CN2826429Y - Novel gas chromatographic detector - Google Patents
Novel gas chromatographic detector Download PDFInfo
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- CN2826429Y CN2826429Y CN 200520106417 CN200520106417U CN2826429Y CN 2826429 Y CN2826429 Y CN 2826429Y CN 200520106417 CN200520106417 CN 200520106417 CN 200520106417 U CN200520106417 U CN 200520106417U CN 2826429 Y CN2826429 Y CN 2826429Y
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Abstract
The utility model discloses a novel gas chromatography detector such as a nitrogen phosphorous detector, a flame photometry detector and an electron capture detector. The utility model comprises a chromatographic column interface cavity which is connected with a chromatographic column, a three-way switching valve which is connected with the chromatographic column interface cavity, and a gas discharge pipe. The three-way switching valve comprises one inlet and two outlets, wherein the inlet is connected with a gas source; a first outlet is communicated with the chromatographic column interface cavity in a position above the port of the chromatographic column; a second outlet is communicated with the chromatographic column interface cavity in a position below the port of the chromatographic column; the gas discharge pipe is communicated with the chromatographic column interface cavity in a position below the port of the chromatographic column. With the application of the gas chromatography detector, the service life of the detector can be greatly prolonged, and in addition, the using range of the detector is also enlarged.
Description
Technical field
The utility model relate generally to gas chromatography detector is in particular to novel nitrogen phosphorous detector, flame photometric detector (FPD) and electron capture detector (ECD).
Background technology
Nitrogen phosphorous detector (NPD) is a kind of gas chromatography (GC) detecting device of ionization type, and it has very high selectivity and sensitivity for the organic principle that comprises nitrogen (N) and/or phosphorus (P).Fig. 1 shows a kind of principle schematic of existing nitrogen phosphorous detector, below this is done simple the introduction.
A critical component of nitrogen phosphorous detector is a pearl 1, and it is to be made by the glass of the alkalinous metal that comprises rubidium or caesium etc.In the atmosphere of high temperature and air, hydrogen, pearl 1 can form the surface with catalytic activity.Pearl 1 stretches in the chamber of gatherer 2 some or all ofly.Gatherer 2 has electric conductivity, generally is offset to certain electromotive force (for example positive potential).During work, pearl 1 is heated to 600～800 ℃ by electrical heating method.Air 4 is introduced into by the road, and make-up gas? (or be called and supply gas, be identical with carrier gas composition in the chromatographic column usually) and/or hydrogen are introduced into from pipeline 5, and the sample (also comprising solvent usually) that contains nitrogen and/or phosphorus passes through chromatographic column 6 and is introduced under carrier gas drives.Each gas flow as shown in Figure 2.As shown in Figure 2, after sample gas and make-up gas? converge, flow through shower nozzle 3 together and enter collector chamber, the catalytically active surface of sample sets branch and pearl 1 is had an effect and is produced negative ion then, and shifts to gatherer 2 under electric field action, thereby produces signal.The pot (not shown) that is electrically connected with gatherer 2 amplifies, measures the electric current that gatherer 2 places form.Can learn relevant composition information in the analyzed gas by the variation of analyzing electric current.
A main deficiency of NPD detecting device of the prior art is its performance variation in time and gradually, and serviceable life is shorter.Through measuring, under the situation of not introducing actual sample idle running, about 1000 hours of the serviceable life of pearl 1.But when sample is analyzed, then can be reduced to the serviceable life of pearl 1 about 400 hours in actual use.Cause the main cause of this situation to have two: (A) in the analyte detection process, the introducing of solvent and sample causes the surface temperature of pearl 1 sharply to descend, thereby causes the surface structure breakage of pearl 1, and then has reduced the serviceable life of pearl; (B) surface reaction of sample component and pearl 1 has consumed the active component of bead surface, has reduced serviceable life.
The main deficiency of another of NPD detecting device of the prior art is that it is to choice of Solvent.Because some solvent, chloroform for example has great destructiveness to the surface of pearl, so be not suitable for the NPD detecting device.But chloroform is the common solvent in the stratographic analysis experiment, and for many application scenarios, chloroform is owing to its efficient and excellent performance becomes optimal selection.So just make the usable range of NPD detecting device dwindle greatly.
Other well known to a person skilled in the art gas chromatography detector, and for example flame photometric detector (FPD) (FPD) and electron capture detector (ECD) (ECD) also exist serviceable life than similar problem such as weak points.
Therefore, need a kind of method and apparatus that can make things convenient for, prolong economically the serviceable life of gas chromatography detector (for example NPD detecting device, FPD detecting device or ECD detecting device) and/or enlarge its usable range.
The utility model content
In view of above-mentioned deficiency of the prior art, it is a kind of with low cost, simple in structure, applied widely and have the NPD detecting device in serviceable life of prolongation and FPD detecting device, an ECD detecting device that the utility model provides.
The utility model is by being connected a three-way switch valve on the hub cavity that links to each other in gas chromatography detector and chromatographic column and a gas outlet solves above-mentioned technical matters.
On the one hand, the utility model provides a kind of nitrogen phosphorous detector, comprises pearl, gatherer and the chromatographic column hub cavity that is connected with chromatographic column, comprises a three-way switch valve and a gas outlet in addition; And this transfer valve comprises an inlet and two outlets; Inlet is connected with a gas source; First position of outlet more than the chromatographic column port is connected with the chromatographic column hub cavity; And second position of outlet below the chromatographic column port is connected with the chromatographic column hub cavity; The position of gas outlet below the chromatographic column port is connected with the chromatographic column hub cavity.
On the other hand, the utility model provides a kind of flame photometric detector (FPD), it comprises illuminated chamber and is used to hold chromatographic column, the chromatographic column hub cavity that is communicated with illuminated chamber, comprise a three-way switch valve in addition, and gas outlet that is communicated with the chromatographic column hub cavity, wherein three-way switch valve comprises an inlet and two outlets, the inlet of three-way switch valve is connected with a make-up gas? source, the position of outlet more than the chromatographic column port is connected with the chromatographic column hub cavity, another outlet position below the chromatographic column port is connected with the chromatographic column hub cavity, and the position of gas outlet below the chromatographic column port is connected with the chromatographic column hub cavity.
On the other hand, the utility model provides a kind of electron capture detector (ECD), it comprises anode, negative electrode, radioactive source and the chromatographic column hub cavity that is used to hold chromatographic column, comprise a three-way switch valve in addition, and gas outlet that is communicated with the chromatographic column hub cavity, wherein three-way switch valve has an inlet and two outlets, inlet is connected with a make-up gas? source, the position of outlet more than the chromatographic column port is connected with the chromatographic column hub cavity, another outlet position below the chromatographic column port is connected with the chromatographic column hub cavity, and the position of gas outlet below the chromatographic column port is connected with the chromatographic column hub cavity.
Description of drawings
Fig. 1 is a schematic structure cut-open view of existing NPD detecting device.
Fig. 2 is the internal gas flow schematic diagram of existing NPD detecting device shown in Figure 1 in working order the time.
Fig. 3 is the structural representation according to the novel NPD detecting device of an embodiment of the utility model.
Fig. 4 A, 4B show the gas flow synoptic diagram that NPD detecting device shown in Figure 3 is worked respectively under normal mode and cleaning model.
Fig. 5 is the novel FPD detector arrangement synoptic diagram according to an embodiment of the utility model.
Fig. 6 is the new E CD detector arrangement synoptic diagram according to an embodiment of the utility model.
Embodiment
For the ease of understanding the utility model better, some embodiment of the present utility model will be described below.But should be realized that, these embodiment just can embody the concrete example of the utility model spirit, it is exemplary but not exhaustive, and those skilled in the art is under the instruction of these embodiment, be easy to the following specific embodiment that provides is made alternative, distortion and improved, so the utility model is not limited to following specific embodiment.In addition, in explanation and describing, some known structure, parts, feature, method are not elaborated, have obscured the utility model in order to avoid a presumptuous guest usurps the role of the host.In the accompanying drawings, unless specialize, identical or similar label is represented identical or similar elements or step.
Fig. 3 shows the NPD detecting device 300 according to an embodiment of the utility model.The NPD detecting device 300 of present embodiment comprises pearl 301, gatherer 302, shower nozzle 303 and the chromatographic column hub cavity 310 that is connected with chromatographic column 306, and air and/or hydrogen are introduced into from pipeline 304.In addition, this NPD detecting device 300 also comprises the controller 370 of a three-way switch valve 350 and gas outlet 380 and and valve 350 electric coupling.This transfer valve 350 comprises 351 and two outlets 356,358 of an inlet.Inlet 351 is connected with make-up gas? source (not shown); First outlet 356 is connected with chromatographic column hub cavity 310 in the position of chromatographic column 306 ports more than 361; And second outlet 358 is connected with chromatographic column hub cavity 310 in the position of chromatographic column 306 ports below 361.And gas outlet 380 is connected with chromatographic column hub cavity 310 in the position of chromatographic column 306 ports below 361.
Note, here " more than ", " following " just have relative meaning, usually the direction that flows along sample gas in the NPD detecting device cavity is defined as to " on ", and opposite direction is defined as to D score.
The three-way switch valve here is meant to have 3 connected entrances that link to each other with the external world (inlet and two outlets) and can switch any valve of the direction of flow of flowing through wherein.This valve is well known to a person skilled in the art.According to the specific requirement to valve size, flow and switching mode, those skilled in the art can select and buy the transfer valve of required suitable types from various known three-way switch valves.For the utility model, the valve that electromagnetism switches is preferred, because this valve can be controlled blocked operation automatically by programming.For example, the Fluid Automation Systems company model of producing is the NPD detecting device that the valve of CH-1290 Versoix is specially adapted to the utility model embodiment.
In addition, note that here three-way switch valve, gas outlet are schematically, draw for principle of the present utility model is described, rather than draw in proportion.Actual three-way switch valve may be very little, for example can be integrated in NPD detecting device enclosure interior, and gas outlet also can be integrated in NPD detecting device enclosure interior, the feasible like this NPD detecting device according to the utility model embodiment has size and the appearance profile same with traditional NPD detecting device, can cooperate existing gas chromatography system easily, and not need the physical construction of chromatographic system is made any change.
Because the existence of three-way switch valve 350, make-up gas? just can enter chromatographic column hub cavity 310 two different positions, and this is corresponding to two kinds of operator schemes of NPD detecting device 300.When transfer valve switches to second outlet 358 the time, make-up gas? enters chromatographic column hub cavity 310 from the position of chromatographic column 306 ports 361 below, and the NPD detecting device is in " normally " mode of operation (shown in Fig. 4 A) at this moment.When transfer valve switches to first outlet 356 the time, make-up gas? enters chromatographic column hub cavity 310 from the position of chromatographic column 306 ports 361 or more, and the NPD detecting device is in " cleaning " mode of operation (shown in Fig. 4 B) at this moment.
From Fig. 4 A as can be known, during normal mode, make-up gas? enters chromatographic column hub cavity 310 from the position of chromatographic column 306 ports below 361.Part make-up gas? is discharged from gas outlet 380, and another part make-up gas? converges with the sample gas that comes from chromatographic column 306, and upwards enters collector chamber through shower nozzle 303 together, the sample gas component therein with pearl 301 surface reactions, thereby detect normally.As seen, under normal mode, similar to the NPD detecting device of prior art according to the operation of NPD of the present utility model.
From Fig. 4 B as can be known, during cleaning model, make-up gas? enters chromatographic column hub cavity 310 from chromatographic column 306 ports more than 361; Because the flow of make-up gas? is usually greater than the flow of sample gas, this part make-up gas? has been suppressed the sample gas that comes from chromatographic column 306, force sample gas to turn to, consequently nearly all in fact sample gas is all discharged from gas outlet 380, and make-up gas? upwards enters collector chamber through shower nozzle 303.That is to say that under cleaning model, sample gas does not enter collector tank, but directly discharge from gas outlet 380; What enter collector tank all is the make-up gas? of inertia, thus pearl 1 not can with the component reaction of sample gas, being reflected on the spectrogram is exactly a basic straight line concordant with baseline.
Switching between these two kinds of patterns is to carry out according to the steering order of controller 370.Usually, after the start operation, the NPD300 acquiescence is in normal manipulation mode; And when desired components does not flow out in the sample gas, normal manipulation mode is changed into cleaning model from chromatographic column, desired components is directly discharged from gas outlet; After desired components has all flowed out, revert to normal manipulation mode at this more subsequently, continue to detect normally.Here " not desired components " is meant does not need the component that detects or the component harmful to pearl 301, for example hazardous solvent (as chloroform etc.).Like this, in case in the sample gas certain not desired components (for example hazardous solvent) from chromatographic column, flow out, just directly discharge, and can pass through pearl 301, thereby avoided integument to destroy or corrode from gas outlet 380; And in case this not desired components is discharged fully, NPD 300 promptly reverts to normal manipulation mode, and analyte detection process is continued and can not be subjected to any adverse influence.That is to say that NPD 300 allows optionally " filtration " to fall certain component or solvent.So just advantageously prolong the serviceable life of pearl, and can not interrupt normal analyzing and testing; Simultaneously, also enlarged the usable range of NPD detecting device, because the use of solvent is no longer limited.
As for the time of occurrence of desired components not in the sample, can determine according to experimenter's experience or condition experiment.Usually, before carrying out formal stratographic analysis experiment, the experimenter can carry out repeatedly condition experiment (preliminary experiment) earlier and grope the chromatographic run parameter.And just can pre-estimate out the general time (retention time) that certain component flows out in the sample from chromatographic column in case in condition experiment, determined chromatographic run parameter, testing crew.For example, many samples will use halogenated hydrocarbon solvent, and this kind solvent is mordant to pearl.After having optimized the chromatographic run parameter through condition experiment, the time of occurrence of solvent peak is just basic in the chromatogram has determined.Utilize these information, controller 370 just can be realized the control to transfer valve 350, avoids not desired components (for example halogenated hydrocarbon solvent) to the damage of pearl.
For controller 370, those skilled in the art can realize various forms of controllers as required.For example, controller 370 can be independently a hardware circuit or an integrated circuit, or the firmware that wherein has program stored therein, or circuit board or processor etc.Perhaps, controller 370 also can be realized by the existing controller in gas chromatograph or the nitrogen phosphorous detector or CPU are carried out reprogramming.It will be understood by those skilled in the art that these ways of realization can mutual alternative.Preferably directly utilize existing controller or CPU in the gas chromatograph, realize controller 370, because do not need existing nitrogen phosphorous detector parts are carried out bigger change like this by reprogramming.
According to a preferred embodiment of the present utility model, for the ease of control transfer valve 350, can comprise a storer in the controller 370, wherein store a logical time table.The experimenter can set this timetable before experiment, the time period of desired components is recorded in this table estimating to occur not.Like this, in formal analysis experimentation, controller just can read this time-event table, sends instruction in the specific time and makes transfer valve carry out blocked operation.For example, under the situation of using halogenated hydrocarbon solvent, just the peak period that goes out of solvent peak can be recorded in the time-event table; Thereby in the stratographic analysis experimentation, in the time of appointment, controller 370 will send instruction makes NPD 300 switch to " cleaning " operator scheme, makes solvent walk around pearl, thereby avoids the damage to pearl; After solvent was walked around pearl, controller 370 sends instruction once more made NPD 300 switch to " normally " operator scheme.Any technician with basic computer software and hardware knowledge can realize said process by simple computer programming, and concrete implementation procedure depends on the concrete model of transfer valve 350 and controller 370, just repeats no more here.
Here, it is emphasized that the NPD detecting device that utilizes the utility model embodiment, the flowing to before entering the NPD detecting device of the sample gas in the gas chromatograph is unaffected; It is to occur in detecting device inside that the flow direction of sample gas changes.Such benefit is, do not need the physical construction of gas chromatograph itself is carried out big change, and the physical construction that only needs to change detecting device itself gets final product.
NPD detecting device according to embodiment of the present utility model goes for various existing gas chromatographs, for example, and 6890GC, 6820GC and 6850GC type gas chromatograph that Agilent company produces.
Utilization can reduce corrosion and the destruction of harmful constituent to pearl according to the NPD detecting device of embodiment of the present utility model, and this just can prolong the serviceable life of pearl greatly; Simultaneously also enlarged the usable range of NPD detecting device, because go for all kinds of solvents, even this solvent has corrosive attack to pearl according to the NPD detecting device of embodiment of the present utility model.
Though illustrated and described specific embodiments of the present utility model here, these instantiations are not intended to limit the utility model.In scope of the present utility model, can carry out many modifications, replacement and variation.For example, according to inventive concept of the present utility model, can design novel flame photometric detector (FPD) (FPD) and electron capture detector (ECD) (ECD)
For example, Fig. 5 shows a kind of novel FPD detecting device 500, and it comprises illuminated chamber 505, be used to the chromatographic column hub cavity 510 holding chromatographic column 506, be communicated with illuminated chamber 505, and air/oxygen is introduced from pipeline 509.In addition, FPD500 also comprise a three-way switch valve 550, with controller 570 and a gas outlet 580 that is communicated with chromatographic column hub cavity 510 of transfer valve 550 electric coupling, wherein the inlet of three-way switch valve 550 is connected with a make-up gas? source, the position of outlet more than chromatographic column 506 ports is connected with chromatographic column hub cavity 510, another outlet position below chromatographic column 506 ports is connected with chromatographic column hub cavity 510, and the position of gas outlet 580 below chromatographic column 506 ports is connected with chromatographic column hub cavity 510.
The transfer valve 550 here, controller 570 and gas outlet 580 are all similar at aspects such as principle, function, operation and technique effects to the counter structure of top embodiment about NPD 300, just repeat no more.
In addition, Fig. 6 shows a kind of new E CD detecting device 600, and it comprises anode 621, negative electrode 622, radioactive source 624,, the chromatographic column hub cavity 610 that be used to hold chromatographic column 606 630 adjacent with the ECD pond.In addition, ECD600 also comprise a three-way switch valve 650, with controller 670 and a gas outlet 680 that is communicated with chromatographic column hub cavity 610 of transfer valve 650 electric coupling, wherein the inlet of three-way switch valve 650 is connected with a make-up gas? source, the position of outlet more than chromatographic column 606 ports is connected with chromatographic column hub cavity 610, another outlet position below chromatographic column 606 ports is connected with chromatographic column hub cavity 610, and the position of gas outlet 680 below chromatographic column 606 ports is connected with chromatographic column hub cavity 610.
The transfer valve 650 here, controller 670 and gas outlet 680 are all similar at aspects such as principle, function, operation and technique effects to the counter structure of top embodiment about NPD 300, just repeat no more.
More than the utility model is described in detail, wherein stated a lot of concrete features, but the utility model is not limited to be implemented with above-mentioned ad hoc fashion in conjunction with specific embodiment.In each specific embodiment, above-mentioned various concrete features also are not limited to described combination.Any falling into all should be considered as falling within the protection domain of the present utility model to the substituting of the utility model specific embodiment, distortion and improvement and equivalent thereof in the scope of the present utility model that claims limit.
Claims (8)
1. a nitrogen phosphorous detector comprises pearl (301), gatherer (302) and the chromatographic column hub cavity (310) that is connected with chromatographic column (306), it is characterized in that also comprising:
A three-way switch valve (350), this transfer valve (350) comprise an inlet (351) and two outlets (356,358); Inlet (351) is connected with a gas source; First outlet (356) position more than chromatographic column (306) port (361) is connected with chromatographic column hub cavity (310); And second outlet (358) position below chromatographic column (306) port (361) is connected with chromatographic column hub cavity (310); And
A gas outlet (380), the position of this gas outlet (380) below chromatographic column (306) port (361) is connected with chromatographic column hub cavity (310).
2. nitrogen phosphorous detector as claimed in claim 1 is characterized in that: described nitrogen phosphorous detector also comprises a controller (370) of blocked operation with transfer valve (350) electric coupling, control transfer valve (350).
3. nitrogen phosphorous detector as claimed in claim 1 is characterized in that: the gas source that is connected with the inlet (351) of transfer valve (350) is the make-up gas? source.
4. nitrogen phosphorous detector as claimed in claim 1 is characterized in that: transfer valve (350) and gas outlet (380) all are integrated in the enclosure interior of described nitrogen phosphorous detector.
5. flame photometric detector (FPD) detecting device, the chromatographic column hub cavity (510) that it comprises illuminated chamber (505) and is used to hold chromatographic column (506), is communicated with illuminated chamber (505) is characterized in that also comprising:
A three-way switch valve (550), this three-way switch valve (550) comprises an inlet and two outlets, inlet is connected with a make-up gas? source, an outlet is connected with chromatographic column hub cavity (510) in the position of chromatographic column (506) more than the port, and another outlet is connected with chromatographic column hub cavity (510) in the position of chromatographic column (506) below the port; And
A gas outlet (580), this gas outlet (580) is connected with chromatographic column hub cavity (510) in the position of chromatographic column (506) below the port.
6. flame photometric detector (FPD) detecting device as claimed in claim 5 also comprises a controller (570) with described three-way switch valve (550) electric coupling, control transfer valve (550) blocked operation.
7. electron capture detector (ECD), it comprises anode (621), negative electrode (622), radioactive source (624) and the chromatographic column hub cavity (610) that is used to hold chromatographic column (606), it is characterized in that also comprising:
A three-way switch valve (650), this three-way switch valve (650) has an inlet and two outlets, inlet is connected with a make-up gas? source, an outlet is connected with chromatographic column hub cavity (610) in the position of chromatographic column (606) more than the port, and another outlet is connected with chromatographic column hub cavity (610) in the position of chromatographic column (606) below the port; And
A gas outlet (680), this gas outlet (680) is connected with chromatographic column hub cavity (610) in the position of chromatographic column (606) below the port.
8. electron capture detector (ECD) as claimed in claim 7 is characterized in that also comprising the controller (670) with transfer valve (650) electric coupling, control transfer valve (650) blocked operation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520106417 CN2826429Y (en) | 2005-08-24 | 2005-08-24 | Novel gas chromatographic detector |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520106417 CN2826429Y (en) | 2005-08-24 | 2005-08-24 | Novel gas chromatographic detector |
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| CN2826429Y true CN2826429Y (en) | 2006-10-11 |
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| CN 200520106417 Expired - Fee Related CN2826429Y (en) | 2005-08-24 | 2005-08-24 | Novel gas chromatographic detector |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324166A (en) * | 2015-07-03 | 2017-01-11 | 中国科学院大连化学物理研究所 | Gas chromatography detector |
| CN110554126A (en) * | 2019-10-21 | 2019-12-10 | 江苏天瑞仪器股份有限公司 | electron capture detector and gas phase device |
-
2005
- 2005-08-24 CN CN 200520106417 patent/CN2826429Y/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106324166A (en) * | 2015-07-03 | 2017-01-11 | 中国科学院大连化学物理研究所 | Gas chromatography detector |
| CN106324166B (en) * | 2015-07-03 | 2017-11-03 | 中国科学院大连化学物理研究所 | A kind of gas chromatography detector |
| CN110554126A (en) * | 2019-10-21 | 2019-12-10 | 江苏天瑞仪器股份有限公司 | electron capture detector and gas phase device |
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| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20061011 |