CN204287133U - For detecting the device of organic compound concentrations in soil - Google Patents
For detecting the device of organic compound concentrations in soil Download PDFInfo
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- CN204287133U CN204287133U CN201420853853.5U CN201420853853U CN204287133U CN 204287133 U CN204287133 U CN 204287133U CN 201420853853 U CN201420853853 U CN 201420853853U CN 204287133 U CN204287133 U CN 204287133U
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Abstract
The utility model relates to a kind of pick-up unit, being specifically related to a kind of device for detecting organic compound concentrations in soil, comprising following five parts: the pressurization of pedotheque High Temperature High Pressure solvent extraction unit, high pure nitrogen and purging unit, sample filtering condensing unit, sample concentration unit, sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit.The utility model pedotheque organic compound extraction rate is fast, and extraction ratio is high; Sample filtering separation efficiency is high, and organic compound loss is few, and filtrate condensing rate is fast, and without the need to human contact's hazardous solvent and organic compound, overall process is airtight, health environment-friendly; The concentrated speed of sample extracting solution is fast, and constant volume is accurate; Can carry out express-analysis test to the organic compound ingredient in pedotheque and concentration, resolution is high, reliable results.
Description
Technical field
The utility model relates to a kind of pick-up unit, is specifically related to a kind of device for detecting organic compound concentrations in soil.
Background technology
Domestic Soil Environmental Pollution situation is day by day severe, for grasping the orgnic compound pollution situation of soil, needs to detect organic compound concentrations in soil.But with regard to present stage, the equipment possessing organic compound function in direct-detection soil is seldom shown in.
Utilize gas chromatography or gas chromatography mass spectrometer to analyze the concentration of organic compound after mostly taking the organic pre-treatment of soil in laboratory, lack the equipment being used for organic compound function in direct-detection soil.Artificial organic pre-treating method of current pedotheque has Puffing and trapping, ultrasonic extraction method and soxhlet extraction.Puffing and trapping will add water in soil and be heated to nitrogen after 50 DEG C to purge organism in water again through the laggard gas chromatographic analysis of cold trap trapping desorb, the organic compound that Puffing and trapping can measure is limited in scope, extraction ratio is low, only can measure the lower volatile organic matter of soil mid-boiling point, the organic compound that boiling point is higher cannot be measured, be difficult to obtain the more comprehensive information of organic compound in pedotheque.Ultrasonic extraction method utilizes Rotary Evaporators to boil off solvent and completes and concentrated finally enter gas chromatography or gas chromatography mass spectrometer analysis after utilizing ultrasonic assistant solvent extraction, ultrasonic extraction method has that organic compounds extraction ratio is low, soil and solvent filter separation efficiency is low, solvent volatilizees seriously easily causes the shortcoming that organic compound loses, rotary evaporation constant volume is inaccurate, human contact's hazardous solvent exists potential hazard.Soxhlet extraction utilizes solvent high-temperature pressure to extract organic compound in soil, extracts needs one time, and speed is slow, organic compound extraction ratio is low.It is large all to there is artificial dependence in above-mentioned three kinds of methods, the shortcoming that speed is slow, extraction ratio is low.
Utility model content
According to above deficiency of the prior art, the technical problems to be solved in the utility model is: provide a kind of device for detecting organic compound concentrations in soil, pedotheque organic compound extraction rate is fast, extraction ratio is high, sample filtering separation efficiency is high, organic compound loses less, filtrate condensing rate is fast, without the need to human contact's hazardous solvent and organic compound, the concentrated speed of sample extracting solution is fast, constant volume is accurate, express-analysis test can be carried out to the organic compound ingredient in pedotheque and concentration, resolution is high, reliable results.
The utility model solves the technical scheme that its technical matters adopts:
Device for detecting organic compound concentrations in soil described in the utility model, comprise extraction apparatus, extraction apparatus outside is coated with aluminum heating jacket, and extraction apparatus top is provided with the 3rd tensimeter and the first needle-valve, extraction apparatus by the first tee ball valve respectively with the first peristaltic pump, second tee ball valve is connected, first peristaltic pump is connected with solvent bottle, first electrically heated rod and the first thermopair are inserted in aluminum heating jacket, aluminum heating jacket is placed on magnetic stirring apparatus, asbestos heat-insulation layer is coated with outside aluminum heating jacket, first sample-transporting tube extend into the inside of extraction apparatus, the first sample-transporting tube, first ball valve, filtrator, second ball valve is connected successively with material condenser, and the top of material condenser is provided with the second needle-valve, and material condenser side is provided with water condensation circulation pipe, and the second sample-transporting tube extend into the inside of material condenser, the second sample-transporting tube, 3rd ball valve, permeable membrane exsiccator, second peristaltic pump, 4th ball valve is connected successively with concentrator, and the second electrically heated rod and the second thermopair are inserted into the inside of concentrator, and the inside of concentrator is provided with nitrogen sparge tube, nitrogen sparge tube, 6th ball valve is connected successively with the first mass-flow gas meter, the first mass-flow gas meter by the second tee ball valve respectively with the first tee ball valve, first tensimeter is connected, the first tensimeter, first reduction valve is connected successively with High Purity Nitrogen gas cylinder, and thickener underflow is provided with liquid level sensor, and concentrator is connected with oil-sealed rotary pump, and the 3rd sample-transporting tube extend into the inside of concentrator, the 3rd sample-transporting tube, 5th ball valve, 3rd peristaltic pump, six-way valve, injection port, gas chromatographic column, Proton-Transfer Reactions ion gun, drift tube massenfilter, electron channel particle detector is connected successively with computer, and six-way valve is provided with quantitative loop, and six-way valve is connected with waste liquid bottle, injection port, second mass-flow gas meter, second tensimeter, second reduction valve is connected successively with high-pure helium gas cylinder, and gas chromatographic column is arranged on column oven inside, Proton-Transfer Reactions ion gun, drift tube massenfilter and electron channel particle detector are arranged on vacuum cavity inside, and vacuum cavity is connected with molecular pump, temperature controller respectively with the first electrically heated rod, first thermopair, second electrically heated rod, second thermopair is connected.
The utility model comprises following five parts: the pressurization of pedotheque High Temperature High Pressure solvent extraction unit, high pure nitrogen and purging unit, sample filtering condensing unit, sample concentration unit, sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit.
Pedotheque passes through successively: extract concentrated in organic compound, sample filtering condensing unit inner filtration wash cooling, sample concentration unit in soil desolventizing in pedotheque High Temperature High Pressure solvent extraction unit, finally enter sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit inner analysis measures organic compound concentrations, high pure nitrogen pressurization with purge unit nitrogen high pressure is provided and as but nitrogen blows concentrated source of the gas.
With the organic compound in solvent extraction soil under pedotheque High Temperature High Pressure solvent extraction unit high-temperature and high-pressure conditions, comprising: temperature controller, the first electrically heated rod, the first thermopair, asbestos heat-insulation layer, magnetic stirring apparatus, extraction apparatus, aluminum heating jacket, the first tee ball valve, the first needle-valve, the 3rd tensimeter, the first peristaltic pump, solvent bottle, the first sample-transporting tube, the first ball valve.
High pure nitrogen pressurization with purge unit and be used for: pressurizeing in pedotheque High Temperature High Pressure solvent extraction unit fills high pure nitrogen and is convenient to rapid extraction organic compound, provides power by improving pressure reduction that nitrogen pressure produces for the sample filtering step in sample filtering condensing unit, for nitrogen purge step in sample concentration unit provides high pure nitrogen, comprising: High Purity Nitrogen gas cylinder, the first reduction valve, the first tensimeter, the second tee ball valve, the first mass-flow gas meter.
Sample filtering condensing unit is used for: cross and filter the remaining soil, the condensing high temperature sample extracting solution that have extracted organic compound, comprising: filtrator, the second ball valve, water condensation circulation pipe, material condenser, the second needle-valve, the 3rd ball valve, the second sample-transporting tube.
Sample concentration unit is used for: the mode concentrating sample extract taking heating, decompression, nitrogen to purge, removes most of solvent, and utilize liquid level sensor to be concentrated into Stationary liquid same volume.Comprise: permeable membrane exsiccator, the second peristaltic pump, the 4th ball valve, the 5th ball valve, the 6th ball valve, the second electrically heated rod, the second thermopair, nitrogen sparge tube, the 3rd sample-transporting tube, concentrator, liquid level sensor, oil-sealed rotary pump.
Sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit are used for: get fixed volume quantitatively concentrated after fluid sample injection gas chromatography Proton-Transfer Reactions flight time mass spectrum detect the concentration analyzing each organic compound.Comprise: the 3rd peristaltic pump, six-way valve, quantitative loop, waste liquid bottle, injection port, the second mass-flow gas meter, high-pure helium gas cylinder, the second reduction valve, the second tensimeter, gas chromatographic column, column oven, Proton-Transfer Reactions ion gun, drift tube massenfilter, electron channel particle detector, vacuum cavity, molecular pump, computer.
1, pedotheque High Temperature High Pressure solvent extraction unit:
The first described electrically heated rod and the first thermopair for heating aluminum heating jacket, and carry out high-temperature heating extraction organic compound wherein by heat transfer to pedotheque in extraction apparatus.
Temperature controller regulates the rate of heat addition of the first electrically heated rod and the second electrically heated rod respectively according to the first thermopair and the second thermocouple measuring temperature, and then accurately controls the temperature of extraction apparatus and concentrator, temperature stabilization.
Asbestos heat-insulation layer is used for being incubated aluminum heating jacket.Be coated with asbestos heat-insulation layer outside aluminum heating jacket, be beneficial to and maintain extraction apparatus temperature constant.
Magnetic stirring apparatus utilizes the liquid-solid mixture material of magneton to the solvent in extraction apparatus and pedotheque composition to carry out magnetic agitation, is beneficial to the extraction of organic compound in pedotheque.
Extraction apparatus is used for: under heating pressurization closed condition, utilize the organic compound in the liquid solvent rapid extraction pedotheque in solvent bottle.Extraction apparatus comprises stainless steel cover, teflon gasket, stainless steel base, and stainless steel cover and stainless steel base by thread and the teflon gasket added between stainless steel cover and stainless steel base realize excellent sealing.
Aluminum heating jacket is used for the high temperature of the first electrically heated rod to pass to extraction apparatus by aluminium heat exchange pattern.Aluminum heating jacket is cylindric, and column type inside groove has been dug for holding extraction apparatus in centre, and aluminum heating jacket adopts making of pure aluminum, and heat-transfer effect is good.Aluminum heating jacket can cushion the first electrically heated rod and directly heats the large problem of the extraction apparatus range of temperature that may cause in addition, is conducive to keeping extraction apparatus temperature constant.
First tee ball valve is used for: with the solvent of the first peristaltic pump in extraction apparatus in filling solvent bottle, utilize nitrogen in High Purity Nitrogen gas cylinder to pressurize to extraction apparatus, and airtight extraction apparatus carries out organic compound extraction in soil.
First needle-valve is used for pressure in sealing or emptying extraction apparatus.
3rd tensimeter is for showing pressure in extraction apparatus.
Solvent bottle extracts the liquid solvent of organic compound in soil for storing.
First sample-transporting tube is used for: after opening the first ball valve, in soil organic compound extract after the transfer of material.
2, high pure nitrogen pressurization and purging unit:
By the switching of the second tee ball valve, realize on the one hand: in the extraction apparatus in pedotheque High Temperature High Pressure solvent extraction unit, pressurization fills high pressure nitrogen, by pressurizeing and then improving solvent and organic compound boiling point, thus improve the heating-up temperature of material, be convenient to rapid extraction organic compound.Realize on the other hand: by regulating the first reduction valve of High Purity Nitrogen gas cylinder to increase the first tensimeter registration, improve nitrogen pressure reduction in extraction apparatus, for the sample filtering step of carrying out in the filtrator in sample filtering condensing unit provides power.The third aspect, for the nitrogen purge step of carrying out in concentrator in sample concentration unit provides high pure nitrogen source of the gas.
3, sample filtering condensing unit:
Filtrator is used for isolated by filtration soil residue and contains organic compound extract.Filtrator is detachable, and shell is stainless steel, and by thread seal, filter interior adopts candle to cross and filters soil residue, and candle without absorption, can not lose the organic compound in extract to the organic compound in extract after filtration.
Material condenser is used for condensation extract.Material condenser is provided with water condensation circulation pipe, by passing into condensation cycle water, high temperature extract is cooled to room temperature.
Second sample-transporting tube is used for cooled extract to be transferred in concentrator by material condenser.
Second needle-valve is used for the pressure on the extract top after being cooled to room temperature in emptying material condenser.
4, sample concentration unit:
Permeable membrane exsiccator is used for the drying of extract, adopts permeable membrane drying to dewater, compares traditional drying agent material filling type exsiccator and have the advantage that rate of drying soon, does not lose water-soluble organic compounds in sample.
Second peristaltic pump is used for the extract in material condenser to be delivered in concentrator through Sample introduction pipe.
4th ball valve and the 5th ball valve are used for airtight concentrator when extract carries out enrichment method.
Second electrically heated rod is connected with temperature controller with the second thermopair, keeps temperature constant for heated concentrator.
Liquid level sensor is for measuring liquid level in concentrator.
Nitrogen sparge tube blows the evaporation of extract accelerated solvent for nitrogen makes extract finally be concentrated into 1ml.Utilize liquid level sensor level sensing, when extract by heat and the mode reduced pressure is concentrated into 3ml time, the second electrically heated rod stops heating, and nitrogen sparge tube starts to pass into high pure nitrogen and purges extract and be concentrated into 1ml.
Extract completes concentrated in concentrator.Concentrator has glass vision panel, and the liquid level of extract is high-visible and by liquid level sensor Measurement accuracy.Thickener underflow is provided with small-bore and indicates the cavity of volume markings line, and cavity is implosion guard material, can by the screw thread at cavity top from concentrator lower end dismounting cavity.1ml concentrate is finally stored in the small-bore cavity of concentrator lower end.
3rd sample-transporting tube is for shifting 1ml concentrated extracting solution in concentrator to six-way valve.
Oil-sealed rotary pump is in decompression state for maintaining concentrator, and accelerated solvent evaporates, and is beneficial to rapid concentration extract.
5, sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit:
3rd peristaltic pump is used for the 1ml concentrate conveying in concentrator to arrive six-way valve.
Quantitative loop is for measuring the concentrate of Stationary liquid same volume to gas chromatography Proton-Transfer Reactions flight time mass spectrum sample introduction.
The internal duct of six-way valve can freely switch, and by switching, is full of concentrate for injection port sample introduction with six-way valve in the quantitative loop be connected, and residue concentrate enters in the waste liquid bottle be connected with six-way valve.Injection port keeps the condition of high temperature, and concentrate sample enters gas chromatographic column temperature programme and is separated after injection port fully gasifies.Gas chromatography column temperature is controlled by column oven and realizes temperature programme.Each organic compound is separated through gas chromatographic column and in chronological sequence flows out the Proton-Transfer Reactions ion gun that chromatographic column enters gas chromatography Proton-Transfer Reactions flight time mass spectrum successively.
Proton-Transfer Reactions ion gun is used for the ionization of organic compound molecule in concentrate.In Proton-Transfer Reactions ion gun, make reaction reagent IONS OF H by cathode glow discharging
3o
+with the molecule generation Proton-Transfer Reactions of gaseous sample to be measured, ionization generates the specific molecular ion of generating strap proton.
Drift tube massenfilter is for separating of the molion with different mass-to-charge ratio.Drift tube massenfilter is a kind of without magnetic dynamic mass analyzer, different according to the speed of ion in field-free Disengagement zone of different mass-to-charge ratio, cause the difference of drift time to realize separation, the quality of ion is less, working time is shorter, more early arrives electron channel particle detector.
Electron channel particle detector gathers the molion of each organic compound for detecting, and arrives computer after molion signal being carried out amplification process.In pedotheque, each organic compound concentrations detection data and corresponding detection spectrogram show at computer.
Proton-Transfer Reactions ion gun, drift tube massenfilter and electron channel particle detector are positioned at vacuum cavity inside, the high vacuum state of vacuum cavity is constantly vacuumized by molecular pump and maintains, high vacuum state effectively can reduce the interference of background, avoids unnecessary ion-molecule reaction occurs.
In computer display pedotheque, each organic compound concentrations detects data and corresponding detection spectrogram, can also control and revise the instrument parameter comprising Proton-Transfer Reactions ion gun, drift tube massenfilter and electron channel particle detector to arrange.
Principle of work and process:
Use the device detecting organic compound concentrations in soil for front, first utilize the mixed standard solution of organic compound to demarcate gas chromatography Proton-Transfer Reactions flight time mass spectrum, establish each organic compound concentrations and the calibration relation between the peak area detecting molecular ion peak corresponding in spectrogram.First open high-pure helium gas cylinder switch, regulate the second reduction valve and the second manometric registration, and by the second mass-flow gas meter for injection port provides the helium as gas chromatographic column carrier gas of firm discharge.Opening molecular pump power supply makes vacuum cavity maintain high vacuum state all the time, then open Proton-Transfer Reactions ion gun, drift tube massenfilter, electron channel particle detector, and the temperature of injection port, the ionogenic temperature of Proton-Transfer Reactions, the instrument parameter such as detection voltage of electron channel particle detector ready are set by computer.The organic compound mixed standard solution of six concentration known prepared is injected successively in the small-bore cavity of concentrator lower end, switch pipeline through the 3rd peristaltic pump pumps and six-way valve, the organic compound mixed standard solution with same volume be full of in quantitative loop is injected injection port.Chromatographic column temperature programme is controlled by column oven, and each organic compound standard material is separated through gas chromatography column and programmed temperature, and flows out gas chromatographic column successively by retention time length.Afterwards successively through Proton-Transfer Reactions ion gun generation Proton-Transfer Reactions thus ionization, drift tube massenfilter is separated according to difference drift time, electron channel particle detector detects and gathers and will obtain chromatogram and the mass spectrogram of the organic compound mixed standard solution of six concentration known after signal transacting amplification at computer, computer is utilized to carry out linear equation recurrence to the sample introduction concentration of each organic compound standard material and the peak area of molecular ion peak, obtain the equation of linear regression being applicable to each organic compound calibration curve, and be stored in computer, ready for measuring organic compound concentrations in pedotheque.
Opening temp. control instrument power supply, with the first electrically heated rod by aluminum heating mantle heats to suitable high-temperature temperature, and utilize temperature controller and the first thermopair accurate temperature controlling and keep temperature constant, the asbestos heat-insulation layer insulation of aluminum heating jacket outside.
Pedotheque after weighing is placed in extraction apparatus, puts into magneton, utilize screw thread and teflon gasket sealing extraction apparatus.Close the first ball valve and the first needle-valve, rotate the first tee ball valve and the first peristaltic pump is communicated with extraction apparatus, then opening the first peristaltic pump will be used for extracting the solvent delivery of the fixed volume of organic compound in pedotheque in extraction apparatus in solvent bottle.
Open High Purity Nitrogen gas cylinder switch, rotating the first reduction valve makes the registration of high pressure pressure shown in the first tensimeter identical with the pressure values that extraction apparatus extracts needed for pedotheque, rotate the second tee ball valve and the first tee ball valve, high pressure nitrogen is filled in extraction apparatus, pressure in 3rd tensimeter display extraction apparatus, complete high pressure nitrogen when the 3rd tensimeter registration no longer increases to fill, then close the second tee ball valve and the first tee ball valve.
Extraction apparatus is placed in aluminum heating jacket, opens magnetic stirring apparatus and utilize magneton to stir, under high-temperature and high-pressure conditions, utilize the organic compound in solvent extraction pedotheque.The extraction that suitable raised temperature is conducive to accelerating organic compound in pedotheque improves extraction ratio simultaneously.Fill high pressure nitrogen by pressurization in extraction apparatus and then improve solvent and organic compound boiling point, thus improve material can heating-up temperature, be also beneficial to rapid extraction organic compound and improve extraction ratio.
After organic compound in pedotheque extracts, close the 3rd ball valve, open the second ball valve and the first ball valve successively.Utilize the high pressure that extraction apparatus carries, after solid-liquid mixture is filtered desilt automatically, liquid extract enters material condenser.Close the first ball valve, extraction apparatus is taken out in aluminum heating jacket and is cooled to room temperature, open after the first needle-valve emptying gas makes extraction apparatus return to normal pressure and then close the first needle-valve.Open the first peristaltic pump and regulate the first tee ball valve, in extraction apparatus, injecting appropriate solvent for cleaning a small amount of solid-liquid mixture remained in extraction apparatus, stopping the first peristaltic pump.Rotating the first reduction valve makes the first tensimeter registration extract pressure values height 0.5MPa needed for pedotheque than extraction apparatus, rotates the second tee ball valve and the first tee ball valve, in extraction apparatus, fills high pressure nitrogen, pressure value in the 3rd tensimeter display extraction apparatus.Open the first ball valve, utilize 0.5MPa pressure reduction by the solvent press-in filtrator in extraction apparatus, the organic compound be mixed with in ceramic core surface attachment soil in washing filter.Cleansing solution enters material condenser through the second ball valve and to mix with extract and merge.
Close the second ball valve, the first tee ball valve and the second tee ball valve successively, the water condensation circulation pipe to material condenser passes into condensation cycle water and high temperature extract is cooled to room temperature.Open in the second needle-valve emptying material condenser the nitrogen on the extract top after being cooled to room temperature, open the 3rd ball valve, the 4th ball valve and the second peristaltic pump successively, extract in material condenser extracts transfer through the second sample-transporting tube pump, the drying of permeable membrane exsiccator dewaters, after the second peristaltic pump pumps conveying, concentrator is entered by Sample introduction pipe, thickener underflow is provided with small-bore cavity, cavity is implosion guard material and indicates volume markings line, can by the screw thread dismounting cavity at cavity top.
In concentrator, purge by heating, decompression, nitrogen the enrichment method that the mode combined realizes extract and become 1ml concentrate.Close the 4th ball valve, the 5th ball valve and the 6th ball valve, open the power supply of the second electrically heated rod, oil-sealed rotary pump and liquid level sensor.Extract in concentrator is heated to boiling with the second electrically heated rod, utilizes temperature controller and the second thermopair accurate temperature controlling and keep extract temperature constant; Utilize oil-sealed rotary pump to maintain concentrator simultaneously and be in decompression state, be beneficial to accelerated solvent evaporation, realize rapid concentration extract.In extract concentration and evaporation process, liquid level sensor detects the liquid level of extract in concentrator in real time, when extract by heat and the mode reduced pressure is concentrated into 3ml time, second electrically heated rod stop heating.Regulate the first reduction valve be connected with High Purity Nitrogen gas cylinder, suitable nitrogen pressure is selected according to the first tensimeter registration, open the 6th ball valve, rotate the second tee ball valve, high pure nitrogen arrives nitrogen sparge tube after accurately controlling nitrogen flow by the first mass-flow gas meter.Nitrogen sparge tube blows the evaporation of extract accelerated solvent for nitrogen to be made extract finally be concentrated into 1ml and is stored in the small-bore cavity of concentrator lower end.
After extract has concentrated, open the 5th ball valve, utilize the 3rd peristaltic pump and the 3rd sample-transporting tube that the 1ml concentrated extracting solution in concentrator is delivered into six-way valve, concentrate is full of in the quantitative loop be connected with six-way valve, switch six-way valve sample introduction, injection port concentrate in quantitative loop being sent into gas chromatograph-mass spectrometer detects organic compound concentrations, and residue concentrate enters the waste liquid bottle be connected with six-way valve.
Injection port keeps the condition of high temperature, and concentrate sample enters gas chromatographic column temperature programme and is separated after injection port fully gasifies.Gas chromatography column temperature is controlled by column oven and realizes temperature programme.Each organic compound is separated through gas chromatographic column and flows out chromatographic column successively by appearance time difference.
Proton-Transfer Reactions ion gun is used for the ionization of organic compound molecule in concentrate.In Proton-Transfer Reactions ion gun, make reaction reagent IONS OF H by cathode glow discharging
3o
+with the molecule generation Proton-Transfer Reactions of gaseous sample to be measured, ionization generates the specific molecular ion of generating strap proton.
Drift tube massenfilter is for separating of the molion with different mass-to-charge ratio.Drift tube massenfilter is a kind of without magnetic dynamic mass analyzer, different according to the speed of ion in field-free Disengagement zone of different mass-to-charge ratio, cause the difference of drift time to realize separation, the quality of ion is less, working time is shorter, more early arrives electron channel particle detector.
Electron channel particle detector gathers the molion of each organic compound for detecting, and arrives computer after molion signal being carried out amplification process.In pedotheque, the detection chromatogram of each organic compound, mass spectrogram and corresponding concentration thereof show at computer.
Proton-Transfer Reactions ion gun, drift tube massenfilter and electron channel particle detector are positioned at vacuum cavity inside, vacuum cavity is connected with molecular pump, the high vacuum state of vacuum cavity is constantly vacuumized by molecular pump and maintains, high vacuum state effectively can reduce the interference of background, avoids unnecessary ion-molecule reaction occurs.
The peak area of the molecular ion peak of the chromatogram of each organic compound, mass spectrogram and correspondence thereof in computer display pedotheque, and according to the equation of linear regression of each organic compound calibration curve, computing machine calculates organic compound concentrations in pedotheque automatically.Utilize computer to control and revise the instrument parameter comprising Proton-Transfer Reactions ion gun, drift tube massenfilter and electron channel particle detector and arrange.
After filtrator has often filtered ten pedotheques, change the candle in filtrator.First close the first ball valve and the 3rd ball valve, then open the second ball valve and the second needle-valve successively, by the pressure in the second needle-valve vent filters and pipeline thereof, the screw thread then turning on filtrator changes candle.
The beneficial effect that the utility model has is:
1. the utility model is furnished with pedotheque High Temperature High Pressure solvent extraction unit, and sample preparation speed is fast, and organic compound extraction ratio is high, and heating rate is fast, temperature stabilization.The mode adopting electrical heating intensification, nitrogen pressurization, solvent extraction to combine realizes the rapid extraction of organic compound in pedotheque at extraction apparatus, sample preparation speed is fast, organic compound extraction ratio is high, the stainless steel cover of extraction apparatus and stainless steel base by thread and teflon gasket sealing, good sealing effect, convenient disassembly, changes pedotheque quick.First electrically heated rod heating rate is fast, and temperature controller temperature control accurate temperature is constant.Adopt the first electrically heated rod Fast Heating aluminum heating jacket simultaneously, and by heat transfer, high-temperature heating extraction organic compound is carried out to pedotheque in extraction apparatus, aluminum heating jacket arranges and can cushion the first electrically heated rod and directly heat the large problem of the extraction apparatus range of temperature that may cause, and is conducive to keeping extraction apparatus temperature constant.
2. the utility model is furnished with sample filtering condensing unit, and isolated by filtration efficiency is high, and organic compound loss is few, and manually do not contact hazardous solvent and organic compound, overall process is airtight, environment protection health, and filtrate condensing rate is fast, time saving and energy saving.The utility model utilizes the airtight filtration desilt of nitrogen pressure reduction to isolate extract and presses the organic compound be mixed with in washing filter soil with solvent bank, isolated by filtration efficiency is high, soil clean result is good, extract is true and reliable representative, and organic compound loss is few, without the need to filtration washing manually, time saving and energy saving, human body does not contact hazardous solvent and organic compound, and overall process is airtight, health environment-friendly.Filtrator and material condenser are by thread seal, quick detachable, easy to use.Material condenser is provided with water condensation circulation pipe, passes into condensation cycle water, and filtrate condensing rate is fast.
3. the utility model is furnished with sample concentration unit, and the concentrated speed of sample extracting solution is fast, and it is accurate that concentrate concentrates constant volume, and saturating membrane dryer rate of drying is fast and dry run does not lose water-soluble organic compounds.Adopt heating, decompression, nitrogen to purge three kinds of mode concentrated extracting solutions be combined with each other, concentrate speed fast, adopt liquid level sensor to detect liquid level in real time, final accurately concentrating is settled to 1ml.When liquid level volume realizes rapid concentration higher than adopting the second electrically heated rod to add thermal oil-sealed rotary pump pressure reducing mode during 3ml, passing into nitrogen purging when liquid level volume is less than 3ml in nitrogen sparge tube and realizing accurately concentrating being settled to 1ml in conjunction with oil-sealed rotary pump decompression.Saturating membrane dryer is compared traditional drying agent material filling type exsiccator and is had the advantage that rate of drying soon, does not lose water-soluble organic compounds in sample.
4. the utility model is furnished with sample feeding and gas chromatography Proton-Transfer Reactions flying time mass spectrum analysis unit, express-analysis test can be carried out to the organic compound ingredient in pedotheque and concentration, resolution is high, reliable results, and it is accurate that quantitative loop arranges sampling volume.Constituent analysis and the measurement of concetration that the mode combined with mass spectrometry quantitative test realizes the organic compound in pedotheque is separated by gas chromatography.Gas chromatography Proton-Transfer Reactions flight time mass spectrum resolution is high, and mass number can be accurate to 2 significant digits, and organic compound qualitative, quantitative result is more reliable.Realize quantitative loop by the switching of six-way valve internal duct measure the concentrate sample through fixed volume and inject injection port, sampling volume is accurate.
Accompanying drawing explanation
Fig. 1 is the utility model structural representation;
In figure: 1, extraction apparatus; 2, aluminum heating jacket; 3, the 3rd tensimeter; 4, the first needle-valve; 5, the first tee ball valve; 6, the first peristaltic pump; 7, solvent bottle; 8, the second tee ball valve; 9, the first electrically heated rod; 10, the first thermopair; 11, magnetic stirring apparatus; 12, asbestos heat-insulation layer; 13, the first sample-transporting tube; 14, the first ball valve; 15, filtrator; 16, the second ball valve; 17, material condenser; 18, the second needle-valve; 19, water condensation circulation pipe; 20, the second sample-transporting tube; 21, the 3rd ball valve; 22, permeable membrane exsiccator; 23, the second peristaltic pump; 24, concentrator; 25, the second electrically heated rod; 26, the second thermopair; 27, nitrogen sparge tube; 28, the first mass-flow gas meter; 29, the first tensimeter; 30, the first reduction valve; 31, High Purity Nitrogen gas cylinder; 32, liquid level sensor; 33, oil-sealed rotary pump; 34, the 3rd sample-transporting tube; 35, the 5th ball valve; 36, the 3rd peristaltic pump; 37, six-way valve; 38, injection port; 39, gas chromatographic column; 40, Proton-Transfer Reactions ion gun; 41, drift tube massenfilter; 42, electron channel particle detector; 43, computer; 44, quantitative loop; 45, waste liquid bottle; 46, the second mass-flow gas meter; 47, the second tensimeter; 48, the second reduction valve; 49, high-pure helium gas cylinder; 50, column oven; 51, vacuum cavity; 52, molecular pump; 53, temperature controller; 54, the 4th ball valve; 55, the 6th ball valve.
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present utility model is described further:
As shown in Figure 1, the utility model comprises extraction apparatus 1, and extraction apparatus 1 outside is coated with aluminum heating jacket 2, and extraction apparatus 1 top is provided with the 3rd tensimeter 3 and the first needle-valve 4, extraction apparatus 1 by the first tee ball valve 5 respectively with the first peristaltic pump 6, second tee ball valve 8 is connected, first peristaltic pump 6 is connected with solvent bottle 7, first electrically heated rod 9 and the first thermopair 10 are inserted in aluminum heating jacket 2, aluminum heating jacket 2 is placed on magnetic stirring apparatus 11, asbestos heat-insulation layer 12 is coated with outside aluminum heating jacket 2, first sample-transporting tube 13 extend into the inside of extraction apparatus 1, the first sample-transporting tube 13, first ball valve 14, filtrator 15, second ball valve 16 is connected successively with material condenser 17, the top of material condenser 17 is provided with the second needle-valve 18, material condenser 17 side is provided with the inside that water condensation circulation pipe 19, second sample-transporting tube 20 extend into material condenser 17, the second sample-transporting tube 20, 3rd ball valve 21, permeable membrane exsiccator 22, second peristaltic pump 23, 4th ball valve 54 is connected successively with concentrator 24, and the second electrically heated rod 25 and the second thermopair 26 are inserted into the inside of concentrator 24, and the inside of concentrator 24 is provided with nitrogen sparge tube 27, nitrogen sparge tube 27, 6th ball valve 55 is connected successively with the first mass-flow gas meter 28, the first mass-flow gas meter 28 by the second tee ball valve 8 respectively with the first tee ball valve 5, first tensimeter 29 is connected, the first tensimeter 29, first reduction valve 30 is connected successively with High Purity Nitrogen gas cylinder 31, and concentrator 24 bottom is provided with liquid level sensor 32, and concentrator 24 is connected with oil-sealed rotary pump 33, and the 3rd sample-transporting tube 34 extend into the inside of concentrator 24, the 3rd sample-transporting tube 34, 5th ball valve 35, 3rd peristaltic pump 36, six-way valve 37, injection port 38, gas chromatographic column 39, Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41, electron channel particle detector 42 is connected successively with computer 43, six-way valve 37 is provided with quantitative loop 44, and six-way valve 37 is connected with waste liquid bottle 45, injection port 38, second mass-flow gas meter 46, second tensimeter 47, second reduction valve 48 is connected successively with high-pure helium gas cylinder 49, and it is inner that gas chromatographic column 39 is arranged on column oven 50, Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41 and electron channel particle detector 42 are arranged on that vacuum cavity 51 is inner, and vacuum cavity 51 is connected with molecular pump 52, temperature controller 53 respectively with the first electrically heated rod 9, first thermopair 10, second electrically heated rod 25, second thermopair 26 is connected.
Use the device detecting organic compound concentrations in soil for front, first utilize the mixed standard solution of organic compound to demarcate gas chromatography Proton-Transfer Reactions flight time mass spectrum, establish each organic compound concentrations and the calibration relation between the peak area detecting molecular ion peak corresponding in spectrogram.First open high-pure helium gas cylinder 49 switch, regulate the registration of the second reduction valve 48 and the second tensimeter 47, and by the second mass-flow gas meter 46 for injection port 38 provides the helium as gas chromatographic column 39 carrier gas of firm discharge.Opening molecular pump 52 power supply makes vacuum cavity 51 maintain high vacuum state all the time, then open Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41, electron channel particle detector 42, and the instrument parameter such as temperature, the temperature of Proton-Transfer Reactions ion gun 40, the detection voltage of electron channel particle detector 42 of injection port 38 is set by computer 43 and ready.The organic compound mixed standard solution of six concentration known prepared is injected successively in the small-bore cavity of concentrator 24 lower end, switch internal duct through the 3rd peristaltic pump 36 extraction and six-way valve 37, the organic compound mixed standard solution with same volume be full of in quantitative loop 44 is injected injection port 38.Chromatographic column temperature programme is controlled by column oven 50, and each organic compound standard material is separated through gas chromatography column and programmed temperature, and flows out gas chromatographic column 39 successively by retention time length.Proton-Transfer Reactions is there is thus ionization successively afterwards through Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41 is separated according to difference drift time, electron channel particle detector 42 detects and gathers and will obtain chromatogram and the mass spectrogram of the organic compound mixed standard solution of six concentration known after signal transacting amplification at computer 43, computer 43 is utilized to carry out linear equation recurrence to the sample introduction concentration of each organic compound standard material and the peak area of molecular ion peak, obtain the equation of linear regression being applicable to each organic compound calibration curve, and be stored in computer 43, ready for measuring organic compound concentrations in pedotheque.
Opening temp. control instrument 53 power supply, is heated to suitable high-temperature temperature with the first electrically heated rod 9 by aluminum heating jacket 2, and utilizes temperature controller 53 and the first thermopair 10 accurate temperature controlling and keep temperature constant, and aluminum heating jacket 2 outside asbestos heat-insulation layer 12 is incubated.
Pedotheque after weighing is placed in extraction apparatus 1, puts into magneton, utilize screw thread and teflon gasket sealing extraction apparatus 1.Close the first ball valve 14 and the first needle-valve 4, rotating the first tee ball valve 5 makes the first peristaltic pump 6 communicate with extraction apparatus 1, and then opening the first peristaltic pump 6 will be used for extracting the solvent delivery of the fixed volume of organic compound in pedotheque in extraction apparatus 1 in solvent bottle 7.
Open High Purity Nitrogen gas cylinder 31 switch, rotating the first reduction valve 30, to make the first pressure 29 show shown high pressure pressure registration identical with the pressure values that extraction apparatus 1 extracts needed for pedotheque, rotate the second tee ball valve 8 and the first tee ball valve 5, high pressure nitrogen is filled in extraction apparatus 1,3rd tensimeter 3 shows pressure in extraction apparatus 1, complete high pressure nitrogen when the 3rd tensimeter 3 registration no longer increases to fill, then close the second tee ball valve 8 and the first tee ball valve 5.
Extraction apparatus 1 is placed in aluminum heating jacket 2, opens magnetic stirring apparatus 11 and utilize magneton to stir, under high-temperature and high-pressure conditions, utilize the organic compound in solvent extraction pedotheque.The extraction that suitable raised temperature is conducive to accelerating organic compound in pedotheque improves extraction ratio simultaneously.Fill high pressure nitrogen by pressurization in extraction apparatus 1 and then improve solvent and organic compound boiling point, thus improve material can heating-up temperature, be also beneficial to rapid extraction organic compound and improve extraction ratio.
After organic compound in pedotheque extracts, close the 3rd ball valve 21, open the second ball valve 16 and the first ball valve 14 successively.Utilize the high pressure that extraction apparatus 1 carries, solid-liquid mixture is automatically after filter 15 filters desilt, and liquid extract enters material condenser 17.Close the first ball valve 14, extraction apparatus 1 is taken out and is cooled to room temperature in aluminum heating jacket 2, opens after the first needle-valve 4 emptying gas makes extraction apparatus 1 return to normal pressure and then close the first needle-valve 4.Open the first peristaltic pump 6 and regulate the first tee ball valve 5, in extraction apparatus 1, injecting appropriate solvent for cleaning a small amount of solid-liquid mixture remained in extraction apparatus, stopping the first peristaltic pump 6.Rotating the first reduction valve 30 makes the first tensimeter 29 registration extract pressure values height 0.5MPa needed for pedotheque than extraction apparatus 1, rotate the second tee ball valve 8 and the first tee ball valve 5, in extraction apparatus 1, fill high pressure nitrogen, the 3rd tensimeter 3 shows pressure value in extraction apparatus 1.Open the first ball valve 14, utilize 0.5MPa pressure reduction by the solvent press-in filtrator 15 in extraction apparatus 1, the organic compound be mixed with in ceramic core surface attachment soil in washing filter 15.Cleansing solution enters material condenser 17 through the second ball valve 16 and to mix with extract and merge.
Close the second ball valve 16, first tee ball valve 5 and the second tee ball valve 8 successively, the water condensation circulation pipe 19 to material condenser 17 bottom passes into condensation cycle water and high temperature extract is cooled to room temperature.Open in the second needle-valve 18 emptying material condenser 17 nitrogen on the extract top after being cooled to room temperature, open the 3rd ball valve 21, the 4th ball valve 54 and the second peristaltic pump 23 successively, after extract in material condenser 17 draws transfer through the second sample-transporting tube 20 successively, permeable membrane exsiccator 22 drying dewaters, the second peristaltic pump 23 extracts conveying, concentrator 24 is entered by Sample introduction pipe, concentrator 24 bottom is provided with small-bore cavity, cavity is implosion guard material and indicates volume markings line, can by the screw thread dismounting cavity at cavity top.
In concentrator 24, purge by heating, decompression, nitrogen the enrichment method that the mode combined realizes extract and become 1ml concentrate.Close the 4th ball valve 54, the 5th ball valve 35 and the 6th ball valve 55, open the power supply of the second electrically heated rod 25, oil-sealed rotary pump 33 and liquid level sensor 32.Extract in concentrator 24 is heated to boiling with the second electrically heated rod 25, utilizes temperature controller 53 and the second thermopair 26 accurate temperature controlling and keep extract temperature constant; Utilize oil-sealed rotary pump 33 to maintain concentrator 24 simultaneously and be in decompression state, be beneficial to accelerated solvent evaporation, realize rapid concentration extract.In extract concentration and evaporation process, liquid level sensor 32 detects in real time the liquid level of extract in concentrator 24, when extract by heat and mode reduce pressure is concentrated into 3ml time, the second electrically heated rod 25 stops heating.Regulate the first reduction valve 30 be connected with High Purity Nitrogen gas cylinder 31, suitable nitrogen pressure is selected according to the first tensimeter 29 registration, open the 6th ball valve 55, rotate the second tee ball valve 8, high pure nitrogen arrives nitrogen sparge tube 27 after accurately controlling nitrogen flow by the first mass-flow gas meter 28.Nitrogen sparge tube 27 blows the evaporation of extract accelerated solvent for nitrogen to be made extract finally be concentrated into 1ml and is stored in the small-bore cavity of concentrator 24 lower end.
After extract has concentrated, open the 5th ball valve 35, utilize the 3rd peristaltic pump 36 and the 3rd sample-transporting tube 34 that the 1ml concentrated extracting solution in concentrator 24 is delivered into six-way valve 37, concentrate is full of in the quantitative loop 44 be connected with six-way valve 37, switch six-way valve 37 sample introduction, the injection port 38 that gas chromatograph-mass spectrometer sent into by concentrate in quantitative loop 44 is detected organic compound concentrations, and residue concentrate enters the waste liquid bottle 45 be connected with six-way valve 37.
Injection port 38 keeps the condition of high temperature, and concentrate sample enters gas chromatographic column temperature programme and is separated after injection port 38 fully gasification.Gas chromatographic column 39 temperature is controlled by column oven 50 and realizes temperature programme.Each organic compound is separated through gas chromatographic column and flows out chromatographic column successively by appearance time difference.
Proton-Transfer Reactions ion gun 40 is for the ionization of organic compound molecule in concentrate.In Proton-Transfer Reactions ion gun 40, make reaction reagent IONS OF H by cathode glow discharging
3o
+with the molecule generation Proton-Transfer Reactions of gaseous sample to be measured, ionization generates the specific molecular ion of generating strap proton.
Drift tube massenfilter 41 is for separating of the molion with different mass-to-charge ratio.Drift tube massenfilter 41 is a kind of without magnetic dynamic mass analyzer, different according to the speed of ion in field-free Disengagement zone of different mass-to-charge ratio, cause the difference of drift time to realize separation, the quality of ion is less, working time is shorter, more early arrives electron channel particle detector 42.
Electron channel particle detector 42 gathers the molion of each organic compound for detecting, and arrives computer 43 after molion signal being carried out amplification process.In pedotheque, the detection chromatogram of each organic compound, mass spectrogram and corresponding concentration thereof show at computer 43.
It is inner that Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41 and electron channel particle detector 42 are positioned at vacuum cavity 51, vacuum cavity 51 is connected with molecular pump 52, the high vacuum state of vacuum cavity 51 is constantly vacuumized by molecular pump 52 and maintains, high vacuum state effectively can reduce the interference of background, avoids unnecessary ion-molecule reaction occurs.
Computer 43 shows the peak area of the molecular ion peak of the chromatogram of each organic compound in pedotheque, mass spectrogram and correspondence thereof, and according to the equation of linear regression of each organic compound calibration curve, computing machine calculates organic compound concentrations in pedotheque automatically.Utilize computer 43 to control and revise the instrument parameter comprising Proton-Transfer Reactions ion gun 40, drift tube massenfilter 41 and electron channel particle detector 42 and arrange.
After filtrator 15 has often filtered ten pedotheques, change the candle in filtrator 15.First close the first ball valve 14 and the 3rd ball valve 21, then open the second ball valve 16 and the second needle-valve 18 successively, by the pressure in the second needle-valve 18 vent filters 15 and pipeline thereof, the screw thread then turning on filtrator 15 changes candle.
Claims (1)
1. one kind for detecting the device of organic compound concentrations in soil, comprise extraction apparatus (1), it is characterized in that extraction apparatus (1) outside is coated with aluminum heating jacket (2), extraction apparatus (1) top is provided with the 3rd tensimeter (3) and the first needle-valve (4), extraction apparatus (1) by the first tee ball valve (5) respectively with the first peristaltic pump (6), second tee ball valve (8) is connected, first peristaltic pump (6) is connected with solvent bottle (7), first electrically heated rod (9) and the first thermopair (10) are inserted in aluminum heating jacket (2), aluminum heating jacket (2) is placed on magnetic stirring apparatus (11), aluminum heating jacket (2) outside is coated with asbestos heat-insulation layer (12), first sample-transporting tube (13) extend into the inside of extraction apparatus (1), first sample-transporting tube (13), first ball valve (14), filtrator (15), second ball valve (16) is connected successively with material condenser (17), the top of material condenser (17) is provided with the second needle-valve (18), material condenser (17) side is provided with water condensation circulation pipe (19), second sample-transporting tube (20) extend into the inside of material condenser (17), second sample-transporting tube (20), 3rd ball valve (21), permeable membrane exsiccator (22), second peristaltic pump (23), 4th ball valve (54) is connected successively with concentrator (24), second electrically heated rod (25) and the second thermopair (26) are inserted into the inside of concentrator (24), the inside of concentrator (24) is provided with nitrogen sparge tube (27), nitrogen sparge tube (27), 6th ball valve (55) is connected successively with the first mass-flow gas meter (28), first mass-flow gas meter (28) by the second tee ball valve (8) respectively with the first tee ball valve (5), first tensimeter (29) is connected, first tensimeter (29), first reduction valve (30) is connected successively with High Purity Nitrogen gas cylinder (31), concentrator (24) bottom is provided with liquid level sensor (32), concentrator (24) is connected with oil-sealed rotary pump (33), 3rd sample-transporting tube (34) extend into the inside of concentrator (24), 3rd sample-transporting tube (34), 5th ball valve (35), 3rd peristaltic pump (36), six-way valve (37), injection port (38), gas chromatographic column (39), Proton-Transfer Reactions ion gun (40), drift tube massenfilter (41), electron channel particle detector (42) is connected successively with computer (43), six-way valve (37) is provided with quantitative loop (44), six-way valve (37) is connected with waste liquid bottle (45), injection port (38), second mass-flow gas meter (46), second tensimeter (47), second reduction valve (48) is connected successively with high-pure helium gas cylinder (49), it is inner that gas chromatographic column (39) is arranged on column oven (50), Proton-Transfer Reactions ion gun (40), it is inner that drift tube massenfilter (41) and electron channel particle detector (42) are arranged on vacuum cavity (51), vacuum cavity (51) is connected with molecular pump (52), temperature controller (53) respectively with the first electrically heated rod (9), first thermopair (10), second electrically heated rod (25), second thermopair (26) is connected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420853853.5U CN204287133U (en) | 2014-12-29 | 2014-12-29 | For detecting the device of organic compound concentrations in soil |
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| CN201420853853.5U CN204287133U (en) | 2014-12-29 | 2014-12-29 | For detecting the device of organic compound concentrations in soil |
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| CN204287133U true CN204287133U (en) | 2015-04-22 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103851A1 (en) * | 2016-12-08 | 2018-06-14 | Büchi Labortechnik AG | Device, particularly extraction devices or evaporation device, and method |
| CN108801721A (en) * | 2017-04-27 | 2018-11-13 | 中国科学院寒区旱区环境与工程研究所 | Stable carbon isotope apparatus for pre-analysis treatment in the carbonate dissolved in a kind of water body |
| CN109738242A (en) * | 2019-01-11 | 2019-05-10 | 成都市环境保护科学研究院 | Volatile organic contaminant acquisition device in soil |
| CN111855373A (en) * | 2020-07-26 | 2020-10-30 | 复旦大学 | Device and method for online measurement of trace polar organic matters in atmospheric concentrated particulate matters |
| CN112630092A (en) * | 2020-12-15 | 2021-04-09 | 阜阳科优检测科技有限公司 | Soil pollution in-situ detection device based on semipermeable membrane |
| CN113532997A (en) * | 2021-07-28 | 2021-10-22 | 东南大学 | Extraction and separation device for isoprenoid quinone in soil |
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2014
- 2014-12-29 CN CN201420853853.5U patent/CN204287133U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018103851A1 (en) * | 2016-12-08 | 2018-06-14 | Büchi Labortechnik AG | Device, particularly extraction devices or evaporation device, and method |
| CN108801721A (en) * | 2017-04-27 | 2018-11-13 | 中国科学院寒区旱区环境与工程研究所 | Stable carbon isotope apparatus for pre-analysis treatment in the carbonate dissolved in a kind of water body |
| CN109738242A (en) * | 2019-01-11 | 2019-05-10 | 成都市环境保护科学研究院 | Volatile organic contaminant acquisition device in soil |
| CN111855373A (en) * | 2020-07-26 | 2020-10-30 | 复旦大学 | Device and method for online measurement of trace polar organic matters in atmospheric concentrated particulate matters |
| CN112630092A (en) * | 2020-12-15 | 2021-04-09 | 阜阳科优检测科技有限公司 | Soil pollution in-situ detection device based on semipermeable membrane |
| CN112630092B (en) * | 2020-12-15 | 2023-12-19 | 阜阳科优检测科技有限公司 | Soil pollution normal position detection device based on semi-permeable membrane |
| CN113532997A (en) * | 2021-07-28 | 2021-10-22 | 东南大学 | Extraction and separation device for isoprenoid quinone in soil |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
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Granted publication date: 20150422 Termination date: 20181229 |