CN101625315A - Energy-saving and low-cost atomic absorption photometer of tungsten coil furnace - Google Patents
Energy-saving and low-cost atomic absorption photometer of tungsten coil furnace Download PDFInfo
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- CN101625315A CN101625315A CN200910131797A CN200910131797A CN101625315A CN 101625315 A CN101625315 A CN 101625315A CN 200910131797 A CN200910131797 A CN 200910131797A CN 200910131797 A CN200910131797 A CN 200910131797A CN 101625315 A CN101625315 A CN 101625315A
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Abstract
The invention provides an energy-saving and low-cost atomic absorption photometer of a tungsten coil furnace. A metal tungsten wire with the diameter of 0.5 mm is wound into a sampling hole with the inside diameter of 1.6 mm, the diameter of a steel bar is 6 mm, and an end cap has the inside diameter of 7 mm and the length of 20 mm. Pyrolysis graphite caps (the end cap) are sleeved at two ends of the tungsten coil and have the thickness of 0.4 mm, the length of 2 mm and the ring inside diameter of 4 mm. The tungsten coil is heated to pass through a graphite ring which is contained in water-cooled jackets of an upper flat plate and a lower flat plate. Sintering zirconium oxide insulating rings with the width of 4 mm and the thickness of 1 mm are sleeved at the two ends of the tungsten coil. A pyrolysis graphite piece with the dimension of 7.5*17.5*0.4 mm respectively and tightly attached in the front of a permanent magnet and at the back of the permanent magnet is inserted into a lower graphite ring, and the lower graphite ring and an upper graphite ring maintain the clearance to be 0.5 mm in the attached figure, the Zeeman atomic absorption photometer of the tungsten coil furnace with a transverse magnetic field form. m0exp<*> values of 62 elements at different atomization temperature are acquired through an experiment, which can be analyzed by using non-standard analysis software.
Description
Use tungsten coil furnace to set up energy-saving and low-cost atomic absorption photometer of tungsten coil furnace.
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 Instrument s 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 absorption photometer in detail below.
The present invention includes the making of (one) two ends band caps (end cap) tungsten wire ring.
See Fig. 1 with the use steel mold, sample holes steel mold (1) 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 on binding post (Fig. 3) when mounted.The tungsten wire ring two ends put end cap pyrolytic graphite cap, and 0.5mm is thick, and the long 2mm of cap internal diameter 7mm just in time puts tungsten wire ring, and cap ring internal diameter 4mm sees Fig. 2.The patent " fixed metal tungsten or tantalum platform graphite tube preparation method " (application number 200810093774.8, April 21 2008 applying date) that the tungsten wire ring that makes proposes by the present inventor, processing 0.02-0.1mm thickness pyrolytic graphite coating.But thickness coating increases energy consumption, and being controlled at energy consumption, to be no more than 25V60A be 1500W.The patent that proposes with the present inventor " tungsten of band permanent matrix modifier or the method for making of tantalum platform-graphite tube " (application number 200810134853.9 again, August 4 2008 applying date), add 3mgIr+3mgZr on the pyrolytic graphite coating end cap tungsten wire ring or 3mgRu+3mgZr is a permanent matrix modifier having.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 element to be measured owing to when atomization, generate the MX molecule, atomization efficiency is descended significantly, matrix effect increases, X can be O, Cl, S, F, Br, I, CN, C
2, etc.Molecule absorption that matrix produces and background absorption increase, and promptly M (matrix) X increases, and PO, SO, CN, C
2Deng increase, the direct injection analysis of solid suspension particularly, molecule and background absorption also are difficult to deduction greatly to 3.0 with Zeeman deduction background.Therefore do not have in tungsten coil furnace 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, and is when for example surveying cobalt, higher more than 70 times than no hydrogen atomization efficiency in argon gas with 10% hydrogen.Therefore the use of 10% hydrogen is necessary with tungsten coil furnace the time.Hydrogen Preparation and the available electrolysis dilute sulfuric acid water liquid of generation, 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, and 1 minute 10% hydrogen is 0.2l/min (0.0033l/s), so the electrolysis electricity consumption is very low.By the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen with argon gas.
(2) transverse zeeman end cap tungsten coil furnace body structure.
The patent that furnace binding and present inventor propose " no standard analysis is with laterally heating graphite furnace transverse magnetic Zeeman atomic absorption photometer " (application number 200710097222.X, April 29 2007 applying date) is similar.Endcap tungsten wire ring (1) two ends put the wide 1mm heavy insulation of 3mm ring (18), and 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, and injection port (2) is so that sample introduction.There is the outer tracheae (10) of argon in following water collar central authorities, and respectively there is tracheae (9) in the argon both sides, stops the supple of gas or steam when atomization.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), keeps the 0.5mm gap with last graphite annulus.Permanent magnet (8) is wrapped up in one deck teflon insulation layer (5), and 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 on fixed screw by spring (15) is arranged.
Replace the end cap THGA graphite furnace of widespread use to face many new problems with energy-efficient and low-cost end cap tungsten coil furnace, promptly use the argon gas that adds 10% hydrogen, can guarantee that atomization efficiency reaches 1.00.This remains be experimental results show that.The graphite furnace greater than end capTHGA is lost in diffusion between the circle of tungsten coil furnace, and 10% hydrogen is lost also in the argon gas diffusion and lost greater than the diffusion of argon gas.Therefore when using no standard analysis, originally be applicable to the m of end cap THGA graphite furnace
0Cal, m
0Exp
*Value has not been suitable for tungsten coil furnace, need obtain 62 ms of element when different atomization temperature that are suitable for tungsten coil furnace again
0Cal, m
0Exp
*Value, promptly new table one.New table one has been arranged, just the patent " the Zeeman deduction background graphite furnace atomic absorption photometer does not have standard analysis software " (application number 200810093773.3, April 21 2008 applying date) that can propose with the present inventor.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).M when experiment redeterminates that 62 elements are at different atomization temperature in the end cap tungsten coil furnace Zeeman atomic absorption photometer
0Cal, m
0Exp
*Value is made new table 1.Calibrating correction coefficient K with 6 standard solution, the Q when tortuosity factor β and typical curve counter-rotating
AValue (A
rValue) 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 frequent use time-consuming of common inorganic analysis, the molten sample that difficulty is loaded down with trivial details, separate and determination step, also can break away from the loaded down with trivial details time-consuming step that corresponding reagent blank of bringing into and purification reagent need.Each instrument also can be simultaneously with being the standard metering instrument, as balance in the gravimetric method, and various capacity measuring instruments in the volumetric method.The function that the numerous and diverse standard model of similar quantity kind is also arranged simultaneously is as the standard tool for transmitting.
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.
Claims (3)
1. the present invention relates to the energy-efficient and low-cost tungsten wire coil atomic absorption photometer.
The present invention includes the making of (one) two ends band caps (end cap) tungsten wire ring.See Fig. 1 with the use steel mold, sample holes steel mold (1) 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 on binding post (Fig. 3) when mounted.The tungsten wire ring two ends put end cap pyrolytic graphite cap, and 0.5mm is thick, and the long 2mm of cap internal diameter 7mm just in time puts tungsten wire ring, and cap ring internal diameter 4mm sees Fig. 2.The patent " fixed metal tungsten or tantalum platform graphite tube preparation method " (application number 200810093774.8, April 21 2008 applying date) that the tungsten wire ring that makes proposes by the present inventor, processing 0.02-0.1mm thickness pyrolytic graphite coating.But thickness coating increases energy consumption, and being controlled at energy consumption, to be no more than 25V60A be 1500W.The patent that proposes with the present inventor " tungsten of band permanent matrix modifier or the method for making of tantalum platform-graphite tube " (application number 200810134853.9 again, August 4 2008 applying date), add 3mgIr+3mgZr on the pyrolytic graphite coating end cap tungsten wire ring or 3mgRu+3mgZr is a permanent matrix modifier having.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 element to be measured owing to when atomization, generate the MX molecule, atomization efficiency is descended significantly, matrix effect increases, X can be O, Cl, S, F, Br, I, CN, C
2, etc.Molecule absorption that matrix produces and background absorption increase, and promptly M (matrix) X increases, and PO, SO, CN C
2Deng increase, the direct injection analysis of solid suspension particularly, molecule and background absorption also are difficult to deduction greatly to 3.0 with Zeeman deduction background.Therefore do not have in tungsten coil furnace 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, and is when for example surveying cobalt, higher more than 70 times than no hydrogen atomization efficiency in argon gas with 10% hydrogen.Therefore the use of 10% hydrogen is necessary with tungsten coil furnace the time.Hydrogen Preparation and the available electrolysis dilute sulfuric acid water liquid of generation, 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, and 1 minute 10% hydrogen is 0.2l/min (0.0033l/s), so the electrolysis electricity consumption is very low.By the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen with argon gas.
(2) transverse zeeman end cap tungsten coil furnace body structure.
The patent that furnace binding and present inventor propose " no standard analysis is with laterally heating graphite furnace transverse magnetic Zeeman atomic absorption photometer " (application number 200710097222.X, April 29 2007 applying date) is similar.Endcap tungsten wire ring (1) two ends put the wide 1mm heavy insulation of 3mm ring (18), and 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, and injection port (2) is so that sample introduction.There is the outer tracheae (10) of argon in following water collar central authorities, and respectively there is tracheae (9) in the argon both sides, stops the supple of gas or steam when atomization.Be close to each a slice 17 of 11mm gap permanent magnet (8) front and back, 5X17.5X0.4mm pyrolytic graphite sheet (4) is inserted in down graphite annulus, keeps the 0.5mm gap with last graphite annulus.Permanent magnet (8) is wrapped up in one deck teflon insulation layer (5), and 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 on fixed screw by spring (15) is arranged.
Replace the end cap THGA graphite furnace of widespread use to face many new problems with energy-efficient and low-cost end cap tungsten coil furnace, promptly use the argon gas that adds 10% hydrogen, can guarantee that atomization efficiency reaches 1.00.This remains be experimental results show that.The graphite furnace greater than end cap THGA is lost in diffusion between the circle of tungsten coil furnace, and 10% hydrogen is lost also in the argon gas diffusion and lost greater than the diffusion of argon gas.Therefore when using no standard analysis, originally be applicable to the m of end cap THGA graphite furnace
0Cal, m
0Exp
*Value has not been suitable for tungsten coil furnace, need obtain 62 ms of element when different atomization temperature that are suitable for tungsten coil furnace again
0Cal, m
0Exp
*Value, promptly new table one.New table one has been arranged, just the patent " the Zeeman deduction background graphite furnace atomic absorption photometer does not have standard analysis software " (application number 200810093773.3, April 21 2008 applying date) that can propose with the present inventor.
2. described according to claim 1;
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.
3, described by claim 1;
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).M when experiment redeterminates that 62 elements are at different atomization temperature in the end cap tungsten coil furnace Zeeman atomic absorption photometer
0Cal, m
0Exp
*Value is made new table 1.Calibrating correction coefficient K with 6 standard solution, the Q when tortuosity factor β and typical curve counter-rotating
AValue (A
rValue) 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 frequent use time-consuming of common inorganic analysis, the molten sample that difficulty is loaded down with trivial details, separate and determination step, also can break away from the loaded down with trivial details time-consuming step that corresponding reagent blank of bringing into and purification reagent need.Each instrument also can be simultaneously with being the standard metering instrument, as balance in the gravimetric method, and various capacity measuring instruments in the volumetric method.The function that the numerous and diverse standard model of similar quantity kind is also arranged simultaneously is as the standard tool for transmitting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101317978A CN101625315B (en) | 2009-04-02 | 2009-04-02 | Energy-saving and low-cost atomic absorption photometer of tungsten coil furnace |
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| CN2009101317978A CN101625315B (en) | 2009-04-02 | 2009-04-02 | Energy-saving and low-cost atomic absorption photometer of tungsten coil furnace |
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| CN101625315A true CN101625315A (en) | 2010-01-13 |
| CN101625315B CN101625315B (en) | 2012-02-22 |
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Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5018855A (en) * | 1988-10-26 | 1991-05-28 | Athens Corp. | Atomic absorption process monitoring |
| 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 |
| CN101285766A (en) * | 2008-04-21 | 2008-10-15 | 马怡载 | Immobilized metal tungsten or tantalum platform graphite tube preparation method |
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