CN103743678B - The sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water - Google Patents
The sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water Download PDFInfo
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- CN103743678B CN103743678B CN201310752517.1A CN201310752517A CN103743678B CN 103743678 B CN103743678 B CN 103743678B CN 201310752517 A CN201310752517 A CN 201310752517A CN 103743678 B CN103743678 B CN 103743678B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000001301 oxygen Substances 0.000 title claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 11
- 239000002352 surface water Substances 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000007789 gas Substances 0.000 claims abstract description 42
- 230000010354 integration Effects 0.000 claims abstract description 23
- 238000001228 spectrum Methods 0.000 claims abstract description 23
- 230000008676 import Effects 0.000 claims abstract description 16
- 238000005259 measurement Methods 0.000 claims abstract description 16
- 239000000523 sample Substances 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- -1 cold-trap Substances 0.000 claims abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 239000005431 greenhouse gas Substances 0.000 abstract description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 46
- 239000001272 nitrous oxide Substances 0.000 description 22
- 230000000694 effects Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000003068 static effect Effects 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000013535 sea water Substances 0.000 description 4
- 238000012937 correction Methods 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000008358 core component Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000926 atmospheric chemistry Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
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- 238000003860 storage Methods 0.000 description 1
- 239000005437 stratosphere Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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Abstract
In a kind of surface water, the sub-nitrogen spread for continuous profiling of dissolved oxygen, relates to a kind of monitoring equipment of greenhouse gases.Be provided with top layer water pump, filter plant, temperature and salimity measurement equipment, flow controller, moisture balance device, temp probe, cold-trap, air pump, Water-proof electrode, from axle integration chamber output spectrum detecting device, Standard Gases steel cylinder, top layer pump intake is arranged under water, top layer pump outlet takes over filter equipment entrance, filter plant outlet jointing temp and salimity measurement equipment, temperature and salimity measurement equipment export and connect flow controller import, flow controller outlet water receiving vapour evener, the air out being located at moisture balance device top connects cold-trap import, temp probe is located in moisture balance device, cold-trap outlet connects air pump import, water electrode is taken over control in air pump outlet, Water-proof electrode outlet connects detecting device import and the outlet of Standard Gases steel cylinder, detector output end connects secondary evener, the bottom in moisture balance device is located at by secondary evener, waste water discharge opening is established bottom moisture balance device.
Description
Technical field
The present invention relates to a kind of monitoring equipment of greenhouse gases, especially relate to the sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water.
Background technology
Nitrous oxide gas all has material impact to global climate and atmospheric chemistry process.Greenhouse effect Deng material amount nitrous oxide are 200 ~ 300 times of carbon dioxide.Meanwhile, its photochemical product NO in stratosphere can with O
3reaction, destroys atmospheric ozone layer (Crutzen, 1970).IPCC reports AR4(2007) point out, in air, nitrous oxide concentration is risen to about the 319ppb of 2006 by 270 ± 1ppb before the industrial revolution, and still with annual about 0.25% speed increment.6 years only between IPCC third time report (2001) and the 4th report (2007), the sub-nitrogen partial pressure increase of atmospheric oxidn about 5ppb, corresponding Radiative Forcing increased by 11%.Therefore, when mankind's limit production use fluorochlorohydrocarbon and cause its atmospheric concentration decline year by year, nitrous oxide not only surmounts fluorochlorohydrocarbon in greenhouse effect contribution, become the third-largest greenhouse effect contribution gas, more become 21 century topmost depletion of the ozone layer gas (Ravishankaraetal, 2009).
At present, vapor-phase chromatography GC-ECD or GC-MS is generally adopted to detect nitrous oxide in the world, the complete manual operation of method, transport laboratory back from the sampling of on-the-spot website, pre-service, sample introduction analysis need a large amount of manpowers and longer time, therefore sea area coverage rate, data resolution, time continuity are all difficult to reach the requirement of accurately estimation sea table methane spatial and temporal distributions, extra large gas methane Flux.Butler etc. (1989) achieve the coupling by water-gas balanced system and gas chromatography first, after this have again evener successful Application (Bangeetal., 1994 after more improvement; RehderandSuess, 2001).But vapor-phase chromatography needs a part of static headspace gas in expending equilibrium system, cause water in balanced system-gas balance to be interrupted, METHOD FOR CONTINUOUS DETERMINATION truly can not be realized.
Summary of the invention
The object of the invention is to propose quick with scene, high-resolution observed pattern and can not break the sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water of nitrous oxide in moisture balance, continuously automatic Observation water body.
The present invention be provided with top layer water pump, filter plant, temperature and salimity measurement equipment, flow controller, moisture balance device, temp probe, cold-trap, air pump, Water-proof electrode, from axle integration chamber output spectrum detecting device, Standard Gases steel cylinder;
The water inlet of described top layer water pump is arranged under water, the water delivering orifice of top layer water pump connects the entrance of filter plant, the outlet jointing temp of filter plant and salimity measurement equipment, the outlet of temperature and salimity measurement equipment connects the import of flow controller, the outlet water receiving vapour evener of flow controller, the air out being located at moisture balance device top connects the import of cold-trap, temp probe is located in moisture balance device, the outlet of cold-trap connects the import of air pump, gas delivery side of pump takes over control water electrode, the outlet of Water-proof electrode connects the outlet of import from axle integration chamber output spectrum detecting device and Standard Gases steel cylinder respectively by valve, output terminal from axle integration chamber output spectrum detecting device connects secondary evener by valve, the bottom in moisture balance device is located at by secondary evener, waste water discharge opening is established in the bottom of moisture balance device.
Described top layer pump intake can be arranged on boats and ships stem 1 ~ 5m place under water.
Beneficial effect of the present invention is as follows:
Compared with current other nitrous oxide scope, the present invention have simple to operate, power consumption is low, the feature such as sturdy and durable, is the ideal tools of the rugged surroundings such as sea, field condition.From axle integration chamber output spectrum method be now state-of-the-art do not consume nitrous oxide and can realize continuous and automatic observation nitrous oxide concentration instrument, the present invention can obtain high-precision data, good stability, long-term very reduced-maintenance can be realized automatically run, such as, on the platforms such as the boats and ships navigated by water or buoy, realize the Continuous Observation to the high-resolution long time scale of the large area of the water surface, air.Compared to current manual website sampling, transport laboratory treatment back, analyze that it is with the obvious advantage, save a large amount of labour, operator seldom needs to carry out maintenance and operation, full automation to it after installation.Time is quick, and detection system can show at that time in real time, local nitrous oxide concentration, and takes back lab analysis and may have passed through the some months even longer time to going out data.In addition, relative to the recording geometry of other kinds, the present invention devises emphatically the safeguard procedures of detection system water inlet, except cold-trap is except water vapour, is also provided with Water-proof electrode, for detection system increases insurance together, guarantees security of system.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
See Fig. 1, the embodiment of the present invention be provided with top layer water pump 1, filter plant 2, temperature and salimity measurement equipment 3, flow controller 4, moisture balance device 5, temp probe 6, cold-trap 7, air pump 8, Water-proof electrode 9, from axle integration chamber output spectrum detecting device 10, Standard Gases steel cylinder 11.
The water inlet of described top layer water pump 1 is arranged under water, the water delivering orifice of top layer water pump 1 connects the entrance of filter plant 2, the outlet jointing temp of filter plant 2 and salimity measurement equipment 3, the outlet of temperature and salimity measurement equipment 3 connects the import of flow controller 4, the outlet water receiving vapour evener 5 of flow controller 4, the air out 51 being located at moisture balance device 5 top connects the import of cold-trap 7, temp probe 6 is located in moisture balance device 5, the outlet of cold-trap 7 connects the import of air pump 8, water electrode 9 is taken over control in the outlet of air pump 8, the outlet of Water-proof electrode 9 connects the outlet of import from axle integration chamber output spectrum detecting device 10 and Standard Gases steel cylinder 11 respectively by valve, output terminal from axle integration chamber output spectrum detecting device 10 connects secondary evener 52 by valve, the bottom in moisture balance device 5 is located at by secondary evener 52, waste water discharge opening 53 is established in the bottom of moisture balance device 5.In FIG, mark A is waste gas, and B is air, and C is waste water.
Described top layer pump intake can be arranged on boats and ships stem 1 ~ 5m place under water, by constant for surface seawater suction laboratory, first after filtration the impurity in seawater and bulky grain thing filter by equipment, prevent from these foreign material from entering moisture balance device to result in blockage, seawater is through excess temperature and salinity measuring apparatus, in-situ temperature, the salinity of real-time measurement seawater, image data frequency suggestion for 1min once.
Use traffic controller controls water velocity and maintains fixing horizontal, flow velocity fast as far as possible can accelerate the balance between gas-liquid two-phase, but too fast flow velocity can cause the air in evener to be taken out of with current, cause negative pressure in evener, non-counter-balanced ambient atmosphere enters moisture balance device in a large number.
Be separated into fine drop by top after current enter moisture balance device and air exchange balances, in moisture balance device, temperature serviceability temperature probe carries out real-time monitored, and with 1min interval record.Static headspace gas is connected with ambient atmosphere by pore, object is that the air pressure maintained in moisture balance device is consistent with atmospheric pressure, due to ambient atmosphere enter may cause gas-liquid imbalance can carry out pre-equilibration by the secondary evener installing another one additional small-sized, ensure that the balance of main evener is not broken.
After gas-liquid two-phase reaches balance, by air pump, static headspace gas is extracted out, first the most of water vapor in gas circuit is removed through cold-trap (-4 DEG C), then a Water-proof electrode is entered, the effect of this Water-proof electrode is, once touch the existence of aqueous water, triggers good program prepared in advance immediately, by the mode of Vavle switching, gas circuit is emptying, fundamentally ensure the safety from axle integration chamber output spectrum detecting device 1.Gas circuit is finally entering before the output spectrum detecting device of axle integration chamber, through a filtration unit to remove the molecule impurity that may exist in gas circuit, the setting of this filtration unit is because the core component in the optical cavity from axle integration chamber output spectrum detecting device is the mirror of a pair high reflectance, very easily stain and reduced the order of reflection of light path in chamber, greatly shorten and absorb light path, thus the high-precision detection for nitrous oxide can be had influence on.
Adopt from axle integration chamber output spectrum method from axle integration chamber output spectrum detecting device, should be as follows from the characteristic of axle integration chamber output spectrum detecting device:
Operating temperature: 0 ~ 45 DEG C;
Ambient humidity: 0 ~ 100%;
Measurement range: 1 ~ 100ppm;
Finding speed: 1Hz;
Repeatability/precision: 0.2ppb.
The built-in (SuSE) Linux OS of the present invention, without the need to worrying the interference of extraneous software virus, has the storage space of 10G, and connect display and can obtain visual operation, data and chart can obtain visualize.
Except hardware device, also work out a set of special software to realize automation mechanized operation.By the design of software, realize often observing the sub-nitrogen of dissolved oxygen in 3h water body, observe the nitrous oxide concentration in 5min air by the mode of Vavle switching, be then switched to calibrating gas and carry out, from the correction of axle integration chamber output spectrum detecting device, circulating with this.And by the date, the time, longitude and latitude, temperature (original position and evener), salinity is that interval is stored in internal memory with 1min.
To be arranged on the boats and ships of navigation, first this equipment to be arranged on boat-carrying laboratory, to connect power supply.Top layer water pump is arranged on 1 ~ 5m place under stem waterline, in water inlet, temperature, salinity measuring apparatus (SBE21 are installed, Seabird), to obtain temperature, the salinity of original position water body, be convenient to solubleness and the saturation degree of nitrous oxide in subsequent calculations water body, adopt the highly dense water pipe of certain length that current are introduced laboratory.The injection port of air be arranged on boats and ships top layer deck and as far as possible away from the position of chimney to avoid polluting.Current enter moisture balance device through flow controller, flow velocity is adjusted to about 3L/min, current are through the sheet plastic at top, this thin plate is covered with tiny space, current are dispersed into water droplet, increase the contact area of gas-liquid two-phase to realize nitrous oxide at two alternate Fast-Balances by reducing drop volume.
Moisture balance device belongs to " air bubble type " (other two kinds is " laminar-type " and " spraying type ") in three kinds of General balance devices, moisture balance device height 35cm, diameter 15cm, shape is right cylinder, volume is about 6L, after water body enters moisture balance device, remaining head space volume is about 3L, and the height of water level is maintained by U trap.The secondary evener of a scaled down version is also had in moisture balance device center of inside, ambient atmos enters this secondary evener by pipeline, gas circuit through being also introduced into secondary evener when axle integration chamber output spectrum detecting device returns, namely the effect that it plays is for main evener provides pre-equilibration, and avoiding non-counter-balanced air to enter main evener disequilibrates.Because evener communicates with air, internal pressure is considered to equal atmospheric pressure all the time.This evener belongs to secondary evener theoretically, but due to its volume very little, current and the gas residence time is inside relatively short, can be reduced to the one-level evener mixed.Install temp probe one in moisture balance device, the model of suggestion is PT100, and degree of accuracy is 0.1 DEG C, for the temperature variation in real-time monitored moisture balance device.According to Henry's law, by measuring the concentration of trace gas in moisture balance device static headspace gas, the concentration (Weiss, 1980) of gas in liquid phase can be calculated:
C
N2O=XF(T
eq,S)
In formula: C
n2Oit is the sub-nitrogen concentration (nmol/L) of dissolved oxygen in water body;
X is the mole fraction (ppm) of nitrous oxide in static headspace gas;
F dissolves function, is water temperature T
eq, salinity S function (nmol/L).
The mole fraction of nitrous oxide concentration detected from axle integration chamber output spectrum detecting device, measure the temperature T of water body in moisture balance device
eqobtain F value with salinity S, the sub-nitrogen concentration of dissolved oxygen in water body can be calculated.
With air pump, the static headspace gas in evener is extracted out uniformly, first through de-watering apparatus to remove water vapor excessive in gas circuit.The present invention adopts cold-trap (-4 DEG C) to realize, and needs change condenser pipe every day, to ensure that water removal effect is best, needs to prepare 3-5 root glass cold traps in advance with for subsequent use.Theoretically; cold-trap water removal effect can reach the object removing water vapor completely; but for safety we add loading electrode after cold-trap; the principle of this Water-proof electrode is; once touch the existence of aqueous water; trigger the program woven in advance immediately, switch three-way valve is emptying and realize absolute protection to detecting device by gas circuit.
Gas circuit finally enters still to be needed through a filtration unit before the output spectrum detecting device of axle integration chamber, this is owing to very easily being stain from mirror in optical cavity in the output spectrum detecting device of axle integration chamber thus reducing reflectivity, reduce the order of reflection of light path in optical cavity and shorten absorption light path, thus have impact on the precision that nitrous oxide is measured, and the material stain can have assimilation effect to light path, causes the measurement result of nitrous oxide to occur deviation.
The core component from axle integration chamber output spectrum detecting device that the present invention uses is the mirror (reflectivity R ~ 0.9999) of a pair high reflectance and the LASER Light Source of high degree of specificity, and gas circuit is by detection cell (volume: 0.55 × 10
-3m
2, length: 0.2m) time, laser beam enters to inject optical cavity with very little angle, and due to the mirror of high reflectance, light path can in intracavity reflecting (1 ~ 10) × 10
4secondary, produce (2 ~ 20) × 10
3the absorption light path of m.Even if tested gas is very low to the absorption coefficient of laser, light intensity still can be made to obtain effective attenuation by the way infinitely increasing absorption light path and be detected the high-precision measuring realizing trace gas by detecting device.Temperature and pressure in optical cavity (106hpa, changes with energy level after suppressing nitrous oxide molecule absorption photon the absorption peak caused by the negative pressure that maintains about 106hpa in measuring cell and widen) is also by synchro measure.The measurement range of this system is 1 ~ 100ppm, and sample frequency is 1Hz, and operating temperature is 0 ~ 45 DEG C, ambient humidity 0 ~ 100%, turnover gas interface be the big Lip river of generation gram model (Swageloktype3/8 ", 1/4 ").
By customized software contribute data as date, time, longitude and latitude, evener temperature, salinity etc. with 1min interval export and mate with boat-carrying in-situ temperature, air pressure.Before starting to measure, first function software carries out the correction of Standard Gases of zero standard gas, variable concentrations, and be stored in after having measured in internal memory, the survey frequency of Standard Gases is set to 1Hz, mensuration 5min.Next start to survey 15min air, then start to measure the sub-nitrogen of dissolved oxygen in 3h water body, the mode that above operation is all switched by software autocontrol valve realizes.The data of mensuration air, water body are 1min interval record, circulate thus, are finally terminated by the correction of Standard Gases, and the data of every day produce one with the file of date name, are then corrected by the data of interpolation method to period.The detection data of nitrous oxide can be displayed in the mode of distribution graph in time by display, be convenient to the exceptional value of scientific research personnel's Timeliness coverage nitrous oxide concentration, more directly perceived, for marine environment monitoring and find that nitrous oxide exceptional leakage point has fast relative to classic method, accuracy rate is high, the advantage of saving manpower, its scientific research, social effect are conducive to it and apply.
Claims (2)
1. the sub-nitrogen spread for continuous profiling of dissolved oxygen in surface water, it is characterized in that being provided with top layer water pump, filter plant, temperature and salimity measurement equipment, flow controller, moisture balance device, temp probe, cold-trap, air pump, Water-proof electrode, from axle integration chamber output spectrum detecting device, Standard Gases steel cylinder;
The water inlet of described top layer water pump is arranged under water, the water delivering orifice of top layer water pump connects the entrance of filter plant, the outlet jointing temp of filter plant and salimity measurement equipment, the outlet of temperature and salimity measurement equipment connects the import of flow controller, the outlet water receiving vapour evener of flow controller, the air out being located at moisture balance device top connects the import of cold-trap, temp probe is located in moisture balance device, the outlet of cold-trap connects the import of air pump, gas delivery side of pump takes over control water electrode, the outlet of Water-proof electrode connects the outlet of import from axle integration chamber output spectrum detecting device and Standard Gases steel cylinder respectively by valve, output terminal from axle integration chamber output spectrum detecting device connects secondary evener by valve, the bottom in moisture balance device is located at by secondary evener, waste water discharge opening is established in the bottom of moisture balance device.
2. the sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water as claimed in claim 1, is characterized in that described top layer pump intake is arranged on boats and ships stem 1 ~ 5m place under water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310752517.1A CN103743678B (en) | 2013-12-31 | 2013-12-31 | The sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water |
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| CN201310752517.1A CN103743678B (en) | 2013-12-31 | 2013-12-31 | The sub-nitrogen spread for continuous profiling of dissolved oxygen in a kind of surface water |
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| CN114279996B (en) * | 2021-12-28 | 2023-02-03 | 哈尔滨工业大学 | Gas-phase hydrogen peroxide concentration detection system based on off-axis integration cavity |
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| CN203025013U (en) * | 2013-01-08 | 2013-06-26 | 中国工程物理研究院核物理与化学研究所 | Portable tritiated water sampling device |
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