CN1300559C - Microwave extinguishing instrument - Google Patents
Microwave extinguishing instrument Download PDFInfo
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- CN1300559C CN1300559C CNB031785190A CN03178519A CN1300559C CN 1300559 C CN1300559 C CN 1300559C CN B031785190 A CNB031785190 A CN B031785190A CN 03178519 A CN03178519 A CN 03178519A CN 1300559 C CN1300559 C CN 1300559C
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- 229910000831 Steel Inorganic materials 0.000 claims abstract description 45
- 239000010959 steel Substances 0.000 claims abstract description 45
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 18
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- 238000012360 testing method Methods 0.000 claims abstract description 16
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
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- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
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Abstract
The present invention discloses a microwave extinguishing instrument which comprises a front pressure container, a back microwave transmission system and a pressure sensing container. A safety valve and a pressure release valve are arranged on the top of a steel cylinder, and an inner layer is a corrosion preventing inner cavity composed of various components made of PTFE materials and engineering plastics. The microwave emitting system is arranged on the back part of the instrument, and an antenna of a magnetron, a pressure sensor and an electric heating pipe penetrate into the inner cavity of a pressure container from the bottom of the steel cylinder. A test tube filled with a sample and extinguishing reagents is positioned in the inner cavity to generate high-temperature and high-voltage extinguishing samples in the sealed pressure container by microwave heating and electrical heating to realize the operation of automated instruments for sample treatment.
Description
The present invention relates to a kind of instrument, a kind of being used for carried out pre-treatment to sample in the analytical chemistry field, makes it the specialized equipment of digest and decompose.
Chemico-analytic sample pre-treatments is a global problem, the effort that AC is long-term, and the prior art that is occurred is not generally accepted by the chemical analysis industry so far.Traditional Specimen eliminating method mainly is dry incineration method and wet type resolution method, uses till today as national standard method always.In the current prior art, utilizing micro-wave oven and pressure dispelling jar to be used in combination and clear up sample, is comparatively popular a kind of new technologies of nearly more than ten years.The MARS-5 type intelligent microwave high pressure sample-preparing system of U.S. CE M company development for example, patent (ZL942394143) the optical fiber pressure automatic control closed microwave digestion system of Shanghai microwave applications technical institute.So-called digestion system is a kind of small pressure jar and the household microwave oven group of having reequiped and together.This head tank, double-decker, skin are engineering plastics, internal layer is teflon (to call PTFE an in the following text) inner bag, has sealing gasket.Sample and acid reagent are inserted in the jar, make the interior supercharging of sealable tank reach the purpose of clearing up sample by microwave heating.The advantage of its maximum is that speed is exceedingly fast, finish the Specimen eliminating overall process about 20 minutes, but also be his critical defect, temperature and pressure sharply raises in several minutes, volume in jar only has 50 milliliters, and energy can not discharge, and easily produces the UHV (ultra-high voltage) phenomenon, High Temperature High Pressure causes the distortion of PTFE inner bag, and sealing gasket bursts apart.Simultaneously because the position difference of head tank in micro-wave oven, the energy difference that is absorbed, reproducibility of analysis results is relatively poor.So prior art is difficult for promoting, and fails during the last ten years to popularize, this series products also is like this both at home and abroad.
Purpose of the present invention, be to overcome the defective of current prior art, a kind of Specimen eliminating instrument is provided, combine with electrical heating with microwave heating, designed the inner bag that a kind of seal-off pressure container replaces micro-wave oven, cancellation pressure dispelling jar the glass test tube that sample and reagent are housed, places and clears up sample in the closed pressure vessel.Be actually the pressure vessel that the head tank of 50 milliliters of single volumes has been become about 15 liters big volumes, temperature and pressure is controlled in the lower scope, and the chemical reaction velocity of sample and reagent is slowed down, and the Specimen eliminating process is slowly stablized.
Technical solution of the present invention is, instrument is divided in two parts, and the front portion is a pressure vessel, and the rear portion is a microwave transmission system.Described pressure vessel, drum can also can be pressed nonstandard design of pressure vessels as the rectangle microwave burner hearth by the design of GB Steel Pressure Vessels.It is a double-decker, and skin is a steel design, and internal layer is that the molded inner bag of PTFE material membrane is made corrosion protective lining, and high-strength engineering plastic is done heat-insulation layer, has the pressure-bearing function concurrently.This cylindric Steel Pressure Vessels is placed with horizontal type.Described microwave launcher system, also comprise pressure sensor diagnostics, electric heater unit, blind controller system.The magnetron launched microwave enters airtight pressure vessel through waveguide, after starting microwave emission dress system, places sample and reagent in the glass test tube in the pressure vessel, clears up sample under high temperature, condition of high voltage.As run into the sample that is difficult to clear up, can use the heating of microwave heating and electrothermal tube simultaneously, instrument A.T.C and pressure.Maximum operating temperature is 180 ℃, and pressure is 1MPa to the maximum, can prevent that chemical reaction from causing that temperature, pressure sharply raise, and reach the purpose of clearing up sample lentamente.
The present invention improves magnetron, the antenna of magnetron appropriateness lengthening, and magnetron removes cooling fins, with aluminium matter water pipe seal welding, reaches very high radiating efficiency by tap water mobile, and magnetron can be worked continuously for a long time.
The present invention is an one with microwave heating and electric heater unit and pressure vessel group, microwave and electric heating double energy have been utilized, the rapid rising of control temperature, pressure, the sample in the glass test tube is being cleared up under the seal-off pressure container environment of term harmonization, is directly exposed in microwave radiation and the electric radiation field, accept energy even, handling safety, stable performance can not produce the UHV (ultra-high voltage) phenomenon because of chemical reaction, improve the quality of clearing up of sample, eliminated unsafe factor.
The present invention is described in further detail below in conjunction with accompanying drawing.
Fig. 1 is a microwave dissolver side of the present invention position cross-sectional schematic.
Fig. 2 is a microwave dissolver normotopia synoptic diagram of the present invention.
Fig. 3 is that microwave dissolver of the present invention is along Figure 1A-A cross-sectional schematic.
Fig. 4 is another embodiment side position cross-sectional schematic of microwave dissolver of the present invention.
Fig. 5 is another embodiment normotopia synoptic diagram of microwave dissolver of the present invention.
Fig. 6 is the dual microwave transmission synoptic diagram of another embodiment of microwave dissolver of the present invention
Shown in Figure 1, the structure of microwave dissolver is divided the two large divisions basically, and the front portion is a pressure vessel, is made up of various devices; The rear portion is microwave transmission system, pressure sensor diagnostics, electric heater unit, blind controller system.Pressure vessel is a double-decker, and outer field steel vessel 2 is welded into container with flange 3 at the bottom of by steel cylinder 1 and steel cylinder, and blind flange 4 is connected with flange 3 usefulness swing bolts 5, and swing bolt 5 is fixed on the journal stirrup 6, and journal stirrup 6 is welded on the seat that combines of steel cylinder 1 and flange 3.Pressure vessel is to place with horizontal type, and the total weight of instrument is that forward rear support 7 bears.The top of pressure vessel is provided with safety valve 8 and 9, two valves of blowdown valve are communicated with pressure vessel is inside and outside.The inwall of the steel cylinder 1 of pressure vessel will have good processing smooth finish, and the metal of one deck high conductivity should be plated in the surface, helps the reflection of microwave.
The pressure vessel internal layer, owing to be to clear up sample under certain temperature, pressure, acid vapor ambient condition, the various devices of container intracavity all are to use the PTFE material.The inner bag 10 of the container internal layer surface 2-3 millimeters thick that to be PTFE make through compression molding tightly is lining in inwall.Outside the inner bag 10 and between steel cylinder 1 inwall, with the cylinder heat-insulation layer 11 that high-strength engineering plastic is made, it has the effect of bearing pressure concurrently.Above blind flange 4 inner faces are bonded in the PTFE plate, form adhesive surface 12, one, anticorrosion, the 2nd, insulation.The sealing surface of blind flange 4 and flange 3 has PTFE rubber gasket 13, and whole like this internal layer forms an anticorrosion inner chamber.The test tube rack 14 of clearing up sample is arranged in the anticorrosion inner chamber, arrange test tube 15 on the test tube rack 14, test tube rack 15 is placed on the PTFE material waffle slab 16.Used auxiliary member such as pad and so on all are the PTFE material in the inner chamber.
The rear portion of microwave dissolver is made up of microwave transmission system, pressure sensor diagnostics, electric heater unit, blind controller system.The main devices of microwave transmission system is by magnetron 17, and antenna (coupling mechanism) 18, waveguide 19, commutation diode 20, high voltage stabilizing transformer 21 (high-voltage capacitor does not mark) form resonant circuit.Magnetron 17 by fixed head 22 at the bottom of the steel cylinder outside 2 the center fix.In order to adapt to the special requirement of this instrument, magnetron structures is through changing a social system: the one, and antenna 18 lengthenings are because the steel plate thickness of the bottom of pressure vessel is in 25 millimeter, the commodity magnetron antenna is too short, must lengthening, surpass and a little more than steel plate thickness, to guarantee enough emission efficiencies; The 2nd, remove the cooling fins 23 at antenna 18 rear portions, the both sides of former fin and aluminium matter water pipe seal welding connect water inlet pipe and water outlet pipe solenoid valve 24,25 are housed outside casing, and its effect is to have replaced cooling fins and fan, fundamentally improve cooling effectiveness, assurance magnetron 17 can be worked for a long time.Waveguide 19 is copper pipe materials, and the cylinder hollow shape is coated with a floor height conductance metal, is guaranteeing under the length of effective transfer function, and it passes at the bottom of the steel cylinder after 2 steel plates, becomes the circular horn shape.Outside inner bag 10 bottoms, the front end of antenna 18 has formed horn-like hollow section like this.Because inner bag 10 has only the 2-3 millimeter thin, in order to prevent the impact of downforce in working order,, embed the cushion block 26 of a high-strength engineering plastic at the horn-like hollow section of antenna 18 front ends, protection antenna 18 is unlikely impaired.
2 penetrate in the pressure vessel chamber at the bottom of the pressure vessel steel cylinder, and pressure transducer 27 is housed above, and the probe of sensor 27 is by the PTFE film wrapped; Electrothermal tube 28 is housed below, and electrothermal tube 28 can be withstand voltage quartz ampoule, also can be the electrothermal tube of metal, and making electrothermal tube with metal should be at the dispersed PTFE anticorrosive coat of top layer coated.The rear projection of instrument partly is provided with instrument 29 control system panels, and it mainly is made up of the hardware of microprocessor, connects each device of instrument, the follow procedure design is automatically to microwave transmission system, pressure transducer 27, electrothermal tube 28 sends instruction, finishes the Specimen eliminating operation.Instrument casing 30 sheet metal processing and fabricating.
Shown in Figure 2, be the normotopia synoptic diagram of Fig. 1, on blind flange 4 facades of pressure vessel switch knob 31, flange shaft ear 32, pivot pin 33 are arranged.
Shown in Figure 3, be along Figure 1A-A pressure vessel steel cylinder 1 diagrammatic cross-section, be PTFE material inner bag 10 from inside to outside successively, be the cylindric heat-insulation layers 11 of engineering plastics between outer and steel cylinder 1 inwall of inner bag 10, outermost one deck is a casing 30; Lumen centers is test tube rack 14, test tube 15; Safety valve 8 and pressure-release valve 9 are arranged before and after the steel cylinder 1 outer wall top; Have pressure transducer 27, waffle slab 17 times electrothermal tube 28 to be arranged above the inner chamber, the back of inner bag 10 bottom centre's dashed region has pressure-bearing pad fast 26, is thereafter antenna 18 and waveguide 19 hollow sections.
Shown in Figure 4, the structural drawing of another embodiment of microwave dissolver, it is the rectangle Steel Pressure Vessels with nonstandard design, it is high that rectangle inwall smooth finish machining precision is wanted.On steel cylinder 1 outer wall plane, can be vertical, also can be horizontal, four direction is provided with waveguide 19 in length and breadth, waveguide 19 central upper are settled magnetron 17, after antenna 18 passed waveguide tube wall 19, every end of waveguide 19 had an inclined-plane reflecting plate 34 and the steel cylinder under the inclined-plane reflecting plate 1 to have radio frequency channel window 35, and this structure is to utilize dual and multiple microwave function.
Shown in Figure 5, be another embodiment Fig. 4 normotopia synoptic diagram, solid line has shown square type blind flange 4, handle 31, journal stirrup 32, pivot pin 33.The profile of dotted line has shown the seat and the geometric configuration of rectangular inner cavity top magnetron 17, antenna 18, waveguide 19 and other each assemblies, in just electrothermal tube 28 is installed in top of chamber above, the probe of sensor 27 is installed in below the intracavity bottom.
Fig. 6 is another embodiment normotopia perspective diagram, has provided rectangular pressure vessels the steel cylinder 1 dual or multiple microwave transmission reflective condition behind the madial wall.Square shaped steel cylindrical shell 1 top inner wall can only show the reflecting plate 34 and the waveguide window 35 of waveguide mouth rear and front end among the figure, the microwave that sends from two windows has certain phase difference, has increased the emitting area of microbeam at furnace chamber.Several reflection bars 36 are equipped with in steel cylinder 1 inwall both sides, also can make the circular metal projection and be distributed on the inwall of both sides, and this structure makes the homogeneous radiation in container as much as possible of microwave energy, improve the quality of clearing up of sample.
During operation, behind sample and reagent adding glass test tube 15, be placed on the test tube rack 14, once can put 16 test tubes.Push swing bolt 5 open, draw back blind flange 4, test tube rack 14 is sent into the pressure vessel inner chamber, be placed on the waffle slab 16, shut blind flange 4, fix swing bolt 5 with handle 31.After the energising, by the character of sample and the complexity of clearing up, design temperature, pressure, time.Maximum operating temperature is 180 ℃, and pressure is 1Mpa, and digestion time generally at 2-3 hour, controlled automatically by instrument by Specimen eliminating, staged heats up, and first low temperature, low pressure kept 1-2 hour, after treating that chemical reaction is fully finished, be raised to predetermined temperature and pressure at last, be incubated about 1 hour.Clear up end, after the half an hour of cutting off the power supply, open blowdown valve 9, slowly unload to be depressed into and arrive atmospheric pressure state in the pressure vessel, stopped slightly several minutes, unclamp swing bolt 5, open blind flange 4, take out sample, little yellow that sample is transparent clarification gets final product.
Claims (6)
1. microwave dissolver, comprise anterior pressure vessel, the microwave transmission system at rear portion, pressure sensor diagnostics, electric heater unit, the blind controller system two large divisions forms, it is characterized in that: described pressure vessel is a double-decker, skin is by steel cylinder (1), at the bottom of the steel cylinder (2), the cylindric pressure vessel that flange (3) is welded into, flange (3) is to be connected with swing bolt (5) with blind flange (4), swing bolt (5) is fixed on the journal stirrup (6), journal stirrup (6) is welded on steel cylinder (1) and flange (3) junction, be provided with safety valve (8) and blowdown valve (9) above the outer wall of steel cylinder (1), Steel Pressure Vessels is placed with horizontal type, and instrument is by front and back bearing (7) load-bearing; The inner bag of internal layer (10), adhesive surface (12), gasket seal (13) are to be made by PTFE materials processing, cylinder heat-insulation layer (11) is to be processed into by engineering plastics, they have constituted anticorrosion cavity, and the test tube rack (14) in the cavity is gone up and arranged test tube (15), is placed on the waffle slab (16); Described microwave transmission system has magnetron (17), antenna (18), waveguide (19), commutation diode (20), high-tension transformer (21) to form resonant circuit, and magnetron (17) center outside (2) at the bottom of the steel cylinder is fixing by fixed head (22); Described pressure transducer (27) penetrates in the pressure vessel above (2) at the bottom of steel cylinder, and electrothermal tube (28) penetrates pressure vessel below (2) at the bottom of the steel cylinder; Described instrument (29) control system is made up of microprocessor hardware, connects each electron device of instrument; Tool housing (30) is to be made by metallic sheet stock.
2. microwave dissolver according to claim 1 is characterized in that: the antenna (18) of magnetron (17) lengthening, pass (2) center at the bottom of the steel cylinder, and slightly exceed one centimetre of steel plate; The no cooling fins of magnetron (17) (23), with aluminum water pipe seal welding, by the mobile heat radiation of tap water, magnetron can be worked continuously for a long time, and water pipe is by instrument (29) control electromagnetic valve (24), (25) water inlet and water outlet.
3. microwave dissolver according to claim 1; it is characterized in that: waveguide (19) is copper hollow cylindrical; pass (2) center at the bottom of the steel cylinder; become the circular horn shape; cylinder insulation bottom (11) center of antenna (18) front end in the waveguide (19) is cut out one, has formed hollow section, the outer pressure-bearing cushion block (26) that is equipped with in the inner courage of hollow section (10) bottom; prevent the impact of working pressure, protection antenna (18) is unlikely impaired.
4. microwave dissolver according to claim 1 is characterized in that: after pressure transducer (27) penetrated in the pressure vessel, its detecting head surface had PTFE film anticorrosive coat to coat; Electrothermal tube (28) device is to use the metal tube manufacturing, and its top layer coated with PTFE is divided the bulk cargo anticorrosive coat.
5. microwave dissolver, it is characterized in that: skin is welded into rectangular vessel by (2), flange (3) at the bottom of steel cylinder (1), the steel cylinder, blind flange (4) cuts into rectangle by circle, and four jiaos keep certain radian, swing bolt (5) joint flange (3) and blind flange (4); Safety valve (8), blowdown valve (9) are installed on the plane, steel cylinder (1) external wall of upper portion forward position, about side by side; Internal layer inner bag (10) is to make rectangular cavities by the PTFE material, and heat-insulation layer (11) is to make rectangular cavities by engineering plastics, and adhesive surface (12) and sealing gasket (13) are to make rectangular shape by the PTFE material; On steel cylinder (1) outer wall plane, waveguide (19) vertically is set, settle magnetron (17) in waveguide (19) central upper portion, after antenna (18) passes the waveguide tube wall, every end of waveguide (19) has an inclined-plane reflecting plate (34), and the steel cylinder (1) under the reflecting plate (34) has waveguide window (35); Support the related electric elements of magnetron (17) emission coefficient still to be arranged on the instrument rear portion; Pressure transducer (27) penetrates inner chamber below (2) at the bottom of steel cylinder, electrothermal tube (28) is penetrating inner chamber above (2) at the bottom of the steel cylinder.
6. a kind of microwave dissolver according to claim 5 is characterized in that: in the rectangle Steel Pressure Vessels, several projectioies are housed respectively on the sidewall of the interior both sides of steel cylinder (1), the metallic reflection bar (36) that smooth finish is good helps microwave radiation and evenly distributes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031785190A CN1300559C (en) | 2003-07-08 | 2003-07-08 | Microwave extinguishing instrument |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031785190A CN1300559C (en) | 2003-07-08 | 2003-07-08 | Microwave extinguishing instrument |
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| CN1566922A CN1566922A (en) | 2005-01-19 |
| CN1300559C true CN1300559C (en) | 2007-02-14 |
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| CNB031785190A Expired - Fee Related CN1300559C (en) | 2003-07-08 | 2003-07-08 | Microwave extinguishing instrument |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102713557A (en) * | 2009-11-03 | 2012-10-03 | 7685297加拿大有限公司 | Systems and methods for preparing samples for chemical analysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102713557B (en) * | 2009-11-03 | 2015-04-15 | 7685297加拿大有限公司 | Systems and methods for preparing samples for chemical analysis |
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| Publication number | Publication date |
|---|---|
| CN1566922A (en) | 2005-01-19 |
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