CN1616945A - Method and device for pretreatment of speeding chemical matter detection - Google Patents
Method and device for pretreatment of speeding chemical matter detection Download PDFInfo
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- CN1616945A CN1616945A CN 200410067890 CN200410067890A CN1616945A CN 1616945 A CN1616945 A CN 1616945A CN 200410067890 CN200410067890 CN 200410067890 CN 200410067890 A CN200410067890 A CN 200410067890A CN 1616945 A CN1616945 A CN 1616945A
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Abstract
The present invention relates to fast chemical matter pre-treating method and device. After the gasifying bottle with held sample is set inside microwave equipment, the magneton inside the gasifying bottle is rotated to stir the sample liquid and the electromagnetic wave the microwave equipment generates actives the molecules of the sample liquid to make the chemical matter in the sample liquid to be analyzed and measured gasify in short time for absorption and/or adsorption with medium under the outer controlled temperature. The present invention can shorten the sample pre-treating time greatly, increase the sampled amount of the chemical matter, lower the detection limit and omit the use of organic solvent.
Description
Technical field:
The present invention is that a kind of speeding chemical matter detects pretreated method and apparatus, especially refer to a kind of sampling pretreatment time significantly can being dwindled, quickening is to the pretreatment time of the chemical substance sampling to be analyzed of half volatile, difficult volatility or low volatility, but and reduction detecting limit.
Background technology:
Known when the organism in the complex sample is analyzed, usually adopt be liquid-liquid extract mutually (Liquid-liquid extraction, LLE) and solid phase extraction (solid phase extraction, technology such as SPE).But these methods are the defective on the various degrees all, as the infringement to human body of: expense height, complicated operation, time-consuming and poisonous organic solvent.
And a kind of solid-phase microextraction method (solid phasemicroextraction that U.S. SUPELCO releases, SPME) defective of technology traditional sample pretreatment technology before having overcome, it need not solvent and complex appts, it can directly gather volatilization and nonvolatile compound from liquid or gaseous sample, can be directly at gas chromatograph (GC), gas chromatography/mass spectrum (GC/MS), combined instrument and liquid chromatography (LC) instrument (HPLC) are gone up and are analyzed, and can with the gas phase and the logotype of liquid chromatography (LC) instrument of any model, have manually and two kinds of auto injections.
In addition, extraction (headspace method in space on a kind of top, HS) in the past for many years in, in the analytical test process, the head space method is used for detecting the volatile matter of food, blood, soil, water, mud, cosmetics, soap, pharmacy and packing material gradually.In some countries,, use static head space method to replace dynamic head space method such as Japan.In recent years, the head space method obtained using more widely in China.
Headspace technique comprises several different sampling techniques.Mainly include dynamic head space or be called purge and trap, solid-phase microextraction, static headspace technique etc.Wherein promoted widely as a kind of The application of new technique with static headspace technique.Static headspace technique (being called for short the headspace sampling technology) is mainly used in measures those volatilizable analytes under 200 degrees centigrade, and the sample that relatively is difficult to carry out pre-treatment.
Use headspace technique and in the analytical test process, possess many advantages.Use headspace sampling to reduce the time that is used for sample pre-treatments very effectively, and save many funds, need not from matrix, to extract analyte to carry out the liquid sample introduction; Usually, the volatility composition in the measuring samples is cleaner than measuring whole liquid sample, and this has just reduced time and expense that sampling system is safeguarded; In addition, in many application, the content of the sample solvent that injects in the head space method lacks than the contained quantity of solvent of liquid sample introduction, and like this, solvent signal peak just diminishes, thereby can reduce the interference of solvent signal peak to interested mensuration component signal peak.
The head space method is widely used in the analysis of volatile matter in the matrixes such as environmental sample soil, mud and water.For example, such class volatile organic matters such as methenyl choloride, phenixin, triclene, zellon, bromoform in the water, because the suction of its composition causes serious harm to the liver of humans and animals, therefore, relevant administrative authority has worked up about strict steering needle such as potable water, source water, sewage effluent, and water quality monitoring department widespread use headspace sampling technology is carried out monitoring analysis work.
But the aforementioned method of carrying, the disappearance that one maximum is all arranged on it uses, that pretreatment time of just taking a sample is still very long, and is used in the sampling of volatile organic contaminant mostly, and can't sample to boiling point higher half volatile or difficult volatile organic contaminant.
Summary of the invention:
Fundamental purpose of the present invention is to solve above-mentioned known disappearance, significantly dwindles at the pretreatment time of how will taking a sample, and this preprocessor can be finished in several minutes, and provides a kind of speeding chemical matter to detect equipment of pretreatment.
This equipment can be taken a sample to the chemical substance to be analyzed of half volatile, difficult volatility or low volatility, and pretreatment time is short.
Adopt this equipment increasing the sampling and measuring amount of this chemical substance to be analyzed, but reduce detecting limit.
Another purpose of the present invention provides a kind of speeding chemical matter to detect pretreated method and does not need with an organic solvent in the sampling pre-service, so do not reduce running cost only, exempt the safety problem with an organic solvent derived, health problem, and discarded solvent processing problem yet.
Speeding chemical matter of the present invention detects the pre-processing device system bottle of will vaporize and is arranged at the inside of this microwave device and connects a control temperature device, and this vaporization bottle inside is equipped with a magneton.Utilize a magneton to drive device and drive the inner magneton rotation of this vaporization bottle, when chemical substance to be determined places this vaporization bottle, can stir this chemical substance to be determined by this magneton of rotation makes it even, utilize the electromagenetic wave radiation of this microwave device to impel the molecule activation of this sample liquid to move fast simultaneously, cause the chemical substance of mensuration to be analyzed in this sample liquid in the very extremely short time, to vaporize to the interior pipe of head space temperature control sampling pipe.Again by the turnover of the water cycle of the blasthole of this head space temperature control sampling pipe and apopore, the temperature of pipe in the may command, also because this temperature controlling, the chemical substance of this vaporization will be cooled to a cloud, and the position system of this adsorbing medium of when operation pipe in head space temperature control sampling pipe changes into liquid cloud according to the chemical substance of mensuration to be analyzed by gaseous state and is decided, and the chemical substance of this mensuration to be analyzed adsorbing medium that can be the absorption of sample device absorbs (attached) by this.
Description of drawings:
Fig. 1 is an equipment synoptic diagram of the present invention.
Fig. 2 is an enforcement sample attitude synoptic diagram of the present invention.
Wherein: 10-microwave device 11-perforation 30-head space temperature control sampling pipe
31-blasthole 32-apopore 33-linkage section (pipe)
34-set collar 40-absorption of sample device 41-adsorbing medium
50-blasthole 51-blasthole 52-apopore
53-cyclic space 60-sample 61-vaporizer
71-magneton 70-magneton drives device
Embodiment:
Relevant detailed technology content of the present invention and preferred embodiment thereof are as follows, but can not limit content of the present invention, and conjunction with figs. is described as follows.
See also shown in Figure 1ly, be equipment synoptic diagram of the present invention.This equipment comprises: a microwave device 10, as the micro-wave oven known to commonly using; One vaporization bottle 20, this vaporization bottle 20 is the inside that is arranged at this microwave device 10, and these vaporization bottle 20 inside are equipped with a magneton 71.One magneton drives device 70, system is arranged at this microwave device 10 inner bottom surface, and be positioned at this vaporization bottle 20 belows, magneton drives magneton 71 rotations that device 70 can drive these vaporization bottle 20 inside by this, rotation by this magneton 71, when chemical substance to be determined during, can stir this chemical substance to be determined and make it even by rotating this magneton 71 in this vaporization bottle 20.
Again, these microwave device 10 inside comprise that still one is selected from one of them made recirculated cooling water cover 50 of organic or inorganic material such as glass, plastics or pottery, this recirculated cooling water cover 50 is to be located at this vaporization bottle 20 and 70 in this magneton drive device, and cover this magneton and drive device 70, slacken microwave power by this, make this magneton drive the radiation effect that device 70 is not subjected to microwave.This recirculated cooling water cover 50 has a blasthole 51 and an apopore 52, has one to be full of the cyclic space 53 of protecting water layer between inwall and outer wall, and according to the characteristic of general microwave, these cyclic space 53 thickness are best must be more than 2 centimeters.
One head space temperature control sampling pipe 30, system comprises the concentric tube type flow type temperature-controlled tube of a blasthole 31 and an apopore 32 external temperature control water cycle machine (not shown), the perforation 11 that the below has a linkage section 33 to see through these microwave device 10 end faces is connected with the mouth of vaporization bottle 20, and there is a set collar 34 top.Wherein, this head space temperature control sampling pipe 30 can utilize same circulation (not shown) to reach the purpose of its water cycle with recirculated cooling water cover 50 certainly.And the temperature control method of this head space temperature control sampling pipe 30 dewaters outside the round-robin mode, still can be mechanical temperature control, electric temperature control, and freezing chip temperature control.
One sample absorption plant 40, this absorption of sample device 40 is to can be a solid-phase microextraction (SPME) device, and one of this absorption of sample device 40 end is provided with an adsorbing medium 41, by aforesaid set collar 34, absorption of sample device 40 can be fixed in this head space temperature control sampling pipe 30 tops, and this adsorbing medium 41 is managed within the cooling of head space temperature control sampling pipe 30 temperature controls, and highly be positioned at 32 of this blasthole 31 and this apopores, in order to absorb (attached) vaporization chemical substance of pipe in the head space temperature control sampling pipe 30 when the operation present device.
Again, these adsorbing medium 41 fibrous roots are selected its material according to molecular weight, volatility and the polarity of institute's analyte.
Now be described as follows with regard to its method of operating, see also shown in " the 2nd figure ", be the present invention's enforcement sample attitude synoptic diagram, for conveniently seeing inside clearly, the door of this microwave device 10 is represented with opening ways among the figure.The present invention's speeding chemical matter detects pretreated method and comprises following phases:
Phase one, at first the matter sample to be tested of liquid or solid state powder is inserted vaporization bottle 20, drink to add moisture content and regulate pH-value and become a sample liquid 60, wherein the pH-value of this sample liquid 60 system according to the chemical substance of mensuration to be analyzed regulate.
Subordinate phase, make magneton 71 be subjected to magneton to drive device 70 starts and stir this sample liquid 60 and make it even, utilize this sample liquid 60 of electromagenetic wave radiation Fast Heating of this microwave device 10 simultaneously, impel the chemical substance of mensuration to be analyzed in this sample liquid 60 to vaporize to the interior pipe of head space temperature control sampling pipe 30.At this moment, can pass in and out by the blasthole 31 of this head space temperature control sampling pipe 30 and the water cycle of apopore 32, the temperature of pipe in the may command, also because this temperature controlling, the chemical substance of this vaporization will be cooled to a cloud 61, and the position system of this adsorbing medium 41 of when operation pipe in head space temperature control sampling pipe 30 in is decided by the cloud 61 that gaseous state changes into liquid state according to the chemical substance of mensuration to be analyzed, and the chemical substance of this mensuration to be analyzed adsorbing medium 41 that can be absorption of sample device 40 absorbs (attached) by this.
Wherein, this microwave irradiation power train is according to the characteristic adjustment of the chemical substance of mensuration to be analyzed.For example: sampling chlorophenol microwave irradiation power 132W under the best research parameter in water sample (soil), these 41 about 5 minutes of sampling times of extraction of adsorbing medium.Under irradiation power 145W, this adsorbing medium 41 extracts about 30 minutes of sampling times for polycyclic aromatic hydrocarbons in the water sample (PAHs).
Phase III, will absorb (attached) and perform an analysis in the mensuration chemical substance injection gas chromatography separation to be analyzed of adsorbing medium 41 and the various detecting device of attaching troops to a unit.
For surfactant, the headspace analysis of the trace impurity in high molecular polymer and the solid sample, the environmental analysis of water sample, aroma analysis in the food, various pollutant analysis in the soil, analyses such as vegetable and fruit remains of pesticide, set on fire or the forensic analysis of explosive sample etc., the present invention has utilized the about 122mm of wavelength of microwave device 10, respective frequencies is the electromagnetic wave of 2450MHz, and its can make in the sample liquid 60 molecule with it together with the characteristic of identical hunting of frequency, make in the sample liquid 60 molecule and intermolecular motion more and more fierce, high-speed rotation, run foul of each other and rub, thereby generation heat, can in the very short time (several minutes), the chemical substance of mensuration to be analyzed be vaporized, the quickening of this vaporescence, also accelerated material to be analyzed to adsorbing medium 41 amount on every side, cause adsorbing medium 41 can adsorb the amount that it is enough measured fast, and easy and simple to handle.
Material to be analyzed for half volatile, difficult volatility or low volatility also will be accelerated the vibration of its molecule because of electromagnetic characteristic, accelerate its volatility, make vaporization in its short time.This also has positive effect to the sampling amount of chemical substance to be analyzed in some sample liquid 60, and is can be because of content of chemical substances to be analyzed not few and be difficult for obtaining the amount of enough detections, but reduces detecting limit greatly.
Simultaneously, the present invention takes a sample in the pre-service, because do not need with an organic solvent, does not so reduce running cost only, also exempts the safety problem of with an organic solvent being derived, health problem, and discarded solvent processing problem.
Above-mentioned is preferred embodiment of the present invention only, is not to be used for limiting scope of the invention process, and promptly all equalizations of being done according to the present patent application claim change and modify, and are all claim of the present invention and contain.
Claims (11)
1, a kind of speeding chemical matter detects equipment of pretreatment, it is characterized in that this equipment comprises:
One microwave device (10);
One vaporization bottle (20), this vaporization bottle (20) are to be arranged at microwave device (10) inside, and this vaporization bottle (20) inside is equipped with a magneton (71);
One can drive the magneton drive device (70) that this magneton (71) rotates, and is to be arranged at microwave device (10) inner bottom surface, and is positioned at this vaporization bottle (20) below,
One head space temperature control sampling pipe (30), system comprises the concentric tube type flow type temperature-controlled tube of a blasthole (31) and an apopore (32), the perforation (11) that the below has a linkage section (33) to see through this microwave device (10) end face is connected with the bottleneck of vaporization bottle (20), and there is a set collar (34) top;
One sample absorption plant (40) is to be fixed in this head space temperature control sampling pipe (30) top by said fixing ring (34), in order to absorb and/or the vaporization chemical substance of absorption in the interior pipe of head space temperature control sampling pipe (30) temperature control cooling.
2. equipment as claimed in claim 1, it is characterized in that this microwave device (10) inside still comprises a recirculated cooling water cover (50), described vaporization bottle (20) is located at by this recirculated cooling water cover (50) and described magneton drives between device (70), and covers this magneton drive device (70).
3. equipment as claimed in claim 2 is characterized in that this recirculated cooling water cover (50) has a blasthole (51) and an apopore (52), has one to be full of the cyclic space (53) of protecting water layer between inwall and outer wall.
4. equipment as claimed in claim 2 is characterized in that this recirculated cooling water cover (50) is that to be selected from the organic or inorganic material of glass, plastics or pottery made.
5. equipment as claimed in claim 1, the temperature control method that it is characterized in that this head space temperature control sampling pipe (30) are mechanical temperature control, electric temperature control or freezing chip temperature control.
6. equipment as claimed in claim 1 is characterized in that this absorption of sample device (40) is a solid-phase micro-extracting device.
7. equipment as claimed in claim 1, an end that it is characterized in that this absorption of sample device (40) is provided with the interior pipe of an adsorbing medium (41) in the cooling of head space temperature control sampling pipe (30) temperature control, and highly is positioned between the blasthole (31) and this apopore (32) of described pre-empty temperature control sampling pipe 30.
8. the application process of a speeding chemical matter detection pre-processing device as claimed in claim is characterized in that the method comprises the following steps:
1) sample is inserted vaporization bottle (20), drinks to add moisture content and regulate pH-value to become a sample liquid (60);
2) make magneton (71) be subjected to magneton to drive device (70) start and stir this sample liquid (60) and make it even, utilize this microwave device (10) this sample liquid of microwave heating (60) simultaneously, impel the chemical substance of mensuration to be analyzed in this sample liquid (60) to vaporize, and in head space temperature control sampling pipe (30), be cooled to a cloud (61) and absorbed and/or adsorb by the adsorbing medium (41) of this absorption of sample device (40) to the interior pipe of head space temperature control sampling pipe (30);
3) the mensuration chemical substance to be analyzed that will absorb or invest adsorbing medium (41) is injected gas chromatography and is separated and performed an analysis by the various detecting device of attaching troops to a unit.
9. method as claimed in claim 8, the pH-value system that it is characterized in that this sample liquid (60) according to the chemical substance of mensuration to be analyzed regulate.
10. method as claimed in claim 8 is characterized in that the characteristic adjustment of this microwave irradiation power train according to the chemical substance of mensuration to be analyzed.
11. method as claimed in claim 8 is characterized in that the position system of this adsorbing medium (41) pipe in head space temperature control sampling pipe (30) is decided by the cloud (61) that gaseous state changes into liquid state according to the chemical substance of mensuration to be analyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100678904A CN1293376C (en) | 2004-11-05 | 2004-11-05 | Method and device for pretreatment of speeding chemical matter detection |
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| CNB2004100678904A CN1293376C (en) | 2004-11-05 | 2004-11-05 | Method and device for pretreatment of speeding chemical matter detection |
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| CN1616945A true CN1616945A (en) | 2005-05-18 |
| CN1293376C CN1293376C (en) | 2007-01-03 |
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| CNB2004100678904A Expired - Fee Related CN1293376C (en) | 2004-11-05 | 2004-11-05 | Method and device for pretreatment of speeding chemical matter detection |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103768828B (en) * | 2014-01-28 | 2015-05-06 | 安徽省农业科学院园艺研究所 | Balancing device for solid phase microextraction of fruit fragrance and extraction method |
| CN105606409A (en) * | 2015-12-28 | 2016-05-25 | 成都科林分析技术有限公司 | Multi-channel headspace extraction needle |
| CN107167335A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of compound with low volatility and detection |
| CN107167334A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of the temperature influence of compound with low volatility and detection |
| CN108389773A (en) * | 2018-03-22 | 2018-08-10 | 北京雪迪龙科技股份有限公司 | A kind of headspace sampling device and headspace sampling analysis system and method |
| CN109073561A (en) * | 2016-01-29 | 2018-12-21 | 梁庆耀 | Detection of Organic Chemicals |
Family Cites Families (4)
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| WO2000039558A1 (en) * | 1998-12-28 | 2000-07-06 | Pawliszyn Janusz B | Process and device for carrying out continuous membrane extraction with a sorbent interface |
| US6267015B1 (en) * | 1999-12-17 | 2001-07-31 | The Goodyear Tire & Rubber Company | Sampling device for condensable gases |
| CN1806165B (en) * | 2003-04-14 | 2011-04-20 | 珀金埃尔默健康科学股份有限公司 | System and method for extracting headspace vapor |
| CN1320355C (en) * | 2003-04-22 | 2007-06-06 | 江南大学 | Method for analyzing fragrancer matter in apple wine |
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- 2004-11-05 CN CNB2004100678904A patent/CN1293376C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103768828B (en) * | 2014-01-28 | 2015-05-06 | 安徽省农业科学院园艺研究所 | Balancing device for solid phase microextraction of fruit fragrance and extraction method |
| CN105606409A (en) * | 2015-12-28 | 2016-05-25 | 成都科林分析技术有限公司 | Multi-channel headspace extraction needle |
| CN105606409B (en) * | 2015-12-28 | 2018-06-05 | 成都科林分析技术有限公司 | Multichannel head space extracts pin |
| CN109073561A (en) * | 2016-01-29 | 2018-12-21 | 梁庆耀 | Detection of Organic Chemicals |
| CN109073561B (en) * | 2016-01-29 | 2022-06-03 | 梁庆耀 | Detection of organic chemicals |
| CN107167335A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of compound with low volatility and detection |
| CN107167334A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of the temperature influence of compound with low volatility and detection |
| CN108389773A (en) * | 2018-03-22 | 2018-08-10 | 北京雪迪龙科技股份有限公司 | A kind of headspace sampling device and headspace sampling analysis system and method |
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| CN1293376C (en) | 2007-01-03 |
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