CN202676680U - Device capable of detecting low-concentration freon in seawater - Google Patents

Device capable of detecting low-concentration freon in seawater Download PDF

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CN202676680U
CN202676680U CN 201220340704 CN201220340704U CN202676680U CN 202676680 U CN202676680 U CN 202676680U CN 201220340704 CN201220340704 CN 201220340704 CN 201220340704 U CN201220340704 U CN 201220340704U CN 202676680 U CN202676680 U CN 202676680U
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interface
gas
valve
solenoid valve
way
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郑晓玲
何鹰
王保栋
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First Institute of Oceanography SOA
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First Institute of Oceanography SOA
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Abstract

The utility model provides a device capable of detecting low-concentration freon in seawater. The device capable of detecting the low-concentration freon in the seawater comprises an air lifting component, a trapping desorbing component, a chromatographic detecting component, a system control component, and an air supply component, wherein the air lifting component is provided with a blowing pipe, a water-air separator, a first three-way magnetic valve and a second three-way magnetic valve. The trapping desorbing component is provided with a trapping desorbing room, a trapping pipe, a high-temperature liquid pool, a heater, a low-temperature liquid pool, a refrigerator, a third three-way magnetic valve, a fourth three-way magnetic valve, a fifth three-way magnetic valve, a sixth three-way magnetic valve, a seventh three-way magnetic valve, a eighth three-way magnetic valve, a first micropump and a second micropump. The chromatographic detecting component is provided with a gas chromatograph and a computer. The system control component is provided with a first six-way valve, a second six-way valve and a programmable logic controller (PLC). The air supply component is provided with blowing gas, high-purity carrier gas and standard gas. The device capable of detecting the low-concentration freon in the seawater has the advantages that a chemical reagent is not required, pollution does not exist, detection is accurate, and automatic operation of the detecting process is achieved, and cost is saved. Meanwhile, the device capable of detecting the low-concentration freon in the seawater is especially suitable for freon detection for far-reaching survey ships or scientific research ships, and real-time, online and continuous monitoring is conducted for a long time.

Description

Low dose fluoride Leon device in a kind of detection seawater
Technical field
The utility model relates to the ocean monitoring technologytechnologies field, relates in particular to low dose fluoride Leon device in a kind of detection seawater, specifically a kind of far-reaching extra large freon chemical tracing technology, device of the Leon enrichment of realization Trace Fluoride, testing process of being applied to.
Background technology
Freon is also referred to as fluorochlorohydrocarbon (CFCs), be several fluorine methyl chlorides and the fluorine chloric ethane of being made by the mankind fully, modal is fluoro trichloromethane (CFC-11), difluorodichloromethane (CFC-12), trifluorotrichloroethane (CFC-113).They at room temperature are gas or volatile liquid, stable chemical nature, and flammable the and utmost point hypotoxicity of tool is not extensive for commercial applications.Just point out that as far back as Molina in 1974 and Rowland freon destroys the mechanism of ozone, Farman in 1985 with more strong digital proof the former theoretical correctness, cause thus human environment and the increasingly extensive concern of health problem that freon is caused.
Because the chemical inertness of freon, its destruction is long-term.On the other hand, scientist finds that freon stability can be applied to chemical tracing, is the effective tool of the water body motion of research ocean and the exchange of extra large gas.Lovelock proposed freon first as inertia tracer research ocean water body in 1973, based on the eighties in 20th century of global ocean Loop experiment (World Ocean Circulation Experiment) so far, the Marine Sciences In International man is by setting up the analytical approach of freon in the seawater, accumulated freon a large amount of observational data in ocean and the atmosphere, and be applied to ocean circulation, sea gas exchange, the tracer study of mixed process, the freon chemical tracing has become a kind of ocean tracer technique that has using value, but the correlative study report is very few at home.Therefore, in order to improve China's thalassochemistry tracer technique, catch up with and surpass world ocean power, it is great to carry out the far-reaching extra large freon chemical tracing Research Significance of boat-carrying, and each component concentration of freon is its important prerequisite that is applied to tracer technique in the seawater and detect fast, accurately, quantitatively.
External freon spike detects and mainly depends on boat-carrying gas chromatography-electron capture detection (GC-ECD) system, transports the laboratory, land back after part scientific worker seals sample collection and analyzes mensuration.Electron capture detector (ECD) is highly sensitive, selectivity good, the range of linearity is narrow, but the seawater sample matrix is complicated, though higher boiling or strong polar impurity are low-response in chromatogram, but the high several orders of magnitude of its concentration ratio freon detected components, a large amount of strong polar impurities enter the ECD pond, be adsorbed on paper tinsel surface, ECD pond, cause the detector performance degradation, especially electron capture detector has the Ni radioactive source, aboard ship use, maintenance is very inconvenient in the laboratory that special maintenance prevention need to be arranged.The all previous marine scientific investigation activity of China does not all have the gas chromatograph of boat-carrying electron capture detector, so is not suitable for China's marine boat-carrying investigation use.
The content of freon is very low in the ocean, as the concentration of far-reaching extra large CFC-11 about 1pmol/kg, utilize existing instrument and equipment all can not directly measure it, no matter be the boat-carrying on-the site analysis, or the laboratory, land is detected, sample all must be through enrichment, and enrichment method commonly used has: solid-phase microextraction, liquid-liquid extraction method, Static Headspace method, molecular sieve adsorption concentration method, air lift cold trap trapping method etc.More than each method need loaded down with trivial details treatment step, sample composition is complicated, operating cost is large, detection time is long, greatly impact analysis speed and accuracy, and be difficult to realize on a large scale, the automatic monitoring of continuous real-time online.
Summary of the invention
The purpose of this utility model is to solve present domestic prior art and design concept defective and deficiency in the field, according to the later development proposition of Modern Analytical Chemistry and instrumental analysis.The technical scheme that its technical matters that solves the utility model adopts is: adopt high-purity carrier gas that volatility freon is purged air lift from seawater sample, through cryogenic trapping, make the concentration of freon obtain enrichment, after finishing, capture makes its desorb by being rapidly heated, being pushed gas-phase chromatographic capillary column by high-purity carrier gas separates, adopt each component concentration of electrolytic conductivity detector (ELCD) detection of freon, thereby realize the detection to low dose fluoride Leon in the far-reaching seawater.The utility model utilization purges the technology components such as air lift, cryogenic trapping, desorption under high temperature, gas chromatography separation, electrolytic conductance detection and automatic control system, form the pick-up unit of the system integration, measurement result is reliable and stable, can long-time continuous operation in the scientific investigation in far-reaching sea and investigation.
The purpose of this utility model is realized by following technical scheme, developed low dose fluoride Leon device in a kind of detection seawater, this device is to be made of air lift assembly, capture desorb assembly, chromatogram detection components, system's Control Component, gas supply assembly, and it is characterized in that: the air lift assembly arranges scavenging duct 1-1, moisture separator 1-2, the first three-way solenoid valve 1-3, the second three-way solenoid valve 1-4; Capture the desorb assembly capture desorption chamber 2-1, trap tube 2-2, high temperature liquid pool 2-11, well heater 2-12, low temperature liquid pool 2-13, refrigerator 2-14, the 3rd three-way solenoid valve 2-4, the 4th three-way solenoid valve 2-5, the 5th three-way solenoid valve 2-6, the 6th three-way solenoid valve 2-7, the 7th three-way solenoid valve 2-9, the 8th three-way solenoid valve 2-10 and the first micropump 2-3, the second micropump 2-8 are set; The chromatogram detection components arranges gas chromatograph 3-1, computing machine 3-2; System's Control Component arranges the first six-way valve 4-1, the second six-way valve 4-2, PLC plc 4-3; Gas supply assembly arranges sweep gas 5-1, high-purity carrier gas 5-2, Standard Gases 5-3.
Described scavenging duct 1-1 is a withstand voltage horminess glass tube, the upper end is provided with injection port, the core glass sheet is arranged at the bottom, the lower end is import, the top is outlet, connect with teflon seal respectively, the center is provided with teflon hose, the import of scavenging duct lower end is connected with the second three-way solenoid valve 1-4, top exit and moisture separator 1-2 entrance in succession, moisture separator 1-2 outlet is connected with the first three-way solenoid valve 1-3 entrance, the first three-way solenoid valve 1-3 controls the activation of moisture separator and entering of sample gas, an outlet is connected with the first six-way valve 4-1 interface III3a, another outlet water pipe emptying of running in; Moisture separator 1-2 is designed to the stainless steel rectangular parallelepiped, be provided with heating member and temperature controller outward, in the aqueous vapor separator tube is arranged, fill dehydrated adsorbent in the pipe, the second three-way solenoid valve 1-4 control sweep gas enter discharging with seawater sample, lower interface is connected with sweep gas 5-1, and side interface is that water sample is emptying.
Trap tube 2-2 is installed in the described capture desorption chamber 2-1, fill adsorbent in the pipe, the entrance of trap tube 2-2 is connected with the second six-way valve 4-2 the second interface 2b, outlet is connected with the second six-way valve 4-2 the 5th interface 5b, and the capture low temperature, the desorb high temperature that capture desorption chamber 2-1 are provided by the heat-conducting medium dimethyl silicon oil in low temperature liquid pool, the high temperature liquid pool respectively.
Capillary separation column and electrolytic conductivity detector are installed in the described gas chromatograph 3-1, gas chromatograph 3-1 entrance is connected with the second six-way valve 4-2 the 4th interface 4b, sample gas from the sucking-off of trap tube solution, emptying behind capillary separation column, electrolytic conductivity detector respectively under the promotion of carrier gas, computing machine 3-2 control chromatographic signal sampling, calculating.
Conversion between described six-way valve 4-1 Quality control sample introduction and the calibrate is provided with six interface two states, and the sample introduction state is that interface I 1a and interface II2a are logical, interface III3a is logical with interface IV4a, interface V5a and interface VI6a lead to; The demarcation state is that interface I1a and interface VI6a are logical, interface II2a is logical with interface III3a, interface IV4a and interface V5a lead to; The connected mode of six interfaces: interface I1a is that floss hole is connected with conduit, interface II2a is connected with interface V 5a by quantity tube, interface III interface 3a is connected with the first three-way solenoid valve 1-3, connection interface IV mouth 4a is connected with the second six-way valve 4-2 first interface 1b, and interface VI6a is connected with Standard Gases 5-3; The second six-way valve 4-2 Quality control capture with measure between conversion, be provided with six interface two states, the capture state is that first interface 1b is logical with the second interface 2b, the 3rd interface 3b and the 4th interface 4b leads to, the 5th interface 5b and the 6th interface 6b lead to; The mensuration state is that first interface 1b and land interface 6b are logical, the second interface 2b is logical with the 3rd interface 3b, the 4th interface 4b and the 5th interface 5b lead to; The connected mode of six interfaces: first interface 1b is connected with the first six-way valve 4-1 interface IV4a, the second interface 2b is connected with trap tube 2-2 entrance, the 3rd interface 3b is connected with high-purity carrier gas 5-2, the 4th interface 4b is connected with gas chromatograph 3-1 gas circuit entrance, the 5th interface 5b is connected with trap tube 2-2 outlet, and the 6th interface 6b is that floss hole is connected with conduit.
Described sweep gas 5-1 is connected with the second three-way solenoid valve 1-4 through reduction valve, purification pipe, flow regulator; High-purity carrier gas 5-2 is connected with the second six-way valve 4-2 the 3rd interface 3b through reduction valve, purification pipe, flow regulator; Standard Gases 5-3 is connected with the first six-way valve 4-1 the 6th interface 6a through reduction valve, purification pipe, flow regulator.
Characteristics of the present utility model and beneficial effect are: this device need not any chemical reagent, can not cause secondary pollution to environment and water body, testing process quick and precisely, favorable reproducibility, the result is reliable and stable, can realize the testing process automatic operating, save a large amount of manpower and materials costs, be suitable for the detection of freon concentration in the various water bodys, be particularly suitable for far-reaching sea investigation boats and ships or scientific investigation ship and carry out the needs that freon detects, and can be for a long time in real time, online, continuous monitoring, comprehensive, extensibility is strong, suitablely extensively promote.
Description of drawings
Fig. 1 is the utility model flowage structure synoptic diagram.
Embodiment
Referring to Fig. 1, the utility model has been developed low dose fluoride Leon device in a kind of detection seawater, takes following steps:
Low dose fluoride Leon device in a kind of detection seawater, this device is to be made of air lift assembly, capture desorb assembly, chromatogram detection components, system's Control Component, gas supply assembly, and it is characterized in that: the air lift assembly arranges scavenging duct 1-1, moisture separator 1-2, the first three-way solenoid valve 1-3, the second three-way solenoid valve 1-4; Capture the desorb assembly capture desorption chamber 2-1, trap tube 2-2, high temperature liquid pool 2-11, well heater 2-12, low temperature liquid pool 2-13, refrigerator 2-14, the 3rd three-way solenoid valve 2-4, the 4th three-way solenoid valve 2-5, the 5th three-way solenoid valve 2-6, the 6th three-way solenoid valve 2-7, the 7th three-way solenoid valve 2-9, the 8th three-way solenoid valve 2-10 and the first micropump 2-3, the second micropump 2-8 are set; The chromatogram detection components arranges gas chromatograph 3-1, computing machine 3-2; System's Control Component arranges the first six-way valve 4-1, the second six-way valve 4-2, PLC plc 4-3; Gas supply assembly arranges sweep gas 5-1, high-purity carrier gas 5-2, Standard Gases 5-3.
Described scavenging duct 1-1 is a withstand voltage horminess glass tube, the upper end is provided with injection port, the core glass sheet is arranged at the bottom, the lower end is import, the top is outlet, connect with teflon seal respectively, the center is provided with teflon hose, the import of scavenging duct lower end is connected with the second three-way solenoid valve 1-4, top exit and moisture separator 1-2 entrance in succession, moisture separator 1-2 outlet is connected with the first three-way solenoid valve 1-3 entrance, the first three-way solenoid valve 1-3 controls the activation of moisture separator and entering of sample gas, an outlet is connected with the first six-way valve 4-1 interface III3a, another outlet water pipe emptying of running in; Moisture separator 1-2 is designed to the stainless steel rectangular parallelepiped, be provided with heating member and temperature controller outward, in the aqueous vapor separator tube is arranged, fill dehydrated adsorbent in the pipe, the second three-way solenoid valve 1-4 control sweep gas enter discharging with seawater sample, lower interface is connected with sweep gas 5-1, and side interface is that water sample is emptying.
Trap tube 2-2 is installed in the described capture desorption chamber 2-1, fill adsorbent in the pipe, the entrance of trap tube 2-2 is connected with the second six-way valve 4-2 the second interface 2b, outlet is connected with the second six-way valve 4-2 the 5th interface 5b, and the capture low temperature, the desorb high temperature that capture desorption chamber 2-1 are provided by the heat-conducting medium dimethyl silicon oil in low temperature liquid pool, the high temperature liquid pool respectively.
Capillary separation column and electrolytic conductivity detector are installed in the described gas chromatograph 3-1, gas chromatograph 3-1 entrance is connected with the second six-way valve 4-2 the 4th interface 4b, sample gas from the sucking-off of trap tube solution, emptying behind capillary separation column, electrolytic conductivity detector respectively under the promotion of carrier gas, computing machine 3-2 control chromatographic signal sampling, calculating.
Conversion between described six-way valve 4-1 Quality control sample introduction and the calibrate is provided with six interface two states, and the sample introduction state is that interface I1a and interface II2a are logical, interface III3a is logical with interface IV4a, interface V5a and interface VI6a lead to; The demarcation state is that interface I1a and interface VI6a are logical, interface II2a is logical with interface III3a, interface IV4a and interface V5a lead to; The connected mode of six interfaces: interface I1a is that floss hole is connected with conduit, interface II2a is connected with interface V 5a by quantity tube, interface III interface 3a is connected with the first three-way solenoid valve 1-3, connection interface IV mouth 4a is connected with the second six-way valve 4-2 first interface 1b, and interface VI6a is connected with Standard Gases 5-3; The second six-way valve 4-2 Quality control capture with measure between conversion, be provided with six interface two states, the capture state is that first interface 1b is logical with the second interface 2b, the 3rd interface 3b and the 4th interface 4b leads to, the 5th interface 5b and the 6th interface 6b lead to; The mensuration state is that first interface 1b and land interface 6b are logical, the second interface 2b is logical with the 3rd interface 3b, the 4th interface 4b and the 5th interface 5b lead to; The connected mode of six interfaces: first interface 1b is connected with the first six-way valve 4-1 interface IV4a, the second interface 2b is connected with trap tube 2-2 entrance, the 3rd interface 3b is connected with high-purity carrier gas 5-2, the 4th interface 4b is connected with gas chromatograph 3-1 gas circuit entrance, the 5th interface 5b is connected with trap tube 2-2 outlet, and the 6th interface 6b is that floss hole is connected with conduit.
Described sweep gas 5-1 is connected with the second three-way solenoid valve 1-4 through reduction valve, purification pipe, flow regulator; High-purity carrier gas 5-2 is connected with the second six-way valve 4-2 the 3rd interface 3b through reduction valve, purification pipe, flow regulator; Standard Gases 5-3 is connected with the first six-way valve 4-1 the 6th interface 6a through reduction valve, purification pipe, flow regulator.
Each assembly specific requirement and detection principle are as follows in the utility model:
The air lift assembly is mainly finished the gas extraction task of freon in the seawater, because freon concentration is very low in the seawater, need a certain amount of seawater sample, could obtain the freon sample of enough concentration, because freon has good volatility, can be blown out by the gas of continuous flow again.Therefore, the air lift component design is the horminess glass tube of a straight shape, the bottom is lined with the core glass sheet, but the seawater sample of splendid attire certain volume in the pipe, when high-purity sweep gas produces a large amount of bubbles during by the core glass sheet, freon in the water sample is purged out, enter moisture separator, dehydrated dose of absorption of water vapor wherein, freon enters the capture resolution component under the promotion of carrier gas.When the dehydrated adsorbent in the moisture separator reaches capacity, make moisture separator rise to uniform temperature by temperature controller, the aqueous vapor in the adsorbent is removed and regenerate, the water that removes is by the outlet discharging of three-way solenoid valve.Make the volatile sulfur compounds gas stripping efficiency reach optimum condition by adjusting carrier gas flux, flow velocity, purge time.After each mensuration finished, the seawater in the scavenging duct was discharged by the switching three-way solenoid valve.
The major function that captures the desorb assembly is to make the freon from the air lift assembly obtain enrichment and desorb.Adopt semiconductor cooler as the refrigeration source of low temperature liquid pool, thermal resistor is as the heating source of high temperature liquid pool.In capturing desorption chamber trap tube is installed, inserts adsorbent in the pipe, so that freon is adsorbed in the trap tube at low temperatures, reach the enrichment purpose, the temperature by regulating the low temperature liquid pool, sweep gas flow velocity, capture time are to obtain the best effect that captures.Must be through thermal desorption ability so that sample be finally detected after capture is finished, the medium of high temperature liquid pool flows into and captures desorption chamber during desorb, freon desorb from trap tube is discharged, and high-purity carrier gas is carried sample gas and is entered gas-phase chromatographic capillary column and separate.
The major function of gas chromatographic detection assembly is to finish the separation and detection task of freon.Contain multiple freon compound in the seawater, wherein some compound property is close, the common separation post can not separate these compounds fully, the electrolytic conductivity detector that utilization of the present invention has a high selectivity to halogen detects the concentration of freon in the seawater, select a kind of separating column that freon is had the good separation performance, can finish separation and detection to multiple freon in the seawater.By means of chromatographic work station, can finish qualitative, the quantitative evaluation work to freon.
The major function of system's Control Component is the robotization control of implement device flow process.This system component mainly is comprised of three-way solenoid valve, six-way valve, flow regulator, temperature controller, PLC Programmable Logic Controller, computing machine etc.Three-way solenoid valve is mainly used in controlling entering and discharging of liquids and gases, and the switching of carrier flow direction in high temperature liquid pool and the low temperature liquid pool; Six-way valve is mainly used in the conversion between Quality control sample introduction, calibrate, sample capture and the mensuration; Flow regulator can be regulated and the flow of controlling gas and flow velocity; The PLC plc can the regulating and controlling three-way solenoid valve, the handoff functionality of six-way valve, sends operating instruction, computer realization good in interactive function can also for temperature controller, flow regulator.
Gas supply assembly is mainly realized supply, conversion and the flow regulation of gas.Sweep gas is mainly used in the purging of the freon in the scavenging duct is taken out of, and will send into trap tube.High-purity gas carrier is mainly used in the flowing carrier of desorb, chromatographic resolution and the detection of freon sample.Standard Gases is the freon standard mixture of Known Species, concentration, is used for qualitative, quantitative and standard working curve drafting and demarcation.
The utility model groundwork program is as follows:
Initialize routine 1: make all three-way solenoid valves be in normally off, open three-way solenoid valve, start micropump, air is under the effect of micropump, enter the capture desorption chamber along three-way solenoid valve, the cryogenic media that air will capture in the desorption chamber pushes back the low temperature liquid pool along three-way solenoid valve, and unnecessary air is discharged from the pore at low temperature liquid pool 3 tops, closes micropump 2-3.
Initialize routine 2: make all three-way solenoid valves be in normally off, open three-way solenoid valve, start micropump, air is under the effect of micropump, enter the capture desorption chamber along three-way solenoid valve, the high-temperature medium that air will capture in the desorption chamber pushes back the high temperature liquid pool along T-valve, and unnecessary air is discharged from high temperature liquid pool top pore, closes micropump.
Capture desorption chamber low-temperature working program: after finishing initialize routine 1, make all three-way solenoid valves be in normally off; Start micropump, heat-conducting medium is extracted out from the low temperature liquid pool, enters the capture desorption chamber along three-way solenoid valve, micropump, three-way solenoid valve, and after being full of whole capture desorption chamber, flows back to the low temperature liquid pool through three-way solenoid valve successively.
Capture desorption chamber hot operation program: after finishing initialize routine 2, make all three-way solenoid valves be in normally off; Open three-way solenoid valve, start micropump, heat-conducting medium is extracted out from the high temperature liquid pool, enters the capture desorption chamber along T-valve, micropump, three-way solenoid valve, be full of whole capture desorption chamber after, flow back to the high temperature liquid pool through three-way solenoid valve successively.
The concrete detection method of the utility model is as follows:
1, instrumental calibration
Arrange respectively: sweep gas 100mL/min, carrier gas 40mL/min, freon gas 30mL/min, quantity tube volume 0.5mL captures temperature-20 ℃, captures time 5min, and 200 ℃ of resolution temperatures are resolved time 3min.Select " standard test " button, at this moment, six-way valve is in the sample introduction state, six-way valve is in the capture state, Standard Gases is interfaced to emptying along six-way valve, calibrating gas is full of quantity tube, behind the 3min, six-way valve is the demarcation state, sweep gas enters trap tube and captures along three-way solenoid valve, scavenging duct, moisture separator, three-way solenoid valve, six-way valve interface, six-way valve interface, this process sweep gas is written into trap tube with the freon gas in the quantity tube, and the sweep gas of collection at large is then emptying behind the six-way valve interface.5min captures and finishes, the autoshutdown Standard Gases, six-way valve still is the demarcation state, six-way valve switches to the mensuration state, at this moment, captures 200 ℃ of the resolution temperatures that the Resolution Room temperature rises to setting, behind the 3min, high-purity carrier gas along the six-way valve interface enter trap tube, six-way valve is interfaced to the gas chromatograph entrance, high-purity carrier gas pushes gas chromatograph with the freon that parses and detects through the switching of six-way valve.Computing machine chromatographic work station real-time rendering working curve.In " standard test " process, carried out synchronously by capture desorption chamber low-temperature working program, capture desorb hot operation program, initialize routine 1, the initialize routine 2 of PLC control.
According to the said determination process, adopt the freon gas of variable concentrations to capture-resolve-to measure, can draw the freon standard working curve.
2, sample determination
Arrange respectively: sweep gas 100mL/min, carrier gas 40mL/min captures temperature-20 ℃, captures time 10min, and 200 ℃ of resolution temperatures are resolved time 3min.The seawater of certain volume injects scavenging duct from injection port.
Select " sample determination " button, six-way valve is in the sample introduction state, and six-way valve is in the capture state.At this moment, sweep gas enters trap tube along three-way solenoid valve, scavenging duct, moisture separator, three-way solenoid valve, six-way valve interface six-way valve interface and captures (this process sweep gas is blown into trap tube with the freon in the scavenging duct seawater), and the sweep gas of collection at large is then emptying behind the six-way valve interface.10min captures and finishes autoshutdown sweep gas, switching three-way solenoid valve, seawater is discharged from the three-way solenoid valve escape hole of scavenging duct bottom, after seawater drains, switch three-way valve, make sweep gas pass into scavenging duct, the heating water gas separating device makes water vapor discharge from the T-valve outlet simultaneously.Meanwhile, six-way valve switches to the demarcation state, six-way valve switches to the mensuration state, capture 200 ℃ of the resolution temperatures that the Resolution Room temperature rises to setting, behind the 3min, high-purity carrier gas along the six-way valve interface enter trap tube, six-way valve is interfaced to the gas chromatograph entrance, i.e. high-purity carrier gas pushes gas chromatograph with the freon that parses and detects through the switching of six-way valve.Computing machine chromatographic work station real-time rendering working curve.In " sample determination " process, carried out synchronously by capture desorption chamber low-temperature working program, capture desorption chamber hot operation program, initialize routine 1, the initialize routine 2 of PLC control.Can calculate the concentration of freon in the given volume seawater according to standard working curve.
In addition, the utility model and not meaning that by synoptic diagram and instructions limits to, and can change to some extent under the prerequisite that does not break away from design aim and principle thereof.

Claims (6)

1. one kind is detected low dose fluoride Leon device in the seawater, this device is to be made of air lift assembly, capture desorb assembly, chromatogram detection components, system's Control Component, gas supply assembly, and it is characterized in that: the air lift assembly arranges scavenging duct (1-1), moisture separator (1-2), the first three-way solenoid valve (1-3), the second three-way solenoid valve (1-4); Capture the desorb assembly capture desorption chamber (2-1) is set, trap tube (2-2), high temperature liquid pool (2-11), well heater (2-12), low temperature liquid pool (2-13), refrigerator (2-14), the 3rd three-way solenoid valve (2-4), the 4th three-way solenoid valve (2-5), the 5th three-way solenoid valve (2-6), the 6th three-way solenoid valve (2-7), the 7th three-way solenoid valve (2-9), the 8th three-way solenoid valve (2-10) and the first micropump (2-3), the second micropump (2-8); The chromatogram detection components arranges gas chromatograph (3-1), computing machine (3-2); System's Control Component arranges the first six-way valve (4-1), the second six-way valve (4-2), PLC plc (4-3); Gas supply assembly arranges sweep gas (5-1), high-purity carrier gas (5-2), Standard Gases (5-3).
2. low dose fluoride Leon device in the detection seawater according to claim 1, it is characterized in that: described scavenging duct (1-1) is a withstand voltage horminess glass tube, the upper end is provided with injection port, the core glass sheet is arranged at the bottom, the lower end is import, the top is outlet, connect with teflon seal respectively, the center is provided with teflon hose, the import of scavenging duct lower end is connected with the second three-way solenoid valve (1-4), top exit and moisture separator (1-2) entrance in succession, moisture separator (1-2) outlet is connected with the first three-way solenoid valve (1-3) entrance, the first three-way solenoid valve (1-3) control activation of moisture separator and entering of sample gas, an outlet is connected with the first six-way valve (4-1) interface III (3a), another outlet water pipe emptying of running in; Moisture separator (1-2) is designed to the stainless steel rectangular parallelepiped, be provided with heating member and temperature controller outward, in the aqueous vapor separator tube is arranged, fill dehydrated adsorbent in the pipe, the second three-way solenoid valve (1-4) control sweep gas enter discharging with seawater sample, lower interface is connected with sweep gas (5-1), and side interface is that water sample is emptying.
3. low dose fluoride Leon device in the detection seawater according to claim 1, it is characterized in that: trap tube (2-2) is installed in the described capture desorption chamber (2-1), fill adsorbent in the pipe, the entrance of trap tube (2-2) is connected with the second six-way valve (4-2) the second interface (2b), outlet is connected with the second six-way valve (4-2) the 5th interface (5b), and the capture low temperature, the desorb high temperature that capture desorption chamber (2-1) are provided by the heat-conducting medium dimethyl silicon oil in low temperature liquid pool, the high temperature liquid pool respectively.
4. low dose fluoride Leon device in the detection seawater according to claim 1, it is characterized in that: capillary separation column and electrolytic conductivity detector are installed in the described gas chromatograph (3-1), gas chromatograph (3-1) entrance is connected with the second six-way valve (4-2) the 4th interface (4b), sample gas from the sucking-off of trap tube solution, emptying behind capillary separation column, electrolytic conductivity detector respectively under the promotion of carrier gas, computing machine (3-2) control chromatographic signal sampling, calculating.
5. low dose fluoride Leon device in the detection seawater according to claim 1, it is characterized in that: the conversion between described six-way valve (4-1) Quality control sample introduction and the calibrate, be provided with six interface two states, the sample introduction state is that interface I (1a) is logical with interface II (2a), interface III (3a) is logical with interface IV (4a), interface V (5a) is logical with interface VI (6a); The demarcation state is that interface I (1a) is logical with interface VI (6a), interface II (2a) is logical with interface III (3a), interface IV (4a) is logical with interface V (5a); The connected mode of six interfaces: interface I (1a) is that floss hole is connected with conduit, interface II (2a) is connected with interface V (5a) by quantity tube, interface III interface (3a) is connected with the first three-way solenoid valve (1-3), connection interface IV mouth (4a) is connected with the second six-way valve (4-2) first interface (1b), and interface VI (6a) is connected with Standard Gases (5-3); Conversion between the second six-way valve (4-2) Quality control captures and measures, be provided with six interface two states, the capture state is that first interface (1b) is logical with the second interface (2b), the 3rd interface (3b) is logical with the 4th interface (4b), the 5th interface (5b) is logical with the 6th interface (6b); The mensuration state is that first interface (1b) is logical with land interface (6b), the second interface (2b) is logical with the 3rd interface (3b), the 4th interface (4b) is logical with the 5th interface (5b); The connected mode of six interfaces: first interface (1b) is connected with the first six-way valve (4-1) interface IV (4a), the second interface (2b) is connected with trap tube (2-2) entrance, the 3rd interface (3b) is connected with high-purity carrier gas (5-2), the 4th interface (4b) is connected with gas chromatograph (3-1) gas circuit entrance, the 5th interface (5b) is connected with trap tube (2-2) outlet, and the 6th interface (6b) is that floss hole is connected with conduit.
6. low dose fluoride Leon device in the detection seawater according to claim 1, it is characterized in that: described sweep gas (5-1) is connected with the second three-way solenoid valve (1-4) through reduction valve, purification pipe, flow regulator; High-purity carrier gas (5-2) is connected with the second six-way valve (4-2) the 3rd interface (3b) through reduction valve, purification pipe, flow regulator; Standard Gases (5-3) is connected with the first six-way valve (4-1) the 6th interface (6a) through reduction valve, purification pipe, flow regulator.
CN 201220340704 2012-07-07 2012-07-07 Device capable of detecting low-concentration freon in seawater Expired - Fee Related CN202676680U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102650623A (en) * 2011-02-28 2012-08-29 国家海洋局第一海洋研究所 Device for detection of low-concentration Freon in seawater and production method thereof
CN103808820A (en) * 2014-01-09 2014-05-21 中国人民解放军海军医学研究所 Freon gas detection warning device and detection method thereof
CN104215724A (en) * 2014-09-19 2014-12-17 北京大学 Constant temperature adsorption heat analyzer for atmospheric volatile organic compound measurement
CN110879281A (en) * 2018-09-05 2020-03-13 中国科学院地理科学与资源研究所 Method for determining age of underground water

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102650623A (en) * 2011-02-28 2012-08-29 国家海洋局第一海洋研究所 Device for detection of low-concentration Freon in seawater and production method thereof
CN103808820A (en) * 2014-01-09 2014-05-21 中国人民解放军海军医学研究所 Freon gas detection warning device and detection method thereof
CN104215724A (en) * 2014-09-19 2014-12-17 北京大学 Constant temperature adsorption heat analyzer for atmospheric volatile organic compound measurement
CN104215724B (en) * 2014-09-19 2015-07-22 北京大学 Constant temperature adsorption heat analyzer for atmospheric volatile organic compound measurement
CN110879281A (en) * 2018-09-05 2020-03-13 中国科学院地理科学与资源研究所 Method for determining age of underground water

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