CN102944631A - Device for GC-MS (gas chromatography-mass spectrometer) analysis and sample preparation with physical assistance in PCBs (polychlorinated biphenyls) elution link - Google Patents

Device for GC-MS (gas chromatography-mass spectrometer) analysis and sample preparation with physical assistance in PCBs (polychlorinated biphenyls) elution link Download PDF

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Publication number
CN102944631A
CN102944631A CN2012104388549A CN201210438854A CN102944631A CN 102944631 A CN102944631 A CN 102944631A CN 2012104388549 A CN2012104388549 A CN 2012104388549A CN 201210438854 A CN201210438854 A CN 201210438854A CN 102944631 A CN102944631 A CN 102944631A
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China
Prior art keywords
syringe
ultrasonic transducer
elastic force
endless belt
pcbs
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CN2012104388549A
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Chinese (zh)
Inventor
李榕生
干宁
李天华
曾少林
任元龙
周汉坤
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Ningbo University
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Ningbo University
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Priority to CN2012104388549A priority Critical patent/CN102944631A/en
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Abstract

The invention relates to a device for GC-MS (gas chromatography-mass spectrometer) analysis and sample preparation with physical assistance in a PCBs (polychlorinated biphenyls) elution link and belongs to the field of analysis and test. The target elution technology in the GC-MS detection and sample preparation procedure of the water trace PCBs, i.e. the polychlorinated biphenyls is too old-fashioned, and the scheme aims at the problem. According to the scheme, on the structure basis of a common needle cylinder and a needle cylinder filter, further, the outer wall surface of the needle cylinder is sheathed with an elastic circular band, the inner side surface of the elastic circular band is attached and provided with a microminiature blocky ultrasonic transducer, and the ultrasonic transducer is pressed on the outer wall surface of the needle cylinder through the elastic force. The device realizes the elution link reinforcement in the following application modes: ultrasonic waves in high frequency spectrums are exerted before the needle cylinder is conducted with a negative pressure source, the desorption and the mass transfer of target objects are forcibly promoted, during the suction filtration when the needle cylinder filter is conducted with the negative pressure source, the ultrasonic waves in high frequency spectrums still continue the radiation, and the re-adsorption of the target objects in the suction filtration process is forcibly prevented. The device provided by the scheme is convenient to dismount and mount.

Description

PCBs wash-out link is able to the auxiliary GC-MS of physics and analyzes standby sample device
Technical field
The present invention relates to a kind of PCBs wash-out link and be able to the auxiliary standby sample device of GC-MS analysis of physics, belong to the analytical test field.
Background technology
Character group PCBs refers to polychlorinated biphenyl, and it refers to implication for analyzing the professional this character group, is known.
Be the origin of Trace Polychlorinated Biphenyls and the general background of analyzing and testing thereof about trace PCBs in the environment water, 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 PCBs wash-out link to be able to the auxiliary GC-MS of physics and analyzes standby sample device, this PCBs character group refers to polychlorinated biphenyl, 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 the elastic force endless belt, this elastic force endless belt is to have the ringwise ribbon of flexible its overall profile, and, ultrasonic transducer, it is block that its profile of this ultrasonic transducer is, a face of this ultrasonic transducer attaches and is installed on the inner surface of this elastic force endless belt, this attaching is installed on the inner surface that ultrasonic transducer on the elastic force endless belt inner surface has occupied an elastic force endless belt part, carry elastic force endless belt its profile shape such as ring of ultrasonic transducer, the inner surface of the remainder of this elastic force endless belt holds on the outer wall surface that is fitted in syringe, holding its elasticity strength of elastic force endless belt that is fitted on the syringe outer wall surface causes 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, carry structural relation between elastic force endless belt itself and the syringe of ultrasonic transducer and be and be easy to the independent assortment structural relation that mutually breaks away from, 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 in opposite directions with the face of mentioning before, relative, that set each other off, corresponding.
Described elastic force endless belt, referring to joins end to end is closed into its overall profile ribbon of being made by elastic material in the form of a ring of the one of ring.
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 the ultrasonic transducer of hypomegetic bulk, the ultrasonic transducer of various hypomegetic bulks all has commercially available, also can customize to ultrasound wave specialized factory.
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.
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, further be set with its inboard elastic force endless belt that is equiped with the block ultrasonic transducer of microminiature that attaches in the syringe outer wall surface, rely on the elasticity strength of this elastic force endless belt, this ultrasonic transducer is positioned on the syringe outer wall surface, making the factor of this ultrasonic transducer location is the frictional resistance factor, contiguous syringe bottom, its position location of this ultrasonic transducer, 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 the reinforcement of reaching wash-out by following mechanism: the ultrasound wave that before connecting negative pressure source, applies high-frequency band, desorb, the mass transfer 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.
Ultrasonic transducer in this case apparatus structure is easy to shirk in the lump from syringe together with its elastic force endless belt that depends on; In other words, the structure of this case device is a flexibly structure that dismounting is convenient to both.
The application of this case device can be so that be similar to the trapping agent that its such inside of magnetic active carbon has the huge brute force of the specific surface in large and small duct of flood tide, 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, the elastic force endless belt, the 3rd, syringe filter, the 4th, higher-order of oscillation electric signal transmission cable, the 5th, ultrasonic transducer is not drawn 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 3, port of this syringe filter 3 and the injection port of this syringe 1 are socketed mutually, emphasis is, the structure of this device also comprises elastic force endless belt 2, this elastic force endless belt 2 is to have the ringwise ribbon of flexible its overall profile, and, ultrasonic transducer 5, it is block that these ultrasonic transducer 5 its profiles are, a face of this ultrasonic transducer 5 attaches and is installed on the inner surface of this elastic force endless belt 2, this attaching is installed on the inner surface that ultrasonic transducer 5 on elastic force endless belt 2 inner surfaces has occupied elastic force endless belt 2 parts, carry elastic force endless belt 2 its profile shape such as rings of ultrasonic transducer 5, the inner surface of the remainder of this elastic force endless belt 2 holds on the outer wall surface that is fitted in syringe 1, holding elastic force endless belt 2 its elasticity strength that are fitted on syringe 1 outer wall surface causes these ultrasonic transducer 5 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 5 its locations of structures on syringe 1 outer wall surface, carry structural relation between elastic force endless belt 2 itself and the syringe 1 of ultrasonic transducer 5 and be and be easy to the independent assortment structural relation that mutually breaks away from, these ultrasonic transducer 5 its radiable ultrasonic frequency scopes are between 100kHz and 12MHz, and, higher-order of oscillation electric signal transmission cable 4, an end of this higher-order of oscillation electric signal transmission cable 4 is connected with described ultrasonic transducer 5.
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 5 can attach on the inner surface that is fixed on the elastic force endless belt by any mode; For example, this ultrasonic transducer 5 can carry out the gluing fixedly purpose of described attaching of reaching with epoxy resin adhesive, also can use fixedly purpose of the described attaching of the gluing realization of hot melt adhesive; Etc.; Certainly, reach described attaching with the auxiliary of rivet and so on and fix, also allow.
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 4 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 5 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 3, 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 3 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 3; Described annex is more for example: with the negative pressure source equipment of described filtrate receiver and syringe filter 3 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 3, be not limited to accompanying drawing legend structure, related syringe filter 3 general reference similar function members.
The ultrasonic transducer 5 that is suitable for this case is that hypomegetic its profile is block ultrasonic transducer, the described bulk that is, refer to the fritter form that its profile presents several faces, this wherein also comprises the ultrasonic transducer of ring-type, the ultrasonic transducer of column certainly, etc.
The implementation of this case is not limited to this case accompanying drawing legend.

Claims (5)

1.PCBs the wash-out link is able to the auxiliary GC-MS of physics and analyzes standby sample device, this PCBs character group refers to polychlorinated biphenyl, 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 the elastic force endless belt, this elastic force endless belt is to have the ringwise ribbon of flexible its overall profile, and, ultrasonic transducer, it is block that its profile of this ultrasonic transducer is, a face of this ultrasonic transducer attaches and is installed on the inner surface of this elastic force endless belt, this attaching is installed on the inner surface that ultrasonic transducer on the elastic force endless belt inner surface has occupied an elastic force endless belt part, carry elastic force endless belt its profile shape such as ring of ultrasonic transducer, the inner surface of the remainder of this elastic force endless belt holds on the outer wall surface that is fitted in syringe, holding its elasticity strength of elastic force endless belt that is fitted on the syringe outer wall surface causes 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, carry structural relation between elastic force endless belt itself and the syringe of ultrasonic transducer and be and be easy to the independent assortment structural relation that mutually breaks away from, 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. PCBs wash-out link according to claim 1 is able to the auxiliary GC-MS of physics and analyzes standby sample 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. PCBs wash-out link according to claim 1 is able to the auxiliary GC-MS of physics and analyzes standby sample device, it is characterized in that its radiable ultrasonic frequency scope of this ultrasonic transducer is between 300kHz and 12MHz.
4. PCBs wash-out link according to claim 1 is able to the auxiliary GC-MS of physics and analyzes standby sample 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. PCBs wash-out link according to claim 1 is able to the auxiliary GC-MS of physics and analyzes standby sample device, it is characterized in that its material of this syringe is quartz glass material or stainless steel.
CN2012104388549A 2012-10-25 2012-10-25 Device for GC-MS (gas chromatography-mass spectrometer) analysis and sample preparation with physical assistance in PCBs (polychlorinated biphenyls) elution link Pending CN102944631A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101871920A (en) * 2010-06-13 2010-10-27 中国环境科学研究院 Multistage improvement column for quickly pre-processing and purifying polychlorinated biphenyl in biological sample
CN102279231A (en) * 2011-06-28 2011-12-14 中国科学院生态环境研究中心 Quick qualitative detection method for polychlorinated biphenyl pollutants
CN102507808A (en) * 2011-11-10 2012-06-20 宁波大学 Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)
CN102650599A (en) * 2012-03-08 2012-08-29 宁波大学 Self-cleaning glass carbon electrode with resistance against adsorption pollution and for electrogenerated chemiluminescence
CN102650600A (en) * 2012-03-08 2012-08-29 宁波大学 Electric and acoustic dual-excited bundled composite glass carbon electrode
CN102680459A (en) * 2012-04-23 2012-09-19 宁波大学 Function-extended electrochemiluminescence analysis and test device
CN102680591A (en) * 2012-03-26 2012-09-19 宁波大学 Method for quickly detecting trace polychlorinated biphenyls (PCBs) based on carbon nano tube modification technology

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101871920A (en) * 2010-06-13 2010-10-27 中国环境科学研究院 Multistage improvement column for quickly pre-processing and purifying polychlorinated biphenyl in biological sample
CN102279231A (en) * 2011-06-28 2011-12-14 中国科学院生态环境研究中心 Quick qualitative detection method for polychlorinated biphenyl pollutants
CN102507808A (en) * 2011-11-10 2012-06-20 宁波大学 Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)
CN102650599A (en) * 2012-03-08 2012-08-29 宁波大学 Self-cleaning glass carbon electrode with resistance against adsorption pollution and for electrogenerated chemiluminescence
CN102650600A (en) * 2012-03-08 2012-08-29 宁波大学 Electric and acoustic dual-excited bundled composite glass carbon electrode
CN102680591A (en) * 2012-03-26 2012-09-19 宁波大学 Method for quickly detecting trace polychlorinated biphenyls (PCBs) based on carbon nano tube modification technology
CN102680459A (en) * 2012-04-23 2012-09-19 宁波大学 Function-extended electrochemiluminescence analysis and test device

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Application publication date: 20130227