CN202814873U - Detector for volatile sulphides in surface seawater and atmosphere - Google Patents
Detector for volatile sulphides in surface seawater and atmosphere Download PDFInfo
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- CN202814873U CN202814873U CN 201220278297 CN201220278297U CN202814873U CN 202814873 U CN202814873 U CN 202814873U CN 201220278297 CN201220278297 CN 201220278297 CN 201220278297 U CN201220278297 U CN 201220278297U CN 202814873 U CN202814873 U CN 202814873U
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Abstract
The utility model provides a detector for volatile sulphides in surface seawater and atmosphere. The detector is has a structure that a sample collecting assembly is connected with a gathering and desorbing assembly, the gathering and desorbing assembly is connected with an oxidization detection assembly, and the oxidization detection assembly is connected with a gas circuit conversion assembly and a gas supply system. The detector for volatile sulphides in surface seawater and atmosphere has the characteristics and beneficial effects that the detector has two channels, can detect volatile sulphides in surface seawater and atmosphere at the same time without any chemical agents, does not cause secondary pollution to the environment and water bodies, and is quick and accurate in detection process, good in repeatability, stable and reliable in result and suitable for detecting concentrations of volatile sulphides in various water bodies and in particular suitable for dynamical detection by an ocean research vessel or a scientific research vessel in an underway manner. The detector can detect automatically and monitor in real time for a long time, online and continuously, so that the detector is suitable for being widely applied.
Description
Technical field
The utility model relates to the ocean monitoring technologytechnologies field, relates in particular to volatile sulfur compounds pick-up unit in a kind of surface seawater and the atmosphere, and this application of installation detects volatile sulfur compounds concentration in surface seawater and the atmosphere walking the boat mode.
Background technology
Ocean source of students organic sulfide is a focus in scientific research of seas and the marine eco-environment monitoring field always.Ocean source of students organic sulfide mainly contains dimethyl disulfide, methyl mercaptan, carbon disulphide, cos, dimethyl sulfoxide, DMDS etc., wherein dimethyl disulfide is the abundantest ocean volatile sulfur compounds, mainly produce and be released in the seawater by sea life, account for 95% of ocean sulphur emissions, account for 1/2 of atmosphere natural sulphur emission source.In global sulfur cycle, dimethyl disulfide is participated in climate change and acid rain forming process directly, has vital role in Atmospheric Chemistry and biomass geochemistry, and its research comes into one's own day by day.Moreover, because biocenological variation such as common composition such as source of students organic sulfide the production of material and phytoplankton, animal plankton and bacterium etc. is closely related in the seawater, thereby be the important indicator of coastal ocean eco-environmental quality.A large amount of land-sourced pollutants enters the marine site with the earth's surface runoff, cause the variation of chemical constitution and physical condition in the seawater, these variations affect the variation of producing closely-related marine community with the orgainc sulfur compounds dimethyl disulfide significantly, and then affect the biological production of dimethyl disulfide and the ecologic environment in marine site thereof.Therefore; set up a kind of assay method of ocean-atmosphere interface volatile sulfur compounds of boat-carrying boating type; carry out accurately, fast, on a large scale, the continuous change in time and space of volatile sulfur compounds in long-term observation ocean and the atmosphere; estimate it to the impact of weather and environment generation; be ecologic environment and the corresponding safeguard measure of formulation of protection China littoral sea, tool is of great significance.
Because the content of source of students organic sulfide is very low in ocean and the atmosphere, as the concentration of dimethyl disulfide in the surface seawater 10～10
2Between the ng/L, utilize existing instrument and equipment all can not directly measure it, must be through the enrichment pre-treatment.Usually the analytical approach that adopts both at home and abroad is first sample to be carried out the enrichment pre-treatment, then adopts the vapor-phase chromatography of flame photometric detector (FPD) to detect.The difference of method is that enrichment pre-treatment mode is different, 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.Above each side fado number needs loaded down with trivial details treatment step, sample composition is complicated, operating cost is large, enrichment and detect all needs time of growing, analysis speed and accuracy have greatly been affected, can't carry out on a large scale, automatic monitor for continuously, can not realize away that more the boat mode is to detecting when volatile sulfur compounds in surface seawater and the atmosphere.
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: walks in the boat process at boat-carrying, and by the mode of capture desorb, volatile sulfur compounds in the overhead atmosphere in enrichment ocean, the concentration of measuring and calculate the Atmospheric Sulfur compound is C
1Marine atmosphere and surface seawater are reached mobile equilibrium through fountain aqueous vapor evener, by the capture desorption mode, volatile sulfur compounds in the enrichment Balance Air, the concentration of measuring and calculate the Balance Air medium sulphide content is C
2With Balance Air medium sulphide content concentration C
2Deduct Atmospheric Sulfur compound concentration C
1, the concentration that calculates volatile sulfur compounds in the surface seawater is Δ C
s=C
2-C
1By constantly to C
1, C
2Detect, can realize the boat of walking of volatile sulfur compounds in surface seawater and the atmosphere is detected, and be applied to marine environmental monitoring.The utility model adopts the binary channels design, by walking the boat mode, detects simultaneously volatile sulfur compounds in surface seawater and the atmosphere, measurement result accurately and reliably, need not any chemical reagent, avoid secondary pollution, can realize that boat-carrying is walked to navigate, continuous, real-time, the online detection.
The purpose of this utility model is realized by following technical scheme, developed volatile sulfur compounds pick-up unit in a kind of surface seawater and the atmosphere, this device is to be connected with capture desorb assembly by the sample collection assembly, capture the desorb assembly and be connected with the oxidation detection components, the oxidation detection components is connected with the gas circuit transition components and is connected with air supply system.
Described sample collection assembly arranges pneumatic pump 1-1, aqueous vapor evener 1-2, moisture separator 1-3, and pneumatic pump 1-1 upper channel directly is connected with the plasmas channel of moisture separator 1-3, and lower channel is connected with the gas access of aqueous vapor evener 1-2; Aqueous vapor evener 1-2 lower end is provided with air intake, and the top is provided with the Balance Air outlet, and seawater entrance 1-4 is connected with the boat-carrying submersible pump, and seawer outlet 1-5 connecting duct is emptying, and the gas vent on top is connected with the Balance Air passage of moisture separator 1-3; The outlet of moisture separator 1-3 plasmas channel is connected with the second six-way valve 4-2 first interface B1b by the first three-way diverter valve 1-6, and moisture separator 1-3 Balance Air channel outlet is connected with the first six-way valve 4-1 first interface A1a by the second three-way diverter valve 1-7; The first three-way diverter valve 1-6 and the second three-way diverter valve 1-7 respectively have a floss hole, and pipeline and interface are all used teflon hose and seal.
Described capture desorb assembly arranges and captures desorption chamber 2-1, Balance Air trap tube 2-2, atmosphere trap tube 2-3, thermal resistor 2-4, semiconductor cooler 2-5, Balance Air trap tube 2-2 entrance is connected with six-way valve 4-1 the second interface A2a, and outlet is connected with the first six-way valve 4-1 the 5th interface A5a; Atmosphere trap tube 2-3 entrance is connected with six-way valve 4-2 the second interface B2b, and outlet is connected with the second six-way valve 4-2 the 5th interface B5b; Capture desorption chamber 2-1 thermal resistor 2-4 and semiconductor cooler 2-5 are installed.
Described oxidation detection components arranges catalytic oxidation stove 3-5, atmosphere crystal reaction tube 3-6, Balance Air crystal reaction tube 3-7, the first film drying tube 3-8, the second film drying tube 3-9, UV vluorescent tester 3-10, industrial computer 3-11, atmosphere crystal reaction tube 3-6 entrance is connected with the first gas mixer 3-1, outlet is connected with the first film drying tube 3-8, enters the atmosphere sense channel of UV vluorescent tester; Balance Air crystal reaction tube 3-7 entrance is switched by three-way diverter valve 3-4, can be connected with the second gas mixer 3-2, the 3rd gas mixer 3-3 respectively, outlet is connected with the second film drying tube 3-9, enter the Balance Air sense channel of UV vluorescent tester, industrial computer 3-11 realizes man-machine conversation, data acquisition, the data calculating of testing process.
Described gas circuit transition components arranges the first six-way valve 4-1, the second six-way valve 4-2, the 3rd six-way valve 4-3, the capture that the first six-way valve 4-1 control Balance Air enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface A1a and the second interface A2a are logical, the 3rd interface A3a is logical with the 4th interface A4a, the 5th interface A5a and the 6th interface A6a lead to; Desorption state is that first interface A1a and the 6th interface A6a are logical, the second interface A2a is logical with the 3rd interface A3a, the 4th interface A4a and the 5th interface A5a lead to; The connected mode of six interfaces: first interface A1a is connected with the second three-way diverter valve 1-7, the second interface A2a is connected with Balance Air trap tube 2-2 entrance, the 3rd interface A3a is connected with the 4th flow regulator 7-2, zero gas cylinder 7-1, the 4th interface A4a is connected with the second gas mixer 3-2, the 5th interface A5a is connected with trap tube 2-2 outlet, and the 6th interface A6a is exhaust outlet; The capture that the second six-way valve 4-2 control atmosphere enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface B1b and the second interface B2b are logical, the 3rd interface B3b is logical with the 4th interface B4b, the 5th interface B5b and the 6th interface B6b lead to; Parse state is that first interface B1b and the 6th interface B6b are logical, the second interface B2b is logical with the 3rd interface B3b, the 4th interface B4b and the 5th interface B5b lead to; The connected mode of six interfaces: first interface B1b is connected with the first three-way diverter valve 1-6, the second interface B2b is connected with trap tube 2-3 entrance, the 3rd interface B3b is connected with the 5th flow regulator 7-3, zero gas cylinder 7-1, the 4th interface B4b is connected with the first gas mixer 3-1, the 5th interface B5b is connected with atmosphere trap tube 2-3 outlet, and the 6th interface B6b is exhaust outlet; The 3rd six-way valve 4-3 Quality control is measured with the gas circuit of calibrate and is connected and conversion, be provided with six interfaces of two kinds of states, the mensuration state is that first interface C1c and the second interface C2c are logical, the 3rd interface C3c is logical with the 4th interface C4c, the 5th interface C5c and the 6th interface C6c lead to; The demarcation state is that first interface C1c and the 6th interface C6c are logical, the second interface C2c and the 3rd interface C3c) logical, the 4th interface C4c and the 5th interface C5c lead to; First interface C1c is connected with the 3rd gas mixer 3-3, the second interface C2c is connected with the gas cylinder 7-1 of being connected with the 6th flow regulator 7-4, be connected by quantity tube between the 3rd interface C3c and the 6th interface C6c, the 4th interface C4c is connected with flow regulator 6-2, gas steel cylinder 6-1, and the 5th interface C5c is exhaust outlet.
Described air supply system arranges combustion-supporting gas cylinder 5-1, gas steel cylinder 6-1, zero gas cylinder 7-1, combustion-supporting gas cylinder 5-1 gas is divided into three the tunnel through the reduction valve outlet, be connected with first flow regulator 5-2, the second flow regulator 5-3, the 3rd flow regulator 5-4 respectively, first flow regulator 5-2 is connected with the 3rd gas mixture 3-3, the second flow regulator 5-3 is connected with the second gas mixture 3-2, and the 3rd flow regulator 5-4 is connected with the first gas mixture 3-1; Gas steel cylinder 6-1 gas is connected with the 3rd six-way valve 4-3 interface the 4th interface C4c through reduction valve, flow regulator 6-2; Zero gas cylinder 7-1 gas is divided into three the tunnel through the reduction valve outlet, be connected with the 4th flow regulator 7-2, the 5th flow regulator 7-3, the 6th flow regulator 7-4 respectively, the 4th flow regulator 7-2 is connected with the first six-way valve 4-1 interface the 3rd interface A3a, the 5th flow regulator 7-3 is connected with the second six-way valve 4-2 the 3rd interface B3b, and the 6th flow regulator 7-4 is connected with the 3rd six-way valve 4-3 interface the second interface C2c.
Characteristics of the present utility model and beneficial effect are: adopt the binary channels design, can detect simultaneously volatile sulfur compounds in surface seawater and the atmosphere, 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, be suitable for the detection of various water body volatile sulfur compounds concentration, be particularly suitable for oceanographic research ship or scientific investigation ship to walk to navigate the mode detection of dynamic, and can realize the testing process automatic operating, for a long time real-time, online, continuous monitoring, suitable extensively popularization.
Description of drawings
Fig. 1 is the utility model structural representation.
Embodiment
Referring to Fig. 1, the utility model has been developed volatile sulfur compounds pick-up unit in a kind of surface seawater and the atmosphere, takes following steps:
This device is to be connected with capture desorb assembly by the sample collection assembly, captures the desorb assembly and is connected with the oxidation detection components, and the oxidation detection components is connected with the gas circuit transition components and is connected with air supply system.
Described sample collection assembly arranges pneumatic pump 1-1, aqueous vapor evener 1-2, moisture separator 1-3, and pneumatic pump 1-1 upper channel directly is connected with the plasmas channel of moisture separator 1-3, and lower channel is connected with the gas access of aqueous vapor evener 1-2; Aqueous vapor evener 1-2 lower end is provided with air intake, and the top is provided with the Balance Air outlet, and seawater entrance 1-4 is connected with the boat-carrying submersible pump, and seawer outlet 1-5 connecting duct is emptying, and the gas vent on top is connected with the Balance Air passage of moisture separator 1-3; The outlet of moisture separator 1-3 plasmas channel is connected with the second six-way valve 4-2 first interface B1b by the first three-way diverter valve 1-6, and moisture separator 1-3 Balance Air channel outlet is connected with the first six-way valve 4-1 first interface A1a by the second three-way diverter valve 1-7; The first three-way diverter valve 1-6 and the second three-way diverter valve 1-7 respectively have a floss hole, and pipeline and interface are all used teflon hose and seal.
Described capture desorb assembly arranges and captures desorption chamber 2-1, Balance Air trap tube 2-2, atmosphere trap tube 2-3, thermal resistor 2-4, semiconductor cooler 2-5, Balance Air trap tube 2-2 entrance is connected with six-way valve 4-1 the second interface A2a, and outlet is connected with the first six-way valve 4-1 the 5th interface A5a; Atmosphere trap tube 2-3 entrance is connected with six-way valve 4-2 the second interface B2b, and outlet is connected with the second six-way valve 4-2 the 5th interface B5b; Capture desorption chamber 2-1 thermal resistor 2-4 and semiconductor cooler 2-5 are installed.
Described oxidation detection components arranges catalytic oxidation stove 3-5, atmosphere crystal reaction tube 3-6, Balance Air crystal reaction tube 3-7, the first film drying tube 3-8, the second film drying tube 3-9, UV vluorescent tester 3-10, industrial computer 3-11, atmosphere crystal reaction tube 3-6 entrance is connected with the first gas mixer 3-1, outlet is connected with the first film drying tube 3-8, enters the atmosphere sense channel of UV vluorescent tester; Balance Air crystal reaction tube 3-7 entrance is switched by three-way diverter valve 3-4, can be connected with the second gas mixer 3-2, the 3rd gas mixer 3-3 respectively, outlet is connected with the second film drying tube 3-9, enter the Balance Air sense channel of UV vluorescent tester, industrial computer 3-11 realizes man-machine conversation, data acquisition, the data calculating of testing process.
Described gas circuit transition components arranges the first six-way valve 4-1, the second six-way valve 4-2, the 3rd six-way valve 4-3, the capture that the first six-way valve 4-1 control Balance Air enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface A1a and the second interface A2a are logical, the 3rd interface A3a is logical with the 4th interface A4a, the 5th interface A5a and the 6th interface A6a lead to; Desorption state is that first interface A1a and the 6th interface A6a are logical, the second interface A2a is logical with the 3rd interface A3a, the 4th interface A4a and the 5th interface A5a lead to; The connected mode of six interfaces: first interface A1a is connected with the second three-way diverter valve 1-7, the second interface A2a is connected with Balance Air trap tube 2-2 entrance, the 3rd interface A3a is connected with the 4th flow regulator 7-2, zero gas cylinder 7-1, the 4th interface A4a is connected with the second gas mixer 3-2, the 5th interface A5a is connected with trap tube 2-2 outlet, and the 6th interface A6a is exhaust outlet; The capture that the second six-way valve 4-2 control atmosphere enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface B1b and the second interface B2b are logical, the 3rd interface B3b is logical with the 4th interface B4b, the 5th interface B5b and the 6th interface B6b lead to; Parse state is that first interface B1b and the 6th interface B6b are logical, the second interface B2b is logical with the 3rd interface B3b, the 4th interface B4b and the 5th interface B5b lead to; The connected mode of six interfaces: first interface B1b is connected with the first three-way diverter valve 1-6, the second interface B2b is connected with trap tube 2-3 entrance, the 3rd interface B3b is connected with the 5th flow regulator 7-3, zero gas cylinder 7-1, the 4th interface B4b is connected with the first gas mixer 3-1, the 5th interface B5b is connected with atmosphere trap tube 2-3 outlet, and the 6th interface B6b is exhaust outlet; The 3rd six-way valve 4-3 Quality control is measured with the gas circuit of calibrate and is connected and conversion, be provided with six interfaces of two kinds of states, the mensuration state is that first interface C1c and the second interface C2c are logical, the 3rd interface C3c is logical with the 4th interface C4c, the 5th interface C5c and the 6th interface C6c lead to; The demarcation state is that first interface C1c and the 6th interface C6c are logical, the second interface C2c and the 3rd interface C3c) logical, the 4th interface C4c and the 5th interface C5c lead to; First interface C1c is connected with the 3rd gas mixer 3-3, the second interface C2c is connected with the gas cylinder 7-1 of being connected with the 6th flow regulator 7-4, be connected by quantity tube between the 3rd interface C3c and the 6th interface C6c, the 4th interface C4c is connected with flow regulator 6-2, gas steel cylinder 6-1, and the 5th interface C5c is exhaust outlet.
Described air supply system arranges combustion-supporting gas cylinder 5-1, gas steel cylinder 6-1, zero gas cylinder 7-1, combustion-supporting gas cylinder 5-1 gas is divided into three the tunnel through the reduction valve outlet, be connected with first flow regulator 5-2, the second flow regulator 5-3, the 3rd flow regulator 5-4 respectively, first flow regulator 5-2 is connected with the 3rd gas mixture 3-3, the second flow regulator 5-3 is connected with the second gas mixture 3-2, and the 3rd flow regulator 5-4 is connected with the first gas mixture 3-1; Gas steel cylinder 6-1 gas is connected with the 3rd six-way valve 4-3 the 4th interface C4c through reduction valve, flow regulator 6-2; Zero gas cylinder 7-1 gas is divided into three the tunnel through the reduction valve outlet, be connected with the 4th flow regulator 7-2, the 5th flow regulator 7-3, the 6th flow regulator 7-4 respectively, the 4th flow regulator 7-2 is connected with the first six-way valve 4-1 the 3rd interface A3a, the 5th flow regulator 7-3 is connected with the second six-way valve 4-2 the 3rd interface B3b, and the 6th flow regulator 7-4 is connected with the 3rd six-way valve 4-3 the second interface C2c.
Each assembly specific requirement and detection principle are as follows in the utility model:
The sample collection assembly: this assembly need to gather atmosphere and Balance Air sample simultaneously, and atmosphere is directly by the pneumatic pump Real-time Collection, and Balance Air is that surface seawater and atmosphere are when reaching mobile equilibrium and obtain in the aqueous vapor evener.Surface seawater continuously is pumped to fountain aqueous vapor evener, flow from top to bottom, atmosphere pumps into from aqueous vapor evener bottom, flow in opposite directions with seawater, the Balance Air of setting up after the mobile equilibrium enters moisture separator from the top, and the seawater after the balance is discharged from aqueous vapor evener bottom, the continuous operation of whole process is so that aqueous vapor arrives mobile equilibrium, Balance Air enters moisture separator, dehydrated dose of absorption of water vapor, and orgainc sulfur compounds enters the capture resolution component under the promotion of air.When the dewatering agent in the moisture separator reaches capacity, make moisture separator rise to uniform temperature by heating member and 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 gas flow, flow velocity, purge time.
Capture the desorb assembly: this assembly need to capture volatile sulfur compounds in enrichment atmosphere and the Balance Air sample simultaneously, in capturing desorption chamber, two trap tubes are installed, insert adsorbent of molecular sieve in the pipe, under cryogenic conditions, capture respectively atmosphere and Balance Air medium sulphide content, capture and finish the intensification desorb.Regulate the temperature of semiconductor cooler, to obtain the best effect that captures, capture is finished, and thermistor heats up trap tube rapidly, thereby makes volatile sulfur compounds desorb from trap tube, and zero gas is as carrier gas, and sample gas enters the oxidation detection components under carrier gas promotes.
Oxidation detection components: be sulphuric dioxide with atmosphere and Balance Air medium sulphide content Quantitative yield respectively, and detect.Designed a kind of small switch formula constant temperature catalytic reaction stove, two crystal reaction tubes are installed in the stove, catalyst filling in the pipe, atmosphere and Balance Air sample are mixed into crystal reaction tube with combustion-supporting gas respectively, under uniform temperature and catalyst action, be oxidized to rapidly sulphuric dioxide and water, process film drying tube removes moisture wherein, enters UV vluorescent tester, and it is 214nm that content of sulfur dioxide detects wavelength.Zero gas is determined as baseline value, by measuring the response of concentration known sulphuric dioxide calibrating gas, measures the response of unknown concentration sample again, just can calculate the content of sulphuric dioxide in the sample.Testing process is calculated by industrial computer control, operation, data.
The gas circuit transition components: be comprised of three six-way valves and connecting pipe, each six-way valve has two kinds of states, and six interfaces realize that respectively atmospheric sample capture desorb, Balance Air sample capture desorb, sample determination is connected and translation function with the gas circuit of calibration process.
Air supply system: the supply, conversion and the flow regulation that mainly realize gas.Combustion-supporting gas is air or oxygen, is mainly used in auxiliary organic sulfide and is converted into sulphuric dioxide; Standard Gases is the sulphuric dioxide calibrating gas of concentration known, is used for quantitative measurement, standard working curve drafting and calibrate; Zero gas can be high pure nitrogen or high-purity helium for not containing the blank gas of sulphuric dioxide, is equivalent to the carrier gas effect in capture, desorb, oxidizing process, is equivalent to the background baseline in testing process.
The concrete detection method of the utility model is as follows:
1, instrumental calibration
Arrange respectively: zero gas 200mL/min, combustion-supporting gas 200mL/min, sulphuric dioxide gas 50mL/min, sulphuric dioxide gas concentration 10ppm, quantity tube volume 0.5mL, 280 ℃ of the temperature of catalytic oxidation stove.
Select " standard test " button at System menu, six-way valve 4-1 is that Balance Air captures state, and six-way valve 4-2 is that atmosphere captures state, and six-way valve 4-3 is in the mensuration state.Zero gas 7-1 is through flow regulator 7-4, after entering gas mixer 3-3 and combustion-supporting gas mixes along six-way valve 4-3 the second interface C2c, first interface C1c, successively by catalytic oxidation stove 3-5, crystal reaction tube 3-7, film drying tube 3-9, enter UV vluorescent tester 3-10, discharge from the outlet port of detecting device.Meta-concentration curve when demonstrating in real time on display, this curve are baseline.Sulphuric dioxide gas 6-1 is through flow regulator 6-2, and emptying along six-way valve 4-3 the 4th interface C4c, the 3rd interface C3c, quantity tube, the 6th interface C6c, the 5th interface C5c outlet, quantity tube is also filled in the gas flushing.
Select " demarcation " button at System menu, six-way valve 4-1 is that Balance Air captures state, and six-way valve 4-2 is that atmosphere captures state, and six-way valve 4-3 is in the demarcation state.Zero gas 7-1 is through flow regulator 7-4, after entering gas mixer 3-3 and combustion-supporting gas mixes along six-way valve 4-3 the second interface C2c, the 3rd interface C3c, quantity tube, the 6th interface C6c, first interface C1c, successively by catalytic oxidation stove 3-5, crystal reaction tube 3-7, film drying tube 3-9, enter UV vluorescent tester 3-10, discharge from the outlet port of detecting device.Zero gas is brought the sulphuric dioxide calibrating gas in the quantity tube into UV vluorescent tester and is detected, and meta-concentration curve when demonstrating in real time on display is for curve is the data that gas is measured.
2, sample determination
2.1 Atmospheric Sulfur compound content C
1Mensuration:
Arrange respectively: atmosphere 80mL/min, zero gas 200mL/min, combustion-supporting gas 200mL/min, sulphuric dioxide gas 50mL/min, sulphuric dioxide gas concentration 10ppm, quantity tube volume 0.5mL, 280 ℃ of catalytic oxidation furnace temperatures capture temperature-10 ℃, capture time 5min, 200 ℃ of desorption temperatures, desorption time 2min.
Select " atmosphere mensuration " button at System menu, at this moment, six-way valve 4-1 is that Balance Air captures state, and six-way valve 4-2 is that atmosphere captures state, and six-way valve 4-3 is the mensuration state.Zero gas 7-1 is through flow regulator 7-3, after entering gas mixer 3-1 and combustion-supporting gas mixes along six-way valve 4-2 the 3rd interface B3b, the 4th interface B4b, successively by catalytic oxidation stove 3-5, crystal reaction tube 3-6, film drying tube 3-8, enter UV vluorescent tester atmosphere sense channel, discharge from the exhaust outlet of detecting device.Meta-concentration curve when demonstrating in real time on display, this curve are baseline.
Click " measuring beginning " button, marine atmosphere successively by moisture separator 1-3, three-way diverter valve 1-6, six-way valve 4-2 first interface B1b, the second interface B2b, enters that atmosphere trap tube 2-3 captures, the gas of collection at large is emptying behind the 5th interface B5b, the 6th interface B6b of six-way valve 4-2 by pneumatic pump 1-1.After 5 minutes, does software eject dialog box and " carries out desorb and mensuration? " selection " being ", capture desorption chamber 2-1 automatic heating, six-way valve 4-2 automatically switches to parse state, six-way valve 4-3 still keeps the mensuration state, after 2 minutes, zero gas 7-1 is through flow regulator 7-3, along six-way valve 4-2 the 3rd interface B3b, the second interface B2b enters atmosphere trap tube 2-3, carry out sulfide gas, through six-way valve 4-2 the 5th interface B5b, the 4th interface B4b enters gas mixer 3-1 to be mixed with combustion-supporting gas, catalytic oxidation stove 3-5, crystal reaction tube 3-6, film drying tube 3-8, UV vluorescent tester atmosphere sense channel, the sample gas that is sulfur compound in the atmosphere is to enter UV vluorescent tester behind the sulfur dioxide gas to detect by catalytic oxidation, can observe the real-time change curve of sulfur dioxide concentration on display screen, be the data that atmospheric sample is measured, and instrument calculates the concentration C of organic sulfide in the atmosphere automatically according to the result of calibration and demarcation
1
2.2 the content C of organic sulfur in the Balance Air
2Measure:
Arrange respectively: Balance Air 80mL/min, zero gas 200mL/min, combustion-supporting gas 200mL/min, sulphuric dioxide gas 50mL/min, sulphuric dioxide gas concentration 10ppm, quantity tube volume 0.5mL, 280 ℃ of catalytic oxidation furnace temperatures capture temperature-10 ℃, 5 minutes capture time, 200 ℃ of desorption temperatures, desorption time 2 minutes.
Select " Balance Air mensuration " button at System menu, at this moment, six-way valve 4-1 is that Balance Air captures state, and six-way valve 4-2 is that atmosphere captures state, and six-way valve 4-3 is the mensuration state.Zero gas 7-1 is through flow regulator 7-2, after entering gas mixer 3-2 and combustion-supporting gas mixes along six-way valve 4-1 the 3rd interface A3a, the 4th interface A4a, successively by catalytic oxidation stove 3-5, crystal reaction tube 3-7, film drying tube 3-9, enter UV vluorescent tester Balance Air sense channel, discharge from the exhaust outlet of detecting device.Meta-concentration curve when demonstrating in real time on display, this curve are baseline.
Click " measuring beginning " button, marine atmosphere passes through aqueous vapor evener 1-2, moisture separator 1-3, three-way diverter valve 1-7, six-way valve 4-1 first interface A1a, the second interface A2a successively by pneumatic pump 1-1, enter Balance Air trap tube 2-2 and capture, the gas of collection at large is emptying through six-way valve 4-1 the 5th interface A5a, the 6th interface A6a.After 5 minutes, does software eject dialog box and " carries out desorb and mensuration? " selection " being ", capture desorption chamber 2-1 automatic heating, six-way valve 4-1 automatically switches to parse state, six-way valve 4-3 still keeps the mensuration state, after 2 minutes, zero gas 7-1 is through flow regulator 7-2, along six-way valve 4-1 the 3rd interface A3a, the second interface A2a enters Balance Air trap tube 2-2, carry out sulfide gas, through six-way valve 4-1 the 5th interface A5a, the 4th interface A4a enters gas mixer 3-2 to be mixed with combustion-supporting gas, successively by catalytic oxidation stove 3-5, crystal reaction tube 3-7, film drying tube 3-9, UV vluorescent tester Balance Air sense channel, the sample gas that is sulfur compound in the Balance Air is to enter UV vluorescent tester behind the sulfur dioxide gas to detect by catalytic oxidation, on display screen, can observe the real-time change curve of sulfur dioxide concentration, be the data of Balance Air sample measurement, instrument calculates the concentration C of organic sulfide in the Balance Air automatically according to the result of calibration and demarcation
2
Atmosphere and Balance Air carry out simultaneously in capture, desorb, mensuration process.
2.3 the assay of orgainc sulfur compounds in the surface seawater:
With the Balance Air medium sulphide content concentration C that detects
2Deduct Atmospheric Sulfur compound concentration C
1, calculate the concentration of orgainc sulfur compounds in the surface seawater.
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. volatile sulfur compounds pick-up unit in surface seawater and the atmosphere, this device be by the sample collection assembly with capture the desorb assembly and be connected, capture desorb assembly is connected with the oxidation detection components, the oxidation detection components is connected with the gas circuit transition components and is connected with air supply system.
2. volatile sulfur compounds pick-up unit in surface seawater according to claim 1 and the atmosphere, it is characterized in that: described sample collection assembly arranges pneumatic pump (1-1), aqueous vapor evener (1-2), moisture separator (1-3), pneumatic pump (1-1) upper channel directly is connected with the plasmas channel of moisture separator (1-3), and lower channel is connected with the gas access of aqueous vapor evener (1-2); Aqueous vapor evener (1-2) lower end is provided with air intake, the top is provided with the Balance Air outlet, seawater entrance (1-4) is connected with the boat-carrying submersible pump, and seawer outlet (1-5) connecting duct is emptying, and the gas vent on top is connected with the Balance Air passage of moisture separator (1-3); The outlet of moisture separator (1-3) plasmas channel is connected with the second six-way valve (4-2) first interface B (1b) by the first three-way diverter valve (1-6), and moisture separator (1-3) Balance Air channel outlet is connected with the first six-way valve (4-1) first interface A (1a) by the second three-way diverter valve (1-7); The first three-way diverter valve (1-6) and the second three-way diverter valve (1-7) respectively have a floss hole, and pipeline and interface are all used teflon hose and seal.
3. volatile sulfur compounds pick-up unit in surface seawater according to claim 1 and the atmosphere, it is characterized in that: described capture desorb assembly arranges and captures desorption chamber (2-1), Balance Air trap tube (2-2), atmosphere trap tube (2-3), thermal resistor (2-4), semiconductor cooler (2-5), Balance Air trap tube (2-2) entrance is connected with six-way valve (4-1) the second interface A (2a), and outlet is connected with the first six-way valve (4-1) the 5th interface A (5a); Atmosphere trap tube (2-3) entrance is connected with six-way valve (4-2) the second interface B (2b), and outlet is connected with the second six-way valve (4-2) the 5th interface B (5b); Capture desorption chamber (2-1) thermal resistor (2-4) and semiconductor cooler (2-5) are installed.
4. volatile sulfur compounds pick-up unit in surface seawater according to claim 1 and the atmosphere, it is characterized in that: described oxidation detection components arranges catalytic oxidation stove (3-5), atmosphere crystal reaction tube (3-6), Balance Air crystal reaction tube (3-7), the first film drying tube (3-8), the second film drying tube (3-9), UV vluorescent tester (3-10), industrial computer (3-11), atmosphere crystal reaction tube (3-6) entrance is connected with the first gas mixer (3-1), outlet is connected with the first film drying tube (3-8), enters the atmosphere sense channel of UV vluorescent tester; Balance Air crystal reaction tube (3-7) entrance is switched by three-way diverter valve (3-4), can be connected with the second gas mixer (3-2), the 3rd gas mixer (3-3) respectively, outlet is connected with the second film drying tube (3-9), enter the Balance Air sense channel of UV vluorescent tester, industrial computer (3-11) is realized man-machine conversation, data acquisition, the data calculating of testing process.
5. volatile sulfur compounds pick-up unit in surface seawater according to claim 1 and the atmosphere, it is characterized in that: described gas circuit transition components arranges the first six-way valve (4-1), the second six-way valve (4-2), the 3rd six-way valve (4-3), the capture that the first six-way valve (4-1) control Balance Air enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface A (1a) is logical with the second interface A (2a), the 3rd interface A (3a) and the 4th interface A (4a) are logical, the 5th interface A (5a) and the 6th interface A (6a) are logical; Desorption state is that first interface A (1a) is logical with the 6th interface A (6a), the second interface A (2a) is logical with the 3rd interface A (3a), the 4th interface A (4a) is logical with the 5th interface A (5a); The connected mode of six interfaces: first interface A (1a) is connected with the second three-way diverter valve (1-7), the second interface A (2a) is connected with Balance Air trap tube (2-2) entrance, the 3rd interface A (3a) is connected with the 4th flow regulator (7-2), zero gas cylinder (7-1), the 4th interface A (4a) is connected with the second gas mixer (3-2), the 5th interface A (5a) is connected with trap tube (2-2) outlet, and the 6th interface A (6a) is exhaust outlet; The capture that the second six-way valve (4-2) control atmosphere enters trap tube is connected with the gas circuit of desorb and switching, be provided with six interfaces of two kinds of states, the capture state is that first interface B (1b) is logical with the second interface B (2b), the 3rd interface B (3b) is logical with the 4th interface B (4b), the 5th interface B (5b) is logical with the 6th interface B (6b); Parse state is that first interface B (1b) is logical with the 6th interface B (6b), the second interface B (2b) is logical with the 3rd interface B (3b), the 4th interface B (4b) is logical with the 5th interface B (5b); The connected mode of six interfaces: first interface B (1b) is connected with the first three-way diverter valve (1-6), the second interface B (2b) is connected with trap tube (2-3) entrance, the 3rd interface B (3b) is connected with the 5th flow regulator (7-3), zero gas cylinder (7-1), the 4th interface B (4b) is connected with the first gas mixer (3-1), the 5th interface B (5b) is connected with atmosphere trap tube (2-3) outlet, and the 6th interface B (6b) is exhaust outlet; The 3rd six-way valve (4-3) Quality control is measured with the gas circuit of calibrate and is connected and conversion, be provided with six interfaces of two kinds of states, the mensuration state is that first interface C (1c) is logical with the second interface C (2c), the 3rd interface C (3c) is logical with the 4th interface C (4c), the 5th interface C (5c) is logical with the 6th interface C (6c); The demarcation state is that first interface C (1c) is logical with the 6th interface C (6c), the second interface C (2c) is logical with the 3rd interface C (3c), the 4th interface C (4c) is logical with the 5th interface C (5c); First interface C (1c) is connected with the 3rd gas mixer (3-3), the second interface C (2c) is connected with the gas cylinder of being connected (7-1) with the 6th flow regulator (7-4), be connected by quantity tube between the 3rd interface C (3c) and the 6th interface C (6c), the 4th interface C (4c) is connected with flow regulator (6-2), gas steel cylinder (6-1), and the 5th interface C (5c) is exhaust outlet.
6. volatile sulfur compounds pick-up unit in surface seawater according to claim 1 and the atmosphere, it is characterized in that: described air supply system arranges combustion-supporting gas cylinder (5-1), gas steel cylinder (6-1), zero gas cylinder (7-1), combustion-supporting gas cylinder (5-1) gas is divided into three the tunnel through the reduction valve outlet, respectively with first flow regulator (5-2), the second flow regulator (5-3), the 3rd flow regulator (5-4) connects, first flow regulator (5-2) is connected with the 3rd gas mixture (3-3), the second flow regulator (5-3) is connected with the second gas mixture (3-2), and the 3rd flow regulator (5-4) is connected with the first gas mixture (3-1); Gas steel cylinder (6-1) gas is connected with the 3rd six-way valve (4-3) the 4th interface C (4c) through reduction valve, flow regulator (6-2); Zero gas cylinder (7-1) gas is divided into three the tunnel through the reduction valve outlet, be connected with the 4th flow regulator (7-2), the 5th flow regulator (7-3), the 6th flow regulator (7-4) respectively, the 4th flow regulator (7-2) is connected with the first six-way valve (4-1) the 3rd interface A (3a), the 5th flow regulator (7-3) is connected with the second six-way valve (4-2) the 3rd interface B (3b), and the 6th flow regulator (7-4) is connected with the 3rd six-way valve (4-3) the second interface C (2c).
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| CN 201220278297 CN202814873U (en) | 2012-06-07 | 2012-06-07 | Detector for volatile sulphides in surface seawater and atmosphere |
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| CN103364385A (en) * | 2013-08-06 | 2013-10-23 | 山东省科学院海洋仪器仪表研究所 | Device and method for on-line detection of sulfide concentrations in water sample by utilization of fluorescence spectrophotometry |
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| CN107271364A (en) * | 2017-07-29 | 2017-10-20 | 中国地质调查局油气资源调查中心 | A kind of water air interface methane and carbon dioxide on-line monitoring system and method |
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