Method and device that a kind of ruhende electrode control mercury drips
Technical field
The present invention relates to the ruhende electrode using in polarographic analysis equipment in Electrochemical Detection.
Background technology
Clinical examination trace element project, mainly contain two kinds of technology, respectively atomic absorption method and electrochemical method, the ruhende electrode of using in electrochemical detection method mostly is dropping-mercury electrode or controls mercury and drip the volume of formation by changing time that solenoid valve opens, the mercury that dropping-mercury electrode expends is too many, substantially do not re-use, it is to flow downward along kapillary by the deadweight of mercury that mercury drips formation, in order to ensure that mercury drips smooth formation, mercury cup need have enough height to capillary end, to produce enough pressure, increase length capillaceous, internal diameter capillaceous is very little, the moment of opening at solenoid valve, form vibrations and moment negative pressure can drive the mercury column moment fast reciprocating of kapillary inside to move, because kapillary is very long, be very easy to occur air block, mercury column is divided into discontinuous mercury section, have a strong impact on the reliability of ruhende electrode, simultaneously, the volume that each formation mercury drips is also difficult to ensure homogeneity.
Summary of the invention
In order to overcome the existing ruhende electrode of controlling mercury and drip the volume of formation by changing time that solenoid valve opens, the moment of opening at solenoid valve, form vibrations and moment negative pressure can drive the mercury column moment fast reciprocating of kapillary inside to move, the volume that each formation mercury drips is also difficult to ensure the deficiency of homogeneity, the invention provides method and device that a kind of ruhende electrode control mercury drips, this device promotes mercury with syringe pump and drips formation, the volume that mercury drips can arrange arbitrarily, mercury drips average rate and forms, friction, change without pressure reduction, improved the reliability of electrode.
The technical solution adopted for the present invention to solve the technical problems is: the device that a kind of ruhende electrode control mercury drips, comprise storage mercury container and the kapillary that is arranged on its bottom, it is characterized in that: described storage mercury container is the cylindrical container that upper top and the inside surface of going to the bottom are taper surface, upper top taper surface top end is provided with inlet, water tank with solenoid valve is housed on inlet, the taper surface lowest part of going to the bottom be provided with connect capillaceous go out mercury mouth, and platinum filament extraction electrode is housed, storage mercury container side wall upper part is equipped with syringe pump, storage mercury container inner bottom part is mercury solution layer, top is deionized water liquid layer.
Described kapillary is arranged on storage mercury container bottom by adapter sleeve, and kapillary is gluing to be connected in adapter sleeve, and adapter sleeve is threaded with storage mercury container.
Described syringe pump is push-down syringe pump, and its push rod is connected with stepping motor control apparatus.
Described solenoid valve is normally closed solenoid valve.
Between described adapter sleeve top and storage mercury container, be provided with O-ring seal.
Using method of the present invention is: will add mercury Jiao Gai and be enclosed within below capillaceous, to seal lower outlet capillaceous, open solenoid valve, in water tank, add quantitative mercury solution, the quantitative deionized water of annotating again, syringe pump is stepped back and is moved to range place, shut electromagnetic valve, to add mercury Jiao Gai takes off, the push rod of syringe pump promotes forward deionized water under the control of stepper motor, the pressure producing will make the mercury solution in kapillary move down, finally forming in lower port capillaceous the mercury hanging drips, because the shrinkage factor of water is very little, and mercury solution layer is very little to the distance of lower end capillaceous, density and difference in height generation pressure by mercury can be very not large yet, work as closed electromagnetic valve, in container, there is no air, syringe pump stops, under the enough little state of internal diameter capillaceous, mercury solution can stop in kapillary still, the mercury that lower port formation capillaceous is hung drips also and remains static, become the ruhende electrode needing.In the time that the stroke of syringe pump is finished, to add mercury Jiao Gai and be enclosed within below capillaceous, to seal lower outlet capillaceous, open solenoid valve, supplement quantitative deionized water to water tank, syringe pump moves to range place, shut electromagnetic valve, will add mercury Jiao Gai and take off, and just can continue to use, drip demand according to mercury, capacity that can appropriate change syringe pump.
The invention has the beneficial effects as follows that promoting mercury with syringe pump drips formation, the volume that mercury drips can arrange arbitrarily, and mercury drips average rate and forms, and friction changes without pressure reduction, has improved the reliability of electrode.It is simple that the present invention has device structure, and reliability is high, measures advantage accurately.
Brief description of the drawings
Fig. 1 is structural representation of the present invention,
In figure, 1. water tank, 2. solenoid valve, 3. storage mercury container, 4. deionized water liquid layer, 5. mercury solution layer, 6. platinum filament extraction electrode, 7. O-ring seal, 8. goes out mercury mouth, 9. adapter sleeve, 10. kapillary, 11. syringe pumps, 12. add mercury Jiao Gai.
Embodiment
The specific embodiment of the present invention is, as shown in the figure:
Embodiment 1, the device that a kind of ruhende electrode control mercury drips, comprises storage mercury container 3 and the kapillary 10 that is arranged on its bottom, and kapillary is arranged on storage mercury container bottom by adapter sleeve 9, and kapillary is gluing to be connected in adapter sleeve, and adapter sleeve is threaded with storage mercury container.Between described adapter sleeve top and storage mercury container, be provided with O-ring seal 7.Described storage mercury container is the cylindrical container that upper top and the inside surface of going to the bottom are taper surface, upper top taper surface top end is provided with inlet, water tank 1 with solenoid valve 2 is housed on inlet, the taper surface lowest part of going to the bottom be provided with connect capillaceous go out mercury mouth 8 platinum filament extraction electrode is housed, storage mercury container side wall upper part is equipped with syringe pump 11, and storage mercury container inner bottom part is that mercury solution layer 5, top are deionized water liquid layer 4.
Described syringe pump is push-down syringe pump, and its push rod is connected with stepping motor control apparatus.Described solenoid valve is normally closed solenoid valve.
Using method of the present invention is: will add mercury glue lid 12 and be enclosed within the below of kapillary 10, with the lower outlet of sealing kapillary 10, open solenoid valve 2, in water tank 1, add quantitative mercury solution, the quantitative deionized water of annotating again, syringe pump 11 is stepped back and is moved to range place, shut electromagnetic valve 2, to add mercury glue lid 12 takes off, the push rod of syringe pump 11 promotes forward deionized water under the control of stepper motor, the pressure producing will make the mercury solution in kapillary 10 move down, finally forming in the lower port of kapillary 10 mercury hanging drips, because the shrinkage factor of water is very little, and mercury solution layer 5 is very little to the distance of the lower end of kapillary 10, density and difference in height generation pressure by mercury can be very not large yet, when solenoid valve 2 cuts out, in container 3, there is no air, syringe pump stops, under the enough little state of internal diameter capillaceous, mercury solution can stop in kapillary still, the mercury that lower port formation capillaceous is hung drips also and remains static, become the ruhende electrode needing.In the time that the stroke of syringe pump 11 is finished, to add mercury glue lid 12 and be enclosed within the below of kapillary 10, with the lower outlet of sealing kapillary 10, open solenoid valve 2, supplement quantitative deionized water to water tank 1, syringe pump 11 is stepped back and is moved to range place, shut electromagnetic valve 2, will add mercury glue lid 12 and take off, and just can continue to use, drip demand according to mercury, capacity that can appropriate change syringe pump.