CN204314264U - Organism automatic analyzer - Google Patents
Organism automatic analyzer Download PDFInfo
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- CN204314264U CN204314264U CN201420846514.4U CN201420846514U CN204314264U CN 204314264 U CN204314264 U CN 204314264U CN 201420846514 U CN201420846514 U CN 201420846514U CN 204314264 U CN204314264 U CN 204314264U
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Abstract
The utility model provides a kind of organism automatic analyzer, this organism automatic analyzer, comprise: solid-phase microextraction module, sample introduction discharge opeing module, air feed control module and chromatogram detection module, solid-phase microextraction module respectively and sample introduction stock layout module, have connecting pipeline between air feed control module and chromatogram detection module; Sample introduction discharge opeing module, the Quality control repeated multiple times turnover solid-phase microextraction module when extracting, for solid-phase microextraction module sample introduction and discharge opeing; Air feed control module, provides constant gas as carrier gas when desorption to solid-phase microextraction module; Chromatogram detection module, detects the organism from solid-phase microextraction module.In the analyser that the utility model provides, solid-phase microextraction adsorbent equipment original position can complete adsorption and desorption process, extends the serviceable life of adsorbent equipment.
Description
Technical field
The utility model relates to the gas, liquid, solid object detecting areas containing organic contaminant, especially, relates to a kind of organism automatic analyzer.
Background technology
For the analysis of organic pollutants contained in the materials such as gas, potable water, beverage, the solid phase micro-extraction technique that adopts carries out detection analysis more.Solid-phase microextraction (SPME) is a sample pre-treatments and beneficiation technologies of rising the nineties in 20th century, belongs to non-solvent selective extraction method.Solid phase micro-extraction method is by inserting in sample solution or sample gas by adsorbent equipment, stirred sample promotes that absorption reaches balance simultaneously, after adsorption equilibrium to be achieved, adsorbent equipment is taken out from sample, insert gas chromatography vaporizer, heat the organism of freeing on adsorbent equipment.Extract after desorb, is imported in chromatographic column by mobile phase and is carried out detection analysis in vaporizer, to obtain contained organic composition or content in sample.
After having adsorbed in prior art, often adsorbent equipment need be taken out from sample, carry out the detection of desorption post analysis by mechanical arm by adsorbent equipment transfer insertion chromatogram vaporizer.Due to extraction repeatedly, insert the possibility adding adsorbent equipment and damage, shorten the serviceable life of adsorbent equipment simultaneously.When this kind of equipment is used for 24 hours unmanned automatic analysis, be damaged at nobody once adsorbent equipment, within second day, corresponding data cannot be obtained.
Utility model content
The utility model object be to provide adsorbent equipment can situ extracting, desorption organism automatic analyzer, to solve the technical matters that adsorbent equipment in prior art shortens the serviceable life that frequently movement causes.
For achieving the above object, the utility model provides a kind of organism automatic analyzer, comprise: solid-phase microextraction module, sample introduction discharge opeing module, air feed control module and chromatogram detection module, solid-phase microextraction module respectively and sample introduction stock layout module, have connecting pipeline between air feed control module and chromatogram detection module; Sample introduction discharge opeing module, the Quality control turnover solid-phase microextraction module when extracting, for solid-phase microextraction module sample introduction and discharge opeing; Air feed control module, provides constant gas as carrier gas when desorption to solid-phase microextraction module; Chromatogram detection module, detects the organism from solid-phase microextraction module.
Further, solid-phase microextraction module comprises solid-phase microextraction element and well heater; Solid-phase microextraction element is provided with at least one sample flow mouth, sample flow mouth is connected with sample introduction discharge opeing module, on solid-phase microextraction element and sample flow mouth interval, be provided with at least one blow vent, blow vent is connected with air feed control module and/or chromatogram detection module; The inside of solid-phase microextraction element is provided with cavity, and compartment receives adsorbent equipment, and blow vent is connected with cavity with sample flow mouth; Well heater is used for heating cavities to realize desorption.
Further, adsorbent equipment is be provided with the ventilative of sorbing material layer and/or liquid parts, and sorbing material layer is for be made up of arbitrary in strong polar material, Semi-polarity material or low pole material.
Further, adsorbent equipment is bar-shaped, tubulose, wire or netted.
Further, sample introduction discharge opeing module comprises the valve sets and power pump that can make sample feeding or discharge opeing, and power pump is used for Quality control and repeatedly passes in and out solid-phase microextraction element; Valve sets is arranged on the pipeline that sample flow mouth is connected with sample introduction discharge opeing module.
Further, power pump has quantitative effect.
Further, air feed control module comprises: carrier gas reservoir and/or pressure gas source, is communicated with solid-phase microextraction module, provides its work desired gas to solid-phase microextraction module; Constant pressure and flow element, is arranged on each gas delivery pipeline, for making the gaseous tension that moves in each pipeline and constant flow; Valve sets, for controlling gas flowing.
Further, the pipeline that air feed control module is connected with blow vent is provided with three-way control valve, and the one end open of three-way control valve is connected with blow vent, and another two openings of three-way control valve are connected with air feed control module with chromatogram detection module respectively.
Further, chromatogram detection module comprises: chromatographic column unit, for separating of the organism to be measured in the carrier gas from solid-phase microextraction module; Detecting unit, is connected with chromatographic column and detects organism to be measured; Chromatographic column unit comprises capillary column, and capillary column is directly connected with blow vent.
The utility model has following beneficial effect:
1, in the analyser that provides of the utility model, solid-phase microextraction adsorbent equipment original position can complete adsorption and desorption process, extends the serviceable life of adsorbent equipment;
2, in the analyser that provides of the utility model, solid-phase microextraction module is directly connected with the capillary column in chromatographic column module, eliminate the injection port in conventional chromatogram instrument, shorten the motion length of pipe containing organic carrier gas to be measured left from solid-phase microextraction module, thus the possibility of the Adsorption of Organic eliminated in carrier gas on the parts such as tube wall, valve.Further eliminate the heating arrangement needed for pipeline of transmission carrier gas, and then reach the object simplifying pipeline raising equipment dependability.
Except object described above, feature and advantage, the utility model also has other object, feature and advantage.Below with reference to figure, the utility model is described in further detail.
Accompanying drawing explanation
The accompanying drawing forming a application's part is used to provide further understanding of the present utility model, and schematic description and description of the present utility model, for explaining the utility model, is not formed improper restriction of the present utility model.In the accompanying drawings:
Fig. 1 is the schematic diagram of each model calling of the utility model preferred equipment embodiment;
Fig. 2 is the equipment connection schematic diagram of the utility model preferred equipment embodiment 1;
Fig. 3 is the equipment connection schematic diagram of the utility model preferred equipment embodiment 2;
Fig. 4 is the equipment connection schematic diagram of the utility model preferred equipment embodiment 3;
Fig. 5 is the equipment connection schematic diagram of the utility model preferred equipment embodiment 4; And
Fig. 6 is the utility model method for optimizing embodiment schematic flow sheet; And
Fig. 7 is that the utility model method for optimizing embodiment analyser is for extracting sample gained chromatogram;
Fig. 8 is that the utility model method for optimizing embodiment analyser is for extracting sample 30 gained chromatograms;
Fig. 9 is that the utility model method for optimizing embodiment analyser is for extracting sample 10 gained chromatograms.
Marginal data:
100, solid-phase microextraction module; 110, ram pump; 120, solid-phase microextraction element; 130, adsorbent equipment; 140, the first opening; 150, the second opening; 160, the 3rd opening; 200, air feed control module; 210, nitrogen pot; 220, pressure transducer; 300, operation valve module; 310, the first valve; 320, the second valve; 330, the 3rd valve; 340, the 4th valve; 350, the 5th valve; 360, the 6th valve; 370, peristaltic pump; 400, sample introduction discharge opeing module; 410, sample introduction end; 420, mark end is entered; 430, drain side; 440, feed liquor pipeline; 450, ventilation line; 460, pipeline is detected; 500, chromatogram detection module; 510, capillary column; 600, detecting unit.
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present utility model is described in detail, but the multitude of different ways that the utility model can be defined by the claims and cover is implemented.
See Fig. 1 and 2, the utility model provides a kind of organism automatic analyzer, comprise: solid-phase microextraction module 100, sample introduction discharge opeing module 400, air feed control module 200 and chromatogram detection module 500, solid-phase microextraction module 100 respectively and sample introduction stock layout module, have connecting pipeline between air feed control module 200 and chromatogram detection module 500; Sample introduction discharge opeing module 400, the Quality control repeated multiple times turnover solid-phase microextraction module 100 when extracting, for solid-phase microextraction module 100 sample introduction and discharge opeing; Air feed control module 200, provides constant gas as carrier gas when desorption to solid-phase microextraction module 100; Chromatogram detection module 500, detects the organism from solid-phase microextraction module 100.
Adsorbent equipment (or immerses in sample by making sample repeatedly repeatedly pass in and out in solid-phase microextraction module 100 by the organism automatic analyzer that the utility model provides, still can reach the object of extraction, complete the adsorption process of composition to be detected in sample.Avoid, because solid-phase microextraction module 100 is repeatedly repeatedly moving in sampling process the problem appearance causing instrument to damage, extending service life of equipment.Concrete connected mode between each module can pipeline routinely.At the air-flow of necessity or sample Controlling vertex, valve is set to control the flowing of gas or sample.As sample can by being opened in the feature bottom that is provided with solid-phase microextraction element 120 in solid-phase microextraction module 100 or sidewall offers sample flow mouth, and coordinate pipeline to connect, sample repeatedly completes flowing first-in last-out under the driving of power source in pipeline, realizes absorption.
Preferably, solid-phase microextraction module 100 comprises solid-phase microextraction element 120 and well heater; Solid-phase microextraction element 120 is provided with at least one sample flow mouth, sample flow mouth is connected with sample introduction discharge opeing module 400, on solid-phase microextraction element 120 and sample flow mouth interval, be provided with at least one blow vent, blow vent is connected with air feed control module 200 and/or chromatogram detection module 500; The inside of solid-phase microextraction element 120 is provided with cavity, and compartment receives adsorbent equipment 130, and blow vent is connected with cavity with sample flow mouth; Well heater is used for heating cavities to realize desorption.
The sample flow mouth offered bottom preferred solid-phase microextraction element 120, can ensure that all samples entering this element all can fully contact with adsorbent equipment 130.If when handled sample is gas certainly, in respective line, all gas in solid-phase microextraction element 120 can be extracted out by setting, sample flow mouth can be arranged at the gas position of solid-phase microextraction element 120, as top or sidewall.The bottom surface of more preferably solid-phase microextraction element 120 offers sample flow mouth, now by Action of Gravity Field, the speed that sample leaves solid-phase microextraction element 120 can be improved.
Sample flow in sample flow mouth is connected by pipeline by sample introduction discharge opeing module 400.The flowing of sample is controlled by sample introduction discharge opeing module 400.
On solid-phase microextraction element 120 and sample flow mouth interval, be provided with at least one blow vent, blow vent is connected with air feed control module 200 and/or chromatogram detection module 500.In order to improve gas flow rate, multiple blow vent can be set.Preferably a blow vent is only set.Now blow vent is used for passing into carrier gas in solid-phase microextraction element 120, the organism delivery after desorption to be carried out being separated rear detection to chromatographic column.Optimizing breathing mouth is arranged at the top of solid-phase microextraction element 120, and now the motion of gas in this element is more quick, even under gravity.
Under special circumstances, solid-phase microextraction element 120 also only can offer an opening, now by with the pipeline of this opening in communication on T-valve is set, two other opening of T-valve is connected with sample introduction discharge opeing module 400 with air feed control module 200 respectively.When sample introduction, solid-phase microextraction element 120 is connected with sample introduction discharge opeing module 400.After sample introduction completes, after draining the sample in solid-phase microextraction element 120, by T-valve, this interface is connected with air feed control module 200.Pass into carrier gas, and after opening well heater desorption, carry out subsequent detection.
The cavity of solid-phase microextraction element 120 inside can be glass tube so that with changing.Solid-phase microextraction element 120 can be arranged at other fixed parts for the opening of logical sample and carrier gas, adopt as the easy-formation such as metal, plastics material is made.Reduce difficulty of processing.The structure of solid-phase microextraction element 120 can for be made up of the through hole device being arranged at glass cavity two ends.Preferably, the side wall ring of cavity, around being provided with well heater, is convenient to desorption, to make this analyser inner structure compacter.Certain well heater also can be the well heaters such as the heater strip being arranged at solid-phase microextraction element 120 annex.
Further, adsorbent equipment 130 is for being provided with the ventilative of sorbing material layer and/or liquid parts, and sorbing material layer is for be made up of arbitrary in strong polar material, Semi-polarity material or low pole material.
The structure of adsorbent equipment 130 can be varied, as being the different cartridge type of two ends width, only need ensure that sample can through this adsorbent equipment 130.Preferred adsorbent equipment 130 is bar-shaped, tubulose, wire or netted.The adsorbent equipment 130 of this structure is easy to make, is easy to obtain.
Further, air feed control module 200, provides gas to dry up solid-phase microextraction module 100 after extraction completes; Sample introduction discharge opeing module 400 comprises the valve sets and power pump that can make sample feeding or discharge opeing, and power pump is used for Quality control and repeatedly passes in and out solid-phase microextraction element 120.
Air feed control module 200 can also be used for drying up adsorbent equipment 130, to omit special gas supply device.Air feed control module 200 is connected with the cavity in solid-phase microextraction element 120 by pipeline.Valve sets in sample introduction discharge opeing module 400 is arranged on the pipeline that sample introduction discharge opeing module 400 is connected with solid-phase microextraction module 100.To realize, as when sample introduction, by the control of valve sets, sample flow mouth being closed.Power pump sampling is flowed required power in pipeline.Owing to needing during sample introduction to carry out quantitative Treatment to the amount of institute's sample introduction product, by adopting the power pump with quantitative effect, sample introduction can be realized and quantitatively complete simultaneously, reduce quantity pipeline being arranged components and parts, to reduce the volume of analyser, make it easy to carry.The use of power pump can be carried out according to the using method of conventional pumps, on the pipeline that sample introduction discharge opeing module 400 is connected with solid-phase microextraction element 120 as being arranged on by pump.
Certain sample amounts also can come by arranging graduated cylinder with a scale on the pipeline of sample introduction, so that observe.Or scale is set on the cavity sidewalls, control the accuracy of repeated multiple times sample introduction.
Further, air feed control module 200 comprises: carrier gas reservoir and/or pressure gas source, and being communicated with solid-phase microextraction module 100 provides its work desired gas to solid-phase microextraction module 100; Constant pressure and flow element, is arranged on each gas delivery pipeline, for making the gaseous tension that moves in each pipeline and constant flow; Valve sets, for controlling gas flowing.
Because the solid-phase microextraction element 120 in solid-phase microextraction module 100 in use exists three phases, the first stage is the sample introduction stage, needs to be found time or direct and contact air to cavity by the power pump in sample introduction discharge opeing module 400 before.Subordinate phase is blowdown period, now when the cavity in solid-phase microextraction element 120 is not connected with air, needs to provide emptying power.The gas that now can produce by carrier gas reservoir and/or pressure gas source, discharges the sample immersed in cavity.To reduce the contaminated possibility of cavity.If when handled sample is gas certainly, need to carry out evacuation processes by the power pump in sample introduction discharge opeing module 400.After repeated multiple times, close sample introduction discharge opeing module 400, after thermal desorption is added to solid-phase microextraction module 100, enter the phase III for passing into the carrier gas stage, organism now after desorption is in cavity, the carrier gas produced by carrier gas reservoir and/or pressure gas source passes in cavity, is carried by organism wherein and enters in chromatographic column.In order to ensure the stability of testing result, the pipeline of body of also need ventilating in air feed control module 200 is arranged constant pressure and flow element reduce pressure, flow velocity fluctuation to resultant adverse effect.
Further, the pipeline that air feed control module 200 is connected with blow vent is provided with three-way control valve, the one end open of three-way control valve is connected with blow vent, and another two openings of three-way control valve are connected with air feed control module 200 with chromatogram detection module 500 respectively.
In order to reduce analyser volume further; improve pipeline compactedness; reduce equipment needed thereby; the gas produced in air feed control module 200 is except playing carrier gas; sample is brought into outside the effect of chromatogram detection module 500; also play and continue to ventilate body to the capillary column 510 in chromatogram detection module 500, with the effect of protective hair capillary column 510.Because the unique path of gas is at the blow vent place of solid-phase microextraction element 120, thus now can by being provided with three-way control valve on the pipeline be connected with blow vent.Three-way control valve herein can make gas circuit arbitrarily switch between solid-phase microextraction module 100 and chromatogram detection module 500.
Further, chromatogram detection module 500 comprises: chromatographic column, is directly connected for separating of the organism to be measured in the carrier gas from solid-phase microextraction module 100 with blow vent; Detecting unit 600, is connected with chromatographic column and detects organism to be measured.
Chromatographic column unit, comprises capillary column 510 and temperature control unit, for separating of from solid-phase microextraction module 100 containing organic carrier gas after desorption.After this carrier gas enters capillary column 510, in carrier gas, contained organism is separated, thus obtains result by detecting unit 600 detection.The composition stratographic analysis detection method routinely of this module is arranged.Capillary column is directly connected with the blow vent in solid-phase microextraction element 120, decreases the use of injection port in conventional chromatography evaluation instrument, improves detection accuracy.
Carrier gas is produced by nitrogen pot 210.Gas can be not limited thereto herein, is only required to be the conventional various inert gas that can be used for chromatographic resolution.The pressure transducer 220 be connected with nitrogen pot 210 controls the pressure of the gas produced from nitrogen pot 210.Nitrogen pot 210 is connected with detecting unit 600 with solid-phase microextraction element 120 respectively by pipeline.6th valve 360 is arranged on the pipeline that nitrogen pot 210 is connected with the blow vent (in Fig. 2 the 3rd opening 160) on solid-phase microextraction element 120.Sample flow mouth (in Fig. 2 the first opening 140) on solid-phase microextraction element 120 directly and sample introduction end 410 and drain side 430 pass through pipeline connection, pipeline arranges three-way valve, sample introduction end 410 is connected with sample flow mouth with drain side 430 simultaneously.The pipeline that sample flow mouth and sample introduction end 410 are communicated with drain side 430 is also provided with peristaltic pump 370.By forward conveying and the oppositely conveying of peristaltic pump 370, realize sample and repeatedly pass in and out in solid-phase microextraction element 120, thus realize the abundant absorption of organism on adsorbent equipment 130 in sample.Avoid sample adsorption incomplete.And solid-phase microextraction element 120 is without the need to movement, avoids damage, extends serviceable life.When not using, all right adjustments of gas of the 6th valve 360, making gas when not entering solid-phase microextraction element 120, entering in capillary column 510, leading to carrier gas play a protective role to capillary column 510.
Apparatus embodiments
Power part is any one in ram pump, peristaltic pump or volume pump
Embodiment 1
See Fig. 1 and 2, the organism automatic analyzer that the utility model provides comprises solid-phase microextraction module 100, air feed control module 200, sample introduction discharge opeing module 400, chromatogram detection module 500 and detecting unit 600.Solid-phase microextraction module 100 can be solid-phase micro-extracting device conventional in prior art, can be capillary type or bar-shaped sorbing material.By the conveying of sample introduction discharge opeing module 400, sample enters after in solid-phase microextraction module 100, by sorbing material and sample contacts, tested component in sample is adsorbed in adsorbent equipment 130.Air feed control module 200 comprises carrier gas reservoir and pressure gas storer.Carrier gas reservoir provides carrier gas for being communicated with solid-phase microextraction module 100 to solid-phase microextraction module 100.Pressure gas storer is communicated with solid-phase microextraction module 100 provides power to promote discharge opeing to solid-phase microextraction module 100.Carrier gas reservoir and pressure gas storer are that a feeder is connected with solid-phase microextraction module 100 in the present embodiment, afterwards under different operating conditions, play blanking gas and the effect to liquid pressing by controlling whether to pressurize.
Afterwards by adding thermal desorption, air feed control module 200 air feed control module 200 comprises: carrier gas reservoir and/or pressure gas source, and being communicated with solid-phase microextraction module 100 provides its work desired gas to solid-phase microextraction module 100; Constant pressure and flow element, is arranged on each gas delivery pipeline, for making the gaseous tension that moves in each pipeline and constant flow; Valve sets, for controlling gas flowing.Carrier gas is made to enter in solid-phase microextraction module 100, by the substance use after desorption in chromatogram detection module 500.Only comprise capillary column 510 in chromatogram detection module 500, and eliminate injection port.All need by injection port sample introduction during sample introduction in prior art.The utility model by by solid-phase microextraction module 100 and follow-up chromatogram detection module 500 and detecting unit 600 in one apparatus integrated, the capillary column 510 that must comprise in chromatogram detection module 500 is directly connected with the gas outlet of solid-phase microextraction module 100, eliminate injection port indispensable in conventional chromatography evaluation instrument, and then both eliminated longer connecting line and pipeline heating device, eliminate again mechanical arm or manually note sample.Improve the efficiency of sample introduction, simplify device structure, effectively reduce the volume of robotization Analysis of Organic Substances instrument.The utility model, by after cancellation injection port, finds the problem that originally fears are entertained that, does not occur, and can also improve detection efficiency, sample introduction efficiency, sample introduction accuracy and testing result accuracy.
Sample introduction, solid-phase microextraction, stratographic analysis are detected and be integrated on an equipment simultaneously, only need to adopt a set of software can operate equipment set and run, save cost, improve Software match.Each module all can be installed by this area conventional method and be connected above.
Embodiment 2
See Fig. 3, an embodiment in the organism automatic analyzer that the utility model provides comprise solid-phase microextraction module 100, for generation of and to solid-phase microextraction module 100 delivery of carrier gas air feed control module 200, for control carrier gas in air feed control module 200 operation valve module 300, for the sample introduction discharge opeing module 400 to solid-phase microextraction module 100 sample introduction and discharge opeing; For separating of the chromatogram detection module 500 of the thing to be detected in the carrier gas from solid-phase microextraction module 100; And for detecting the detecting unit 600 being separated the material obtained from the capillary column 510 in chromatogram detection module 500.Solid-phase microextraction module 100 comprises ram pump 110, solid-phase microextraction element 120.Sample introduction discharge opeing module 400 comprises sample introduction end 410, enters to mark end 420 and drain side 430.In order to control the opening and closing of the different mouths of sample introduction and discharge opeing, sample introduction end 410 is connected with the 3rd valve 330.Enter to mark end 420 to be connected with the second valve 320.Drain side 430 is connected with the first valve 310.By two three-way pipes, sample introduction end 410, the injection port that enters to mark end 420 and drain side 430 are merged into a feed liquor pipeline 440 afterwards.So that sample introduction.
All kinds of air feed original papers that air feed control module 200 can be commonly used by this area assemble.See Fig. 2, the air feed control module 200 in an embodiment of the present utility model comprises nitrogen pot 210 and pressure transducer 220.Carrier gas is produced by nitrogen pot 210 and the control of the sensor 220 pairs of nebulizer gas pressures that are under pressure.Carrier gas is delivered to solid-phase microextraction module 100 by the conveying of pipeline by the carrier gas left from air feed control module 200.The pipeline of connection air feed control module 200 and solid-phase microextraction module 100 can pass through operation valve module 300, control.
Ram pump 110 refers to and relies on the to-and-fro movement of plunger in cylinder body, makes the volume of seal operation cavity volume change the device realizing absorbing sample and extruding sample.Ram pump 110 comprises axial plunger pump, single-column ram pump, horizontal plunger pump etc.Ram pump 110 comprises cavity and plunger.Cavity is sheathed on plunger at one end.One end of cavity is blind end, and the middle part of blind end offers osculum.The osculum of ram pump 110 is connected with feed liquor pipeline 440.Osculum can feed liquor (gas) or fluid (gas).Another opposite end of cavity is opening end, when plunger fills up cavity completely, still has part to be exposed to outside the opening end of cavity.When plunger moves along cavity to the blind end of cavity, liquid (gas) body be contained in cavity can be released.When plunger moves along cavity to the opening end of cavity, liquid (gas) body can be sucked in cavity.Osculum is herein relatively large mouth, the mouth that aperture area is little.
Solid-phase microextraction element 120 open top is wherein inserted with adsorbent equipment 130.The openend of solid-phase microextraction element 120 is provided with lid, prevents sample loss.The size of solid-phase microextraction element 120 is less.The disturbance that sample occurs in solid-phase microextraction element 120 is comparatively abundant, and mixing effect is better.The bottom of solid-phase microextraction element 120 is blind end.Solid-phase microextraction element 120 bottom is provided with the first opening 140 be connected with feed liquor pipeline 440.First opening 140 is also connected with the nitrogen pot 210 in air feed control module 200 simultaneously.The pipeline that first opening 140 is connected with nitrogen pot 210 is respectively equipped with flow stabilizing valve and the 4th valve 340.So that carrier gas is passed in solid-phase microextraction element 120 from the first opening 140.The top sidewall of solid-phase microextraction element 120 offers the second opening 150.Second opening 150 and contact air.Close with the connected sum of air to control the second opening 150, the pipeline that the second opening 150 is connected with air arranges the 5th valve 350.Second opening 150 is also connected with the nitrogen pot 210 in air feed control module 200 simultaneously.So that air feed pressurization in solid-phase microextraction element 120.Second opening 150 and the connecting pipeline of nitrogen pot 210 are arranged the 5th valve 350 to control gas and circulate.Top sidewall and second opening 150 opposite side of solid-phase microextraction element 120 offer the 3rd opening 160.3rd opening 160 is directly connected with the capillary column 510 in chromatogram detection module 500, and connecting pipeline is directly connect.Preferred 3rd opening 160 place also can be provided with retaining valve, enters in knitting wool tubing string with liquidproof.
Embodiment 3
See Fig. 4, the difference of another embodiment that the utility model provides and embodiment 2 is also to be provided with ventilation line 450.Ventilation line 450 is communicated with the 3rd opening 160 in nitrogen pot 210 and solid-phase microextraction element 120.Carrier gas continues to purge capillary column 510.Protective hair capillary column 510.Do not arrange into mark end 420 and the respective valve be attached thereto.
Embodiment 4
See Fig. 5, the difference of another embodiment that the utility model provides and embodiment 2 is also to be provided with and detects pipeline 460.Detect pipeline 460 and be communicated with nitrogen pot 210 and detecting unit 600.Do not arrange into mark end 420 and the respective valve be attached thereto.
In the utility model, adsorbent equipment 130 used is made for adopting exotic material (as glass, inert metal, pottery etc.), can analyze the organism of boiling temperature more than 300 DEG C, and lose little; Due to capillary column 510 serviceable life limited (general each element can only use 80 to 200 times), in the utility model, capillary column 510 and the 3rd opening 160 can by glued joint or web member mode is connected.When adopting web member, the replacing of capillary column 510 can be facilitated.
The utility model additionally provides a kind of analytical approach of the said equipment on the other hand.
See Fig. 6, step S1 sample introduction: testing sample is inhaled into ram pump 110 from sample introduction end 410.Undertaken quantitatively by ram pump 110 pairs of sampling volumes.Quantitatively also can measuring by arranging the graduated circulation cup of sidewall band at the osculum of ram pump 110 of sample introduction.Close the 3rd valve 330, second valve 320 and the first valve 310 of feed liquor pipeline 440 end.And open the 5th valve 350 with contact air.
Step S2 extracts: the pull bar repeatedly promoting ram pump 110 makes repeated multiple times the entering in solid-phase microextraction element 120 of testing sample.Be as the criterion with the position making sample be no more than each opening of solid-phase microextraction element 120 top sidewall when pushing sample.Sample is in the process repeatedly passing in and out solid-phase microextraction element 120, turbulization, disturbance make the adsorbent equipment 130 in solid-phase microextraction element 120 and sample that the way of contact of similar stirring occur, thus when not moving adsorbent equipment 130, accelerating organism on adsorbent equipment 130 and reaching adsorption equilibrium.Thus avoid adsorbent equipment 130 appearance of damage that causes of movement repeatedly, extend the serviceable life of adsorbent equipment 130.Adsorbent equipment 130 can be selected according to handled sample, various forms of solid-phase microextraction absorptive element can be selected, as extraction bar, extracting fiber, extracting tube etc. can, according to detecting matter property difference, selected solid-phase microextraction absorptive element can adopt the Stationary liquid sorbing materials such as strong polarity, Semi-polarity, low pole.
Step S3 dries up: open the first valve 310.Close the 5th valve 350.Open nitrogen pot 210 pairs of solid-phase microextraction elements 120 in air feed control module 200 to ventilate, and keep the air-flow of a period of time while the sample in solid-phase microextraction element 120 is discharged, dry up adsorbent equipment 130.
Step S4 desorption: close the first valve 310, thermal desorption is added to P region.In solid-phase microextraction element 120, pass into carrier gas simultaneously.
Step S5 detects: the material on adsorbent equipment 130 is directly brought in the capillary column 510 in chromatogram detection module 500 by carrier gas.The separation of the capillary column 510 in chromatogram detection module 500, in sample, contained material of can surveying enters in detection module 600 to detect and bears results.
Result of use
By the analyser in embodiment 1 for the treatment of water sample: containing 1,2,4-trichloro-benzenes, 1,3,5-trichloro-benzenes, the water sample 50ml of each 20ppb of 1,2,3-trichloro-benzenes.
Extraction conditions: water sample turnover solid-phase microextraction module 50 times.
Chromatographic column: MXT-624 Stainless Steel Capillary chromatographic column (30m*0.53*0.25 μm).
Detector temperature: 250 DEG C.
Resolution temperature: 250 DEG C.
Gained extraction pattern as shown in figs. 7-9.Wherein Fig. 7 is for having extracted 50 gained chromatograms.As seen from Figure 7, adopt this sample of this analyser, can detect containing 1,2,4-trichloro-benzenes in sample, 1,3,5-trichloro-benzenes, 1,2,3-trichloro-benzenes.Testing result is accurate.
Fig. 8 adopts same analysis instrument to carry out 30 times under the same conditions to same sample to extract the chromatogram obtained.Fig. 9 adopts same analysis instrument to carry out 10 times under the same conditions to same sample to extract the chromatogram obtained.Compound contained known in sample all can be detected in the gained chromatogram of Fig. 7 ~ 9, not occur other Interference Peaks simultaneously, illustrate and adopt this detecting instrument, testing result is accurate.
Adopt existing chromatograph to configure the Multifunctional sample injection type Combi-PAL of CTC company of Switzerland, because this equipment is sampled by sampling arm, moving-member is many, and device is complicated, and extraction parts vulnerable to pollution in moving process, affects the test result of sample.
Simultaneously because this equipment is provided with injection port, the carrier gas with sample can not directly enter in capillary column, and thus testing result accuracy also decreases.
The foregoing is only preferred embodiment of the present utility model, be not limited to the utility model, for a person skilled in the art, the utility model can have various modifications and variations.All within spirit of the present utility model and principle, any amendment done, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (9)
1. an organism automatic analyzer, is characterized in that, comprising: solid-phase microextraction module, sample introduction discharge opeing module, air feed control module and chromatogram detection module,
Described solid-phase microextraction module respectively and described sample introduction stock layout module, have connecting pipeline between described air feed control module and described chromatogram detection module;
Described sample introduction discharge opeing module, when extracting, Quality control passes in and out described solid-phase microextraction module, for described solid-phase microextraction module sample introduction and discharge opeing;
Described air feed control module, provides constant gas as carrier gas when desorption to described solid-phase microextraction module;
Described chromatogram detection module, detects the described organism from described solid-phase microextraction module.
2. analyser according to claim 1, is characterized in that, described solid-phase microextraction module comprises solid-phase microextraction element and well heater;
Described solid-phase microextraction element is provided with at least one sample flow mouth, and described sample flow mouth is connected with described sample introduction discharge opeing module,
On described solid-phase microextraction element and described sample flow mouth interval, be provided with at least one blow vent, described blow vent is connected with described air feed control module and/or described chromatogram detection module;
The inside of described solid-phase microextraction element is provided with cavity, described compartment receive adsorbent equipment or cavity inner wall attachment sorbing material, described blow vent is connected with described cavity with described sample flow mouth;
Described well heater heats described sorbing material desorption.
3. analyser according to claim 2, is characterized in that, described adsorbent equipment is be provided with the ventilative of sorbing material layer and/or liquid parts, and described sorbing material layer is for be made up of arbitrary in strong polar material, Semi-polarity material or low pole material.
4. analyser according to claim 3, is characterized in that, described adsorbent equipment is bar-shaped, tubulose, wire or netted.
5. analyser according to claim 2, is characterized in that,
Described sample introduction discharge opeing module comprises the valve sets and power pump that can make described sample feeding or discharge opeing, and described power pump is used for Quality control and repeatedly passes in and out described solid-phase microextraction element;
Described valve sets is arranged on the pipeline that described sample flow mouth is connected with described sample introduction discharge opeing module.
6. analyser according to claim 5, is characterized in that, described sample introduction discharge opeing module can be carried out quantitatively sample size.
7. analyser according to claim 2, is characterized in that, described air feed control module comprises:
Carrier gas reservoir and/or pressure gas source, be communicated with described solid-phase microextraction module, provides its work desired gas to described solid-phase microextraction module;
Constant pressure and flow element, is arranged on each gas delivery pipeline, for controlling the gaseous tension that moves in each pipeline and flow;
Valve sets, for controlling gas flowing.
8. analyser according to claim 7, it is characterized in that, the pipeline that described air feed control module is connected with described blow vent is provided with three-way control valve, the one end open of described three-way control valve is connected with described blow vent, and another two openings of described three-way control valve are connected with described air feed control module with described chromatogram detection module respectively.
9. analyser according to claim 2, is characterized in that, described chromatogram detection module comprises:
Chromatographic column unit, for separating of the organism to be measured in the described carrier gas from described solid-phase microextraction module;
Detecting unit, is connected with described chromatographic column and detects described organism to be measured;
Described chromatographic column unit comprises capillary column, and described capillary column is directly connected with described blow vent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420846514.4U CN204314264U (en) | 2014-12-26 | 2014-12-26 | Organism automatic analyzer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420846514.4U CN204314264U (en) | 2014-12-26 | 2014-12-26 | Organism automatic analyzer |
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| CN204314264U true CN204314264U (en) | 2015-05-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458999A (en) * | 2014-12-26 | 2015-03-25 | 力合科技（湖南）股份有限公司 | Automatic organism analyzer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458999A (en) * | 2014-12-26 | 2015-03-25 | 力合科技（湖南）股份有限公司 | Automatic organism analyzer |
| CN104458999B (en) * | 2014-12-26 | 2016-08-17 | 力合科技（湖南）股份有限公司 | Organic substance automatic analyzer |
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