CN104062170A - Automatic online micro-scale sample dilution and mixing system and mixing method - Google Patents
Automatic online micro-scale sample dilution and mixing system and mixing method Download PDFInfo
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Abstract
The invention provides an automatic online micro-scale sample dilution and mixing system and a mixing method. The device includes a syringe pump, a first multi-position switching valve, a second multi-position switching valve, a third multi-position switching valve, a mixer, a six-way valve, a quantitative tube and a sample introduction pump. The first multi-position switching valve comprises a first main port and two first switch ports; the second multi-position switching valve comprises a second main port and two second switch ports; the third multi-position switching valve comprises a third main port and two third switch ports; the mixer is provided with a liquid inlet and outlet port; the quantitative tube and sample introduction pump are connected to the six-way valve; the syringe pump is connected with the first main port; one first switch port is connected with the second main port, and the other first switch port is connected with the six-way valve; one second switch port is connected with one third switch port; and the third main port is connected with the liquid inlet and outlet port. The invention improves versatility of the automatic on-line micro-scale sample dilution mixing system, and meets the requirements of automatic on-line sample dilution and mixing.
Description
Technical field
The present invention relates to chromatographic analysis device, relate in particular to a kind of automatic on-line micro-example dilution commingled system and mixed method.
Background technology
Chromatograph application chromatography is carried out qualitative and quantitative analysis to material, and studies the physics of material, the instrument of chemical characteristic.Chromatograph in use, generally need to first inject quantitative sample, and then injects dilution according to extension rate sample is diluted.Generally, after sample mixes with dilution, need to mix processing, in prior art, conventionally adopt following two kinds of modes: mode one, in the mode stirring, sample and dilution be mixed; The mode of mode two, employing bubbling mixes sample and dilution.Above-mentioned two kinds of modes all can mix fully to heavy dose of sample and dilution, but, dilution for automatic on-line micro-example mixes, the concentration of component is in ppb ~ ppm level, its sample size is only between 10 ~ 200 μ L, for example, due to seldom (: 300 times of the Sample Dilutions of 10 μ L) of the dosage of collected specimens, self volume of its corresponding mixer is just very little.For mode one, due to the small volume of mixer, have no idea to stir in mixer at all; And for mode two, the restriction bubbling effect that is subject on the one hand mixer space is poor, on the other hand, the contained pollutant of air that bubbling uses will affect the measuring accuracy of sample.As from the foregoing, mixer of the prior art cannot meet the dilution mixing requirement of automatic on-line sample.
Summary of the invention
Technical matters to be solved by this invention is: a kind of automatic on-line micro-example dilution commingled system and mixed method are provided, in solution prior art, mixer cannot meet the defect of the dilution mixing requirement of automatic on-line sample, realize the dilution mixing requirement that automatic on-line micro-example dilution commingled system meets automatic on-line sample, improve mixing uniformity.
Technical scheme provided by the invention is that a kind of automatic on-line micro-example dilution commingled system, comprises syringe pump, the first multi-position switching valve, the second multi-position switching valve, mixer, six-way valve, quantity tube and sampling pump; Described the first multi-position switching valve comprises that the first master port and two select with described the first master port the first port switching being communicated with, described the second multi-position switching valve comprises that the second master port and three select with described the second master port the second port switching being communicated with, and described mixer has a liquid inlet/outlet; The two-port of described quantity tube and the import of described sampling pump are connected on described six-way valve, described syringe pump is connected with described the first master port, wherein described in one, the first port switching is connected with described the second master port, described in another, the first port switching is connected with described six-way valve, and wherein described in one, the second port switching is connected with described liquid inlet/outlet.
The present invention also provides a kind of automatic on-line micro-example dilution commingled system, comprises syringe pump, the first multi-position switching valve, the second multi-position switching valve, the 3rd multi-position switching valve, mixer, six-way valve, quantity tube and sampling pump; Described the first multi-position switching valve comprises that the first master port and two select with described the first master port the first port switching being communicated with, described the second multi-position switching valve comprises that the second master port and two select with described the second master port the second port switching being communicated with, described the 3rd multi-position switching valve comprises that the 3rd master port and two select with described the 3rd master port the 3rd port switching being communicated with, and described mixer has a liquid inlet/outlet; The two-port of described quantity tube and the import of described sampling pump are connected on described six-way valve, described syringe pump is connected with described the first master port, wherein described in one, the first port switching is connected with described the second master port, described in another, the first port switching is connected with described six-way valve, wherein described in one the second port switching with wherein described in one the 3rd port switching be connected, described the 3rd master port is connected with described liquid inlet/outlet.
Further, described mixer comprises mixing tube and waterproof ventilated membrane, is provided with described liquid inlet/outlet and air inlet/outlet on described mixing tube, is provided with described waterproof ventilated membrane on described air inlet/outlet.
Further, described mixer comprises flexible pouch, is provided with described liquid inlet/outlet in described flexible pouch.
Further, described six-way valve is six-way injection valve.
Further, described six-way valve comprises two two transfer valves, and described two transfer valves comprise that master port and two select with described master port the port switching being communicated with, and described quantity tube is connected between two described master ports; Described the first multi-position switching valve and described sampling pump respectively with corresponding connection of described port switching of two transfer valves described in one wherein.
Further, described in another, the second port switching is connected with waste liquid barrel.
Further, described in another, the 3rd port switching is connected with waste liquid barrel.
The present invention provides again a kind of automatic on-line Sample Dilution mixed method, adopts above-mentioned automatic on-line micro-example dilution commingled system, and concrete grammar comprises:
Step 1, sample introduction: sample is filled to quantity tube by sampling pump;
Step 2, dilution: by syringe pump, the sample in quantity tube is drawn in syringe pump, and dilution is drawn in syringe pump simultaneously;
Step 3, mixing: syringe pump is injected into the mixed liquor of sample and dilution in mixer by liquid inlet/outlet, then, then draw back the mixed liquor in mixer; So, repeated multiple times.
Automatic on-line micro-example dilution commingled system provided by the invention and mixed method, by adopting quantity tube quantitatively to measure micro-sample, because the volume of quantity tube is fixed, can high precision measure accurately micro-sample, mix and adopt syringe pump to dilute, syringe pump plays in the course of the work dilution and mixes two kinds of effects, syringe pump itself can be set the dilution of multiple accurately to sample, and in the time mixing, repeatedly extract and inject by syringe pump, can make sample and dilution mix fully, and, in extraction and injection process, can not exert an influence to the content of material of mixed liquor itself, can effectively meet the requirement that low dose of sample mixes in the mixer of small volume, realize the dilution mixing requirement that online micro-example dilution commingled system meets automatic on-line sample, improve mixing uniformity.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of automatic on-line micro-example dilution commingled system embodiment mono-of the present invention in sample introduction state;
Fig. 2 is the structural representation of automatic on-line micro-example dilution commingled system embodiment mono-of the present invention in diluted state;
Fig. 3 is the structural representation of automatic on-line micro-example dilution commingled system embodiment mono-of the present invention in admixture;
Fig. 4 is the structural representation of automatic on-line micro-example dilution commingled system embodiment bis-of the present invention;
Fig. 5 is the structural representation of mixer in automatic on-line micro-example dilution commingled system of the present invention.
Embodiment
For making object, technical scheme and the advantage of the embodiment of the present invention clearer, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment mono-
As shown in Figure 1, the present embodiment automatic on-line micro-example dilution commingled system, comprises syringe pump 1, the first multi-position switching valve 2, the second multi-position switching valve 3, the 3rd multi-position switching valve 5, mixer 4, six-way valve 8, quantity tube 9 and sampling pump 7; The first multi-position switching valve comprises that the first master port 21 and two select with the first master port 21 the first port switching 22,23 being communicated with, the second multi-position switching valve 3 comprises that the second master port 31 and two select with the second master port 31 the second port switching 32,33 being communicated with, the 3rd multi-position switching valve 5 comprises that the 3rd master port 51 and two select with the 3rd master port 51 the 3rd port switching 52,53 being communicated with, and mixer 4 has a liquid inlet/outlet 41; The import of the two-port of quantity tube 9 and sampling pump 7 is connected on six-way valve 8, syringe pump 1 is connected with the first master port 21, wherein one first port switching 23 is connected with the second master port 31, another first port switching 22 is connected with six-way valve 8, wherein one second port switching 33 is connected with one the 3rd port switching 52 wherein, and the 3rd master port 51 is connected with liquid inlet/outlet 41.
Particularly, the present embodiment automatic on-line micro-example dilution commingled system can effectively be carried out the sample introduction of micro-example, the quantity tube 9 connecting on six-way valve 8 can be designed to set micro-volume as required, while carrying out sample introduction by sampling pump 7, as shown in Figure 1, six-way valve 8 is communicated with sample, quantity tube 9 and sampling pump 7 streams, in quantity tube 9, will fill sample.And adopt syringe pump 1 to extract sample and the dilution in quantity tube 9, the controller of syringe pump 1 sends pulse and makes the rotation of device stepper motor, and stepper motor drives the screw mandrel of syringe pump 1 to rotatablely move to become rectilinear motion, carry out constant motion with the piston that promotes syringe in syringe pump 1, thereby realize high precision, pulseless fluid transport.Syringe pump 1 in the present embodiment has two kinds of functions: dilution and mixing.Concrete, first, as shown in Figure 2, six-way valve 8 is communicated with dilution, quantity tube 9 and the first multi-position switching valve 2 streams, the first master port 21 and being communicated with the first port switching 22, syringe pump 1 can extract sample and the dilution in quantity tube 9 by the first port switching 22; Then, as shown in Figure 3, the first master port 21 and being communicated with the first port switching 23, the second master port 31 is communicated with the second port switching 33, the 3rd master port 51 and the 3rd port switching 52 are communicated with, and the sample that syringe pump 1 obtains its inner extraction and the mixed liquor of dilution are expelled in mixer 4, after syringe pump 1 has been injected, again mixed liquor in mixer 4 is drawn back, repeatedly inject and extraction until mixed liquor mix.As from the foregoing, mixer 4 only has a liquid inlet/outlet 41, mixed liquor is injected in the process that pump 1 injects and extract via liquid inlet/outlet 41, mixed liquor can effectively be mixed, and because syringe pump 1 precision of infusing can reach 0.5%, fidelity can reach 0.05%, when making the present embodiment automatic on-line micro-example dilution commingled system can meet common sample introduction dilution mixing, can also well meet the dilution mixing requirement of automatic on-line micro-example.Because syringe pump 1 is lower than range below 20% time, there is larger error, this makes directly cannot meet with the micro-sample of syringe pump 1 direct extraction the requirement of precision, and quantity tube 9 can obtain micro-sample accurately, and in the time of dilution, syringe pump 1 can together extract together with sample and dilution, and extraction amount now will exceed the error stroke range of syringe pump 1, thereby obtains the mixed liquor of accurate extension rate.
In addition, after the sample in mixer 4 and dilution mix, extracted completely by syringe pump 1, the second master port 31 is selected to be communicated with the second port switching 32, and syringe pump 1 just can be injected into the mixed liquor mixing in analytical instrument.Simultaneously, syringe pump 1 can also enter into mixer 4 in the identical mode of above-mentioned mixed process by cleaning fluid and clean, after mixer 4 cleans up, the 3rd port switching 53 is communicated with the 3rd master port 51, on the 3rd port switching 53, be connected with waste liquid barrel 6, the cleaning fluid in mixer 4 flow in waste liquid barrel 6 automatically.Meanwhile, the outlet of sampling pump 7 is also connected with waste liquid barrel 6, and in the time of sample introduction, too much sample enters into waste liquid barrel 6.
The present embodiment automatic on-line micro-example dilution commingled system, by adopting quantity tube quantitatively to measure micro-sample, because the volume of quantity tube is fixed, can high precision measure accurately micro-sample, mix and adopt syringe pump to dilute, syringe pump plays in the course of the work dilution and mixes two kinds of effects, syringe pump itself can be set the dilution of multiple accurately to sample, and in the time mixing, repeatedly extract and inject by syringe pump, can make sample and dilution mix fully, and, in extraction and injection process, can not exert an influence to the content of material of mixed liquor itself, can effectively meet the requirement that low dose of sample mixes in the mixer of small volume, realize the dilution mixing requirement that online micro-example dilution commingled system meets automatic on-line sample, improve mixing uniformity.
Embodiment bis-
As shown in Figure 4, the present embodiment automatic on-line micro-example dilution commingled system, comprises syringe pump 1, the first multi-position switching valve 2, the second multi-position switching valve 3, mixer 4, six-way valve 8, quantity tube 9 and sampling pump 7; The first multi-position switching valve 1 comprises that the first master port 21 and two select with the first master port 21 the first port switching 22,23 being communicated with, the second multi-position switching valve 3 comprises that the second master port 31 and three select with the second master port 31 the second port switching 32,33,34 being communicated with, and mixer 4 has a liquid inlet/outlet; The import of the two-port of quantity tube 9 and sampling pump 7 is connected on six-way valve 8, syringe pump 1 is connected with the first master port 21, wherein one first port switching 23 is connected with the second master port 31, another first port switching 22 is connected with six-way valve 8, and wherein one second port switching 33 is connected with liquid inlet/outlet 41.
Particularly, the present embodiment automatic on-line micro-example dilution commingled system is identical with the principle in embodiment mono-, is also to utilize syringe pump 1 to complete sample introduction, dilution and mixing.Difference is: between the first multi-position switching valve 2 and mixer 4, adopt second multi-position switching valve 3 to connect, the second multi-position switching valve 3 has three the second port switchings 32,33,34, the second port switching 32 is for being injected into analytical instrument by the mixed liquor mixing, the second port switching 33 connects mixer 4, and the second port switching 34 is connected with waste liquid barrel 6, and the outlet of sampling pump 7 is also connected with waste liquid barrel 6.
Embodiment tri-
The present embodiment automatic on-line micro-example dilution commingled system is based on above-described embodiment one or embodiment bis-, difference is: as shown in Figure 5, mixer 4 comprises mixing tube 40 and waterproof ventilated membrane 42, on mixing tube 40, be provided with liquid inlet/outlet 41 and air inlet/outlet (not shown), on air inlet/outlet, be provided with waterproof ventilated membrane 42.Concrete, waterproof ventilated membrane 42 has the function of ventilative and waterproof, in the process of mixing at syringe pump 1, pressure in waterproof ventilated membrane 42 energy balance mixing tubes 40, to guarantee that syringe pump 1 moves smoothly, meanwhile, waterproof ventilated membrane 42 can effectively filter and enter into the contained pollutant of mixing tube 40 gases, guarantees the measuring accuracy of sample.
Embodiment tetra-
The present embodiment automatic on-line micro-example dilution commingled system is based on above-described embodiment one or embodiment bis-, and difference is: mixer comprises flexible pouch, is provided with liquid inlet/outlet in flexible pouch.Concrete, mixer adopts the mode of flexible pouch, due to flexible pouch deformable, thus can according to how many variations of adapting to of flexible pouch internal mix liquid, to guarantee that syringe pump 1 moves smoothly.In addition, because flexible pouch is hermetically sealed, do not have the impact of environmental contaminants, guarantee the measuring accuracy of sample.
Embodiment five
The present embodiment automatic on-line micro-example dilution commingled system is based on above-described embodiment one or embodiment bis-, and difference is: as shown in Figure 1, six-way valve 8 is six-way injection valve.Or as shown in Figure 4, six-way valve 8 comprises that 81,82, two transfer valves 81,82 of two two transfer valves comprise that master port (not shown) and two select with master port the port switching (not shown) being communicated with, quantity tube 9 is connected between two master ports; The first multi-position switching valve 2 and sampling pump 7 respectively with corresponding connection of port switching of one or two transfer valve 82 wherein.
Embodiment six
The present invention provides again a kind of automatic on-line Sample Dilution mixed method, adopts above-mentioned automatic on-line micro-example dilution commingled system, and to adopt the automatic on-line micro-example dilution commingled system of embodiment mono-as example, as shown in Figure 1-Figure 3, concrete grammar comprises:
Step 1, sample introduction: sample is filled to quantity tube 9 by sampling pump 7.Concrete, as shown in Figure 1, six-way valve 8 is communicated with sample, quantity tube 9 and sampling pump 7 streams, and sampling pump 7 draw sampless make will fill sample in quantity tube 9.
Step 2, dilution: by syringe pump 1, quantitative sample is drawn in syringe pump 1, and dilution is drawn in syringe pump 1 simultaneously.Concrete, as shown in Figure 2, the first master port 21 and being communicated with the first port switching 22, syringe pump 1 can extract quantitative sample and a certain amount of dilution by the first port switching 22, and sample is diluted with the extension rate of regulation.
Step 2, mixing: syringe pump 1 is injected into the mixed liquor of sample and dilution in mixer 4 by liquid inlet/outlet 41, then, then draw back the mixed liquor in mixer 4; So, repeated multiple times.Concrete, as shown in Figure 3, the first master port 21 and being communicated with the first port switching 23, the second master port 31 is communicated with the second port switching 33, the 3rd master port 51 and the 3rd port switching 52 are communicated with, and the sample that syringe pump 1 obtains its inner extraction and the mixed liquor of dilution are expelled in mixer 4, after syringe pump 1 has been injected, again mixed liquor in mixer 4 is drawn back, repeatedly inject and extraction until mixed liquor mix.
The present embodiment automatic on-line Sample Dilution mixed method, by adopting quantity tube quantitatively to measure micro-sample, because the volume of quantity tube is fixed, can high precision measure accurately micro-sample, mix and adopt syringe pump to dilute, syringe pump plays in the course of the work dilution and mixes two kinds of effects, syringe pump itself can be set the dilution of multiple accurately to sample, and in the time mixing, repeatedly extract and inject by syringe pump, can make sample and dilution mix fully, and, in extraction and injection process, can not exert an influence to the content of material of mixed liquor itself, can effectively meet the requirement that low dose of sample mixes in the mixer of small volume, realize the dilution mixing requirement that online micro-example dilution commingled system meets automatic on-line sample, improve mixing uniformity.
Finally it should be noted that: above embodiment only, in order to technical scheme of the present invention to be described, is not intended to limit; Although the present invention is had been described in detail with reference to previous embodiment, those of ordinary skill in the art is to be understood that: its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement; And these amendments or replacement do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (9)
1. an automatic on-line micro-example dilution commingled system, is characterized in that, comprises syringe pump, the first multi-position switching valve, the second multi-position switching valve, mixer, six-way valve, quantity tube and sampling pump; Described the first multi-position switching valve comprises that the first master port and two select with described the first master port the first port switching being communicated with, described the second multi-position switching valve comprises that the second master port and three select with described the second master port the second port switching being communicated with, and described mixer has a liquid inlet/outlet; The two-port of described quantity tube and the import of described sampling pump are connected on described six-way valve, described syringe pump is connected with described the first master port, wherein described in one, the first port switching is connected with described the second master port, described in another, the first port switching is connected with described six-way valve, and wherein described in one, the second port switching is connected with described liquid inlet/outlet.
2. an automatic on-line micro-example dilution commingled system, is characterized in that, comprises syringe pump, the first multi-position switching valve, the second multi-position switching valve, the 3rd multi-position switching valve, mixer, six-way valve, quantity tube and sampling pump; Described the first multi-position switching valve comprises that the first master port and two select with described the first master port the first port switching being communicated with, described the second multi-position switching valve comprises that the second master port and two select with described the second master port the second port switching being communicated with, described the 3rd multi-position switching valve comprises that the 3rd master port and two select with described the 3rd master port the 3rd port switching being communicated with, and described mixer has a liquid inlet/outlet; The two-port of described quantity tube and the import of described sampling pump are connected on described six-way valve, described syringe pump is connected with described the first master port, wherein described in one, the first port switching is connected with described the second master port, described in another, the first port switching is connected with described six-way valve, wherein described in one the second port switching with wherein described in one the 3rd port switching be connected, described the 3rd master port is connected with described liquid inlet/outlet.
3. automatic on-line micro-example dilution commingled system according to claim 1 and 2, it is characterized in that, described mixer comprises mixing tube and waterproof ventilated membrane, is provided with described liquid inlet/outlet and air inlet/outlet on described mixing tube, is provided with described waterproof ventilated membrane on described air inlet/outlet.
4. automatic on-line micro-example dilution commingled system according to claim 1 and 2, is characterized in that, described mixer comprises flexible pouch, is provided with described liquid inlet/outlet in described flexible pouch.
5. automatic on-line micro-example dilution commingled system according to claim 1 and 2, is characterized in that, described six-way valve is six-way injection valve.
6. automatic on-line micro-example dilution commingled system according to claim 1 and 2, it is characterized in that, described six-way valve comprises two two transfer valves, described two transfer valves comprise that master port and two select with described master port the port switching being communicated with, and described quantity tube is connected between two described master ports; Described the first multi-position switching valve and described sampling pump respectively with corresponding connection of described port switching of two transfer valves described in one wherein.
7. automatic on-line micro-example dilution commingled system according to claim 1, is characterized in that, described in another, the second port switching is connected with waste liquid barrel.
8. automatic on-line micro-example dilution commingled system according to claim 2, is characterized in that, described in another, the 3rd port switching is connected with waste liquid barrel.
9. an automatic on-line Sample Dilution mixed method, is characterized in that, adopts the automatic on-line micro-example dilution commingled system as described in as arbitrary in claim 1-8, and concrete grammar comprises:
Step 1, sample introduction: sample is filled to quantity tube by sampling pump;
Step 2, dilution: by syringe pump, the sample in quantity tube is drawn in syringe pump, and dilution is drawn in syringe pump simultaneously;
Step 3, mixing: syringe pump is injected into the mixed liquor of sample and dilution in mixer by liquid inlet/outlet, then, then draw back the mixed liquor in mixer; So, repeated multiple times.
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