamp filaments. The atomic absorption spectrometer with the hollow cathode lamp consists of a concave surface reflector, a seam-in concave surface reflector, a flame or graphite furnace center, a flat field concave surface grating and a diode array detector. The invention has the advantages that: the hollow cathode lamp and the atomic absorption spectrometer can generate sharp lines with two-dimensional quantity, and break through the obstruction that the hollow cathode lamp is needed to be replaced once when one element is measured in the technical field of atomic absorption at home and abroad, and a plurality of elements are measured by primary sample introduction simultaneously.

Description

Hollow cathode lamp and the Atomic Absorption Spectrometer of making by this hollow cathode lamp
Technical field
The present invention relates to a kind of hollow cathode lamp, the invention still further relates to a kind of Atomic Absorption Spectrometer of making by this hollow cathode lamp.
Background technology
Single element hollow cathode lamp (HCL) is the most frequently used in the atomic absorption analysis method, most important light source, but a kind of element of every measurement will be changed HCL one time.Photron company has developed a kind of multi-element lamp, and 6 hollow cathode wicks are evenly distributed on the same circumferential plane in the lamp housing of diameter 50mm, and the center is public multianode.6 negative electrodes go between respectively and power, use and need the negative electrode power supply of preheating, other negative electrodes are not powered, each hollow cathode, the same with regard to same single element lamp, during use be the axle rotation with the anodes centre, single injected sampling can only be measured an element, frequently changes lamp and will make the aspects such as convenience of analysis speed, amount of information and use be restricted.Jena, Germany company adopts the high xenon short-act lamp continuous light source that focuses on of 300W to replace 70 element lamps as the atomic absorption light source, because spectrum is continuous, must cooperate high-resolution echelle grating double monochromator and high performance CCD linear array detector (512 dot matrix) to unite use, and to adopt the method for length scanning to measure the absorption spectrum of appointment, take analysis time.
Atomic absorption spectroscopy worker all over the world and designer also are being devoted to obtain with a light source research of numerous sharp lines always.The crucial scientific and technological problem that presses for solution is the problem that element of every measurement changes a lamp, presses for haveing breakthrough in theory that atom absorbs, and is used to instruct the production of atomic absorption instrument device, instructs the update of Atomic Absorption Spectrometer product.Because of the expansion of the mankind to the element information amount, this method is to the requirement of analysis speed and convenience, and the metal group research that the new development of life science aspect is got up also has great help.
Summary of the invention
First technical problem that the present invention will solve provides a kind of hollow cathode lamp that can produce the sharp line of two-dimentional quantity.The another one technical problem that solves also is to provide a kind of Atomic Absorption Spectrometer of being made by above-mentioned hollow cathode lamp.Utilize present device can realize that single injected sampling measures a plurality of elements simultaneously.
The technical scheme of hollow cathode lamp of the present invention is: this hollow cathode lamp comprises a plurality of hollow cathode filaments, a hollow cathode filament uses a kind of alloy to make, each hollow cathode filament on hollow cathode lamp uses alloy not of the same race, every kind of alloy contains multiple element, preferred 5 kinds of the kind of contained element.In hollow cathode lamp, a plurality of hollow cathode filaments equidistantly are arranged on the same optical main axis, assign a plurality of hollow anode rings between a plurality of hollow cathode filaments.
The assembly structure that the present invention contains the Atomic Absorption Spectrometer of above-mentioned hollow cathode lamp is: the sharp line transmitting terminal of hollow cathode lamp points to concave mirror, the two-dimentional sharp line that it sent reflexes on the seam concave mirror by concave mirror, at the concave mirror and the two-dimentional sharp line focus place of going into to stitch between the concave mirror flame or graphite furnace center are housed, going into the seam place through the two-dimentional sharp line focus of going into to stitch the concave mirror reflection, and be dispersed on the flat filed concave grating, whole sharp lines focus between the two-end-point of straight line PDAD through the chromatic dispersion of flat filed concave grating.
The invention has the beneficial effects as follows: hollow cathode lamp of the present invention and Atomic Absorption Spectrometer can produce the sharp line of two-dimentional quantity, broken through in the domestic and international atomic absorption technique field and to have measured the obstacle that an element need change a hollow cathode lamp, realized that single injected sampling measures a plurality of elements simultaneously.When having improved analysis speed significantly, also provide great convenience for enlarging the information use amount.
Description of drawings
Below in conjunction with the drawings and specific embodiments the present invention is described in detail.
Fig. 1 is the structural representation of the embodiment of the invention 1.
Fig. 2 is the structural representation of embodiment 2.
Fig. 3 is sequential pulse power voltage supply and luminous intensity figure detection time.
Fig. 4 is the schematic diagram of photovoltage sync detection device.
Number in the figure:
1, hollow cathode lamp 2, hollow cathode filament 3, hollow anode ring
4, cathode leg 5, anode tap 6, concave mirror
7, graphite furnace center 8, go into to stitch concave mirror 9, flat filed concave grating
10, PDAD 11, operating voltage generator 12, sequential pulse distributor
13, microcontroller 14, atom absorb Control Software 15, microcomputer.
Embodiment
Example 1
As shown in Figure 1, hollow cathode lamp 1 of the present invention comprises a plurality of hollow cathode filaments 2, a hollow cathode filament 2 is made by a kind of alloy, each hollow cathode filament 2 on hollow cathode lamp uses alloy not of the same race, every kind of alloy contains multiple element, the element kind is 5 kinds, and the element composition of alloy is chosen according to the boiling point and the application scenario of element.In hollow cathode lamp, a plurality of hollow cathode filaments 2 equidistantly are arranged on the same optical main axis, assign a plurality of hollow anode rings 3 between a plurality of hollow cathode filaments 2, and the quantity of hollow cathode filament 2 is defined as 10 kinds according to the quantity of element to be measured.The cathode leg 4 of hollow cathode filament 2 and the anode tap 5 of hollow anode ring 3 are drawn from an end of hollow cathode lamp 1.
Filament assembled scheme in this example sees Table 1, and this scheme is that the boiling point according to element makes up and helps using the roughly the same lamp current that has, or makes up according to application and to help using.Because in the compound filament ferroalloy is arranged, so iron-filament is not set separately.
Table 1
Filament numbering (1~M) The element numbering (1-M, M=5)
1 1 mercury Hg-2As-3 selenium Se-4K-5Cd
2 1Na-2 zinc Zn-3 magnesium Mg-4 lithium Li-5 strontium Sr
3 The plumbous Pb-4 barium of 1 thallium Tl-2 calcium Ca-3 Ba-5 manganese Mg
4 1 silver medal Ag-2 indium In-3 gallium Ga-4 beryllium Be-5 aluminium Al
5 1 bronze medal Cu-2 tin Sn-3 chromium Cr-4 gold Au-5 nickel
6 1 cobalt Co-2 silicon Si-3 titanium Ti-4 vanadium V-5 cerium Ce
7 1 rhodium Rh-2 platinum Pt-3 boron-4 molybdenum Mo-5 tungsten W
8 1 caesium Cs-2 rubidium Rb-3 ytterbium Yb-4 europium Eu-5 bismuth Bi
9 1 antimony Sb-2 samarium Sm-3 thulium Tm-4 dysprosium Dy-5 holmium Ho
10 1 germanium Ge-2 scandium Sc-3 palladium Pd-4 neodymium Nd-5 erbium Er
11 1 terbium Tb-2 gadolinium Dy-3 yttrium Y-4 lutetium Lu-5 lanthanum La
12 1 praseodymium Pr-2 uranium U-3 ruthenium Ru-4 zirconium Zr-5 iridium Ir
13 1 hafnium Hf-2 niobium Nb-3 thorium Th-4 osmium Os-5 tantalum Ta
017] example 2
As shown in Figure 2, each parts installation desired location that the present invention contains the Atomic Absorption Spectrometer of hollow cathode lamp 1 is: the sharp line transmitting terminal of hollow cathode lamp 1 points to concave mirror 6, the two-dimentional sharp line that it sent reflexes on the seam concave mirror 7 by concave mirror 6, at the concave mirror 6 and the two-dimentional sharp line focus place of going into to stitch between the concave mirror 7 flame or graphite furnace center 8 are housed, going into the seam place through the two-dimentional sharp line focus of going into to stitch concave mirror 7 reflections, and be dispersed on the flat filed concave grating 9, whole sharp lines focus between the two-end-point of straight line PDAD 10 through the chromatic dispersion of flat filed concave grating 9.
The sync detection device of whole sharp line signal strength signal intensity receiving systems and each sharp line photovoltage in back 125 microseconds of its pulse period is housed in the PDAD, can applies sequential pulse voltage M hollow cathode filament and M anode.
Example 3
This example is the whole sharp line signal strength signal intensity receiving systems of sequential.
The core of the whole sharp line signal strength signal intensity receiving systems of the sequential in the PDAD is cover software systems, comprises TDAA interface software and spectrum data gathering assemble software with the VB6.0 establishment, the shared cover communications protocol of two cover softwares.According to the linear relation of dot matrix numbering with sharp line wavelength, preestablish the dot matrix summary sheet of sharp line wavelength correspondence, the function of control circuit board is that sequential ground supplies the sequential pulse voltage for TDHCL, and the time of photon absorbing intensity computing formula detection time tmn=i (tc-1)+mtc/M-0.25tc/M calculating sampling of the discrete signal in the method for pressing, all photon absorbing intensity carries out analog-to-digital conversion, total data deposits in the two-dimentional subscript variable, is used to show absorbance curve over time.See Fig. 3.
Below be the design principle of above-mentioned software:
Sequential pulse power supply order pulse period tc, filament numbering m, the pass of sampling number i and luminous intensity and sampling time tmn is:
tmn?=?i(tc-1)?+?mtc/M?-?0.25tc/M
Pulse frequency ν=200Hz, the pulse power supply duty ratio is 1:5, pulse period t c=5ms, burst length t p=t c/ M, t detection time of luminous intensity dAt burst length t pBack 1/4, promptly take 0.25t p, duty factor=t p/ t c=1/M.
M=5 for example, burst length t p=t c/ M=1ms, luminous intensity t detection time d=1/4=0.25ms.Detect whole sharp line absorptions peak by technology path.Photon absorbing intensity t detection time of discrete signal MnBy formula calculate (1).The absworption peak of sharp line detects at one time on the same filament, and the absworption peak of sharp line detects in sequential time on the different filament.I is the natural integer row of indication cycle's quantity.The frequency that signal produces is consistent with pulse frequency.
The sample rate that NITRATE BY FLAME ATOMIC absorbs is 5 point/seconds, and 1 point is with 200 milliseconds, 200 milliseconds/5 milliseconds=40 points, final signal value be in 40 pulses discrete signal away from value.
The sample rate that no NITRATE BY FLAME ATOMIC absorbs is 20 point/seconds, and 1 point takies the 1000/20=50 millisecond, 50 milliseconds/5 milliseconds=10 points, and final signal value is the average of 10 discrete signals in the pulse.
If two-dimentional hollow cathode lamp is powered simultaneously, then line spectrum overlaps mutually and becomes continuous spectrum, and continuous spectrum can propose very high requirement to the beam splitting system of back.Adopt the spectrum that the sequential pulse power supply then produces can not the phase mutual interference, kept the high resolution of line spectrum.Obtain the high-resolution line spectrum spectral radiation curves of M filament at 1 second or shorter time.
The key that realizes this function is to sequence sequential.The speed of TDAA image data is 5 point/seconds.Obtain M * N and decide the light intensity signal of wavelength points.For NITRATE BY FLAME ATOMIC absorbed, the luminous intensity when measuring distilled water was equivalent to light transmittance T=100% and absorbs.For no NITRATE BY FLAME ATOMIC absorbed, the luminous intensity of measuring the process measurement that does not add sample was equivalent to light transmittance T=100% and absorbs.The luminosity of each dot matrix of CCD detector is saved, and represents with Ti100; During sample solution, the luminosity of each dot matrix is saved, and represents with Tix; The absorbance A i=log of each dot matrix (Ti100/Tix).Ti100 approximately takies 20%~80% of AD converter dynamic range.The AD precision is 16, uses ADS7813, change-over times 20 microsecond, sample rate can reach 50000 times/second.
Example 4
This example is the photovoltage sync detection device in the PDAD.
As shown in Figure 4, operating voltage generator 11 produces needed starting voltage of hollow cathode lamp and normal working voltage, operating voltage is passed through sequential pulse distributor 12 timing allocation to a plurality of negative electrodes of hollow cathode lamp 1, and controls the size of each lamp current respectively.PDAD 10 receives sharp linear light, is carried out data sampling and is stored in the internal memory by STM32 type microcontroller 13.Atom absorbs Control Software 14 and reads sampled data in the sequential pulse generating process by microcomputer 15, can the display light spectral curve on the interface of microcomputer 15 and the resistance to vibration of sharp line.STM32 type microcontroller 13 is the microcontrollers with 32 bit flash memories, uses the Cortex-M3 kernel of ARM company, and this kernel is that specialized designs is used to satisfy high-performance, low-power consumption, the requirement of built-in applied system cheaply.

Claims (3)

1. hollow cathode lamp, it is characterized in that: this hollow cathode lamp (1) comprises a plurality of hollow cathode filaments (2), a hollow cathode filament (2) is made by a kind of alloy, each hollow cathode filament (2) on the hollow cathode lamp (1) uses alloy not of the same race, every kind of alloy content has 5---10 kind element, in hollow cathode lamp (1), a plurality of hollow cathode filaments (2) equidistantly are arranged on the same optical main axis; Between a plurality of hollow cathode filaments (2), assign a plurality of hollow anode rings (3).
2. hollow cathode lamp according to claim 1 is characterized in that: described alloying element kind is 5 kinds.
3. two-dimentional Atomic Absorption Spectrometer of making by the described hollow cathode lamp of claim 1, it is characterized in that: each parts is installed the sharp line transmitting terminal sensing concave mirror (6) that desired location is this hollow cathode lamp (1), the two-dimentional sharp line that it sent reflexes on the seam concave mirror (7) by concave mirror (6), at the concave mirror (6) and the two-dimentional sharp line focus place of going into to stitch between the concave mirror (7) flame or graphite furnace center (8) are housed, going into the seam place through the two-dimentional sharp line focus of going into to stitch concave mirror (7) reflection, and be dispersed on the flat filed concave grating (9), whole sharp lines focus between the two ends of straight line CCD PDAD (10) through the chromatic dispersion of flat filed concave grating (9).
CN 201110099795 2011-04-21 2011-04-21 Hollow cathode lamp and atomic absorption spectrometer manufactured by hollow cathode lamp Expired - Fee Related CN102184834B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103337447A (en) * 2013-06-05 2013-10-02 无锡市金义博仪器科技有限公司 A hollow cathode lamp apparatus
CN103411674A (en) * 2013-07-08 2013-11-27 杭州久傲科技有限公司 Micro fiber spectrometer based oncortex-M3
CN104865206A (en) * 2015-04-24 2015-08-26 上海伯顿医疗设备有限公司 Single photoelectric tube five-channel atomic absorption spectrometer
CN107589083A (en) * 2017-08-14 2018-01-16 北京普析通用仪器有限责任公司 Lead and cadmium elements are the same as the Atomic Absorption Spectrometer and detection method surveyed in a kind of grain
CN113383217A (en) * 2019-02-07 2021-09-10 耶拿分析仪器有限公司 Atomic absorption spectrometer
CN113418879A (en) * 2021-06-24 2021-09-21 宁夏新龙蓝天科技股份有限公司 Copper chloride solution detection method

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JPS55100642A (en) * 1979-01-24 1980-07-31 Hitachi Ltd Light source cathode for zeeman atomic absorption analyzing device
CN2411468Y (en) * 1999-12-29 2000-12-20 吴安林 Multi-cathode element hollow cathode lamp
US20010035717A1 (en) * 1999-01-21 2001-11-01 Imaging & Sensing Technology Corporation Getter flash shield
CN2826408Y (en) * 2005-07-01 2006-10-11 北京博晖创新光电技术股份有限公司 Atom absorption device capable of multielement simultaneous determination
CN101548173A (en) * 2006-12-18 2009-09-30 株式会社岛津制作所 Atomic absorption spectrophotometer
CN101692039A (en) * 2009-04-02 2010-04-07 马怡载 Energy-efficient and low-cost tungsten wire coil furnace atomic absorption photometer for measuring multiple elements forming hollow cathode lamp
CN201655744U (en) * 2010-04-16 2010-11-24 大庆市日上仪器制造有限公司 Multi-cathode multi-anode composite multielement hollow cathode lamp

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3487254A (en) * 1969-01-16 1969-12-30 Perkin Elmer Corp Alloy for hollow cathode lamp
JPS55100642A (en) * 1979-01-24 1980-07-31 Hitachi Ltd Light source cathode for zeeman atomic absorption analyzing device
US20010035717A1 (en) * 1999-01-21 2001-11-01 Imaging & Sensing Technology Corporation Getter flash shield
CN2411468Y (en) * 1999-12-29 2000-12-20 吴安林 Multi-cathode element hollow cathode lamp
CN2826408Y (en) * 2005-07-01 2006-10-11 北京博晖创新光电技术股份有限公司 Atom absorption device capable of multielement simultaneous determination
CN101548173A (en) * 2006-12-18 2009-09-30 株式会社岛津制作所 Atomic absorption spectrophotometer
CN101692039A (en) * 2009-04-02 2010-04-07 马怡载 Energy-efficient and low-cost tungsten wire coil furnace atomic absorption photometer for measuring multiple elements forming hollow cathode lamp
CN201655744U (en) * 2010-04-16 2010-11-24 大庆市日上仪器制造有限公司 Multi-cathode multi-anode composite multielement hollow cathode lamp

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103337447A (en) * 2013-06-05 2013-10-02 无锡市金义博仪器科技有限公司 A hollow cathode lamp apparatus
CN103337447B (en) * 2013-06-05 2016-12-28 无锡市金义博仪器科技有限公司 Hollow cathode lamp device
CN103411674A (en) * 2013-07-08 2013-11-27 杭州久傲科技有限公司 Micro fiber spectrometer based oncortex-M3
CN104865206A (en) * 2015-04-24 2015-08-26 上海伯顿医疗设备有限公司 Single photoelectric tube five-channel atomic absorption spectrometer
CN107589083A (en) * 2017-08-14 2018-01-16 北京普析通用仪器有限责任公司 Lead and cadmium elements are the same as the Atomic Absorption Spectrometer and detection method surveyed in a kind of grain
CN107589083B (en) * 2017-08-14 2020-04-28 北京普析通用仪器有限责任公司 Atomic absorption spectrometer for simultaneously detecting lead and cadmium elements in grains and detection method
CN113383217A (en) * 2019-02-07 2021-09-10 耶拿分析仪器有限公司 Atomic absorption spectrometer
CN113418879A (en) * 2021-06-24 2021-09-21 宁夏新龙蓝天科技股份有限公司 Copper chloride solution detection method

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