CN101692042B - Atomic fluorescence photometer of Zeeman deduction background of constant magnetic field of energy-saving low-price tungsten wire ring furnace - Google Patents
Atomic fluorescence photometer of Zeeman deduction background of constant magnetic field of energy-saving low-price tungsten wire ring furnace Download PDFInfo
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- CN101692042B CN101692042B CN2009101317963A CN200910131796A CN101692042B CN 101692042 B CN101692042 B CN 101692042B CN 2009101317963 A CN2009101317963 A CN 2009101317963A CN 200910131796 A CN200910131796 A CN 200910131796A CN 101692042 B CN101692042 B CN 101692042B
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Abstract
The invention establishes an atomic fluorescence photometer of a Zeeman deduction background of a constant magnetic field of an energy-saving low-price tungsten wire ring furnace. A metal tungsten wire with the diameter of 0.5mm is winded on a mold into the conditions of the internal diameter of 6mm, the external diameter of 7mm, the length of 20mm and a sample introduction hole of 1.6mm. Both ends of a tungsten wire ring are sleeved with a pyrolytic graphite cap (end cap) with the thickness of 0.4mm, the length of 2mm and the ring internal diameter of 4mm. The tungsten wire ring is heated, and graphite rings are contained in an upper flat plate water-cooling jacket and a lower flat plate water-cooling jacket. Both ends of the tungsten wire ring are sleeved with sintering zirconia insulation rings with the width of 4mm and the thickness of 1mm. Each pyrolytic graphite piece which is tightly adhered to the front and the back of the permanent magnet and is 17.5*17.5*0.4mm is inserted at a lower graphite ring and keeps a clearance of 0.5mm from an upper graphite ring, and an atomic fluorescence photometer of a Zeeman tungsten wire ring furnace of a transverse magnetic field is formed. The placement of a hollow cathode lamp and a Rochon prism is disclosed in the attached drawing. The invention can be used for various merchandises of atomic fluorescence photometers. The sensitivity of the invention is 2-3 magnitude orders higher than that of a conventional flame or electric heating quartz pipe atomization device; as the interference of a basal body and a background is effectively eliminated, complicated solid suspension can directly enter the tungsten wire ring furnace and is measured; and the method is quick, simple and convenient, the data are reliable and accurate, and the time-consuming, inconvenient and complicated steps of sample dissolution and reagent purification can be discarded.
Description
Use tungsten coil furnace to set up the energy-efficient and low-cost tungsten wire coil atomic fluorescence photometer of Zeeman deduction background of constant magnetic field.
Design phiolosophy of the present invention is the patent that proposes of present inventor " no standard analysis with fixed metal tungsten or tantalum platform graphite road atomic absorption photometer " (application number 200710097221.5, April 29 2007 applying date) " no standard analysis is with laterally heating the permanent magnetic field of graphite furnace Zeeman atomic absorption photometer " (application number 200710097221.X, April 29 2007 applying date) " fixed metal tungsten or tantalum platform graphite tube preparation method " (application number 200810093774.8, April 21 2008 applying date) " tungsten of band permanent matrix modifier or the method for making of tantalum platform-graphite tube " (application number 200810134853.9, August 4 2008 applying date).After using these patents, need not to set up typical curve directly constituent content to be measured and concentration in assay determination complex fluid or the solid, break away from common inorganic side and analyse the time-consuming of frequent use, the molten sample that difficulty is loaded down with trivial details, separate and determination step, also can break away from the time-consuming loaded down with trivial details step that corresponding reagent blank of bringing into and purification reagent need.Each also can be simultaneously with being the standard metering instrument with device, as balance in the gravimetric method, and various capacity measurement instruments in the amount method of appearance.The function that the numerous and diverse standard model of similar quantity kind is also arranged simultaneously is as the standard tool for transmitting.But use based on end cap THGA WTaPGT graphite furnace power consumption up to 5KW, the graphite furnace power supply volume is big, is unfavorable for instrument miniaturization, and field operation.End cap graphite-pipe costs an arm and a leg, and one in PE company is 150 dollars, and one in German Jena company is 100 dollars.In order to economize on electricity and cheapness, at first expect only staying tungsten filament tantalum piece platform pipe wherein with removing graphite-pipe in tungsten or the tantalum platform-graphite tube (WTaPGT).WETA82 tungsten sheet circle stove from the production of nineteen eighty-two Czech Laboratory Instruments company, power consumption is up to 2.7KW, to the WETA90 power consumption 14V2500A 35KW 0.56s that nineteen ninety produces, directly heating tungsten filament tantalum piece circle stove as can be known can not economize on electricity, and possible power consumption is bigger.Expect further removing the tantalum piece circle for this reason, directly heat tungsten wire ring.Present inventor in 1986 is engaged in electric atomizing (ETV) at professor Harrison of U.S. Virginia university place as the visiting scholar and uses in mass spectrum (MS), because of graphite furnace too huge, therefore design the tungsten coil furnace of small and exquisite energy-efficient and low-cost, power consumption is 25V 40A 1KW only, in conjunction with Harrison professor speciality glow discharge (GD) MS, set up GD tungsten coil furnace light source and be used for emission spectrum, ion gun is used for MS.Harrison teaches in XXVIICSI world spectrum conference in 1991 in Norway Bergan and is making four GDMS that unite one of big report of conference, introduces GD tungsten coil furnace light source and the ion gun of present inventor in proposition in 1986 in the RIMS report.To introduce the energy-efficient and low-cost tungsten wire coil atomic fluorescence photometer of Zeeman deduction background of constant magnetic field in detail below.
The present invention relates to the energy-efficient and low-cost tungsten wire coil atomic fluorescence photometer of Zeeman deduction background of constant magnetic field,
The present invention includes (one) two ends band cap tungsten wire ring, this two ends band cap tungsten wire ring.
Use steel mold, the sample holes rod iron is 30 ° of pyramid rods, and sample holes internal diameter 1.6mm is inserted in diameter 6mm rod iron (2) central authorities, steel mold around on diameter 0.5mm tungsten filament 40 circle, the long tungsten filament of 40mm is left at the tungsten wire ring two ends, passes graphite annulus and water collar when mounted on binding post, and the tungsten wire ring two ends put the pyrolytic graphite cap, 0.5mm it is thick, the long 2mm of cap internal diameter 7mm just in time puts tungsten wire ring, cap ring internal diameter 4mm, the tungsten wire ring that makes processing 0.02-0.1mm thickness pyrolytic graphite coating, but thickness coating increases energy consumption, being controlled at energy consumption, to be no more than 25V60A be 1500W, adds 3mgIr+3mgZr or 3mgRu+3mgZr having on the pyrolytic graphite coating tungsten wire ring, replaces the graphite-pipe can be energy-conservation and cheap with tungsten wire ring, but the reducing atmosphere that does not have carbon in the graphite-pipe during owing to high temperature, its consequence is an element to be measured owing to generate the MX molecule when atomization, and atomization efficiency is descended significantly, and matrix effect increases, X is O, Cl, S, F, Br, I, CN, C
2,, molecule absorption that matrix produces and background absorption increase, and promptly MX increases, and PO, SO, CN, C
2Increase, the direct injection analysis of solid suspension, molecule and background absorption are greatly to 3.0, also be difficult to deduction with Zeeman deduction background, therefore in tungsten coil furnace, do not have under the reducing atmosphere condition of carbon, solution only leans against and adds 10% hydrogen in the argon gas, this is just widely-used in commodity tungsten sheet stove, therefore the use of 10% hydrogen is necessary with tungsten coil furnace the time, Hydrogen Preparation and generation electrolysis dilute sulfuric acid water liquid, each separates negative electrode and anode with anion-exchange membrane and cation-exchange membrane, by faraday's theorem, 2 coulombs is that 2 peaces can produce 22.4 liters of hydrogen in 1 second, 1 minute 10% hydrogen is 0.2l/min (0.0033l/s), so the electrolysis electricity consumption is very low, with argon gas by the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen
(2) transverse zeeman end cap tungsten coil furnace body structure;
Furnace binding is as follows; End cap tungsten wire ring two ends put the wide 1mm heavy insulation of 3mm ring (18), ring is made by zirconia powder sintering in induction furnace, tungsten wire ring two ends 40mm tungsten filament passes graphite annulus (3) and water collar (6) and is connected binding post (17) and is connected with the 25V60A1500W transformer at last with big electric current connection sheet (16), respectively there is a quartz window (7) at last water collar two ends, injection port (2) is so that sample introduction, there is the outer tracheae (10) of argon in following water collar central authorities, respectively there is tracheae (9) in the argon both sides, when atomization, stop the supple of gas or steam, each a slice 17.5 * 17.5 * 0.4mm pyrolytic graphite sheet (4) is inserted in down graphite annulus before and after being close to 11mm gap permanent magnet (8), keep the 0.5mm gap with last graphite annulus, permanent magnet (8) is wrapped up in one deck teflon insulation layer (5), teflon insulation layer (5) is posted in the water collar junction up and down, last lower water jacket respectively has water inlet pipe and water outlet pipe (10), last lower water jacket all is installed on the engineering nylon 20mm slab base (16), be fixed on the base (16) with tighten the screws (14), last water collar is equipped with spring (15) on fixed screw
(3) tungsten coil furnace atomic fluorescence photometer of Zeeman deduction background of constant magnetic field structure is seen Figure of description 6; The 4 usefulness lens focuss of empty negative electrode light enter rotation Rochon prism 5, enter tungsten coil furnace with catoptron 6 focusing, atomic vapour absorbed when the parallel luminous energy of Rochon prism was atomization, produce atomic absorption and the background absorption that comprises molecule absorption, the Rochon prism vertical light does not produce atomic absorption, only produce background absorption, in like manner directional light produces atomic fluorescence and background fluorescence, vertical light only produces background fluorescence, directional light subtracts the atomic fluorescence after vertical light must be detained background, enters extensive stock atomic fluorescence spectrophotometer 2 and register system 3 with the lens focus on the right side of tungsten coil furnace 1 by the catoptron central aperture.
As long as the power consumption of End cap tungsten coil furnace is 1.5KW, and near the 1KW of electric heater, and the power consumption of end cap THGA graphite furnace is up to 5KW, so end cap tungsten coil furnace belongs to energy-saving instrument, is convenient to field operation and instrument miniaturization.End cap THGA graphite-pipe price is expensive, and one in PE company is 150 dollars, and one in German Jena company is 100 dollars.And end cap tungsten coil furnace raw material is a tungsten filament, is family expenses bulb primary raw material, and its price only about in the of 1 dollar, therefore belongs to cheap type instrument.
Its basis of End cap tungsten coil furnace is the patent that proposes of present inventor " no standard analysis with fixed metal tungsten or tantalum platform graphite furnace atomic absorption photometer " (application number 200710097221.5, April 29 2007 applying date) " no standard analysis is with laterally heating the permanent magnetic field of graphite furnace Zeeman atomic absorption photometer " (application number 200710097222.X, April 29 2007 applying date), " fixed metal tungsten or tantalum platform graphite tube preparation method " (application number 200810093774.8, April 21 2008 applying date) " tungsten of band permanent matrix modifier or the method for making of tantalum platform-graphite tube " (application number 200810134853.9, August 4 2008 applying date).Can directly assay determination complexity
Constituent content to be measured and concentration in the solid are broken away from frequent use time-consuming of common inorganic analysis, and complicated loaded down with trivial details molten sample separates and determination step, also can break away from the complicated loaded down with trivial details time-consuming step that corresponding reagent blank of bringing into and purification reagent need.Owing to can effectively eliminate matrix and background interference, can obtain the authentic data and the accuracy of high level.Analyze fast and conveniently, after complicated solid was made into suspending liquid, direct injected was in tungsten coil furnace, and atomization records the integration fluorescence intensity level, gets concentration value by analytic curve.Sampling can be arrived Gamma Magnitude less, to valuable rare sample, and the particularly research work in nanometer field and the monitoring of device of high-tech area, the big effect of lifting.
Lot of domestic and foreign manufacturer production commodity atomic fluorescence spectrophotometer is only limited to flame or electrothermal quartz tube atomizer at present, owing to insufficient sensitivity, need during analytic sample with complicated loaded down with trivial details time-consuming separating step, and the complicated loaded down with trivial details time-consuming step of corresponding purification reagent.After using tungsten coil furnace, sensitivity improves 2-3 the order of magnitude, analyzes fast and conveniently, and complex fluid sample direct injected is in tungsten coil furnace, and atomization records the integration fluorescent value, gets concentration value by analytic curve.Sampling can be arrived micro updating less, to valuable rare sample, and as blood measuring in the human body, the big effect of lifting.
Description of drawings
1; The die drawing that Fig. 1 uses for the coiling tungsten wire ring; (1) sample holes mould rod.(2) around the mould rod of tungsten wire ring.(3) tungsten wire ring.
2; Fig. 2 is an end cap tungsten filament loop graph; (1) sample holes.(2) end cap pyrolytic graphite cap ring.(3) tungsten wire ring.
3; Fig. 3 and Figure of abstract are tungsten coil furnace body structure (X-Z cross section) synoptic diagram; (1) end cap tungsten wire ring.(2) injection port.(3) graphite annulus.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(7) quartz window.(8) magnet.(9) interior tunger tube.(10) outer tunger tube.(11) water pipe.(12) base plate.(13) fixed screw.(14) tighten the screws cap.(15) spring.(16) big electric current plate.(17) tungsten filament connection post is tightened with nut.(18) zirconia dead ring.
4; Fig. 4 is tungsten coil furnace body structure (X-Y cross section) synoptic diagram; (1) end cap tungsten wire ring.(2) injection port.(3) graphite annulus.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(7) quartz window.(8) magnet.(11) water pipe.
5; Fig. 5 is tungsten coil furnace body structure (Y-Z cross section) synoptic diagram (a 1) end cap tungsten wire ring.(2) injection port.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(8) magnet.(9) interior tunger tube.
6; Fig. 6 is a tungsten coil furnace atomic fluorescence spectrophotometer structural drawing; (1) tungsten coil furnace.(2) commodity atom fluorescent photometer.(3) recording system.(4) empty cathode modulation.(5) Rochon prism.(6) concave surface focusing mirror.
Description of drawings
1; The die drawing that Fig. 1 uses for the coiling tungsten wire ring; (1) sample holes mould rod.(2) around the mould rod of tungsten wire ring.(3) tungsten wire ring.
2; Fig. 2 is an end cap tungsten filament loop graph; (1) sample holes.(2) end cap pyrolytic graphite cap ring.(3) tungsten wire ring.
3; Fig. 3 and Figure of abstract are tungsten coil furnace body structure (X-Z cross section) synoptic diagram (1) end cap tungsten wire ring.(2) injection port.(3) graphite annulus.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(7) quartz window.(8) magnet.(9) interior tunger tube.(10) outer tunger tube.(11) water pipe.(12) base plate.(13) fixed screw.(14) tighten the screws cap.(15) spring.(16) big electric current plate.(17) tungsten filament connection post is tightened with nut.(18) zirconia dead ring.
4; Fig. 4 is tungsten coil furnace body structure (X-Y cross section) synoptic diagram; (1) end cap tungsten wire ring.(2) injection port.(3) graphite annulus.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(7) quartz window.(8) magnet.(11) water pipe.
5; Fig. 5 is tungsten coil furnace body structure (Y-Z cross section) synoptic diagram; (1) end cap tungsten wire ring.(2) injection port.(4) pyrolytic graphite sheet.(5) insulation course.(6) water collar.(8) magnet.(9) interior tunger tube.
6; Fig. 6 is a tungsten coil furnace atom fluorescent photometer structural drawing; (1) tungsten coil furnace.(2) commodity atom fluorescent photometer.(3) recording system.(4) empty cathode modulation.(5) Rochon prism.(6) concave surface focusing mirror.
Claims (1)
1. tungsten wire ring atomic fluorescence photometer of Zeeman deduction background of constant magnetic field,
Comprise (one) two ends band cap tungsten wire ring, this two ends band cap tungsten wire ring is used steel mold, and the sample holes rod iron is 30 ° of pyramid rods, sample holes internal diameter 1.6mm, be inserted in diameter 6mm rod iron (2) central authorities, steel mold around on diameter 0.5mm tungsten filament 40 circle, the long tungsten filament of 40mm is left at the tungsten wire ring two ends, pass graphite annulus and water collar when mounted on binding post, the tungsten wire ring two ends put the pyrolytic graphite cap, and 0.5mm is thick, and the long 2mm of cap internal diameter 7mm just in time puts tungsten wire ring, cap ring internal diameter 4mm, the tungsten wire ring that makes processing 0.02-0.1mm thickness pyrolytic graphite coating, but thickness coating increases energy consumption, being controlled at energy consumption, to be no more than 25V60A be 1500W, add 3mgIr+3mgZr or 3mgRu+3mgZr having on the pyrolytic graphite coating tungsten wire ring, replace the graphite-pipe can be energy-conservation and cheap with tungsten wire ring, but owing to there is not the reducing atmosphere of carbon in the graphite-pipe during high temperature, its consequence be an element to be measured owing to generate the MX molecule when atomization, atomization efficiency is descended significantly, matrix effect increases, and X is O, Cl, S, F, Br, I, CN, C
2,, molecule absorption that matrix produces and background absorption increase, and promptly MX increases, and PO, SO, CN, C
2Increase, the direct injection analysis of solid suspension, molecule and background absorption are greatly to 3.0, also be difficult to deduction with Zeeman deduction background, therefore in tungsten coil furnace, do not have under the reducing atmosphere condition of carbon, solution only leans against and adds 10% hydrogen in the argon gas, this is just widely-used in commodity tungsten sheet stove, therefore the use of 10% hydrogen is necessary with tungsten coil furnace the time, Hydrogen Preparation and generation electrolysis dilute sulfuric acid water liquid, each separates negative electrode and anode with anion-exchange membrane and cation-exchange membrane, by faraday's theorem, 2 coulombs is that 2 peaces can produce 22.4 liters of hydrogen in 1 second, 1 minute 10% hydrogen is 0.2l/min (0.0033l/s), so the electrolysis electricity consumption is very low, with argon gas by the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen
(2) transverse zeeman two ends band cap tungsten coil furnace body structure;
Furnace binding is as follows; Band cap tungsten wire ring two ends, two ends put the wide 1mm heavy insulation of 3mm ring (18), ring is made by zirconia powder sintering in induction furnace, tungsten wire ring two ends 40mm tungsten filament passes graphite annulus (3) and water collar (6) and is connected binding post (17) and is connected with the 25V60A1500W transformer at last with big electric current connection sheet (16), respectively there is a quartz window (7) at last water collar two ends, injection port (2) is so that sample introduction, there is the outer tracheae (10) of argon in following water collar central authorities, respectively there is tracheae (9) in the argon both sides, when atomization, stop the supple of gas or steam, each a slice 17.5 * 17.5 * 0.4mm pyrolytic graphite sheet (4) is inserted in down graphite annulus before and after being close to 11mm gap permanent magnet (8), keep the 0.5mm gap with last graphite annulus, permanent magnet (8) is wrapped up in one deck teflon insulation layer (5), teflon insulation layer (5) is posted in the water collar junction up and down, last lower water jacket respectively has water inlet pipe and water outlet pipe (10), last lower water jacket all is installed on the engineering nylon 20mm slab base (16), be fixed on the base (16) with tighten the screws (14), last water collar is equipped with spring (15) on fixed screw
(3) tungsten coil furnace atomic fluorescence photometer of Zeeman deduction background of constant magnetic field structure; Empty negative electrode light enters the rotation Rochon prism with lens focus, enter tungsten coil furnace with focusing mirror, atomic vapour absorbed when the parallel luminous energy of Rochon prism was atomization, produce atomic absorption and the background absorption that comprises molecule absorption, the Rochon prism vertical light does not produce atomic absorption, only produce background absorption, in like manner directional light produces atomic fluorescence and background fluorescence, vertical light only produces background fluorescence, directional light subtracts the atomic fluorescence after vertical light must be detained background, enters extensive stock atomic fluorescence spectrophotometer and register system with the lens focus on the right side of tungsten coil furnace by the catoptron central aperture.
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| CN2009101317963A CN101692042B (en) | 2009-04-02 | 2009-04-02 | Atomic fluorescence photometer of Zeeman deduction background of constant magnetic field of energy-saving low-price tungsten wire ring furnace |
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| CN2009101317963A CN101692042B (en) | 2009-04-02 | 2009-04-02 | Atomic fluorescence photometer of Zeeman deduction background of constant magnetic field of energy-saving low-price tungsten wire ring furnace |
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| CN101692042B true CN101692042B (en) | 2011-09-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021279A (en) * | 2015-07-02 | 2015-11-04 | 北京市理化分析测试中心 | Polarization modulation Zeeman AFS (Atomic Fluorescence Spectroscopy) with constant magnetic filed in light source |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060152A (en) * | 1991-11-09 | 1992-04-08 | 北京三联高技术联合开发公司 | Ultrasonic atomizing automatic specimen handing device |
| CN1563948A (en) * | 2004-04-16 | 2005-01-12 | 广东省测试分析研究所 | Method and appts. for atom absorbing analysis of constant magnetic field reverse zeeman effect |
| CN101294895A (en) * | 2007-04-29 | 2008-10-29 | 马怡载 | Transverse heating graphite furnace constant magnetic field Zeeman atomic absorption photometer for non-standard analysis |
-
2009
- 2009-04-02 CN CN2009101317963A patent/CN101692042B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060152A (en) * | 1991-11-09 | 1992-04-08 | 北京三联高技术联合开发公司 | Ultrasonic atomizing automatic specimen handing device |
| CN1563948A (en) * | 2004-04-16 | 2005-01-12 | 广东省测试分析研究所 | Method and appts. for atom absorbing analysis of constant magnetic field reverse zeeman effect |
| CN101294895A (en) * | 2007-04-29 | 2008-10-29 | 马怡载 | Transverse heating graphite furnace constant magnetic field Zeeman atomic absorption photometer for non-standard analysis |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021279A (en) * | 2015-07-02 | 2015-11-04 | 北京市理化分析测试中心 | Polarization modulation Zeeman AFS (Atomic Fluorescence Spectroscopy) with constant magnetic filed in light source |
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