CN116953088A - Chromatographic and continuous analysis module combined system and method - Google Patents
Chromatographic and continuous analysis module combined system and method Download PDFInfo
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- 238000004458 analytical method Methods 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007789 sealing Methods 0.000 claims description 41
- 239000007789 gas Substances 0.000 claims description 31
- 238000004891 communication Methods 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 20
- 238000004587 chromatography analysis Methods 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 9
- 238000004064 recycling Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims 1
- 238000004868 gas analysis Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 11
- 238000010926 purge Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/56—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition
- B01D46/62—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with multiple filtering elements, characterised by their mutual disposition connected in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/66—Regeneration of the filtering material or filter elements inside the filter
- B01D46/70—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter
- B01D46/72—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter with backwash arms, shoes or nozzles
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
- G01N35/00594—Quality control, including calibration or testing of components of the analyser
- G01N35/00613—Quality control
- G01N35/00623—Quality control of instruments
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
- G01N35/00594—Quality control, including calibration or testing of components of the analyser
- G01N35/00693—Calibration
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Abstract
The invention discloses a chromatographic and continuous analysis module combined system and a chromatographic and continuous analysis module combined system method. Meanwhile, the chromatograph and the continuous analysis module are arranged, and the accurate measurement data of the chromatograph is used for reversely calibrating the continuous analysis module, so that the accurate analysis and the quick response result are achieved after the new measurement model is applied.
Description
Technical Field
The invention relates to the technical field of chromatographic analysis, in particular to a chromatographic and continuous analysis module combined system and a chromatographic and continuous analysis module combined method.
Background
Chromatograph is able to accurately measure the content of each individual compound in a sample, but the instrument characteristics determine that it is periodic and cannot give results quickly. The continuous analysis module can rapidly feed back the concentration value of the single or mixed compound in the sample gas, but in actual measurement, the measured value is inaccurate when the continuous analysis module is used for actually measuring certain single or mixed compound in the sample gas due to the influence of cross interference factors between water vapor and each component, so that the signal value measured by the continuous analysis module is subjected to periodic measurement by utilizing accurate data of the chromatograph and is subjected to correction again, and the concentration value of the measured component of the sample can be accurately and rapidly fed back by the recalibrated data of the continuous analysis module.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a chromatographic and continuous analysis module combined system and a chromatographic and continuous analysis module combined method.
The aim of the invention is realized by the following technical scheme:
the utility model provides a chromatographic and continuous analysis module allies oneself with use system, includes chromatograph, buffer tank, continuous analysis module, carrier gas system, advances a sample filter, first pneumatic two-way ball valve, second pneumatic two-way ball valve, temperature pressure flow sensor, negative pressure assembly and air feed assembly, the analysis entry of chromatograph loops through first pneumatic two-way ball valve and intake pipe and sample entry sealed intercommunication, sample ball valve, advance a sample filter, first tee bend pneumatic ball valve and second tee bend pneumatic ball valve have been set gradually in the intake pipe, just sample ball valve is close to sample entry side sets up, the input of buffer tank with through a plurality of analysis pipeline sealed intercommunication between the intake pipe, every all be provided with on the analysis pipeline continuous analysis module, third tee bend pneumatic ball valve and first flowmeter, third tee bend pneumatic set up between continuous analysis module with between the intake pipe, just the input of analysis pipeline sets up between first tee bend pneumatic ball valve and the second tee bend pneumatic ball valve, the delivery outlet of buffer tank with negative pressure assembly sealed intercommunication has been set up in proper order to have sample ball valve, the buffer tank the input of buffer tank with the second pneumatic two-way ball valve and the second pneumatic ball valve, the second pneumatic ball valve has the seal of two-way pneumatic flow meter and the seal of analysis pipeline, the output of two pneumatic components set up in the continuous analysis module, the first pneumatic two-way ball valve and the second pneumatic ball valve has the seal to open the seal the output of pneumatic flow meter of analysis module, the second pneumatic end of the pneumatic valve and the sample The temperature pressure flow sensor and the measuring signal of the chromatograph are electrically connected with the control center, the input end of the chromatograph is in sealing communication with the air supply assembly, the output end of the chromatograph is in sealing communication with the second air discharge component, the analysis inlet is in sealing communication with the analysis outlet through an analysis pipeline, and a plurality of carrier gas systems are in sealing connection with the analysis pipeline.
Further, the negative pressure assembly comprises first instrument air, a first manual ball valve, a first pressure reducing valve, a venturi pump and a low-pressure return main pipe, wherein the first instrument air sequentially passes through the first manual ball valve, the first pressure reducing valve and the venturi pump and then is communicated with the low-pressure return main pipe in a sealing manner, and an output port of the buffer tank is communicated with the venturi pump in a sealing manner.
Further, the automatic calibration device further comprises a calibration assembly, the calibration assembly comprises a calibration needle valve, a calibration ball valve and a calibration air source, the calibration air source is in sealing communication with the input end of the calibration needle valve through the calibration ball valve, and the second three-way pneumatic ball valve and the third three-way pneumatic ball valve are both in sealing communication with the output end of the calibration needle valve.
Further, the air supply assembly comprises a second instrument air, a second pressure reducing valve and a third pressure reducing valve, wherein the input ends of the second pressure reducing valve and the third pressure reducing valve are respectively communicated with the output end of the second instrument air in a sealing way, the output end of the second pressure reducing valve is communicated with a heating pipeline in the chromatographic analyzer in a sealing way, the output end of the heating pipeline is communicated with a second gas discharge part in a sealing way, and the third pressure reducing valve is communicated with the input end of the driving pipe in a sealing way.
Further, the back cleaning device comprises a back cleaning assembly, wherein the back cleaning assembly comprises third instrument air, a back cleaning ball valve and a fourth pressure reducing valve, and the third instrument air is communicated with the first three-way pneumatic ball valve in a sealing mode after sequentially passing through the back cleaning ball valve and the fourth pressure reducing valve.
Further, a membrane filter is arranged on the air inlet pipe, and the membrane filter is arranged between the first three-way pneumatic ball valve and the second three-way pneumatic ball valve.
Further, the membrane filter is communicated with the input port of the buffer tank in a sealing way through a circulating pipeline, a third flowmeter is arranged on the circulating pipeline, the sample inlet is communicated with a sample source in a sealing way, and the low-pressure return main pipe is communicated with the sample source in a sealing way.
A method of using a chromatography and continuous analysis module in combination system, the method comprising the steps of:
s1: opening the first manual ball valve and the first pressure reducing valve, and driving the venturi pump to work through the first instrument air and enabling the buffer tank to generate negative pressure;
s2: opening the sample ball valve and the first three-way pneumatic ball valve, enabling a sample to sequentially pass through the sample ball valve, the sample introduction filter and the first three-way pneumatic ball valve after coming out of the sample source, then entering the membrane filter, dividing the sample after passing through the membrane filter into a plurality of parts, and enabling a first part of the sample to sequentially pass through a circulating pipeline, the buffer tank, the venturi pump and the low-pressure return header pipe and then return to the sample source to form a rapid circulating loop;
s3: opening the second three-way pneumatic ball valve, the first pneumatic two-way ball valve and the second pneumatic two-way ball valve, enabling a second part of samples to sequentially pass through the second three-way pneumatic ball valve and the first pneumatic two-way ball valve and then enter the chromatographic analyzer for accurate analysis, enabling the samples to sequentially pass through the second pneumatic two-way ball valve and the temperature and pressure flow sensor and then enter the buffer tank for recycling after analysis is completed, enabling sample signals measured by the temperature and pressure flow sensor to be connected to the chromatographic analyzer, and analyzing the signals by the chromatographic analyzer to ensure that the samples currently measured are the samples under a normal circulation flow path;
s4: opening the third three-way pneumatic ball valve, and enabling a third part of the sample to sequentially pass through the third three-way pneumatic ball valve and the continuous analysis module and then enter the buffer tank for recycling;
s5: comparing a first set of data measured in the chromatograph with a second set of data measured in the continuous analysis module, if the first set of data is the same as the second set of data, no reverse calibration is needed, and if the first set of data is different from the second set of data, the continuous analysis module is needed to be calibrated in a reverse calibration mode;
s6: the calibrated continuous analysis module is utilized to rapidly analyze the content of the single or mixed components in the sample to be detected.
Further, in the step S3, when a constant temperature is required during the operation of the chromatograph, the air bath heated gas is provided to the chromatograph through the second instrument air and the second pressure reducing valve to ensure the chromatograph to be at a constant temperature.
Further, in the step S3, when a standard sample source exists, the second three-way pneumatic ball valve, the first pneumatic two-way ball valve and the second pneumatic two-way ball valve are closed, the standard sample is placed in the valve, the calibration needle valve, the calibration ball valve and the third three-way pneumatic ball valve are opened, the standard sample source calibrates the continuous analysis module through the continuous analysis module, and the calibration needle valve and the calibration ball valve are closed after calibration.
The beneficial effects of the invention are as follows:
1) In the system, a chromatographic analyzer and a continuous analysis module are arranged at the same time, and the continuous analysis module is reversely calibrated by accurate measurement data of the chromatographic analyzer, so that a result which can be accurately analyzed and can be responded quickly is achieved after a new measurement model is applied.
2) In the system, through setting up negative pressure subassembly and circulation pipeline for realize recycling after the sample gets into from the sample entry, make things convenient for the input and output of chromatograph to adjust.
3) In this system, set up and back wash the subassembly and can effectually wash the introduction filter, prevent introduction filter jam inefficacy.
4) In the system, the sample introduction filter and the membrane filter are arranged at the same time, so that impurities in a sample can be effectively removed, and pollution of the impurities to a chromatographic analyzer and a continuous analysis module is prevented.
5) In the system, the calibration component is arranged to calibrate the continuous analysis module rapidly, so that the continuous analysis module achieves the purpose of rapid use.
Drawings
FIG. 1 is a connection block diagram of the present system;
in the figure, the 1-chromatograph, 2-buffer tank, 3-continuous analysis module, 4-carrier gas system, 5-sample filter, 6-first pneumatic two-way ball valve, 7-second pneumatic two-way ball valve, 8-temperature pressure flow sensor, 9-intake pipe, 10-sample inlet, 11-sample ball valve, 12-first three-way pneumatic ball valve, 13-second three-way pneumatic ball valve, 14-analysis pipeline, 15-third three-way pneumatic ball valve, 16-first flowmeter, 17-detection pipeline, 18-second flowmeter, 19-first gas discharge component, 20-control center, 21-second gas discharge component, 22-first instrument air, 23-first manual ball valve, 24-first pressure reducing valve, 25-venturi pump, 26-low pressure return manifold, 27-calibration needle valve, 28-calibration ball valve, 29-calibration air source, 30-second pressure reducing valve, 31-second pressure reducing valve, 32-third pressure reducing valve, 33-third instrument air, 34-backwash ball valve, 35-fourth pressure reducing valve, 36-third pressure reducing pipeline, 37-third flowmeter, and 38-third flowmeter.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by a person skilled in the art without any inventive effort, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
a chromatography and continuous analysis module combined system comprises a chromatography analyzer 1, a buffer tank 2, a continuous analysis module 3, a carrier gas system 4, a sample injection filter 5, a first pneumatic two-way ball valve 6, a second pneumatic two-way ball valve 7, a temperature pressure flow sensor 8, a negative pressure assembly and a gas supply assembly, wherein an analysis inlet of the chromatography analyzer 1 is sequentially communicated with a sample inlet 10 in a sealing way through the first pneumatic two-way ball valve 6 and a gas inlet pipe 9, the gas inlet pipe 9 is sequentially provided with the sample ball valve 11, the sample injection filter 5, the first three-way pneumatic ball valve 12 and the second three-way pneumatic ball valve 13, the sample ball valve 11 is arranged near the side of the sample inlet 10, an input port of the buffer tank 2 is communicated with the gas inlet pipe 9 in a sealing way through a plurality of analysis pipelines 14, each analysis pipeline 14 is provided with the continuous analysis module 3, a third three-way pneumatic ball valve 15 and a first flowmeter 16, the third three-way pneumatic ball valve 15 is arranged between the continuous analysis module 3 and the gas inlet pipe 9, an input end of the analysis pipeline 14 is arranged between the first three-way pneumatic ball valve 12 and the second three-way pneumatic ball valve 13, an output port of the buffer tank 2 is communicated with the negative pressure assembly in a sealing way pneumatic two-way pneumatic ball valve 13, an output port of the buffer tank 2 is sequentially communicated with the second pneumatic two-way pneumatic ball valve 1 and the second pneumatic two-way ball valve 7 through the detection pipeline 7 and the temperature sensor 1, the first pneumatic two-way pneumatic ball valve 1 and the temperature sensor 1 are respectively, the second pneumatic sensor 1 is connected with the temperature sensor 1 and the second pneumatic sensor 1, the temperature sensor 1 is respectively, the temperature sensor 1 is arranged in the two-way pneumatic controller is respectively, the two-way pneumatic controller is connected with the temperature sensor 1, the analyzer is respectively, the temperature sensor is connected with the analyzer 1, and the analyzer is arranged in the controller, and the device is 20, and is connected in the device is respectively, and is provided, and is the device is provided and is provided, and is the device, and is provided. The input end of the chromatograph 1 is communicated with the gas supply assembly in a sealing way, the output end of the chromatograph 1 is communicated with the second gas discharge component 21 in a sealing way, the analysis inlet is communicated with the analysis outlet in a sealing way through an analysis pipeline, and a plurality of carrier gas systems 4 are connected to the analysis pipeline in a sealing way. The continuous analysis module 3 is an infrared analysis module in the prior art, and may also be a measurement module such as a thermal conductivity measurement module, an ultraviolet measurement module, a laser measurement module, etc. that can analyze a result for a specific component according to a process condition on site. The continuous analysis module can effectively analyze the samples entering the continuous analysis module 3, the samples entering the continuous analysis module 3 can also enter the chromatograph 1 at the same time, the chromatograph 1 has the function of accurately analyzing the samples entering the chromatograph 1, and the continuous analysis module 3 is reversely calibrated and calibrated through the control center 20 after analysis. The carrier gas system 4 is used for providing carrier gas for the sample entering the chromatographic analyzer 1, the first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 are used for controlling the sample entering the chromatographic analyzer 1, the temperature and pressure flow sensor 8 is in the prior art, the temperature, the pressure and the flow of the sample discharged from the chromatographic analyzer 1 are mainly monitored, the temperature and pressure flow sensor 8 transmits signals to the control center 20, and the control center 20 controls the first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 through the chromatographic analyzer 1. The purpose of buffer tank 2 is to provide a negative pressure so that sample entry through chromatograph 1 and continuous analysis module 3 can be quickly entered into buffer tank 2. The carrier gas system 4 may be provided in one or more, and the continuous analysis module 3 may be provided in one or more. The function of the sample filter 5 is to filter the sample, the function of the negative pressure component is to power the negative pressure of the buffer tank 2, the gas supply component is to power the operation of the system, and the constant temperature is provided for the very stable environment of the chromatographic analyzer 1. The first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 are air pressure regulating valves in the prior art, the first three-way pneumatic ball valve 12 is a three-way pneumatic valve in the prior art, and the second three-way pneumatic ball valve 13 and the third three-way pneumatic ball valve 15 are three-way valves in the prior art. When the calibration assembly works, the sample inlet 10 cannot be communicated with a sample; when the sample inlet 10 is filled with a sample, the calibration assembly stops working, and the calibration assembly and the sample inlet do not work simultaneously. The first and second flow meters 16, 18 are conventional and are primarily used to measure the flow of sample in the respective lines. The data measured by the continuous analysis module are regenerated after the mixed gas is accurately measured according to the chromatograph and the signal data of the selected specific analysis module are modeled, namely the continuous analysis module 3 measures the signal value of the mixed gas, the chromatograph 1 accurately measures the characteristic component value, the chromatograph 1 ensures the accuracy of the data under the measurement of the physical state of the sample by the temperature pressure flow sensor 8, and then the data are calibrated on the signal value of the mixed gas of the continuous analysis module 3, namely new calculation factors are stored and generated after the calibration.
In some embodiments, the negative pressure assembly includes a first meter air 22, a first manual ball valve 23, a first pressure reducing valve 24, a venturi pump 25, and a low pressure return manifold 26, the first meter air 22 passing through the first manual ball valve 23, the first pressure reducing valve 24, and the venturi pump 25 in sequence and being in sealed communication with the low pressure return manifold 26, and the output port of the surge tank 2 being in sealed communication with the venturi pump 25. Wherein the negative pressure assembly may be replaced by a negative pressure pump. In the present technique, the venturi pump 25 and the low pressure return manifold 26 are provided for the purpose of allowing the sample in the buffer tank 2 to enter the low pressure return manifold 26 through the venturi pump 25 in the prior art, and the sample in the low pressure return manifold 26 can be recovered. The first instrument air 22 powers the venturi pump 25, and the first instrument air 22 adjusts the power level of the venturi pump 25 through a first manual ball valve 23 and a first pressure reducing valve 24 in the prior art.
In some embodiments, the device further comprises a calibration assembly, the calibration assembly comprises a calibration needle valve 27, a calibration ball valve 28 and a calibration air source 29, the calibration air source 29 is in sealing communication with the input end of the calibration needle valve 27 through the calibration ball valve 28, and the second three-way pneumatic ball valve 13 and the third three-way pneumatic ball valve 15 are in sealing communication with the output end of the calibration needle valve 27. The calibration component is used for calibrating the continuous analysis module 3, the calibration air source 29 is an air source which is accurately measured, a calibration ball valve 28 and a calibration needle valve 27 in the prior art of samples in the calibration air source 29 enter the continuous analysis module 3, if the data in the continuous analysis module 3 are consistent with the data in the calibration air source 29, the continuous analysis module 3 is not required to be calibrated, if the data in the calibration air source 29 are inconsistent, the continuous analysis module 3 is required to be calibrated, if the data in the calibration air source 29 have a problem, the second three-way pneumatic ball valve 13, the first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 are opened, and the data in the calibration air source 29 can be confirmed through the chromatograph 1.
In some embodiments, the air supply assembly comprises a second instrument air 30, a second pressure relief valve 31 and a third pressure relief valve 32, the inputs of the second pressure relief valve 31 and the third pressure relief valve 32 are each in sealed communication with the output of the second instrument air 30, the output of the second pressure relief valve 31 is in sealed communication with a heated conduit within the chromatograph 1, the output of the heated conduit is in sealed communication with the second gas discharge member 21, and the third pressure relief valve 32 is in sealed communication with the drive tube input. The second instrument air 30 provides an air source for the normal operation of the system, the second instrument air 30 is firstly connected with the input end of a manual valve, the input ends of the second pressure reducing valve 31 and the third pressure reducing valve 32 are both connected with the output end of the manual valve, and the gas with a certain temperature is provided for the chromatographic analyzer 1 through the second pressure reducing valve 31, so that the chromatographic analyzer 1 keeps a constant temperature during operation. The first pneumatic two-way ball valve 6, the second pneumatic two-way ball valve 7 and the first three-way pneumatic ball valve 12 are controlled by the gas of the third pressure reducing valve 32, the flow rate and the switching condition of the first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 are all the wind sources provided by the third pressure reducing valve 32, the first three-way pneumatic ball valve 12 controls two states, one is used for detecting a through sample, the other is used for reversely cleaning the sample injection filter 5 and is used for ventilation, and the two states of the first three-way pneumatic ball valve 12 are also used for controlling the wind sources provided by the third pressure reducing valve 32.
In some embodiments, a back purge assembly is also included, the back purge assembly including a third instrument air 33, a back purge ball valve 34, and a fourth pressure relief valve 35, the third instrument air 33 in turn being in sealing communication with the first three-way pneumatic ball valve 12 after passing through the back purge ball valve 34 and the fourth pressure relief valve 35. Wherein, the back-cleaning ball valve 34 is a manual switch valve in the prior art, the fourth pressure reducing valve 35 is an adjustable valve in the prior art, the third instrument air 33 provides a cleaning air source for back-cleaning, the cleaning air source adjusts the inlet amount in the fourth pressure reducing valve 35 after passing through the back-cleaning ball valve 34, and then the sample filter 5 is reversely cleaned after passing through the first three-way pneumatic ball valve 12.
In some embodiments, a membrane filter 36 is provided on the air inlet pipe 9, the membrane filter 36 being provided between the first three-way pneumatic ball valve 12 and the second three-way pneumatic ball valve 13. The membrane filter 36 is in sealed communication with the input port of the buffer tank 2 via a circulation conduit 37, the circulation conduit 37 is provided with a third flowmeter 38, the sample inlet 10 is in sealed communication with the sample source, and the low pressure return manifold 26 is in sealed communication with the sample source. Wherein the membrane filter 36 is a filter in the prior art, the purpose of the membrane filter 36 is to perform secondary filtration on the sample entering the chromatograph 1 and the continuous analysis module 3, so that the sample contains less impurities, and the membrane filter 36 does not perform filtration on the sample entering the circulation line 37. The sample comes out of the sample source and enters the sample inlet 10, then sequentially passes through the sample ball valve 11, the sample introduction filter 5, the first three-way pneumatic ball valve 12, the membrane filter 36, the circulating pipeline 37, the buffer tank 2 and the low-pressure return manifold 26 and returns to the sample source, so that the sample circulates in the detection process, the flow rate of the sample entering the chromatographic analyzer 1 and the continuous analysis module 3 is conveniently regulated, and the third flowmeter 38 is in the prior art and is mainly used for measuring the flow rate of the sample in the circulating pipeline 37.
A method of using a chromatography and continuous analysis module in combination system, the method comprising the steps of:
(1) The first manual ball valve 23 and the first pressure reducing valve 24 are opened, and the venturi pump 25 is driven to operate by the first instrument air 22 and the buffer tank 2 is caused to generate negative pressure.
(2) The sample ball valve 11 and the first three-way pneumatic ball valve 12 are opened, the sample sequentially passes through the sample ball valve 11, the sample introduction filter 5 and the first three-way pneumatic ball valve 12 and then enters the membrane filter 36 after exiting from the sample source, the sample after passing through the membrane filter 36 is divided into a plurality of parts, and the first part of sample sequentially passes through the circulating pipeline 37, the buffer tank 2, the venturi pump 25 and the low-pressure return manifold 26 and then returns to the sample source to form a rapid circulating loop.
(3) Opening a second three-way pneumatic ball valve 13, a first pneumatic two-way ball valve 6 and a second pneumatic two-way ball valve 7, enabling a second part of samples to sequentially pass through the second three-way pneumatic ball valve 13 and the first pneumatic two-way ball valve 6 and then enter the chromatographic analyzer 1 for accurate analysis, enabling the samples to sequentially pass through the second pneumatic two-way ball valve 7 and the temperature and pressure flow sensor 8 and then enter the buffer tank 2 for recycling after analysis is completed, enabling sample signals measured by the temperature and pressure flow sensor 8 to be connected into the chromatographic analyzer 1, and analyzing the signals by the chromatographic analyzer 1 to ensure that the samples currently measured are samples under a normal circulation flow path. Wherein when a constant temperature is required during operation of the chromatograph 1, the gas supplying air bath heating to the chromatograph 1 through the second instrument air 30 and the second pressure reducing valve 31 ensures that the chromatograph 1 is at a constant temperature. When a standard sample source exists, the second three-way pneumatic ball valve 13, the first pneumatic two-way ball valve 6 and the second pneumatic two-way ball valve 7 are closed, a standard sample is placed in the standard sample source, the calibration needle valve 27, the calibration ball valve 28 and the third three-way pneumatic ball valve 15 are opened, the standard sample source calibrates the continuous analysis module 3 through the continuous analysis module 3, and the calibration needle valve 27 and the calibration ball valve 28 are closed after calibration.
(4) And opening the third three-way pneumatic ball valve 15, and enabling a third part of samples to sequentially pass through the third three-way pneumatic ball valve 15 and the continuous analysis module 3 and then enter the buffer tank 2 for recycling.
(5) Comparing the first set of data measured in the chromatograph 1 with the second set of data measured in the continuous analysis module 3, if the first set of data is the same as the second set of data, no reverse calibration is needed, and if the first set of data is different from the second set of data, the continuous analysis module 3 needs to be calibrated in reverse.
(6) Rapid analysis using the calibrated continuous analysis module 3 requires detection of the content of single or mixed components in the sample.
In the description of the present invention, it should be understood that the directions or positional relationships indicated by the terms "upper", "one side", "inner", "front", "center", "both ends", etc., are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "configured," "connected," "secured," "screwed," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intermediaries, or in communication with each other or in interaction with each other, unless explicitly defined otherwise, the meaning of the terms described above in this application will be understood by those of ordinary skill in the art in view of the specific circumstances.
The foregoing is merely a preferred embodiment of the invention, and it is to be understood that the invention is not limited to the form disclosed herein but is not to be construed as excluding other embodiments, but is capable of numerous other combinations, modifications and environments and is capable of modifications within the scope of the inventive concept, either as taught or as a matter of routine skill or knowledge in the relevant art. And that modifications and variations which do not depart from the spirit and scope of the invention are intended to be within the scope of the appended claims.
Claims (10)
1. A chromatography and continuous analysis module combination system, characterized in that: the device comprises a chromatographic analyzer (1), a buffer tank (2), a continuous analysis module (3), a carrier gas system (4), a sample injection filter (5), a first pneumatic two-way ball valve (6), a second pneumatic two-way ball valve (7), a temperature and pressure flow sensor (8), a negative pressure assembly and a gas supply assembly, wherein an analysis inlet of the chromatographic analyzer (1) sequentially passes through the first pneumatic two-way ball valve (6) and a gas inlet pipe (9) to be communicated with a sample inlet (10) in a sealing manner, the gas inlet pipe (9) is sequentially provided with a sample ball valve (11), the sample injection filter (5), a first three-way pneumatic ball valve (12) and a second three-way pneumatic ball valve (13), the sample ball valve (11) is close to the side of the sample inlet (10), an input port of the buffer tank (2) is communicated with the gas inlet pipe (9) in a sealing manner through a plurality of analysis pipelines (14), each analysis pipeline (14) is provided with the continuous analysis module (3), a third three-way pneumatic ball valve (15) and a first flowmeter (16), the third three-way pneumatic ball valve (15) is arranged between the continuous analysis module (3) and the first pneumatic ball valve (14) and the first pneumatic ball valve (13), the utility model discloses a gas analysis system, including buffer tank (2), negative pressure assembly, continuous analysis module (3), temperature pressure flow sensor (8), chromatograph (1) input end, first gas discharge part (19) are provided with on second pneumatic two-way ball valve (7), the drive tube output in chromatograph (1) respectively with first tee bend pneumatic ball valve (12) first pneumatic two-way ball valve (6) with the sealed intercommunication of second pneumatic two-way ball valve (7), continuous analysis module (3) temperature pressure flow sensor (8) with the measuring signal of chromatograph (1) all is connected with control center (20) electricity, chromatograph (1) input end with gas supply assembly is sealed intercommunication, chromatograph (1) output end with second gas discharge part (21) is connected with analysis system through sealing between a plurality of sealed passageways (4) of analysis system.
2. A chromatography and continuous analysis module combination system according to claim 1, wherein: the negative pressure assembly comprises a first instrument air (22), a first manual ball valve (23), a first pressure reducing valve (24), a venturi pump (25) and a low-pressure return header pipe (26), wherein the first instrument air (22) sequentially passes through the first manual ball valve (23), the first pressure reducing valve (24) and the venturi pump (25) and then is in sealing communication with the low-pressure return header pipe (26), and an output port of the buffer tank (2) is in sealing communication with the venturi pump (25).
3. A chromatography and continuous analysis module combination system according to claim 2, wherein: the automatic calibration device is characterized by further comprising a calibration assembly, wherein the calibration assembly comprises a calibration needle valve (27), a calibration ball valve (28) and a calibration air source (29), the calibration air source (29) is communicated with the input end of the calibration needle valve (27) in a sealing way through the calibration ball valve (28), and the second three-way pneumatic ball valve (13) and the third three-way pneumatic ball valve (15) are communicated with the output end of the calibration needle valve (27) in a sealing way.
4. A chromatography and continuous analysis module combination system according to claim 3, wherein: the gas supply assembly comprises a second instrument air (30), a second pressure reducing valve (31) and a third pressure reducing valve (32), wherein the input ends of the second pressure reducing valve (31) and the third pressure reducing valve (32) are respectively communicated with the output end of the second instrument air (30) in a sealing way, the output end of the second pressure reducing valve (31) is communicated with a heating pipeline in the chromatographic analyzer (1) in a sealing way, the output end of the heating pipeline is communicated with a second gas discharge part (21) in a sealing way, and the third pressure reducing valve (32) is communicated with the input end of the driving pipe in a sealing way.
5. The chromatography and continuous analysis module combination system of claim 4, wherein: the back cleaning device comprises a back cleaning assembly, wherein the back cleaning assembly comprises third instrument air (33), a back cleaning ball valve (34) and a fourth pressure reducing valve (35), and the third instrument air (33) is communicated with the first three-way pneumatic ball valve (12) in a sealing mode after sequentially passing through the back cleaning ball valve (34) and the fourth pressure reducing valve (35).
6. The chromatography and continuous analysis module combination system of claim 5, wherein: the air inlet pipe (9) is provided with a membrane filter (36), and the membrane filter (36) is arranged between the first three-way pneumatic ball valve (12) and the second three-way pneumatic ball valve (13).
7. The chromatography and continuous analysis module combination system of claim 6, wherein: the membrane filter (36) is communicated with the input port of the buffer tank (2) in a sealing way through a circulating pipeline (37), a third flowmeter (38) is arranged on the circulating pipeline (37), the sample inlet (10) is communicated with a sample source in a sealing way, and the low-pressure return manifold (26) is communicated with the sample source in a sealing way.
8. A method of using a chromatography and continuous analysis module according to claim 7, wherein: the method comprises the following steps:
s1: opening the first manual ball valve (23) and the first pressure reducing valve (24), driving the venturi pump (25) to work through the first instrument air (22) and enabling the buffer tank (2) to generate negative pressure;
s2: opening the sample ball valve (11) and the first three-way pneumatic ball valve (12), enabling a sample to sequentially pass through the sample ball valve (11), the sample introduction filter (5) and the first three-way pneumatic ball valve (12) after coming out of the sample source, then entering the membrane filter (36), dividing the sample after passing through the membrane filter (36) into a plurality of parts, and enabling a first part of the sample to sequentially pass through a circulating pipeline (37), the buffer tank (2), a venturi pump (25) and the low-pressure return header pipe (26) and then return to the sample source to form a rapid circulating loop;
s3: opening the second three-way pneumatic ball valve (13), the first pneumatic two-way ball valve (6) and the second pneumatic two-way ball valve (7), enabling a second part of samples to sequentially pass through the second three-way pneumatic ball valve (13) and the first pneumatic two-way ball valve (6) and then enter the chromatographic analyzer (1) for accurate analysis, enabling the samples to sequentially pass through the second pneumatic two-way ball valve (7) and the temperature pressure flow sensor (8) and then enter the buffer tank (2) for circulation after analysis is completed, enabling sample signals measured by the temperature pressure flow sensor (8) to be connected into the chromatographic analyzer (1), and enabling the chromatographic analyzer (1) to analyze the signals so as to ensure that the samples currently measured are the samples under a normal circulation flow path;
s4: opening the third three-way pneumatic ball valve (15), and enabling a third part of the sample to sequentially pass through the third three-way pneumatic ball valve (15) and the continuous analysis module (3) and then enter the buffer tank (2) for recycling;
s5: comparing a first set of data measured in the chromatograph (1) with a second set of data measured in the continuous analysis module (3), if the first set of data is the same as the second set of data, no reverse calibration is required, and if the first set of data is different from the second set of data, the continuous analysis module (3) is required to be subjected to reverse calibration;
s6: rapid analysis using the calibrated continuous analysis module (3) requires detection of the content of single or mixed components in the sample.
9. A method of using a chromatography and continuous analysis module according to claim 8, wherein: in the step S3, when a constant temperature is required in the working process of the chromatographic analyzer (1), the air bath heated gas is provided for the chromatographic analyzer (1) through the second instrument air (30) and the second pressure reducing valve (31) so as to ensure that the chromatographic analyzer (1) is at a constant temperature.
10. A method of using a chromatography and continuous analysis module according to claim 8 or 9, wherein: in the step S3, when a standard sample source exists, the second three-way pneumatic ball valve (13), the first pneumatic two-way ball valve (6) and the second pneumatic two-way ball valve (7) are closed, the standard sample is placed in the standard sample source, the calibration needle valve (27), the calibration ball valve (28) and the third three-way pneumatic ball valve (15) are opened, the standard sample source calibrates the continuous analysis module (3) through the continuous analysis module (3), and the calibration needle valve (27) and the calibration ball valve (28) are closed after calibration.
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