CN114624377A - Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph - Google Patents
Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph Download PDFInfo
- Publication number
- CN114624377A CN114624377A CN202210157760.8A CN202210157760A CN114624377A CN 114624377 A CN114624377 A CN 114624377A CN 202210157760 A CN202210157760 A CN 202210157760A CN 114624377 A CN114624377 A CN 114624377A
- Authority
- CN
- China
- Prior art keywords
- leakage
- liquid
- module
- sensor
- alarm threshold
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 174
- 238000012544 monitoring process Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 36
- 238000001802 infusion Methods 0.000 claims abstract description 34
- 238000009423 ventilation Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 97
- 239000003960 organic solvent Substances 0.000 claims description 36
- 238000001514 detection method Methods 0.000 claims description 23
- 238000004880 explosion Methods 0.000 claims description 16
- 230000007246 mechanism Effects 0.000 claims description 15
- 238000012545 processing Methods 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 4
- 230000000704 physical effect Effects 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 230000009977 dual effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000007784 solid electrolyte Substances 0.000 claims description 2
- 229940090047 auto-injector Drugs 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 230000003321 amplification Effects 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 238000003199 nucleic acid amplification method Methods 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Examining Or Testing Airtightness (AREA)
Abstract
The utility model relates to a leakage double monitoring alarm protection system for a liquid chromatograph, which comprises a column cavity of a column temperature box module, an infusion pump module, an automatic sample injector module, a column temperature box module and a case of a detector module. An organic gas leakage sensor is arranged in a column cavity of the column incubator; the module comprises a module, a circuit control component, a leakage collector, a liquid contact type leakage sensor, a ventilation system, a first mounting area and a second mounting area, wherein the ventilation system is arranged in a case of the module, the first mounting area is used for mounting the circuit control component, the second mounting area is used for mounting the flow path component, the leakage collector and the liquid contact type leakage sensor are sequentially arranged outside the case, the leakage collector is arranged below the second mounting area, and a gas sensor is further arranged at the separation position of the first mounting area and the second mounting area. The technical scheme provided by the utility model adopts a double real-time monitoring mode of the organic gas leakage sensor and the liquid contact type leakage sensor to ensure prompt and treatment in time after leakage and ensure safe operation of the instrument.
Description
Technical Field
The utility model belongs to the field of liquid chromatography detection, and particularly relates to a leakage double-monitoring alarm protection system and method for a liquid chromatograph.
Background
The liquid chromatograph uses a liquid (usually containing an organic solvent) as a mobile phase. During use, there is a possibility that leakage may occur even when the operation of the pipe joint, the flow path member, and the like is irregular or aged. Liquid leakage may occur inside the column cavity of the column oven and outside parts of each module case, such as various pipe joints and the like; it is also possible that flow path components such as buffers, mixers, flow cells, etc. occur. The pipeline joint and the flow path component are distributed in the column cavity of the column incubator or the inside and the outside of each module case in different degrees according to different instrument structures and layouts. Generally, the existing safety measures for liquid leakage are that a drainage device is installed below a position where liquid leakage is likely to occur, leaked liquid is led out to the outside of a case and collected to a contact type liquid leakage sensor position, and a liquid leakage alarm protection mechanism is triggered. The liquid leakage alarm protection mechanism generally cuts off the liquid delivery of a flow path, all heating outputs of a system and the power supply inside a liquid leakage module.
Generally, in the prior art, a thermistor is commonly used as a liquid leakage detection element, when liquid contacts the surface of the thermistor, temperature difference exists between the liquid and the environment, and partial heat is taken away by volatilization of the liquid, so that the temperature of the thermistor changes, the resistance value changes, and finally, an alarm is realized after the temperature is processed by a circuit system. It is not difficult to derive from the above alarm principle that the leaked liquid must be in direct contact with the leakage sensor to trigger an alarm protection mechanism. The conventional leakage sensor is generally arranged at the centralized layout position of the external pipeline joint of the case, so that the pipeline or the component outside the case easily generates leakage to cause a leakage alarm protection mechanism, and even if trace leakage is not converged at the sensor, the trace leakage sensor is easily discovered by an operator to take measures in time. In addition, the potential safety hazard of leakage outside the case is relatively low.
The current liquid leakage alarm technology (direct contact triggering alarm) has obvious defects and major potential safety hazards as follows: firstly, once the liquid that leaks in the quick-witted case of each module can not converge to weeping sensor department because of various reasons, can not initiate the alarm protection mechanism, general operating personnel just also be difficult for discovering the instrument weeping and take corresponding measure. And secondly, liquid leakage is generated on a joint or a component in a column cavity of the column temperature box, and the liquid is easy to volatilize before collection because the column cavity is a temperature control area and the using temperature is higher than the room temperature. The existing leakage alarm technology cannot detect and alarm for protection under the two conditions. The common liquid chromatograph usually uses organic solvent or liquid containing organic solvent as mobile phase, i.e. the liquid leaking from each part generally contains organic solvent, such as common mobile phase methanol, acetonitrile, etc., because the common organic solvent has low boiling point, is very volatile, and has wide explosion limit and very low explosion lower limit, taking methanol as example, the explosion range is 5.5% -44%, the volume of each module cabinet is calculated according to 40L, 3ml of methanol volatilizes to reach the explosion lower limit, while the volume of the column cavity of the common column oven is only 0.5-2L, and the extremely small amount (about 0.1 ml) of methanol volatilizes to reach the explosion lower limit. At this time, if the circuit components or heating components in the cabinet or the column chamber generate sparks, explosion accidents are caused, and the safety of life and property is threatened.
A column oven for a liquid chromatograph and a liquid chromatograph are disclosed in patent publication No. CN107589210A, and the column oven for a liquid chromatograph structurally includes a column temperature adjusting section, a separation column, a leak detection section, and a leak temperature adjusting section; the separation column is arranged in the column temperature adjusting part and used for adjusting the temperature; the liquid leakage detection part consists of a first temperature sensor and a second temperature sensor and is used for detecting liquid formed after the liquid leaks from the separation column to the column temperature regulation part; the leaked liquid temperature adjusting part is used for reducing the temperature of the leaked liquid, so that the difference value between the temperature of the leaked liquid and the ambient temperature after the heat transfer between the leaked liquid and the second temperature sensor is smaller than a preset threshold value, and the detection of the leaked liquid is realized. When the method is applied, the detection efficiency and the detection accuracy of the leaked liquid of the liquid chromatograph can be effectively improved, but a certain amount of leaked liquid is required to be gathered to enable the second temperature sensor to generate temperature change.
Patent publication No. CN209264650U discloses a column oven of a liquid chromatograph capable of monitoring micro leakage, which structurally comprises a box body, a box cover, a chromatographic column and two connecting pieces. Wherein the chromatographic column is arranged in the box body, and two ends of the chromatographic column are respectively connected with the two connecting pieces and are contacted with the supporting block below. Still be equipped with two removal portions in the box, including slider and temperature sensor, temperature sensor installs in the slider top and contacts with the junction of chromatographic column both ends connecting piece, and the box bottom surface is equipped with two spouts of taking the slider, and the slider can slide in the spout. A control box is arranged outside the box body, a PCB welded with a main control module, a power supply module, a processing module and an alarm module is arranged in the control box, and a temperature sensor is connected with the power supply module and the main control module respectively. When the method is applied, only the tiny leakage condition at the joint of the chromatographic column can be monitored and reminded, but the leakage treatment cannot be carried out.
In the above patents, the liquid direct contact type leakage sensor is adopted, and only the external temperature change or the leakage position change is optimized correspondingly, and the condition of volatilization of the leaked liquid cannot be detected, so that the influence on analysis and potential safety hazard caused by the existence of organic solvent vapor in a case or a cavity containing a circuit component or a heating component cannot be avoided. In addition, the aspects of the patent judgment mechanisms are single judgment modes, the judgment accuracy and stability are poor, and the false alarm triggering caused by external environment change cannot be avoided.
Disclosure of Invention
In order to solve the problems, the utility model provides a leakage double monitoring alarm protection system and a leakage double monitoring alarm protection method for a liquid chromatograph, wherein organic gas leakage sensors are used in a column cavity of a column temperature box and the inner part of a case of each module, and a double real-time monitoring mode of a liquid contact type leakage sensor is used at a drainage liquid collection position outside the case of each module so as to ensure prompt and treatment in time after leakage and ensure safe operation of an instrument.
The technical scheme of the utility model is as follows:
a leakage double monitoring alarm protection system for a liquid chromatograph is characterized by structurally comprising a column cavity of a column temperature box module, an infusion pump module, an automatic sample injector module, a column temperature box module and a chassis of a detector module; at least one organic gas leakage sensor is arranged in a column cavity of the column incubator; the device comprises an infusion pump module, an automatic sample injector module, a column temperature box module and a detector module, wherein a ventilation system is arranged in a case of at least one of the infusion pump module, the automatic sample injector module, the column temperature box module and the detector module, a first mounting area for mounting a circuit control part and a second mounting area for mounting a flow path part are arranged in the case, a leakage collector and a liquid contact type leakage sensor are sequentially arranged outside the case, the leakage collector is arranged below the flow path part of the second mounting area, leakage drainage grooves are formed in the surfaces below all the flow path parts where the leakage collector is located, the liquid contact type leakage sensor is arranged at a liquid collection position, and at least one organic gas leakage sensor is further arranged at the separation position of the first mounting area and the second mounting area; the double monitoring is that the organic gas leakage sensor and the liquid contact type leakage sensor respectively carry out double detection monitoring on the leaked organic vapor and the leaked organic liquid. Liquid conveying is realized among the modules through pipelines and pipeline joints, the infusion pump extracts a mobile phase and conveys the mobile phase to the automatic sample injector, the chromatographic column in the column incubator and the detector in sequence, a sample enters the system through the automatic sample injector and is driven to the chromatographic column by the mobile phase for separation, and substances with different components sequentially reach the detector to be detected according to different distribution coefficients. The circuit boards among the modules are connected through communication lines, and the workstation controls the modules.
Preferably, the column cavity of the column oven is a temperature control area for installing the chromatographic column; the ventilation system of the case consists of an air inlet, an air outlet and a power fan, and air in the case can be quickly replaced after the ventilation system is opened.
Preferably, the circuit control component comprises a power supply, a heating element, a circuit board, a component controller; the alternating current is converted into direct current through a power supply to supply power for each circuit board and the component controller, the electric control end of the heating element is connected with the circuit board, the circuit board supplies power and performs heating program control, and the other end of the heating element is arranged in the temperature control area of the column cavity to provide heat for the chromatographic column. The flow path component comprises a mixer, a damper, a pump body, a tee joint, a pipeline and a pipeline joint, wherein the pump body drives a plunger rod to reciprocate through a motor to realize suction and delivery of mobile phases, pressure pulsation formed by reciprocating motion of the plunger rod is eliminated through the damper, then different mobile phases are fully mixed in the mixer, and then the mixed mobile phases are delivered to each module. The pipeline and the joint part of the pipeline are arranged outside the case; the leakage collector is made of organic solvent resistant materials, and the upper plane of the leakage collector is provided with a fluid guide slope.
Preferably, the liquid contact type liquid leakage sensor adopts a thermistor as a sensing element, adopts a two-way thermistor reference detection mode, and is provided with a bridge circuit detection voltage amplification circuit with temperature compensation in a matching circuit, wherein the bridge circuit detection voltage amplification circuit comprises an operational amplifier and an AD converter.
Preferably, the organic gas leakage sensor includes a semiconductor type, a solid electrolyte type, and an electrochemical type, and the semiconductor type uses a sensor element whose conductivity is sensitive to an organic gas.
The utility model also provides a leakage double monitoring and alarming method for the liquid chromatograph, which comprises the following steps:
s1: a user sets a liquid leakage alarm threshold value, the workstation communicates with the CPU, and a recommended gas alarm threshold value is calculated;
s2: selecting a recommended gas alarm threshold or a user-defined gas alarm threshold as an organic gas alarm threshold of the current system;
s3: receiving current values of the organic gas sensor and the liquid contact type leakage sensor, correspondingly comparing the current values with an organic gas alarm threshold value and a liquid leakage alarm threshold value of a current system, judging that the liquid leakage state exists when any current value of the organic gas sensor and the liquid contact type leakage sensor exceeds the corresponding threshold value, and otherwise, judging that the liquid leakage state does not exist;
s4: the workstation issues the current state information to each working module, and the CPU arranged in the working module combines the current liquid leakage alarm state information according to respective characteristics to complete internal processing: if the current state is a liquid leakage state, starting a liquid leakage alarm prompt and protection processing mechanism in each module; if the current state is a non-leakage state, the alarm prompt is released, and except that the infusion pump module maintains the current state, the other modules are restored to the target state set by the user method.
Preferably, the acquiring process of the gas alarm threshold in step S1 is as follows:
s1.1: the CPU receives the method information of the workstation, extracts and identifies the organic solvent information;
s1.2: the CPU calls a built-in common organic solvent physical property table to extract the explosion limit of the currently used organic solvent;
s1.3: and calling a built-in common organic solvent gas concentration-response value relation curve library by the CPU, and circularly comparing and calculating by adopting an interpolation method to obtain a system recommended gas alarm threshold value corresponding to the current organic solvent explosion lower limit.
Preferably, the specific process of step S2 is:
s2.1: prompting a user by the workstation whether to define a gas alarm threshold value by the user, wherein if the gas alarm threshold value is defined by the user, and if the gas alarm threshold value is not defined as the organic gas alarm threshold value of the current system;
s2.2: and judging whether the self-defined gas alarm threshold is lower than the recommended gas alarm threshold by the workstation, if so, defining the self-defined gas alarm threshold as the organic gas alarm threshold of the current system, otherwise, prompting the user to reset the self-defined gas alarm threshold.
Preferably, the operation module in step S4 includes an auto sampler, a column oven and a detector; the infusion pump module adopts an infusion pump, and the infusion pump stops infusion immediately when liquid leakage is confirmed and waits for follow-up examination.
Preferably, the process of S1-S4 is repeatedly executed at intervals of Δ t, and the judgment logics of the operating module and the infusion pump module adopt double judgment logics, and after the CPU issues a command to close the functional component or stop the module from running, the workstation automatically executes the judgment logics once again to complete the processing.
The utility model has the technical effects that:
the utility model adopts a high-sensitivity organic gas sensor in the cavity of the column oven; in addition, a conventional liquid contact type leakage sensor is used at a drainage liquid collection position outside a case of each module (comprising an infusion pump, an automatic sample injector, a column incubator, a detector and the like), and a dual real-time monitoring mode of an organic gas leakage sensor is used inside the case of each module, so that prompt and treatment can be timely performed after leakage is ensured, and safe operation of an instrument can be ensured.
The technical scheme provided by the utility model is structurally characterized in that firstly, a high-sensitivity organic gas leakage sensor is arranged in a column cavity of a column temperature box module; secondly, aiming at the case of each module, a ventilation system capable of quickly replacing air in the case is arranged, the flow path components and the circuit components are spatially isolated in the layout, liquid leakage drainage grooves are arranged below all the flow path components, and a liquid contact type liquid leakage sensor is arranged at a liquid collection position. Therefore, even if liquid leakage occurs in the components, the liquid cannot directly contact any circuit component, and the liquid can be detected after collection to trigger an alarm protection mechanism, so that the hidden danger of safety problems caused by contact of the liquid and a circuit system is avoided. Furthermore, high-sensitivity organic gas sensors are arranged in the column oven cavity and the machine boxes of all the modules, alarm limits are set on a control program, the high-sensitivity organic gas sensors are provided with amplification detection circuits, organic gas which is obviously smaller than the lower explosion limit of common organic solvents can trigger induction, when the concentration of the organic gas in the column oven cavity and the machine boxes of all the modules exceeds the alarm limits, a system alarms, all the modules immediately start a machine box ventilation system, organic gas is quickly removed and replaced, and a liquid leakage protection mechanism is started according to the characteristics of all the modules. After the alarm state is released, the other modules are restored to the target state set by the user method except that the infusion pump module maintains the current state.
The technical scheme provided by the utility model adopts different alarm triggering mechanisms in control according to different characteristics of the liquid leakage sensor and the gas leakage sensor. The liquid contact type leakage sensor adopts a double-path thermistor reference detection mode, and uses a bridge circuit amplifying circuit with temperature compensation in control, so that false alarm caused by environmental temperature fluctuation can be completely avoided. The gas leakage sensor alarm mechanism adopts a control mode that common organic solvent parameters are arranged in a CPU, and the CPU accurately calculates and reserves a safe proportion according to user setting information. And two kinds of weeping sensors adopt the mode of two-way real-time cruise monitoring, carry out the comprehensive control in space and time to instrument outside and inside the column incubator, avoid influencing the analysis because of the weeping does not perceive, avoided the emergence of incident.
Drawings
Fig. 1 is a schematic structural diagram of the apparatus provided in the present invention.
FIG. 2 is a schematic circuit diagram of a bridge circuit detection voltage amplifying circuit in the leakage sensor of the present invention.
Fig. 3 is a flow chart of a method provided by the present invention.
FIG. 4 is a flow chart of obtaining a recommended gas alarm threshold in the system CPU of the present invention.
FIG. 5 is a CPU control logic diagram for an infusion pump.
FIG. 6 is a diagram of the autosampler CPU control logic.
FIG. 7 is a control logic diagram of the column oven CPU.
FIG. 8 is a detector CPU control logic diagram.
In the figure: 1. the liquid leakage detection device comprises a first mounting area, a second mounting area, a power supply, a circuit board, a mixer, a damper, a pump body, a pipeline, a liquid leakage drainage groove, a liquid contact type liquid leakage sensor, a high-sensitivity organic gas sensor, a liquid leakage collector and a liquid leakage detection device, wherein the first mounting area is 2, the second mounting area is 3, the power supply is 4, the circuit board is 5, the mixer is 6, the damper is 7, the pump body is 8, the pipeline is 9, the flow direction of the liquid leakage drainage groove is 10, the liquid contact type liquid leakage sensor is 11, the high-sensitivity organic gas sensor is 12.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in figure 1, the leakage double monitoring and alarming system for the liquid chromatograph comprises a chassis of all modules, a first mounting area 1 for mounting circuit control components and a second mounting area 2 for mounting flow path components are divided in space inside the chassis, the second installation area is close to the front part of the system, the second installation area extends to the position, close to the bottom of the case, outside the case, an integrated type leakage liquid collector 12 and a liquid contact type leakage liquid sensor 10 are installed, all flow path parts and pipeline connectors are installed on the upper portion of the integrated type leakage liquid collector 12, leakage liquid drainage grooves are formed in the surfaces below all the flow path parts where the leakage liquid collector is located, the liquid contact type leakage liquid sensor 10 is arranged at the liquid collection position of the flow direction 9 of the leakage liquid drainage grooves, and a high-sensitivity organic gas sensor 11 is further arranged at the separation position of the first installation area and the second installation area. In addition, in the column cavity of the column oven module, a highly sensitive organic gas sensor 11 is installed.
As an embodiment of the present invention, the system structurally further includes a plurality of modules, specifically, an autosampler, a column oven, a detector, and an infusion pump, each module is disposed in a separate chassis, an organic gas sensor is mounted in each chassis, and a highly sensitive organic gas sensor is also mounted in a column cavity of the column oven module. The conventional liquid contact type leakage sensor is used at the drainage liquid collection position outside the machine cases of all the modules, and the double real-time monitoring mode of the organic gas leakage sensor is used inside the machine cases of all the modules, so that prompt and treatment are timely performed after liquid leakage is ensured, and the safe operation of the instrument is ensured.
And because the risk of leakage outside the case is lower than that inside the case, the pipeline joint and the flow path component are arranged outside the case as much as possible, and the flow path component which is required to be arranged inside the case partially because of functions or other factors is arranged in the flow path component mounting area inside the case.
The leakage collector is made of organic solvent resistant material, the upper plane is provided with a fluid guiding slope part, and the lowest point collection part is connected to the waste liquid collector. After the liquid drops to the leakage collector, the liquid flows along the guide inclined plane and finally is collected to the liquid contact type leakage sensor outside the case.
Wherein the circuit control components comprise a power supply 3, a heating element, a circuit board 4, and a component controller.
The flow path component comprises a mixer 5, a damper 6, a pump body 7, a tee joint, a pipeline 8 and a pipeline joint, and the pipeline joint are arranged outside the case.
If the pipeline joint or the component outside the case leaks, the leaked liquid is collected to the liquid contact type leaked liquid sensor through the leaked liquid drainage groove on the leaked liquid collector exposed outside the case.
In this embodiment, the flow path parts are spatially isolated from the circuit parts, and the leakage drainage grooves are arranged below all the flow path parts to drain to the leakage collector, so that even if the parts leak, the liquid cannot directly contact any circuit part, and the potential safety problem caused by the contact of the liquid and a circuit system is avoided.
As shown in fig. 2, a bridge circuit detection voltage amplifying circuit with temperature compensation is arranged in the liquid contact type leakage sensor, and the bridge circuit detection voltage amplifying circuit comprises an operational amplifier, an AD converter and a thermistor. The liquid leakage sensor adopts the working principle that a bridge circuit with temperature compensation is adopted to detect a voltage amplifying circuit, when fluid flows through a thermistor, the temperature of the fluid changes, resistance value change of the resistor is caused, voltage difference is generated on the bridge circuit, the voltage difference is amplified by the amplifying circuit and is subjected to temperature compensation correction, and then the current value is output. The current value is output to the workstation through the module CPU, and whether to give an alarm or not is judged after the comparison between the workstation and the set value of the user.
In the embodiment, the high-sensitivity organic gas sensors are arranged in the column oven cavity and the machine cases of all the modules, the alarm limit is set on the control program, and the high-sensitivity organic gas sensors are provided with the amplification detection circuit, so that the organic gas which is obviously smaller than the explosion lower limit of the common organic solvent can trigger induction. When the concentration of the organic gas in the cavity of the column incubator or the case exceeds the alarm limit, the system alarms, and each module starts a liquid leakage protection mechanism.
As shown in fig. 3, the present invention further provides a double monitoring and alarming method for liquid leakage of a liquid chromatograph, which adopts a two-way real-time cruise monitoring mode according to the characteristics of two liquid leakage sensors to comprehensively monitor the space and time of the outside of the instrument, the inside of each module case and the column cavity of the column oven, thereby avoiding the invalidation of analysis data and the occurrence of safety accidents caused by the undetected liquid leakage, and comprises the following steps:
s1: a user sets a liquid leakage alarm threshold value, the workstation communicates with the CPU, and a recommended gas alarm threshold value is calculated;
s2: selecting a recommended gas alarm threshold or a user-defined gas alarm threshold as an organic gas alarm threshold of the current system;
s3: receiving current values of the organic gas sensor and the liquid contact type liquid leakage sensor, correspondingly comparing the current values with an organic gas alarm threshold value and a liquid leakage alarm threshold value of a current system, judging that the liquid leakage state exists when any one current value of the organic gas sensor and the liquid contact type liquid leakage sensor exceeds the corresponding threshold value, and otherwise, judging that the liquid leakage state does not exist;
s4: the workstation issues the current state information to each working module, and the CPU arranged in the working module combines the current liquid leakage alarm state information according to respective characteristics to complete internal processing: if the current state is a leakage state, starting a leakage alarm prompt and protection processing mechanism in each module; and if the current state is a non-leakage state, the alarm prompt is released, and the other modules are restored to the target state set by the user method except that the infusion pump module maintains the current state.
As an embodiment of the present invention, as shown in fig. 4, the process of acquiring the gas alarm threshold in step S1 is as follows:
s1.1: the CPU receives the method information of the workstation, extracts and identifies the organic solvent information;
s1.2: the CPU calls a built-in common organic solvent physical property table to extract the explosion limit of the currently used organic solvent;
s1.3: and calling a built-in common organic solvent gas concentration-response value relation curve library by the CPU, and circularly comparing and calculating by adopting an interpolation method to obtain a system recommended gas alarm threshold value corresponding to the current organic solvent explosion lower limit.
For gas alarm, a sensor with higher sensitivity to organic solvents commonly used in liquid chromatography is selected first. Generally, a sensor element sensitive to organic gases with conductivity, such as a tin dioxide (SnO 2) sensor, can be selected, which has a lower conductivity in clean air, and a significantly increased conductivity when organic gas components are present, and which increases with increasing concentration of organic components.
In actual control, a system CPU firstly receives mobile phase information issued by a workstation to obtain the information of the organic solvent in current system operation. Then, a common organic solvent physical property table built in the program is called, and the explosion limit information of the current organic solvent is extracted. The present invention program currently contains, but is not limited to, the following organic solvent physicochemical information: methanol, acetonitrile, n-hexane, cyclohexane, tetrahydrofuran, isopropanol, n-propanol, etc. And then calling a corresponding curve in a built-in relation curve library of response values of the common organic solvent and the gas concentration of the common organic solvent by the CPU, and circularly comparing and calculating by adopting an interpolation method to obtain a system recommended gas alarm threshold value corresponding to the current organic solvent explosion lower limit. The present invention is based on experimental data and the currently built-in curves include, but are not limited to, the following organic solvents: methanol, acetonitrile, n-hexane, cyclohexane, tetrahydrofuran, isopropanol, n-propanol, etc.
As an embodiment of the present invention, as shown in fig. 3, the specific process of step S2 is:
s2.1: prompting a user by the workstation whether to define a gas alarm threshold value by the user, wherein if the gas alarm threshold value is defined by the user, and if the gas alarm threshold value is not defined as the organic gas alarm threshold value of the current system;
s2.2: and judging whether the self-defined gas alarm threshold is lower than the recommended gas alarm threshold or not by the workstation, if so, defining the self-defined gas alarm threshold as the organic gas alarm threshold of the current system, otherwise, prompting a user that the self-defined threshold is not more than a system calculated value, and prompting the user to reset the self-defined alarm threshold.
As an embodiment of the present invention, the operation module in step S4 includes an auto sampler, a column oven, and a detector; and the infusion pump module is used for stopping infusion of the infusion pump when liquid leakage is confirmed and waiting for follow-up examination. The CPU control logic for the infusion pump, autosampler, column oven and detector is shown in fig. 5-8.
As an embodiment of the utility model, the system repeatedly executes the processes of S1-S4 at short time intervals delta t, generally tens of milliseconds, to ensure the real-time monitoring effect, and the judgment logics of the working module and the infusion pump module adopt double judgment logics, after the CPU issues a command to close the functional component or stop the module from running, the workstation automatically executes the judgment logics once again to complete the processing.
No matter the current value of the liquid leakage sensor or the gas sensor exceeds a set threshold value, the leakage monitoring and alarm master control logic judges that leakage exists in the current system, at the moment, the workstation sends real-time alarm information to each module CPU and an infusion pump CPU (when leakage occurs, the infusion pump should stop infusion at first and wait for follow-up investigation), each module CPU starts a ventilation system according to respective characteristics, and gas containing organic steam is replaced at the first time to complete internal judgment and processing. In the processing mechanism, the utility model adopts double closed loop judgment logic, namely, after the CPU issues a command to close the functional part or stop the module from running, the system automatically executes once more to confirm and finally completes the processing.
And according to the real-time monitoring data, when the current state is judged to be a non-leakage state, the alarm prompt of each module is released, the infusion pump module maintains the current state, and the rest modules are restored to the target state set by a user method, such as temperature control of the column oven, light source state of the detector and the like.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the present invention in its spirit and scope. Are intended to be covered by the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A leakage double monitoring alarm protection system for a liquid chromatograph is characterized by structurally comprising a column cavity of a column temperature box module, an infusion pump module, an automatic sample injector module, a column temperature box module and a chassis of a detector module; at least one organic gas leakage sensor is arranged in a column cavity of the column incubator; the device comprises an infusion pump module, an automatic sample injector module, a column temperature box module and a detector module, wherein a ventilation system is arranged in a case of at least one of the infusion pump module, the automatic sample injector module, the column temperature box module and the detector module, a first mounting area for mounting a circuit control part and a second mounting area for mounting a flow path part are arranged in the case, a leakage collector and a liquid contact type leakage sensor are sequentially arranged outside the case, the leakage collector is arranged below the flow path part of the second mounting area, leakage drainage grooves are formed in the surfaces below all the flow path parts where the leakage collector is located, the liquid contact type leakage sensor is arranged at a liquid collection position, and at least one organic gas leakage sensor is further arranged at the separation position of the first mounting area and the second mounting area; the double monitoring is that the organic gas leakage sensor and the liquid contact type leakage sensor respectively carry out double detection monitoring on the leaked organic vapor and the leaked organic liquid.
2. The double monitoring and alarm system for liquid leakage of liquid chromatograph of claim 1, wherein the column cavity of said column oven is a temperature controlled area for installing chromatographic column; the ventilation system of the case consists of an air inlet, an air outlet and a power fan and is used for replacing air in the case.
3. The double monitoring and alarm system for liquid leakage of liquid chromatograph of claim 1, wherein said circuit control components comprise a power supply, a circuit board, a component controller; the flow path component comprises a mixer, a damper, a pump body, a tee joint, a pipeline and a pipeline joint, and the pipeline joint are arranged outside the case; the leakage collector is made of organic solvent resistant materials, and the upper plane of the leakage collector is provided with a fluid guide slope.
4. The dual monitoring and alarming system for liquid leakage of liquid chromatograph of claim 1, wherein said liquid contact type leakage sensor uses thermistor as sensing element, and adopts dual-path thermistor reference detection mode, and a bridge detection voltage amplifying circuit with temperature compensation is arranged in the supporting circuit of said liquid contact type leakage sensor, and said bridge detection voltage amplifying circuit includes operational amplifier and AD converter.
5. The dual monitoring and alarm system for liquid chromatograph leakage of claim 1, wherein said organic gas leakage sensor comprises a semiconductor type, a solid electrolyte type, an electrochemical type, said semiconductor type employing a sensing element whose conductivity is sensitive to organic gases.
6. A double-monitoring alarm protection method for leakage of a liquid chromatograph, based on the double-monitoring alarm protection system for leakage of a liquid chromatograph described in the above claims 1-5, comprising a system CPU, each working module CPU, a workstation, a liquid contact leakage sensor, an organic gas leakage sensor, and a chassis ventilation system, and cooperatively completing real-time leakage monitoring and protection of the liquid chromatograph according to a certain control mode, characterized by comprising the steps of:
s1: after the system is started, a user sets a liquid leakage alarm threshold value, the workstation is communicated with the CPU, and a recommended gas alarm threshold value is calculated;
s2: selecting a recommended gas alarm threshold or a user-defined gas alarm threshold as an organic gas alarm threshold of the current system;
s3: receiving current values of the organic gas sensor and the liquid contact type liquid leakage sensor, correspondingly comparing the current values with an organic gas alarm threshold value and a liquid leakage alarm threshold value of a current system, judging that the liquid leakage state exists when any one current value of the organic gas sensor and the liquid contact type liquid leakage sensor exceeds the corresponding threshold value, and otherwise, judging that the liquid leakage state does not exist;
s4: the workstation issues the current state information to each working module, and the CPU arranged in the working module combines the current liquid leakage alarm state information according to respective characteristics to complete internal processing: if the current state is a leakage state, starting a leakage alarm prompt and protection processing mechanism in each module; and if the current state is a non-leakage state, the alarm prompt is released, and the other modules are restored to the target state set by the user method except that the infusion pump module maintains the current state.
7. The double monitoring and alarming method for liquid leakage of liquid chromatograph of claim 6, wherein the process of obtaining the gas alarm threshold in step S1 is:
s1.1: the CPU receives the method information of the workstation, extracts and identifies the organic solvent information;
s1.2: the CPU calls a built-in common organic solvent physical property table to extract the explosion limit of the currently used organic solvent;
s1.3: and calling a built-in common organic solvent gas concentration-response value relation curve library by the CPU, and circularly comparing and calculating by adopting an interpolation method to obtain a system recommended gas alarm threshold value corresponding to the current organic solvent explosion lower limit.
8. The double monitoring and alarming method for liquid leakage of liquid chromatograph of claim 6, wherein the specific process of step S2 is as follows:
s2.1: prompting a user by the workstation whether to define a gas alarm threshold value by the user, wherein if the gas alarm threshold value is defined by the user, and if the gas alarm threshold value is not defined as the organic gas alarm threshold value of the current system;
s2.2: and judging whether the self-defined gas alarm threshold is lower than the recommended gas alarm threshold or not by the workstation, if so, defining the self-defined gas alarm threshold as the organic gas alarm threshold of the current system, and otherwise, prompting the user to reset the self-defined gas alarm threshold.
9. The double monitoring alarm method for liquid leakage of liquid chromatograph of claim 6, wherein the operation modules in step S4 include an auto-injector, a column oven and a detector; the infusion pump module is an infusion pump, and the infusion pump stops infusion immediately when liquid leakage is confirmed and waits for follow-up examination.
10. The double monitoring and alarming method for liquid leakage of liquid chromatograph of claim 6, wherein the process of S1-S4 is repeatedly executed every Δ t time interval, and the judgment logic of each of the operating module and the infusion pump module adopts double judgment logic, and after the CPU issues a command to shut down the function unit or stop the module from operating, the workstation automatically executes the judgment logic once again to complete the process.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110254353.4A CN112816610A (en) | 2021-03-09 | 2021-03-09 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
| CN2021102543534 | 2021-03-09 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114624377A true CN114624377A (en) | 2022-06-14 |
Family
ID=75863009
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110254353.4A Pending CN112816610A (en) | 2021-03-09 | 2021-03-09 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
| CN202210157760.8A Pending CN114624377A (en) | 2021-03-09 | 2022-02-21 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110254353.4A Pending CN112816610A (en) | 2021-03-09 | 2021-03-09 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN112816610A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112816610A (en) * | 2021-03-09 | 2021-05-18 | 浙江福立分析仪器股份有限公司 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
| CN114280207B (en) * | 2022-01-12 | 2023-03-24 | 上海天美科学仪器有限公司 | Structure capable of distinguishing leakage and condensate generation of vertical column box |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104865318A (en) * | 2014-02-20 | 2015-08-26 | 株式会社岛津制作所 | Liquid chromatograph and column oven for use therein |
| CN207964744U (en) * | 2018-03-16 | 2018-10-12 | 常州三泰科技有限公司 | Monitoring system for liquid chromatographic system |
| CN109185712A (en) * | 2018-09-28 | 2019-01-11 | 杭州若奇技术有限公司 | Gas leakage protects system and method |
| CN208366939U (en) * | 2018-04-23 | 2019-01-11 | 北京宝德仪器有限公司 | Flow Analyzer with leakage detection function |
| CN208921351U (en) * | 2018-10-24 | 2019-05-31 | 江苏峰工电气科技有限公司 | The leakage monitoring and warning note system of electrical equipment gas medium |
| CN110022659A (en) * | 2018-01-09 | 2019-07-16 | 中兴通讯股份有限公司 | A kind of means of defence and device of the liquid cooling leakage of communication apparatus |
| CN110274734A (en) * | 2018-03-14 | 2019-09-24 | 株式会社岛津制作所 | Apparatus for testing weeping, heater box and chromatographic analysis system |
| CN111564024A (en) * | 2020-05-25 | 2020-08-21 | 安徽复盛信息科技有限公司 | Automatic protection method and system based on dangerous gas monitoring alarm |
| CN112816610A (en) * | 2021-03-09 | 2021-05-18 | 浙江福立分析仪器股份有限公司 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
-
2021
- 2021-03-09 CN CN202110254353.4A patent/CN112816610A/en active Pending
-
2022
- 2022-02-21 CN CN202210157760.8A patent/CN114624377A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104865318A (en) * | 2014-02-20 | 2015-08-26 | 株式会社岛津制作所 | Liquid chromatograph and column oven for use therein |
| CN110022659A (en) * | 2018-01-09 | 2019-07-16 | 中兴通讯股份有限公司 | A kind of means of defence and device of the liquid cooling leakage of communication apparatus |
| CN110274734A (en) * | 2018-03-14 | 2019-09-24 | 株式会社岛津制作所 | Apparatus for testing weeping, heater box and chromatographic analysis system |
| CN207964744U (en) * | 2018-03-16 | 2018-10-12 | 常州三泰科技有限公司 | Monitoring system for liquid chromatographic system |
| CN208366939U (en) * | 2018-04-23 | 2019-01-11 | 北京宝德仪器有限公司 | Flow Analyzer with leakage detection function |
| CN109185712A (en) * | 2018-09-28 | 2019-01-11 | 杭州若奇技术有限公司 | Gas leakage protects system and method |
| CN208921351U (en) * | 2018-10-24 | 2019-05-31 | 江苏峰工电气科技有限公司 | The leakage monitoring and warning note system of electrical equipment gas medium |
| CN111564024A (en) * | 2020-05-25 | 2020-08-21 | 安徽复盛信息科技有限公司 | Automatic protection method and system based on dangerous gas monitoring alarm |
| CN112816610A (en) * | 2021-03-09 | 2021-05-18 | 浙江福立分析仪器股份有限公司 | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112816610A (en) | 2021-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114624377A (en) | Liquid leakage double-monitoring alarm protection system and method for liquid chromatograph | |
| JP5379371B2 (en) | Gas detection system and detection method | |
| CN101666784B (en) | Chromatographic instrument calibration device | |
| US6042634A (en) | Moisture extractor system for gas sampling | |
| US9518961B2 (en) | Liquid chromatograph and column oven used therefor | |
| KR101793797B1 (en) | Method and device for measuring the gas content in a liquid, and use of such a device | |
| US20180306682A1 (en) | Smart pump for a portable gas detection instrument | |
| CN108646286A (en) | A kind of reference unit and method of continuous reliable regulation and control precipitation rate of radon | |
| US20040142481A1 (en) | Foam detection/prevention in the context of a purge and trap sample concentrator | |
| CN106880962A (en) | A kind of Portable oil-gas separator | |
| CN112461458A (en) | Helium concentration detection control device for helium mass spectrometer leak detection test system | |
| CN204228687U (en) | A kind of gas analysis sensor | |
| TWI657887B (en) | ALL-IN-ONE VOCs MEASUREMENT INSTRUMENT | |
| JP3178392U (en) | Gas analyzer | |
| JP3446431B2 (en) | Liquid chromatograph | |
| JP2777304B2 (en) | Abnormality diagnosis apparatus and diagnosis method for perfluorocarbon input device | |
| CN111896592B (en) | Controllable jet sensor device and calibration method and system thereof | |
| CN221426605U (en) | Multi-functional smell appearance | |
| CN206557174U (en) | A kind of no carrier gas oil chromatography on-line monitoring system | |
| CN115684503B (en) | Resin VOC detects board for coating with prevent external disturbance | |
| JPH04198861A (en) | Gas chromatograph | |
| JPH06300887A (en) | Failed fuel detector | |
| CN216899000U (en) | Plunger pump cooling monitoring system | |
| CN208847361U (en) | Temperature measures component | |
| CN209559833U (en) | Gas chromatograph easy to remove |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220614 |