CN209878686U - Flow path switching device applied to liquid chromatogram atomic fluorescence combined instrument - Google Patents
Flow path switching device applied to liquid chromatogram atomic fluorescence combined instrument Download PDFInfo
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- CN209878686U CN209878686U CN201920030253.1U CN201920030253U CN209878686U CN 209878686 U CN209878686 U CN 209878686U CN 201920030253 U CN201920030253 U CN 201920030253U CN 209878686 U CN209878686 U CN 209878686U
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Abstract
The utility model relates to a be applied to flow path auto-change over device of liquid chromatogram atomic fluorescence combination instrument, include: the morphology analysis flow path part and the total amount analysis flow path part specifically include: the device comprises a liquid storage bottle, a high-pressure pump I, a high-pressure pump II, a mixer, a six-way valve, a high-pressure switching valve, a chromatographic column I, a chromatographic column II, an ultraviolet digestion interface unit, a total amount analysis sample introduction module, a four-way mixer, a form/total amount switching valve, a gas-liquid separator, a three-stage gas-liquid separator, a gas transmission pipeline, an atomization chamber and a temperature control system; the method has the beneficial effect that the double-column switching in the morphological analysis is realized on the basis of realizing the atomic fluorescence morphology/total amount switching.
Description
Technical Field
The utility model relates to a liquid chromatogram atomic fluorescence allies oneself with technical field, especially relates to a be applied to flow path auto-change over device of liquid chromatogram atomic fluorescence allies oneself with instrument.
Background
The combined technology of atomic fluorescence and liquid chromatography combines the characteristics of high separation performance of liquid chromatography, high sensitivity of atomic fluorescence and low detection limit, and is widely applied to the field of morphological analysis of elements in recent years.
When the liquid chromatogram atomic fluorescence combination instrument is used for total amount and morphological analysis, the connection mode of the pipeline needs to be manually switched before each analysis due to the difference of the connection pipelines, the operation is complex, and the measurement of total amount and morphological analysis samples is carried out in the same set of reaction system, which inevitably causes the pollution of the pipeline. In addition, in the actual morphological analysis experiment, because the separation requirements of different elements are different, the mobile phase and the chromatographic column need to be replaced, and the leakage of the joint is easily caused by repeatedly replacing the chromatographic column.
At present, the improvement about atomic fluorescence total amount and morphological analysis device is mainly to add the multi-ported valve on total amount analysis's basis, thereby realize the switching to the reaction gas flow path, be CN203881724U like the bulletin number of authorizing, the bulletin date of authorizing is the utility model of 2014 10 months 15 days, a novel two chemical reaction systems of liquid chromatogram atomic fluorescence allies oneself with instrument is disclosed, switch the reaction gas flow path before second grade vapour and liquid separator, nevertheless because can produce more steam in the morphological analysis, single vapour and liquid separator can not fine detach, there is the drawback that influences the detectivity. The utility model discloses a liquid chromatography atomic fluorescence instrument analysis function switching device is disclosed in the utility model patent of patent grant publication No. CN 206848220U, the grant publication date is 2018 in 01 month 05, has increased carrier gas distributing valve in the device to respectively independent use vapour and liquid separator and water trap in total amount and morphological analysis flow path, though can realize the switching of different modes, increased the complexity of structure and increased the consumption of carrier gas.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem that probably exists among the above liquid chromatogram atomic fluorescence allies oneself with instrument, the utility model aims to provide a be applied to liquid chromatogram atomic fluorescence allies oneself with flow path auto-change over device of instrument, its beneficial effect has realized the twin columns switching among the morphological analysis on the basis that realizes atomic fluorescence form/total amount switching.
In order to achieve the above purpose, the utility model adopts the technical proposal that:
a flow path switching device applied to a liquid chromatogram atomic fluorescence combined instrument comprises: the morphology analysis flow path part and the total amount analysis flow path part specifically include: the device comprises a liquid storage bottle 1, a high-pressure pump I2, a high-pressure pump II 3, a mixer 4, a six-way valve 5, a high-pressure switching valve 6, a chromatographic column I7, a chromatographic column II 20, an ultraviolet digestion interface unit 8, a total amount analysis sampling module 18, a four-way mixer 17, a form/total amount switching valve 11, a gas-liquid separator 12, a three-stage gas-liquid separator 13, a gas transmission pipeline 14, an atomization chamber 15 and a temperature control system 16;
the liquid storage bottle 1, the high-pressure pump I2, the high-pressure pump II 3, the mixer 4, the six-way valve 5, the high-pressure switching valve 6, the chromatographic column I7, the chromatographic column II 20, the ultraviolet digestion interface unit 8, the form/total amount switching valve 11, the gas-liquid separator 12, the three-stage gas-liquid separator 13, the gas transmission pipeline 14 and the atomization chamber 15 form a form analysis flow path part;
the total analysis sample injection module 18, the four-way mixer 17, the temperature control system 16, the form/total switching valve 11, the gas-liquid separator 12, the three-stage gas-liquid separator 13, the gas transmission pipeline 14 and the atomization chamber 15 form a total analysis flow path part;
the liquid storage bottle 1 is positioned above the high-pressure pump I2 and is connected with the high-pressure pump I2 through a pipeline, the high-pressure pump II 3 is positioned below the high-pressure pump I2 and is connected with the liquid storage bottle 1 through a pipeline, flow path outlets of the high-pressure pump I2 and the high-pressure pump II 3 are both connected with an inlet of a mixer 4, an outlet of the mixer 4 is connected with an inlet end of a six-way valve 5, an outlet end of the six-way valve 5 is connected with an inlet A position of a high-pressure switching valve 6, an inlet A position of the high-pressure switching valve 6 is respectively communicated with a B position of the high-pressure switching valve 6 and a D position of the high-pressure switching valve 6 through rotation of a valve shaft of the high-pressure switching valve 6, an outlet F position of the high-pressure switching valve 6 is respectively communicated with a C position of the high-pressure switching valve 6 and an E position of the high-pressure switching valve 6, a, the position D of the high-pressure switching valve 6 is connected with the inlet of a chromatographic column II 20, the outlet of the chromatographic column II 20 is connected with the position F of the outlet of the high-pressure switching valve 6, the position F of the outlet of the high-pressure switching valve 6 is also connected with the inlet end of an ultraviolet digestion interface unit 8, the outlet of the ultraviolet digestion interface unit 8 is connected with one inlet end of a form/total amount switching valve 11, the total amount analysis sample introduction module 18 is connected with an inlet of a four-way mixer 17, an outlet of the four-way mixer 17 is connected with the other inlet end of the form/total amount switching valve 11, an outlet end of the form/total amount switching valve 11 is connected with an inlet of the gas-liquid separator 12, an outlet of the gas-liquid separator 12 is connected with an inlet end of the third-stage gas-liquid separator 13, an outlet end of the third-stage gas-liquid separator 13 is connected with an inlet of the gas transmission pipeline 14, and an outlet of the gas transmission pipeline 14 is connected with an inlet end of the atomization chamber 15.
On the basis of the scheme, the high-pressure switching valve 6 is a six-position two-way valve, the maximum pressure resistance reaches 130MPa, and different flow paths are switched by rotation of the valve shaft.
On the basis of the above scheme, the form/total amount switching valve 11 is a three-position two-way medium isolation valve or a manual valve, and is used for switching the total amount analysis mode and the form analysis mode.
On the basis of the scheme, the ultraviolet digestion unit 8 comprises: the peristaltic pump I9, the peristaltic pump II 19 and the integrated module 10; the peristaltic pump II 19 is located above the peristaltic pump I9, the peristaltic pump II 19 is used for introducing an ultraviolet digestion oxidant, the peristaltic pump I9 is used for introducing a current-carrying agent and potassium borohydride, the outlet F positions of the peristaltic pump II 19, the peristaltic pump I9 and the high-pressure switching valve 6 are all connected with the integrated module 10, and the integrated module 10 is further connected with one inlet end of the form/total amount switching valve 11.
On the basis of the scheme, the total amount analysis sample injection module 18 adopts a peristaltic pump sample injection mode or an injection pump sample injection mode.
On the basis of the scheme, the temperature control system 16 is used for controlling the temperature of the four-way mixer 17, the form/total amount switching valve 11 and the gas-liquid separator 12 to be kept within the range of 10-50 ℃; the temperature control system 16 is used for controlling the temperature of the three-stage gas-liquid separator 13 to be kept within a range of-5 ℃ to 20 ℃, and the temperature control system 16 is used for controlling the temperature of the gas transmission pipeline 14 to be increased.
On the basis of the scheme, the morphological analysis flow path part adopts a double-liquid-phase high-pressure pump, and can perform gradient elution and isocratic elution procedures.
Drawings
The utility model discloses there is following figure:
fig. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural diagram of the present invention.
In the figure: 1. a liquid storage bottle; 2. a high-pressure pump I; 3. a high-pressure pump II; 4. a mixer; 5. a six-way valve; 6. a high pressure switching valve; 7. a chromatographic column I; 8. an ultraviolet digestion interface unit; 9. a peristaltic pump I; 10. an integration module; 11. a form/total amount switching valve; 12. a gas-liquid separator; 13. a tertiary gas-liquid separator; 14. a gas transmission line; 15. an atomization chamber; 16. a temperature control system; 17. a four-way mixing module; 18. a total amount analysis sample introduction module; 19. a peristaltic pump II; 20. and (4) a chromatographic column II.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
A flow path switching device applied to a liquid chromatography-atomic fluorescence combined instrument is shown in attached figures 1-2 and mainly comprises a morphological analysis flow path part and a total analysis flow path part, and specifically comprises: the device comprises a liquid storage bottle 1, a high-pressure pump I2, a high-pressure pump II 3, a mixer 4, a six-way valve 5, a high-pressure switching valve 6, a chromatographic column I7, a chromatographic column II 20, an ultraviolet digestion interface unit 8, a total amount analysis sampling module 18, a four-way mixer 17, a form/total amount switching valve 11, a gas-liquid separator 12, a three-level gas-liquid separator 13, a gas transmission pipeline 14, an atomization chamber 15 and a temperature control system 16.
The liquid storage bottle 1, the high-pressure pump I2, the high-pressure pump II 3, the mixer 4, the six-way valve 5, the high-pressure switching valve 6, the chromatographic column I7, the chromatographic column II 20, the ultraviolet digestion interface unit 8, the form/total amount switching valve 11, the gas-liquid separator 12, the three-stage gas-liquid separator 13, the gas transmission pipeline 14 and the atomization chamber 15 form a form analysis flow path part;
the total analysis sample injection module 18, the four-way mixer 17, the temperature control system 16, the form/total switching valve 11, the gas-liquid separator 12, the three-stage gas-liquid separator 13, the gas transmission pipeline 14 and the atomization chamber 15 form a total analysis flow path part;
the morphological analysis flow path part adopts a double-liquid-phase high-pressure pump, not only can realize gradient elution, but also can execute an isocratic elution program. The liquid storage bottle 1 is positioned above the high-pressure pump I2 and is connected with the high-pressure pump I2 through a pipeline, the high-pressure pump II 3 is positioned below the high-pressure pump I2 and is connected with the liquid storage bottle 1 through a pipeline, flow path outlets of the high-pressure pump I2 and the high-pressure pump II 3 are both connected with an inlet of a mixer 4, an outlet of the mixer 4 is connected with an inlet end of a six-way valve 5, an outlet end of the six-way valve 5 is connected with an inlet A position of a high-pressure switching valve 6, an inlet A position of the high-pressure switching valve 6 is respectively communicated with a B position and a D position through rotation of a valve shaft of the high-pressure switching valve 6, an outlet F position of the high-pressure switching valve 6 is respectively communicated with a C position of the high-pressure switching valve 6 and an E position of the high-pressure switching valve 6, a B position of the high-pressure switching valve 6 is connected with an inlet of a chromatographic column I7, an, the outlet of the chromatographic column II 20 is connected with the outlet F position of the high-pressure switching valve 6, the outlet F position of the high-pressure switching valve 6 is also connected with the inlet end of the ultraviolet digestion interface unit 8, and the outlet of the ultraviolet digestion interface unit 8 is connected with one inlet end of the form/total amount switching valve 11. The sample and the potassium borohydride solution in the total amount analysis flow path are introduced into a four-way mixer 17 through a total amount analysis sample injection module 18, an outlet of the four-way mixer 17 is connected with the other inlet end of the form/total amount switching valve 11, an outlet end of the form/total amount switching valve 11 is connected with an inlet of the gas-liquid separator 12, an outlet of the gas-liquid separator 12 is connected with an inlet end of the third-stage gas-liquid separator 13, an outlet end of the third-stage gas-liquid separator 13 is connected with an inlet of the gas transmission pipeline 14, and an outlet of the gas transmission pipeline 14 is connected with an.
When isocratic elution is performed, the mobile phase is connected to the inlet end of the six-way valve 5 through the high-pressure pump II 3, and when a gradient elution program is performed, the mobile phase enters the mixer 4 to be mixed after passing through the high-pressure pump I2 and the high-pressure pump II 3 and enters the six-way valve 5.
The high-pressure switching valve 6 is a six-position two-way valve, and different flow paths are switched by rotation of the valve shaft. When the high-pressure switching valve 6 is arranged at the position B, the mobile phase carries a sample to enter the high-pressure switching valve 6 from the position A and enter a chromatographic column I7 through the position B for separation, the separated sample sequentially flows through the position C of the high-pressure switching valve 6, and the position F enters an ultraviolet digestion unit 8. When the high-pressure switching valve 6 is arranged at the position D, the mobile phase carrying the sample enters the high-pressure switching valve 6 from the position A and enters the chromatographic column 20 II through the position D for separation, the separated sample sequentially flows through the position E of the high-pressure switching valve 6, and the position F enters the ultraviolet digestion unit 8.
The form/total amount switching valve 11 is a three-position two-way valve for switching the total amount analysis mode and the form analysis mode, and is located before the gas-liquid separator 12. In the form analysis mode, the sample subjected to the ultraviolet digestion treatment is connected to the gas-liquid separator 12 through the form/total amount switching valve 11. In the total analysis mode, the total analysis sample injection module 18 may adopt a sample injection mode of a peristaltic pump or an injection pump, and a sample is introduced into the four-way mixer 17 from the total analysis sample injection module 18 and enters the gas-liquid separator 12 through the form/total switching valve 11 to perform gas-liquid separation. In order to ensure the high efficiency and consistency of the reaction, the temperature control system 16 is a four-way mixer 17, a form/total amount switching valve 11 and a gas-liquid separator 12 for controlling the temperature.
Hydride or atoms formed by the element to be detected enter the three-stage gas-liquid separator 13 under the carrying of the carrier gas, and the temperature is controlled by the temperature control system 16 to be lower so as to sufficiently remove water vapor in the hydride or atom vapor.
The outlet end of the three-stage gas-liquid separator 13 is connected to an atomization chamber 15 through a gas transmission pipeline 14, and in order to ensure the high efficiency and consistency of atomization efficiency, the temperature control system 16 heats the gas transmission pipeline 14.
The above is the preferred implementation procedure of this embodiment, but the protection scope of the present invention is not limited thereto, and those skilled in the art can easily think of changes or substitutions within the technical scope of the present invention, and all should be covered within the protection scope of the present invention, therefore, the protection scope of the present invention is subject to the claims.
Those not described in detail in this specification are within the skill of the art.
Claims (7)
1. A flow path switching device applied to a liquid chromatogram atomic fluorescence combined instrument is characterized by comprising: the morphology analysis flow path part and the total amount analysis flow path part specifically include: the device comprises a liquid storage bottle (1), a high-pressure pump I (2), a high-pressure pump II (3), a mixer (4), a six-way valve (5), a high-pressure switching valve (6), a chromatographic column I (7), a chromatographic column II (20), an ultraviolet digestion interface unit (8), a total amount analysis sample injection module (18), a four-way mixer (17), a form/total amount switching valve (11), a gas-liquid separator (12), a three-level gas-liquid separator (13), a gas transmission pipeline (14), an atomization chamber (15) and a temperature control system (16);
the device comprises a liquid storage bottle (1), a high-pressure pump I (2), a high-pressure pump II (3), a mixer (4), a six-way valve (5), a high-pressure switching valve (6), a chromatographic column I (7), a chromatographic column II (20), an ultraviolet digestion interface unit (8), a form/total amount switching valve (11), a gas-liquid separator (12), a three-stage gas-liquid separator (13), a gas transmission pipeline (14) and an atomization chamber (15), wherein a form analysis flow path part is formed by the liquid storage bottle, the high-pressure pump I (2);
the total analysis sampling module (18), the four-way mixer (17), the temperature control system (16), the form/total switching valve (11), the gas-liquid separator (12), the three-stage gas-liquid separator (13), the gas transmission pipeline (14) and the atomization chamber (15) form a total analysis flow path part;
the liquid storage bottle (1) is positioned above the high-pressure pump I (2) and is connected with the high-pressure pump I (2) through a pipeline, the high-pressure pump II (3) is positioned below the high-pressure pump I (2) and is connected with the liquid storage bottle (1) through a pipeline, flow path outlets of the high-pressure pump I (2) and the high-pressure pump II (3) are both connected with an inlet of a mixer (4), an outlet of the mixer (4) is connected with an inlet end of a six-way valve (5), an outlet end of the six-way valve (5) is connected with an inlet A position of the high-pressure switching valve (6), through rotation of a valve shaft of the high-pressure switching valve (6), an inlet A position of the high-pressure switching valve (6) is respectively communicated with a B position of the high-pressure switching valve (6) and a D position of the high-pressure switching valve (6), an outlet F position of the high-pressure switching valve (6) is respectively communicated with a C, the B position of the high-pressure switching valve (6) is connected with the inlet of a chromatographic column I (7), the outlet of the chromatographic column I (7) is connected with the C position of the high-pressure switching valve (6), the D position of the high-pressure switching valve (6) is connected with the inlet of a chromatographic column II (20), the outlet of the chromatographic column II (20) is connected with the outlet F position of the high-pressure switching valve (6), the outlet F position of the high-pressure switching valve (6) is also connected with the inlet end of an ultraviolet digestion interface unit (8), the outlet of the ultraviolet digestion interface unit (8) is connected with one inlet end of a form/total amount switching valve (11), a total amount analysis sample injection module (18) is connected with the inlet of a four-way mixer (17), the outlet of the four-way mixer (17) is connected with the other inlet end of the form/total amount switching valve (11), and the outlet end of the form/total amount switching valve (11) is, the outlet of the gas-liquid separator (12) is connected with the inlet end of the three-stage gas-liquid separator (13), the outlet end of the three-stage gas-liquid separator (13) is connected with the inlet of the gas transmission pipeline (14), and the outlet of the gas transmission pipeline (14) is connected with the inlet end of the atomization chamber (15).
2. The flow path switching device applied to the liquid chromatography-atomic fluorescence combined instrument as claimed in claim 1, wherein the high-pressure switching valve (6) is a six-position two-way valve, and the maximum withstand voltage is 130 MPa.
3. The flow path switching device for use in combination of liquid chromatography and atomic fluorescence spectroscopy as set forth in claim 1, wherein the form/total amount switching valve (11) is a three-position two-way medium isolation valve or a manual valve for switching between the total amount analysis mode and the form analysis mode.
4. The flow path switching device applied to the liquid chromatography-atomic fluorescence combined instrument according to claim 1, wherein the ultraviolet digestion interface unit (8) comprises: the peristaltic pump I (9), the peristaltic pump II (19) and the integrated module (10); the peristaltic pump II (19) is located above the peristaltic pump I (9), the peristaltic pump II (19) is used for introducing an oxidant for ultraviolet digestion, the peristaltic pump I (9) is used for introducing current-carrying and potassium borohydride, the outlet F positions of the peristaltic pump II (19), the peristaltic pump I (9) and the high-pressure switching valve (6) are all connected with the integrated module (10), and the integrated module (10) is further connected with one inlet end of the form/total amount switching valve (11).
5. The flow path switching device applied to the liquid chromatography-atomic fluorescence combined instrument as claimed in claim 1, wherein the total amount analysis sample injection module (18) adopts a peristaltic pump sample injection mode or a syringe pump sample injection mode.
6. The flow path switching device for use in a liquid chromatography-atomic fluorescence spectrometer as claimed in claim 1, wherein the temperature control system (16) is configured to control the four-way mixer (17), the form/total amount switching valve (11), and the gas-liquid separator (12) to maintain the temperatures thereof within a range of 10 to 50 ℃; the temperature control system (16) is used for controlling the temperature of the three-stage gas-liquid separator (13) to be kept within a range of-5-20 ℃, and the temperature control system (16) is used for controlling the temperature rise of the gas transmission pipeline (14).
7. The flow path switching device for use in a liquid chromatography-atomic fluorescence spectrometer as claimed in claim 1, wherein the morphological analysis flow path portion employs a dual liquid phase high pressure pump to perform both gradient elution and isocratic elution.
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| CN201920030253.1U CN209878686U (en) | 2019-01-08 | 2019-01-08 | Flow path switching device applied to liquid chromatogram atomic fluorescence combined instrument |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920030253.1U CN209878686U (en) | 2019-01-08 | 2019-01-08 | Flow path switching device applied to liquid chromatogram atomic fluorescence combined instrument |
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| CN209878686U true CN209878686U (en) | 2019-12-31 |
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