CN101625315B - 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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- CN101625315B CN101625315B CN2009101317978A CN200910131797A CN101625315B CN 101625315 B CN101625315 B CN 101625315B CN 2009101317978 A CN2009101317978 A CN 2009101317978A CN 200910131797 A CN200910131797 A CN 200910131797A CN 101625315 B CN101625315 B CN 101625315B
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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 patent " no standard analysis is with fixed metal tungsten or tantalum platform graphite road the atomic absorption photometer " (application number 200710097221.5 that the present inventor proposes; 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 appearance that difficulty is loaded down with trivial details; Separate and determination step; Each also can use simultaneously with device and is the standard metering instrument also can to break away from time-consuming loaded down with trivial details step that corresponding reagent blank of bringing into and purification reagent needs, like 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,
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; WETA90 power consumption 14V2500A 35KW 0.56s to nineteen ninety produces can know that direct heating tungsten filament tantalum piece circle stove 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 in mass spectrum (MS), uses; 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 energy-saving and low-cost atomic absorption photometer of tungsten coil furnace in detail below.
The method for making of two ends band cap tungsten wire ring in a kind of tungsten coil furnace absorption spectrophotometry, it comprises two ends band cap
The making of tungsten wire ring, sample holes steel mold (19) are 30 ° of pyramid rods, and sample holes internal diameter 1.6mm is inserted in diameter 6mm rod iron (20) central authorities.Rod iron 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; The tungsten wire ring two ends put the pyrolytic graphite cap; 0.5mm 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 was the patent CN101285766A " fixed metal tungsten or tantalum platform graphite tube preparation method " on October 15th, 2008 by open day, and particular content does; Use present inventor and metal institute (happy year of horse, Zhang Wentao, Xu Guozhen; Analytical chemistry; 8 (5), 462 pages (1980)) just succeeded in developing pyrolysis coating graphite-pipe production technology as far back as 1977, be generalized to more than ten manufacturer production in the whole nation; Obtain Liaoning Province's science and technology second prize and Chinese Academy of Sciences's third prize, technology has two kinds; (1) use induction furnace, logical people's nitrogen and propane flammable gas are 2: 1, temperature 1850 degree, 2) or use carbon shirt-circuiting furnace, logical people's nitrogen and propane flammable gas are 5: 1, temperature 2000 is spent, and uses in two kinds of technologies any, 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.With the patent CN101550572A " tungsten of band permanent matrix modifier or the method for making of tantalum platform-graphite tube " in open day on October 7th, 2009, particular content does again; Use 20g/l Ir or Ru drips of solution 50 μ l in WTaPGT, by 200 ℃ of 50s, 450 ℃ of 50s; The pyrolysis of 1000 ℃ of 35s programs, 20g/l Zr 50 μ l drip in WTaPGT, by same program pyrolysis; By first Ir or Ru, back Zr repeats twice, three time one in proper order and reinstates logical argon gas impurity in 2500 ℃ of 7s removing permanent matrix modifiers again; Add 3mgIr+3mgZr on the band cap tungsten wire ring of pyrolytic graphite coating two ends or 3mgRu+3mgZr is a permanent matrix modifier having, 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; Preparation of Hydrogen and generation are with electrolysis dilute sulfuric acid water liquid; Each separates negative electrode and anode with anion-exchange membrane and cation-exchange membrane, and through the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen with argon gas.
2, it comprises transverse zeeman two ends band cap tungsten coil furnace body structure a kind of atomic absorption photometer of tungsten coil furnace, and two ends band cap 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) is connected binding post (17), is connected with big electric current connection sheet (16), is connected with the 25V60A1500W transformer at last; Respectively there is a quartz window (7) at last water collar two ends; One injection port (2) is arranged 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; 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), keeps the 0.5mm gap with last graphite annulus, and 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, and water collar respectively has water inlet pipe and water outlet pipe (11) up and down.Last lower water jacket all is installed on the engineering nylon 20mm slab base (16), is fixed on the base (16) with tighten the screws (14), and last water collar is equipped with spring (15) on fixed screw.
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 guaranteeing atomization efficiency to reach 1.00., this remains to be tested proof. and the graphite furnace greater than end cap THGA is lost in the diffusion between the circle of tungsten coil furnace; As long as 10% hydrogen is lost also in the argon gas diffusion and is lost the power consumption of .End cap tungsten coil furnace 1.5KW greater than the diffusion of argon gas; 1KW near 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 expensive; One in PE company is 150 dollars; One in Jena company of Germany is 100 dollars. and end cap tungsten coil furnace raw material is a tungsten filament, is household electrical bulb primary raw material, and its price is only about in the of 1 dollar; Therefore belonging to its basis of cheap type instrument 3.End cap tungsten coil furnace is patent " no standard analysis is with fixed metal tungsten or tantalum platform graphite furnace the atomic absorption photometer " (application number 200710097221.5 that the present inventor proposes; 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). each instrument also can use simultaneously and be the standard metering instrument, the function of the numerous and diverse standard model of similar quantity kind is also arranged simultaneously, as the standard tool for transmitting.
Description of drawings
1: the die drawing that Fig. 1 uses for the coiling tungsten wire ring; (19) sample holes mould rod.(20) mould around tungsten wire ring is excellent.(1) tungsten wire ring.
2; Fig. 2 is an end cap tungsten filament loop graph; (2) injection port.(21) end cap pyrolytic graphite cap ring.(1) 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 connects post and tightens 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 method for making of two ends band cap tungsten wire ring in the atomic absorption photometer of tungsten coil furnace, it comprises the making of two ends band cap tungsten wire ring, sample holes steel mold (19) is 30 ° of pyramid rods; Sample holes internal diameter 1.6mm is inserted in diameter 6mm rod iron (20) central authorities, rod iron 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 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 is used pyrolytic graphite coating production technology, and technology has two kinds; (1) use induction furnace: feeding nitrogen and propane flammable gas is 2: 1, temperature 1850 degree; (2) or use carbon shirt-circuiting furnace; Feeding nitrogen and propane flammable gas is 5: 1, temperature 2000 degree; Use in two kinds of technologies any, 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; Use Ir+Zr or Ru+Zr to be permanent matrix modifier again; Use 20g/l Ir or Ru drips of solution 50 μ l in tungsten wire ring, by 200 ℃ of 50s, 450 ℃ of 50s; The pyrolysis of 1000 ℃ of 35s programs, 20g/l Zr50 μ l drips in tungsten wire ring, by same program pyrolysis; Again by first Ir or Ru; Back Zr repeats to reinstate for twice, three time one logical argon gas in proper order and removes impurity in the permanent matrix modifiers at 2500 ℃ of 7s, adds 3mgIr+3mgZr on the band cap tungsten wire ring of pyrolytic graphite coating two ends or 3mgRu+3mgZr is a permanent matrix modifier having; 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; Preparation of Hydrogen and generation are with electrolysis dilute sulfuric acid water liquid; Each separates negative electrode and anode with anion-exchange membrane and cation-exchange membrane, and through the hydrogen gas electrolysis groove, the control electric weight just can obtain containing the argon gas of 10% hydrogen with argon gas.
2. atomic absorption photometer of tungsten coil furnace, it comprises transverse zeeman two ends band cap tungsten coil furnace body structure, two ends band cap tungsten wire ring (1) two ends put the wide 1mm heavy insulation of 3mm ring (18); Ring is processed 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) earlier and is connected with the 25V60A1500W transformer at last with big electric current connection sheet (16), and respectively there is a quartz window (7) at last water collar two ends, an injection port (2) are arranged 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, stops the supple of gas or steam, and is close to 11mm gap permanent magnet (8)
Each a slice 17.5 * 7.5 * 0.4mm pyrolytic graphite sheet (4) of front and back is inserted in down graphite annulus; Keep 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; Water collar respectively has water inlet pipe and water outlet pipe (11) up and down; Water collar all is installed on the engineering nylon 20mm slab base (16) up and down, is fixed on the base (16) with tighten the screws (14), and last water collar is equipped with spring (15) on fixed screw.
3. atomic absorption photometer of tungsten coil furnace according to claim 2, each instrument also can use simultaneously and be the standard metering instrument, as the standard tool for transmitting.
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| Application Number | Priority Date | Filing Date | Title |
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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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| 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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| CN101625315B true CN101625315B (en) | 2012-02-22 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5018855A (en) * | 1988-10-26 | 1991-05-28 | Athens Corp. | Atomic absorption process monitoring |
| CN101285766A (en) * | 2008-04-21 | 2008-10-15 | 马怡载 | Immobilized metal tungsten or tantalum platform graphite tube preparation method |
| 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 |
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2009
- 2009-04-02 CN CN2009101317978A patent/CN101625315B/en not_active Expired - Fee Related
Patent Citations (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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