CN102937634A - Elution device for gas chromatography-mass spectrometry water body trace amount polychlorinated biphenyl analysis sample preparation - Google Patents
Elution device for gas chromatography-mass spectrometry water body trace amount polychlorinated biphenyl analysis sample preparation Download PDFInfo
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- CN102937634A CN102937634A CN2012104388765A CN201210438876A CN102937634A CN 102937634 A CN102937634 A CN 102937634A CN 2012104388765 A CN2012104388765 A CN 2012104388765A CN 201210438876 A CN201210438876 A CN 201210438876A CN 102937634 A CN102937634 A CN 102937634A
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Abstract
The invention relates to an elution device for gas chromatography-mass spectrometry water body trace amount polychlorinated biphenyl analysis sample preparation, belongs to the fields of analytical testing, and aims at solving the problem that an existing related target object elution technology is too old-fashioned. On the basis of a elution device structure for an ordinary needle cylinder and a needle cylinder filter, an adhering buckle with an ultrasonic transducer is further wound on the surface of an outer wall of the needle cylinder, and the structure position of the ultrasonic transducer subjected to the winding force to be positioned is adjacent to the bottom of the needle cylinder. The elution link is reinforced by the following mechanism in application: ultrasonic waves of a high-frequency frequency band is implemented before the needle cylinder filter is connected with a negative pressure source, mass transfer and desorption of the target object are facilitated with strong force, the ultrasonic waves of the high-frequency frequency band still continues radiating during the period when the needle cylinder filter is connected with the negative pressure source to perform suction filtration, and re-adsorption of a target material in the suction filtration process is avoided with strong force. The elution device is convenient to dismantle and combine freely.
Description
Technical field
The present invention relates to a kind of gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls and analyze standby sample washing device, belong to the analytical test field.
Background technology
About the origin of Trace Polychlorinated Biphenyls in the environment water and the general background of analyzing and testing thereof, can be referring to Chinese invention patent application case 201210099400.3.
In many detection methods of Trace Polychlorinated Biphenyls, comparatively speaking, comparatively accurate, reliable with the GC-MS method in for environment water.Described GC-MS analyzes, and refers to gas chromatography-mass spectrometry, the GC-MS character group its refer to and art-recognized meanings itself for the professional in analysis and testing technology field, be known.
As mentioned above, in environment water Trace Polychlorinated Biphenyls analyzing and testing, the GC-MS method is than the tool advantage, and this point is described in detail in above-mentioned Chinese invention patent application case 201210099400.3.
According to the detailed introduction of Chinese invention patent application case 201210099400.3, among the GC-MS analytical test program for Trace Polychlorinated Biphenyls in the water body, comprise important standby sample step, the namely step of adsorptive separation target substance from water body; Employing is adsorbed target substance through the good magnetic composite nano adsorbent of the hydrophilicity of modification from water body, and through magnetic separation, wash-out, evaporate, dry up, the step such as organic solvent constant volume, finish standby sample, be a more high efficiency sampling method.
Elution step wherein is the focus that this case is paid close attention to.
Analyze in the standby sample for water body Trace Polychlorinated Biphenyls GC-MS existing, its elution step, to be placed within the syringe through the magnetic composite nano adsorbent that from water body, has adsorbed target substance that magnetic separates, and the syringe filtrator in micron order aperture is installed at the syringe front end, with the described magnetic composite nano adsorbent of organic solvent drip washing, and in conjunction with the suction filtration means, reach the purpose of wash-out target substance.
In elution step, such as how the least possible wash-out organic solvent, reach one desirable as far as possible near 100% eluting rate, for saving analysis time, and, the reliability, the accuracy that improve analysis result are all significant, and about this point, any one professional who is engaged in the GC-MS analysis is clear.
In the prior art, comprise that GC-MS analyzes the standby sample program of multiple instrumental analysis of standby sample program, the absorb-elute step of its target substance, usually, all be to adopt simple, traditional syringe to add the apparatus structure of filtrator, and realize wash-out in the mode that the simple drip washing of organic solvent adds suction filtration; Because there is special affinity interaction power in the evaluating objects material usually and between the selected adsorbent, this is the basis that selected adsorbent has good trapping ability, yet, also just because the special affinity interaction power that exists between selected adsorbent and the evaluating objects material is difficult to reach a desirable eluting rate so that the simple drip washing of common organic solvents adds the mode of suction filtration; In other words, selected adsorbent its early stage is to the trapping ability of target substance, with the wash-out difficulty of evaluating objects material in the later stage elution step be the desorb difficulty, both are contradiction each other; Generally speaking, be to improve the eluting rate of evaluating objects material, must take sacrifice adsorbent early stage to the trapping ability of evaluating objects material as prerequisite, vice versa; More particularly, the Capture by Sorbents During ability is weak, comparatively speaking, and just easy wash-out, otherwise, if the Capture by Sorbents During ability is strong, just be not easy to reach desirable eluting rate.
As mentioned above, there is special affinity interaction power in the evaluating objects material usually and between the selected adsorbent, as the specialty chemical worker, this be extremely hold intelligible, as an example, can and evaluating objects material polychlorinated biphenyl between form special π-π combination power, and has again special high-ratio surface, and carry out easily that magnetic separates, certainly the magnetic Nano activated charcoal that first-selected is through hydrophilic modifying, this is the first-selected adsorbent that can reach optimum capture rate, but, just because of the magnetic Nano activated charcoal to polychlorinated biphenyl π-π combination power is strong, specific surface is large especially, it is not strong to capture Z-TEK, so, the problem that causes is exactly that its eluting rate lowers greatly, usual wash-out means become fully unreliable at this, to such an extent as to can't consider to use among the actual analysis Test Application described magnetic Nano activated charcoal to be used as trapping agent or to say adsorbent fully.Just because of this, adopt described magnetic Nano activated charcoal through hydrophilic modifying to be used as the standby sample trapping agent of GC-MS and so on instrumental analysis or say adsorbent, in the prior art basic nobody mention, more report without pertinent literature.
Above-mentioned Chinese invention patent application case 201210099400.3, obviously be that the carbon nano-tube of magnetic coupling captures the polychlorinated biphenyl in the water body not as the trapping agent through the magnetic active carbon of hydrophilic modifying with a kind of trapping ability, the scheme of this application case is real to be a kind of power of capture and eluting rate two-phase balance unavoidable newly measures afterwards.
As seen, if rest on the existing elution technique level always, so, the situation that adsorbent selection face receives greatly to limit to will continue.
In brief, in the so specific field of water body Trace Polychlorinated Biphenyls analytical test work, the wash-out means in the existing standby sample program usually can not be satisfactory; Therefore, how improving the object elution technique in the standby sample program of water body Trace Polychlorinated Biphenyls analytical test, is a problem that merits attention.
Summary of the invention
Technical matters to be solved by this invention is, for the unsafty present situation of elution technique in its standby sample program of water body Trace Polychlorinated Biphenyls analytical test work, researches and develops a kind of new washing device of addressing this problem of helping.
The present invention is by the described technical matters of following solution, this scheme provides a kind of gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls to analyze standby sample washing device, the structure of this device comprises syringe, and, syringe filter, a port of this syringe filter and the injection port of this syringe are socketed mutually, emphasis is, the structure of this device also comprises magic tape, described magic tape has another name called the glochild pull stap, this magic tape is flexible ribbon, and, ultrasonic transducer, it is block that its profile of this ultrasonic transducer is, a face of this ultrasonic transducer is fitted and is fixed on the described magic tape, its head and the tail two ends of this magic tape are as the form that presents as two arms around the syringe of filling the span of a man's arms, present around mutual sticking the taking in its head and the tail two ends of the magic tape of the syringe form of filling the span of a man's arms, head and the tail two ends mutually sticking its squeeze force of magic tape of taking cause another relative face of this ultrasonic transducer to be close on the outer wall surface of syringe, this is close to the bottom of the contiguous syringe of its locations of structures of ultrasonic transducer on the syringe outer wall surface, this ultrasonic transducer that is close on the syringe outer wall surface is one and can takes the releasing of state and follow the member that magic tape is removed in the lump along with magic tape head and the tail two ends are mutually sticking, a function of this magic tape is that the ultrasonic transducer that it is entrained is tied and is positioned on the syringe outer wall surface, another function of this magic tape is to give the mobility that this apparatus structure is disassembled convenient and combination free, its radiable ultrasonic frequency scope of this ultrasonic transducer is between 100KHz and 12MHz, and, higher-order of oscillation electric signal transmission cable, an end of this higher-order of oscillation electric signal transmission cable is connected with described ultrasonic transducer.
Described another relative face refers to another face relative with that face of mentioning before, in opposite directions, the phase mapping.
According to the Baidupedia introduction, magic tape is born in Switzerland mid-term in 20th century, a day of the beginning of the forties, and Switzerland inventor George de Mr. Mestral is with dog to stroll in forest, finds when returning that trousers and dog have sticked barbed Siberian cocklebur with it.This phenomenon has caused De Mr.'s Mestral curiosity.After microscopically was further observed, he has found secret wherein: originally the apex structure of each thorn of Siberian cocklebur was a hooklet, and this exactly structure can be hooked on the trousering of hairiness coil structures it easily.This discovery facilitates De Mr. Mestral to invent by hook and two kinds of magic tapes that structure forms of hair.Hook wherein is just as the hooklet on the Siberian cocklebur, and hair is just as the looped pile on the trousering.
More than about the paragraph of magic tape origin, be for itself the art-recognized meanings of this vocabulary of explaining in detail.
Various magic tape all has commercially available.
Described its art-recognized meanings of ultrasonic transducer one word is known for the ultrasound wave professional and technical personnel; Be suitable for the ultrasonic transducer of this case yes that hypomegetic its profile is block ultrasonic transducer, various hypomegetic its profiles are block ultrasonic transducer all to be had commercially availablely, also can customize to ultrasound wave specialized factory.
Can have various ways that described its profile is block ultrasonic transducer and attach and be fixed on the described magic tape, for example, with epoxy resin adhesive carry out gluing, carry out with hot melt adhesive gluing, etc.; Can certainly allow to come so that the attaching of described ultrasonic transducer is fixed on the described magic tape with the auxiliary of rivet and so on.
Described its art-recognized meanings of higher-order of oscillation electric signal transmission cable one word is known for the ultrasound wave professional and technical personnel; Higher-order of oscillation electric signal transmission cable market is on sale, also can customize to ultrasound wave specialized factory.
The ultrasound wave of described frequency range between 100KHz and 12MHz is the ultrasound wave of the weak high-frequency band of ultrasonic cavitation effect, has many different from the ultrasound wave of the strong low-frequency band of ultrasonic cavitation effect; Its difference is known for the professional and technical personnel of art of ultrasound, is not repeated herein.
The structure of this device of this case can comprise higher-order of oscillation electric signal generator certainly, and the other end of described higher-order of oscillation electric signal transmission cable can be connected with this higher-order of oscillation electric signal generator.Various higher-order of oscillation electric signal generator all has commercially available; Also can customize to ultrasound wave specialized factory.
Its radiable ultrasonic frequency of this ultrasonic transducer, further preferred scope is between 300KHz and 12MHz.
This syringe filter, the aperture of the filter bores of its filter membrane can be the arbitrarily selected apertures between from 0.01 micron to several microns, and still, the preferable range in its filter membrane aperture of this syringe filter is between 0.05 micron and 1.00 microns.Described syringe filter with and interior filter membrane market on sale, also can customize to specialized factory.
Described syringe, its pattern is analogous to usual medical syringe; Its material of described syringe can be plastics, glass, metal, pottery, etc.; Its preferred material of this syringe is quartz glass material or stainless steel.
It is various in style for commercially available magic tape, and preferred magic tape is the elastic force magic tape, and this elastic force magic tape also claims stretch sticking cingulum, and this elastic force magic tape is to have flexible magic tape.Various elastic force magic tape or perhaps stretch sticking cingulum market are on sale.
The structure of this device of this case can also comprise some annexes, described annex for example: the fixed mount that is used for fixing described syringe; Described annex is again for example: the filtrate receiver that is used for receiving filtrate that is connected with syringe filter; Described annex is also for example: with the negative pressure source equipment of described filtrate receiver and syringe filter UNICOM, this negative pressure source refers to any equipment that can make vacuum condition, and described negative pressure source specifically refers to the equipment of vacuum pump and so on; Known with regard to itself art-recognized meanings of vacuum pump one word in the vacuum technique field only; Etc..
Advantage of the present invention is, be that syringe adds on the basis of syringe filter with apparatus structure at usual standby sample, the magic tape that further himself is carried block ultrasonic transducer attaches and is installed on the syringe outer wall surface, and make mutually sticking taking of its head and the tail two ends of this magic tape, form the fill the span of a man's arms form of syringe of magic tape, its head and the tail mutually pressure of sticking this magic tape of taking cause the ultrasonic transducer of its entrained bulk to contact with needle cylinder surface and are positioned on the syringe outer wall surface because of frictional resistance, this is close to syringe bottom because of its position location of block ultrasonic transducer that frictional resistance is positioned on the syringe outer wall surface, so, when application this case device carries out the wash-out operation, can first the adsorbent that has captured target substance be moved in the syringe, and in the syringe filling of adsorbent region or spray wash-out organic solvent, simultaneously, open higher-order of oscillation electric signal generator, form of energy conversion via described ultrasonic transducer, and the sound wave that sees through needle cylinder wall transmits, the adsorbent region sustained radiation ultrasonic cavitation effect ultrasound wave of weak high-frequency band in the syringe, and during this period, connect off and on negative pressure source, off and on suction filtration; Among its application of this case device, it is to reach the raising of elution efficiency and the lifting of eluting rate by following mechanism: the ultrasound wave that before connecting negative pressure source, applies high-frequency band, desorb, mass transfer, movement, disengaging, the escape of target substance facilitated in pressure, and during connection negative pressure source suction filtration, the ultrasound wave of high-frequency band still continues acting on simultaneously, and brute force checks the again absorption of target substance in the suction filtration process; Can so repeat to operate several times according to the needs of actual conditions, to reach desirable wash-out target.
Related magic tape in the device, its function are that the ultrasonic transducer that it is entrained is tied and is positioned on the syringe outer wall surface, and its another function is to give the mobility that this apparatus structure is disassembled convenient and combination free; In brief, the dismounting of this case apparatus structure is convenient to both.
The application of this case device can be so that being similar to its such inside of magnetic active carbon has the trapping agent of the huge brute force of the specific surface in large and small duct of flood tide or says adsorbent, and its target substance that captures no longer is difficult to wash-out; Based on the application of this case device, magnetic active carbon cheap and easy to get application in the standby sample program of instrumental analysis just becomes a kind of actual option that allows.
Description of drawings
Fig. 1 is the brief synoptic diagram of this case apparatus structure.
Among the figure, the 1st, syringe, the 2nd, its profile is block ultrasonic transducer, 3,6 is respectively the head and the tail two ends of magic tape, the 4th, magic tape, the 5th, syringe filter, the 7th, higher-order of oscillation electric signal transmission cable, two arrows among the figure are indicated respectively its action movement direction of filling the span of a man's arms of magic tape head and the tail two ends, do not draw described other annex among the figure.
Embodiment
In this case embodiment that Fig. 1 shows, the structure of this device comprises syringe 1, and, syringe filter 5, port of this syringe filter 5 and the injection port of this syringe 1 are socketed mutually, emphasis is, the structure of this device also comprises magic tape 4, described magic tape 4 has another name called the glochild pull stap, this magic tape 4 is flexible ribbons, and, ultrasonic transducer 2, it is block that these ultrasonic transducer 2 its profiles are, a face of this ultrasonic transducer 2 is fitted and is fixed on the described magic tape 4, these magic tape 4 its head and the tail two ends 3,6 as the form that presents as two arms around the syringe 1 of filling the span of a man's arms, present magic tape 4 its head and the tail two ends 3 around syringe 1 form of filling the span of a man's arms, 6 mutual sticking taking, head and the tail two ends 3,6 glue magic tape 4 its squeeze forces of taking mutually causes these ultrasonic transducer 2 another relative faces to be close on the outer wall surface of syringe 1, this is close to the bottom of the contiguous syringe 1 of ultrasonic transducer 2 its locations of structures on syringe 1 outer wall surface, this ultrasonic transducer 2 that is close on syringe 1 outer wall surface be one can be along with magic tape 4 head and the tail two ends 3,6 mutually stickingly take the releasing of state and follow the member that magic tape 4 is removed in the lump, a function of this magic tape 4 is that the ultrasonic transducer 2 that it is entrained is tied and is positioned on syringe 1 outer wall surface, another function of this magic tape 4 is to give the mobility that this apparatus structure is disassembled convenient and combination free, these ultrasonic transducer 2 its radiable ultrasonic frequency scopes are between 100KHz and 12MHz, and, higher-order of oscillation electric signal transmission cable 7, an end of this higher-order of oscillation electric signal transmission cable 7 is connected with described ultrasonic transducer 2.
The frequency values arbitrarily selected of this scope between 100KHz and 12MHz all is the preferred frequency enforcement value that this case allows.
Among implementing, this ultrasonic transducer 2 can attach by the mode of glueing joint and be fixed on the magic tape 4; Can certainly adopt the mode of any other.
The structure of this embodiment can comprise higher-order of oscillation electric signal generator certainly, and the other end of described higher-order of oscillation electric signal transmission cable 7 can be connected with this higher-order of oscillation electric signal generator.Do not draw described higher-order of oscillation electric signal generator in the accompanying drawing.
Among implementing, these ultrasonic transducer 2 its radiable ultrasonic frequencies, further preferred practical range is between 300KHz and 12MHz; The ultrasonic frequency value of selecting arbitrarily between this 300KHz and 12MHz all is the described further preferred frequency values that this case allows enforcement.
Among implementing, this syringe filter 5, the aperture of the filter bores of its filter membrane can be the arbitrarily selected aperture between from 0.01 micron to several microns, and still, the preferred practical range in its filter membrane aperture of this syringe filter is between 0.05 micron and 1.00 microns; The filter membrane aperture value arbitrarily selected of scope between 0.05 micron and 1.00 microns all is the enforcement value in the described aperture of this case permission.Described syringe filter 5 with and interior filter membrane market all on sale, also can customize to relevant speciality producer.
Described syringe 1, its pattern is analogous to usual medical syringe; Described syringe 1 its enforcement material can be plastics, glass, metal, pottery, etc.; This syringe 1 its preferably to implement material be quartz glass material or stainless steel.
The structure of this device of this case can also comprise some annexes, described annex for example: the fixed mount that is used for fixing described syringe 1; Described annex is also for example: the filtrate receiver that is used for receiving filtrate that is connected with syringe filter 5; Described annex is more for example: with the negative pressure source equipment of described filtrate receiver and syringe filter 5 UNICOMs, this negative pressure source refers to any equipment that can make vacuum condition, and described negative pressure source specifically refers to the equipment of vacuum pump and so on; Known with regard to itself art-recognized meanings of vacuum pump one word in the vacuum technique field only; Etc..Do not draw described annex in the accompanying drawing.
Implement related syringe 1, its pattern is not limited to the pattern in the accompanying drawing; Described syringe 1 also can be the structure that its upper end open-mouth does not have the convex edge.
Implement related syringe 1, the pattern of its injection port is not limited to the pattern in the accompanying drawing.
Implement related syringe 1, make a general reference its similar function member.
Implement related syringe filter 5, be not limited to accompanying drawing legend structure, related syringe filter 5 general reference similar function members.
The implementation of this case is not limited to this case accompanying drawing legend.
Claims (6)
1. gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls is analyzed standby sample washing device, the structure of this device comprises syringe, and, syringe filter, a port of this syringe filter and the injection port of this syringe are socketed mutually, it is characterized in that, the structure of this device also comprises magic tape, described magic tape has another name called the glochild pull stap, this magic tape is flexible ribbon, and, ultrasonic transducer, it is block that its profile of this ultrasonic transducer is, a face of this ultrasonic transducer is fitted and is fixed on the described magic tape, its head and the tail two ends of this magic tape are as the form that presents as two arms around the syringe of filling the span of a man's arms, present around mutual sticking the taking in its head and the tail two ends of the magic tape of the syringe form of filling the span of a man's arms, head and the tail two ends mutually sticking its squeeze force of magic tape of taking cause another relative face of this ultrasonic transducer to be close on the outer wall surface of syringe, this is close to the bottom of the contiguous syringe of its locations of structures of ultrasonic transducer on the syringe outer wall surface, this ultrasonic transducer that is close on the syringe outer wall surface is one and can takes the releasing of state and follow the member that magic tape is removed in the lump along with magic tape head and the tail two ends are mutually sticking, a function of this magic tape is that the ultrasonic transducer that it is entrained is tied and is positioned on the syringe outer wall surface, another function of this magic tape is to give the mobility that this apparatus structure is disassembled convenient and combination free, its radiable ultrasonic frequency scope of this ultrasonic transducer is between 100KHz and 12MHz, and, higher-order of oscillation electric signal transmission cable, an end of this higher-order of oscillation electric signal transmission cable is connected with described ultrasonic transducer.
2. gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls according to claim 1 is analyzed standby sample washing device, it is characterized in that, the structure of this device comprises higher-order of oscillation electric signal generator, and the other end of described higher-order of oscillation electric signal transmission cable is connected with this higher-order of oscillation electric signal generator.
3. gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls according to claim 1 is analyzed standby sample washing device, it is characterized in that its radiable ultrasonic frequency scope of this ultrasonic transducer is between 300KHz and 12MHz.
4. root is dug gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls claimed in claim 1 and is analyzed standby sample washing device, it is characterized in that the aperture of this its filter membrane of syringe filter is between 0.05 micron and 1.00 microns.
5. gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls according to claim 1 is analyzed standby sample washing device, it is characterized in that its material of this syringe is quartz glass material or stainless steel.
6. gas chromatography-mass spectrography water body Trace Polychlorinated Biphenyls according to claim 1 is analyzed standby sample washing device, it is characterized in that, described magic tape is the elastic force magic tape, and this elastic force magic tape also claims stretch sticking cingulum, and this elastic force magic tape is to have flexible magic tape.
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| CN101105477A (en) * | 2007-07-24 | 2008-01-16 | 南京大学 | Method for detecting atmosphere granule trace polychlorinated biphenyls by ion trap tandem mass spectrometry |
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Application publication date: 20130220 |