CN201378146Y - Flow injection-gas-phase molecular absorbing spectrometer - Google Patents
Flow injection-gas-phase molecular absorbing spectrometer Download PDFInfo
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- CN201378146Y CN201378146Y CN200920070613U CN200920070613U CN201378146Y CN 201378146 Y CN201378146 Y CN 201378146Y CN 200920070613 U CN200920070613 U CN 200920070613U CN 200920070613 U CN200920070613 U CN 200920070613U CN 201378146 Y CN201378146 Y CN 201378146Y
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- gas
- phase molecular
- flow injection
- heating arrangement
- molecular absorption
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Abstract
The utility model discloses a flow injection-gas-phase molecular absorbing spectrometer, which comprises a sampling device, a gas-liquid separating device, a drying device and a detecting device. The flow injection-gas-phase molecular absorbing spectrometer is characterized in that the gas-liquid separating device comprises a sampling inlet 1, a reacting cavity 2, a gas outlet 3, a communicating device outlet 4, a waste liquor exhausting port 5 and an air-pressure balancing port 6; the sampling inlet 1 is communicated with the reacting cavity 2, the reacting cavity 2 is communicated with the waste liquor exhausting port 5 and the air-pressure balancing port 6 through the communicating device outlet 4. The utility model provides the flow injection-gas-phase molecular absorbing spectrometer; the operation is simpler, objectivity of the analyzing results is enhanced, analyzing sensitivity and precision are better, automatic on-line heating is realized, and the application range is wider.
Description
Technical field
The utility model relates to the optic analytical instrument technical field, relates in particular to a kind of flow injection-gas phase molecular absorption spectrometer.
Background technology
It is the seventies in 20th century that the theoretical research work of gas-phase molecular absorption spectrometry method starts from.People such as Gresser in 1976 at first propose this method (Gas-Phase Molecular Absorption Spectrometry is called for short GPMAS) Syty and use this method at first and measured SO
2, after this analysts have successfully measured corrosivity, volatile gas, as I
2And Br
2, H
2S, NOCL, HCN, NO
2 [And NO, people such as Rechikov have measured B, N, P, As, Sb, the Si of the hydride gas that the inert gas that is used for semiconductor technology mixes, the hydride of Ge, Sn.But all at that time work all only is confined to laboratory internal theory research to be used, and scientists was built simple reaction unit just according to the principles of chemistry, had tentatively realized this The Application of Technology.Again because the limitation of photoelectric technology at that time, not as people's will, thereby the applied research of gas-phase molecular absorption spectrometry method is lain over aspect the sensitivity of analytical test.
In recent years, the defective of some traditional analytical approachs on using is exposed more and more, such as: complex operation, analytical procedure is too many, when if sample size to be tested is big,, be unfavorable for the requirement of modern society for the analysis result promptness just analysis efficiency sharply reduces; In addition, therefore the traditional analysis method mostly is a colourimetry, is easy to be subjected to water body turbidity and color interference when measuring, especially for the waste water of some matrix complexity, classic method is almost powerless, and the limitation of its range of application is difficult to fully satisfy the modern analysis demand.
So people's the visual field turns to the gas-phase molecular absorption spectrometry method once more, because this method is composition to be determined to be converted into gas measure afterwards again, thereby it is when superiority is analyzed exactly the most intuitively, be subjected to the interference of water body turbidity and color hardly, very Fu Za water body can be measured, and has also just widened the range of application of method greatly.In addition, analysis speed is also obviously accelerated many, the analysis that former half an hour just can finish, only need now one minute less than just can, analysis efficiency improves greatly.And the sensitivity of gas molecule in space absorption process and detection limit all are not less than classic method, and this technology can substitute classic method fully, and have well remedied the deficiency of classic method.The standard method that relevant for this reason application gas-phase molecular absorption spectrometry method is measured has also obtained announcement.
The theoretical foundation of gas-phase molecular absorption spectrometry method is Lambert-Beer's law.Normal conditions, when being in some gas molecule generation vibration of ground state, the energy of absorption is certain, and molecular conecentration is big more, and the energy of absorption is many more, just can judge the concentration of composition to be measured by measuring the energy that absorbs.
According to above-mentioned principle, when measuring,, tested composition is converted into corresponding specific gas by certain chemical reaction, selection can excite the wavelength of this molecular vibration, measures its absorbance, and the concentration and the absorbance of this gas present linear relationship in the certain limit.Can carry out quantitative test to the gas that generates thus, thereby calculate the content of tested composition.
For example: analyze sulfide and measured object can be converted into H
2The S eudiometry; Analyze nitrite and measured object can be converted into NO
2Eudiometry; Analyze total nitrogen and measured object can be converted into the NO eudiometry; Measured object can be reduced to mercury vapour when analyzing mercury content and measure (cold atom principle of absorption).
In the patent No. is 99239921.1 Chinese patent instructions, " a kind of flow injection-gas phase molecular absorption spectrometer; include the flashlight power supply; line source; front and back lens combination; absorption cell; monochromator is disclosed, detecting device, signal processing, control section, read part, the output of flashlight power supply is connected to line source, the front and back lens combination is arranged at the rear and front end of absorption cell, monochromator, detecting device places front lens group successively, after absorption cell and the rear lens group, and signal processing is received in the output of detecting device, control section is received in the output of signal processing, the output of control section is received and is read part, it is characterized in that: this spectrometer further comprises sample product reactor, pneumatic pump, sample product reactor is connected with absorption cell, pneumatic pump is received in the output of control section, and pneumatic pump is connected with sample product reactor; Described absorption cell is designed to double horn type quartz window absorption tube.Described sample product reactor adopts gas-liquid separator.This spectrometer also further includes the gas sampling processing section, and described gas sampling processing section also is connected with absorption cell.It is grournd glass ventilation chock plug that described gas-liquid separator is designed to a top, and the bottom is a reaction bulb, and reaction bulb is built-in with a glass core decollator.”
In the embodiment of above-mentioned patent specification,, mentioned " described sample product reactor employing gas-liquid separator 3 in conjunction with the accompanying drawing 3 of above-mentioned patent specification.It is grournd glass ventilation chock plug 31 that described gas-liquid separator 3 is designed to a top, the bottom is a reaction bulb 32, reaction bulb 32 is built-in with a glass core decollator 33, its analysis to as if gaseous molecular, air can evenly spread from all quarter by glass core decollator 33, make example reaction rapid, can obtain maximum sample concentration.”
Gas-liquid separation device is similar in other words with the gas-liquid separator of mentioning in the preamble, has also enumerated the structure of an a kind of gas-liquid separation device used in the prior art in the application's Figure of description 3.This gas-liquid separator 33 (as Fig. 3-C), comprise reaction bulb 31 (similar test tube structure, hollow circular cylinder, upper end open, as Fig. 3-A) and bottle cap 32 (as Fig. 3-B), bottle cap 32 has mouth of pipe B1, B2 and B3.Its course of work is described below:
1, by transfer pipet and quantitative sample injector reagent and sample are joined in the reaction bulb 31, must guarantee to add the precise volumes of sample;
2, bottle cap 32 is positioned in the reaction bulb 31, shown in Fig. 3-C, the manual unlocking pneumatic pump is pressed into air by B2, after the gas that reaction is produced is loaded into drying agent by B3, enters detection means measure;
3, analytic process briefly is described as successively, connect each parts successively with rubber hose, cleaning reaction bottle 31 and bottle cap 32 add reagent with quantitative sample injector, accurately add sample with transfer pipet, insert bottle cap 32 in the reaction bulb 31 rapidly, screw, open pneumatic pump, ventilation, press zeroing, reading button successively, obtain analysis result at last.
As seen, existing flow injection-gas phase molecular absorption spectrometer operation steps is many, complicated; Need the human intervention test process, influence objectivity; The accuracy of sampling is influenced greatly by operators'skills, thus the impact analysis result; Bottle cap screwing causes gas leakage inadequately easily in the analytic process; The drying agent life-span is low, does not have online heating function, and range of application is restricted.
The utility model content
The purpose of this utility model provides a kind of flow injection-gas phase molecular absorption spectrometer, solution is existing, and flow injection-the gas phase molecular absorption spectrometer operation steps is many, analysis result is influenced greatly by operating personnel's technical ability, gas leakage easily, analysis time is long, the problem that needs human intervention and do not have online heating function.
The technical solution of the utility model is, a kind of flow injection-gas phase molecular absorption spectrometer, comprise sampling device, gas-liquid separation device, drying device and pick-up unit, it is characterized in that, described gas-liquid separation device comprises injection port 1, reaction chamber 2, gas vent 3, linker outlet 4, waste liquid row mouth 5 and air pressure balance mouth 6, described injection port 1 is communicated with described reaction chamber 2, and described reaction chamber 2 is communicated with described waste liquid row mouth 5 and air pressure balance mouth 6 by described linker outlet 4.Described gas vent 3 is communicated with the input of described drying device, and described injection port 1 also is communicated with the output of described sampling device.
Described reaction chamber 2 comprises multilayer hangnail structure 7.
Described flow injection-gas phase molecular absorption spectrometer also comprises heating arrangement, and the output of described sampling device is communicated with the input of described heating arrangement, and measured object enters described heating arrangement through behind the described sampling device, enters described gas-liquid separation device then.
Described heating arrangement is the cylinder 11 of hollow, and described cylinder 11 includes heater 12, and the outside surface spiral twines bend pipe 1.
Described cylinder 11 is carved with spiral groove, and described bend pipe 1 is embedded in this spiral groove.
Described heating arrangement comprises container 21, comprises one section of bend pipe 2 22, heater coil 23 and temperature sensor 24 in this container 21.
Described sampling device comprises peristaltic pump 41, pressure maintaining valve 42 and many siphunculus 43, the reagent of reaction needed and sample are transported at least one input port of described many siphunculus 43 by described peristaltic pump 41, the carrier gas of reaction needed is input at least one other input ports of described many siphunculus 43 by described pressure maintaining valve 42, and the delivery outlet of described many siphunculus 43 leads to described gas-liquid separation device.
Described sampling device comprises peristaltic pump 41, pressure maintaining valve 42 and many siphunculus 43, the reagent of reaction needed and sample are transported at least one input port of described many siphunculus 43 by described peristaltic pump 41, the carrier gas of reaction needed is input at least one other input ports of described many siphunculus 43 by described pressure maintaining valve 42, and the delivery outlet of described many siphunculus 43 leads to described heating arrangement.
The beneficial effects of the utility model are simple to operate, and the objectivity of analysis result is strong, and sensitivity for analysis and precision are good, realize the automatic on-line heating, and range of application is wideer.
Description of drawings
Fig. 1 is the composition module frame chart of flow injection-gas phase molecular absorption spectrometer among the utility model one embodiment
Fig. 2 is that the structure of gas-liquid separation device among the utility model one embodiment is formed synoptic diagram
Fig. 3 is the utility model a kind of gas-liquid separation device synoptic diagram of the prior art
Fig. 4 is a heating arrangement synoptic diagram among the utility model one embodiment
Fig. 5 is a heating arrangement longitudinal profile synoptic diagram among the utility model one embodiment
Fig. 6 is a heating arrangement schematic cross section among the utility model one embodiment
Fig. 7 is a heating arrangement processing synoptic diagram among the utility model one embodiment
Fig. 8 is a heating arrangement schematic surface among the utility model one embodiment
Fig. 9 is a heating arrangement synoptic diagram among the utility model one embodiment
Figure 10 is the composition of pick-up unit among the utility model one embodiment and concerns synoptic diagram with gas-liquid separation device
Figure 11 is the theory of constitution synoptic diagram of sampling device among the utility model one embodiment
Embodiment
Below in conjunction with accompanying drawing concrete enforcement of the present utility model is described in further details.
As shown in Figure 1, the disclosed flow injection-gas phase molecular absorption spectrometer of the utility model comprises sampling device, heating arrangement, gas-liquid separation device, drying device and pick-up unit.Again, as Figure 11, sampling device is input in many siphunculus 43 by the reagent and the sample of peristaltic pump 41 with reaction needed, then simultaneously by the carrier gas of being carried by pressure maintaining valve 42, be that air (or nitrogen) is transported to heating arrangement, form gas and mixtures of liquids in the course of conveying.Peristaltic pump is common on the market four-way or two channel architectures, and many siphunculus can be selected five-way pipe, four-way piece or three-way pipe as required.Potpourri enters gas-liquid separation device through behind the heating arrangement, realizes gas and fluid separation applications, after the gained gas process drying device drying, installs detection computations after testing and obtains analysis result.Simple drying device can adopt the built-in drying agent of hollow glass tube to realize, and for some test item, can not heat, so the heating arrangement here can not need, but as open heating arrangement, then can obviously improve analysis project sensitivity.
Pick-up unit described in the utility model, comprise that common flow injection-gas phase molecular absorption spectrometer all needs light-source system, optical system, testing circuit and the test control software for calculation that comprises, except the measured object through gas-liquid separation device is detected and analytical calculation according to standard, in fact also comprised for finishing gas-phase molecular absorption spectrometry automatically and analyzed necessary control function and necessary optics and circuit for each parts.Figure 10 is the composition of pick-up unit among the utility model embodiment and concerns synoptic diagram with gas-liquid separation device, reacted pick-up unit described in the utility model composition and with the relation of gas-liquid separation device.
As shown in Figure 2, gas-liquid separation device comprises injection port 1, reaction chamber 2, gas vent 3, linker outlet 4, waste liquid row mouth 5 and air pressure balance mouth 6, injection port 1 is communicated with reaction chamber 2, and reaction chamber 2 is communicated with waste liquid row mouth 5 and air pressure balance mouth 6 by linker outlet 4.Gas vent 3 is communicated with the input of drying device, and injection port 1 also is communicated with the output of sampling device.Reaction chamber 2 comprises multilayer hangnail structure 7.In flow injection-gas phase molecular absorption spectrometer sample test process, mixed solution after the heating enters into reaction chamber 2 from injection port 1 under the effect of carrier gas, because action of gravity, most liquid flow out downwards, through linker outlet 4 outlets, emit for 5 mouthfuls from waste liquid row mouth.In addition, entering in the reaction chamber 2 small part steam and gas overflows through gas vent 3 outlets from top.The top of reaction chamber 2 is inwardly long multilayer hangnail structure 7, the part steam interception of upwards overflowing can be reduced steam and overflows from gas vent 3 outlets.Liquid level and linker outlet 4 outlet maintenance levels in the reaction chamber 2, when excess liquid is quiet when eating, by law of connected vessels, redundance will be discharged through linker outlet 4 outlets.The hollow pipe of air pressure balance mouth 6 for communicating with the external world, fundamental purpose is exactly a balance gas-liquid separator inner and outer air pressure.For the manufactured materials of gas-liquid separation device, can select other resistant materials such as simple glass, quartz, teflon.
Flow injection-gas phase molecular absorption spectrometer that the utility model provides also comprises heating arrangement, and sample enters heating arrangement through behind the sampling device, enters described gas-liquid separation device then.
As shown in Figure 4, be a kind of heating arrangement synoptic diagram, Fig. 5 is this heating arrangement longitudinal profile synoptic diagram, and Fig. 6 is this heating arrangement schematic cross section, and described heating arrangement is the cylinder 11 of hollow, includes heater 12, and the outside surface spiral twines bend pipe 1.Cylinder 11 is carved with spiral groove, and bend pipe 1 is embedded in this spiral groove.Being the processing synoptic diagram that is carved with a kind of modifying device of spiral groove on heating arrangement shown in Figure 4 as shown in Figure 7, is the damaged surface synoptic diagram that has spiral groove of heating arrangement shown in Figure 7 as shown in Figure 8.Concrete process is, select for use the material of teflon to make the pipeline of carrying liquid, outer diameter tube is 2～5mm roughly, length 1～4m, liquid is through being transferred, and pipeline is entangled in the groove of well heater outer wall, the heating plate adstante febre, heat is delivered to tube wall by the right cylinder of heat conduction, is delivered to liquid again, thereby allows liquid be heated.Choose one section good aluminium matter or copper and other material etc. of heat conductivility and make right cylinder, the screw-like groove is carved with in the right cylinder outside.The size of groove is consistent with the duct size of carrying liquid, then pipeline is embedded in the groove.A square hole or other shape hole are left in the right cylinder center, place heating plate in the hole, fill with Heat Conduction Material in the gap of heating plate and square hole.The temperature that heating need reach cooperates electronic relay to control by temperature sensor to realize, perhaps directly select for use can the fixed temperature heating heating material.
The utility model also provides another heating arrangement, and as shown in Figure 9, heating arrangement comprises container 21, comprises one section of bend pipe 2 22, heater coil 23 and temperature sensor 24 in this container 22.Principle of work is, holds resistant to elevated temperatures conduction oil in the container, and by the heater coil heating, heating-up temperature cooperates electromagnetic relay to control by temperature sensor.Carry the pipeline of liquid to put into thermostable heat-conductive oil major part, heat is being delivered to liquid, thereby is allowing liquid be heated by tube wall.
Compared with the prior art, the flow injection-gas-phase molecular absorbing spectrometer that provides of the utility model has following features:
1) operation is simpler, can find out obviously that from analytic process existing equipment need to be through 7 step ability Finish analysis, the utility model only needed for 2 steps just can realize sample determination. Use the utility model can be greatly Reduce analytical procedure, make operation simpler, easier quilt is grasped;
2) objectivity of analysis result is stronger, and utility model is not used the accurate utensils such as pipette when the operation sampling, Avoided because operating personnel's analytical skill and the different error of bringing of qualification. Prior art equipment is dividing Must screw lid when analysing, screw in the process usually easily gas leakage, and whole reaction of the present utility model is entirely Carry out in the sealing situation, without any artificial intervention, avoided gas leakage, also guaranteed the visitor of analysis result simultaneously The property seen;
3) sensitivity for analysis is higher, and precision is better, the utility model when measuring gas-liquid separation efficient far above Existing equipment, with isocyatic sample analysis be obtain absorbance signal stronger, sensitivity is also just higher. Unmanned for intervening in the mensuration process, influenced factor is little, so precision is better;
4) operating cost is cheaper, and drier service life is 5 times of existing instrument;
5) the automatic on-line heating can be realized, when total nitrogen or nitrate nitrogen are measured, suitable temperature need to be heated to Reaction just can take place. Like product is to want to utilize sample water bath with thermostatic control to be heated to 70 ± 2 ℃ earlier, and then surveys Fixed. And the technical solution of the utility model does not need to heat in advance by water bath with thermostatic control, can direct injection analysis, Automatically sample is heated to 70 ± 2 ℃ or other temperature. If heat with water bath with thermostatic control in advance in the prior art, This step expends time in needs about 30 minutes, adopts on-line heating can save this part time, therefore big Improved greatly analysis efficiency.
6) range of application is wider, and existing equipment is when measuring the sample of easily foaming, and the foam of generation can enter dried Drying prescription lost efficacy drier, thereby such sample can not be measured by existing equipment, and the utility model provides Technical scheme then can measure, therefore reason is that sample is fully disperseed, and then demulsification, can not Produce a large amount of foams.
Claims (8)
1, a kind of flow injection-gas phase molecular absorption spectrometer, comprise sampling device, gas-liquid separation device, drying device and pick-up unit, it is characterized in that, described gas-liquid separation device comprises injection port (1), reaction chamber (2), gas vent (3), linker outlet (4), waste liquid row mouthful (5) and air pressure balance mouth (6), described injection port (1) is communicated with described reaction chamber (2), described reaction chamber (2) is communicated with described waste liquid row mouthful (5) and air pressure balance mouth (6) by described linker outlet (4), described gas vent (3) is communicated with the input of described drying device, and described injection port (1) also is communicated with the output of described sampling device.
2, flow injection-gas phase molecular absorption spectrometer according to claim 1 is characterized in that described reaction chamber (2) comprises multilayer hangnail structure (7).
3, flow injection-gas phase molecular absorption spectrometer according to claim 1, it is characterized in that, described flow injection-gas phase molecular absorption spectrometer also comprises heating arrangement, the output of described sampling device is communicated with the input of described heating arrangement, measured object enters described heating arrangement through behind the described sampling device, enter described gas-liquid separation device then, described injection port (1) is communicated with the output of described heating arrangement.
4, as flow injection-gas phase molecular absorption spectrometer as described in the claim 3, it is characterized in that described heating arrangement is the cylinder (11) of hollow, described cylinder (11) includes heater (12), and the outside surface spiral twines bend pipe one (13).
5, as flow injection-gas phase molecular absorption spectrometer as described in the claim 4, it is characterized in that described cylinder (11) is carved with spiral groove, described bend pipe one (13) is embedded in this spiral groove.
6, as flow injection-gas phase molecular absorption spectrometer as described in the claim 3, it is characterized in that described heating arrangement comprises container (21), comprise one section of bend pipe two (22), heater coil (23) and temperature sensor (24) in this container (21).
7, flow injection-gas phase molecular absorption spectrometer according to claim 1, it is characterized in that, described sampling device comprises peristaltic pump (41), pressure maintaining valve (42) and many siphunculus (43), the reagent of reaction needed and sample are transported at least one input port of described many siphunculus (43) by described peristaltic pump (41), the carrier gas of reaction needed is input at least one other input ports of described many siphunculus (43) by described pressure maintaining valve (42), and the delivery outlet of described many siphunculus (43) leads to described gas-liquid separation device.
8, as flow injection-gas phase molecular absorption spectrometer as described in the claim 3, it is characterized in that, described sampling device comprises peristaltic pump (41), pressure maintaining valve (42) and many siphunculus (43), the reagent of reaction needed and sample are transported at least one input port of described many siphunculus (43) by described peristaltic pump (41), the carrier gas of reaction needed is input at least one other input ports of described many siphunculus (43) by described pressure maintaining valve (42), and the delivery outlet of described many siphunculus (43) leads to described heating arrangement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200920070613U CN201378146Y (en) | 2009-04-17 | 2009-04-17 | Flow injection-gas-phase molecular absorbing spectrometer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200920070613U CN201378146Y (en) | 2009-04-17 | 2009-04-17 | Flow injection-gas-phase molecular absorbing spectrometer |
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| CN201378146Y true CN201378146Y (en) | 2010-01-06 |
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| CN200920070613U Expired - Lifetime CN201378146Y (en) | 2009-04-17 | 2009-04-17 | Flow injection-gas-phase molecular absorbing spectrometer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106092943A (en) * | 2016-06-02 | 2016-11-09 | 上海北裕分析仪器股份有限公司 | A kind of method using gas-phase molecular absorption spectrometry method to carry out COD test |
| CN107291113A (en) * | 2017-07-04 | 2017-10-24 | 中国科学院国家空间科学中心 | A kind of vacuum temperature control light path purifier |
-
2009
- 2009-04-17 CN CN200920070613U patent/CN201378146Y/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106092943A (en) * | 2016-06-02 | 2016-11-09 | 上海北裕分析仪器股份有限公司 | A kind of method using gas-phase molecular absorption spectrometry method to carry out COD test |
| CN107291113A (en) * | 2017-07-04 | 2017-10-24 | 中国科学院国家空间科学中心 | A kind of vacuum temperature control light path purifier |
| CN107291113B (en) * | 2017-07-04 | 2018-12-04 | 中国科学院国家空间科学中心 | A kind of vacuum temperature control optical path purification device |
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Legal Events
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|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: SHANGHAI BEIYU ANALYTICAL INSTRUMENT CO., LTD. Free format text: FORMER OWNER: CHEN FAN Effective date: 20120331 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 201900 BAOSHAN, SHANGHAI TO: 200941 BAOSHAN, SHANGHAI |
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| TR01 | Transfer of patent right |
Effective date of registration: 20120331 Address after: 200941, room 822, 230 Xin Nan Lu, Shanghai, Baoshan District Patentee after: Shanghai Beiyu Analytical Instruments Co., Ltd. Address before: 201900 No. 800, Fujin Road, Shanghai, Baoshan District Patentee before: Chen Fan |
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| CX01 | Expiry of patent term |
Granted publication date: 20100106 |
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| CX01 | Expiry of patent term |