CN203720155U - Sample feeding device for measuring gas phase of water body release gas - Google Patents

Sample feeding device for measuring gas phase of water body release gas Download PDF

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Publication number
CN203720155U
CN203720155U CN201420051407.2U CN201420051407U CN203720155U CN 203720155 U CN203720155 U CN 203720155U CN 201420051407 U CN201420051407 U CN 201420051407U CN 203720155 U CN203720155 U CN 203720155U
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China
Prior art keywords
gas
water
bottle
sample
sample feeding
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Withdrawn - After Issue
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CN201420051407.2U
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Chinese (zh)
Inventor
刘新红
高岩
张振华
王红莲
易能
范如芹
王岩
严少华
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Jiangsu Academy of Agricultural Sciences
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Jiangsu Academy of Agricultural Sciences
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Abstract

The utility model relates to a sample feeding device for measuring a gas phase of a water body release gas. In order to realize in-situ research of the water body release gas, especially nitrogen release, and solve the problem that interference-free accurate sample feeding to gas chromatography at field in-situ direct collection, accurate quantification, and accurate volume of the water body release gas can not be realized, the utility model discloses a sample feeding device for measuring the gas phase of the water body release gas. The sample feeding device comprises a gas chromatograph sample feeding hole, and further comprises a gas collecting bottle used for collecting the water body release gas, and a water storing tank, wherein a water outlet is formed in the bottom of the water storing tank, the water storing tank is communicated with the water collecting bottle through a water inlet pipe, and the water inlet pipe is inserted into the bottom of the gas collecting bottle through an insertion hole in a bottle plug. The sample feeding device further comprises a sample feeding pipeline, wherein one end of the sample feeding pipeline is arranged at a bottle opening of the gas collecting bottle through the insertion hole in the bottle plug, and the other end of the sample feeding pipeline is communicated with the gas chromatograph sample feeding hole. According to the sample feeding device, normal sample feeding of gas chromatography detection at a normal pressure state is realized, intermediate links such as sampling are prevented, and the problems such as pollution to a sample by air are prevented.

Description

For water body, discharge the sampling device that gas gas phase is measured
Technical field
The present invention relates to environmental monitoring field, particularly relate to water body environment monitoring field, more specifically relate to a kind of sampling device that discharges gas gas phase mensuration for water body.
Background technology
Water body is except having methane isothermal chamber gas discharging, and photosynthesis is understood releasing oxygen, and nitration denitrification process can discharge nitrogen and nitrous oxide gas.Wherein, nitrogen release may be one of water body important channel that especially eutrophication water denitrogenation realization purifies.The rule of further investigation eutrophication water liberating nitrogen gas, significant for the denitrogenation purification of greenhouse gas emission and eutrophication water.Realize directly collection and the research of original position that water body discharges gas, first will solve collection mode and the assay method problem of sample.In air, contain 78% nitrogen and 21% oxygen, and diffusion and mobility extremely strong, very easily cause sample contamination, so must have specific method and strict anti-seep measure, in guarantee sample collection and mensuration process, be not subject to the leakage pollution of air.
Collection method for gaseous sample, common have vacuum airbag method, a Dewar bottle method, in order to guarantee that collecting gas avoids air pollution, therefore these two kinds of gas producing devices are before gas production, all need through application of vacuum, complicated operation and require highly, vacuum suction facility and vacuum airbag, the cost of Dewar bottle with extraordinary sealing-plug mouth are also higher, and field complex environment while especially operating under the water surface operating condition difficulty larger.Secondly, the function of vacuum airbag and Dewar bottle only limits to gas collecting process.When follow-up while carrying out stratographic analysis, particularly during rigorous analysis, gaseous sample must be extracted out, now as easy as rolling off a log generation secondary pollution.Meanwhile, utilize it can not realize the Accurate Measurement of sample overall volume; The 3rd; for the research of water body release gas, be deep into the air release of water-bed and bed mud; in gas collector, often having the foreign material such as shale and algae adheres to; vacuum gas production bag and Dewar bottle by aciculiform sampling thief in sampling process, very easily stop up, be obviously not suitable for the gas collection under this condition.
In addition, for the detection of gaseous sample, as nitrogen, oxygen, this class gas of methane, adopt gas chromatography to carry out the technology of Accurate Analysis more complete, the valve formula sampling system based on six-way valve and ten-way valve is guaranteed the accuracy of sample size.Yet, realize the Accurate Analysis to sample, first need in the sampling system of the input gas chromatography of the accurate ne-leakage of designated volume sample.But, high for content in this air of nitrogen, the easy gas that pollution easily occurs in sample introduction process, headspace sampling method, online sample introduction and direct water sample injection all can not be directly used in the direct injected of atmosphere gas sample.
Summary of the invention
In order to realize water body, discharge the gas original position research that especially nitrogen discharges, solve water body and discharge the directly collection of field original position, accurate quantification and the accurate volume ground of gas to the problem of the noiseless accurate sample introduction of gas chromatography.The invention discloses a kind of sampling device that discharges gas gas phase mensuration for water body, so that more convenient, to realize exactly water body release gas detection, especially nitrogen etc. are easily by the detection of air-polluting gaseous sample.
We disclose a kind of sampling device that discharges gas gas phase mensuration for water body, comprise gas chromatograph injection port, also comprise and collect the gas bottle that has water body to discharge gas, and the bottle stopper that described gas bottle bottleneck is offered two patchholes seals; Also include water tank, the bottom of described water tank offers water delivering orifice, and is communicated with gas bottle by water inlet pipe, and described water inlet pipe is inserted into gas bottle bottom by the patchhole on bottle stopper, is also provided with water valve on described water inlet pipe; Also include sample channel, described sample channel one end is arranged at gas bottle bottle mouth position by the patchhole on bottle stopper, and the other end is communicated with gas chromatograph injection port.
Thereby the water tank, gas bottle, the gas chromatograph that are interconnected have been formed.Between water tank and gas bottle, by water inlet pipe, be communicated with, gas bottle and gas chromatograph, be by sample channel, to be communicated with between the injection port of gas chromatograph specifically, and then form a complete connectivity structure.
Due to the port of water inlet pipe and the port of sample channel, the position in gas bottle is different, specifically, because the port of water inlet pipe is the bottom that is positioned at gas bottle, so the water in water tank enters into the bottom of gas bottle by water inlet pipe, the water liquid layer that height of formation increases gradually; And the port of sample channel is positioned at the bottle mouth position of gas bottle, therefore, it can not interfered by water liquid, gas in gas bottle directly enters into gas chromatograph thus, without further increase the process sampling in gas bottle, avoided the problem of the air pollution sample of as easy as rolling off a log appearance in this flow process.
And in traditional mode, all having sampling---therefore this process of sample introduction, in order to guarantee that in this flow process, sample is not contaminated, is all generally to adopt extremely harsh sampling---sampling condition.For nitrogen, this in air the very high sample of content, its condition is well imagined, so the accuracy of its sample introduction is more doubtful, simultaneously for guarantee that accurate sampling, sample introduction pay condition equipment cost be also great.
Further, we also disclose and on described sample channel, have also been provided with dring silicon sebific duct.Due in continuous sample introduction process, may carry micro-steam, therefore on sample channel, being provided with dring silicon sebific duct can absorption of residual stay ducted moisture, guarantees the drying regime that enters gas chromatograph sample.
Closer, we also disclose and on described sample channel, have also been provided with peristaltic pump.The object of doing is like this to provide the power system of a redundancy, when hydraulic pressure is not enough to gas to be pressed into, utilizes the power of peristaltic pump that gas is imported into gas chromatograph.
Meanwhile, we also disclose 0.5 ~ 1.5 centimetre of the termination distance set gas cylinder bottom of described water inlet pipe.And then the validity of assurance hydraulic pressure to gas effect.
Finally, the distance that we also disclose between the termination of described sample channel and gas bottle bottle stopper bottom is less than 0.5 centimetre.Thereby better guarantee to collect the height of gas, prevent that too much steam from sneaking into.
Meanwhile, we will further supplement disclosed, and the gas bottle is here the first container of gas collection, when using as a kind of container of collecting gas, gas bottle is inverted, and it is full of to water in advance, then utilize draining ratio juris to collect water body and discharge gas.
Based on this theory, we can make the mode that two-part engages by the pipe section outside the pipe section in bottle and bottle.That is to say, water inlet pipe and sample channel be at the partial fixing of gas bottle inside, and at bottle mouth position, a fitting piece is set, and can be glass tube, or spiral connector, then, when different use states, replaces outside pipeline.
Adopt after technical scheme disclosed in this invention, realized under atmospheric pressure state, the direct injected of gas chromatographic detection, has avoided the intermediate links such as sampling, has stopped the problems such as air pollution sample that therefore produce.
Accompanying drawing explanation
Fig. 1 discharges for water body the sampling device schematic diagram that gas gas phase is measured;
Fig. 2 is the schematic diagram under gas bottle gas collection state;
Fig. 3 is that the relative peak area of three kinds of sample modes in different storage times compares schematic diagram;
In Fig. 3, BFW is gas bottle sample detection result; VB is vacuum bag sample detection result; VV is Dewar bottle sample detection result.
Embodiment
Below in conjunction with the drawings and specific embodiments, further illustrate the present invention.
Embodiment 1
As shown in Figure 1, a kind of sampling device that discharges gas gas phase mensuration for water body, comprises gas chromatograph injection port 7, also comprises and collects the gas bottle 4 that has water body to discharge gas, and the bottle stopper that described gas bottle 4 bottlenecks are offered two patchholes seals; Also include water tank 1, the bottom of described water tank 1 offers water delivering orifice, and is communicated with gas bottle 4 by water inlet pipe 2, and described water inlet pipe 2 is inserted into gas bottle 4 bottoms by the patchhole on bottle stopper, on described water inlet pipe 2, is also provided with water valve 3; Also include sample channel 8, described sample channel 8 one end are arranged at gas bottle 4 bottle mouth positions by the patchhole on bottle stopper, and the other end is communicated with gas chromatograph injection port 7.
Thereby the water tank 1, gas bottle 4, the gas chromatograph injection port 7 that are interconnected have been formed.Between water tank 1 and gas bottle 4, by water inlet pipe 2, be communicated with, gas bottle 4 and gas chromatograph, be by sample channel, to be communicated with 8 between the injection port 7 of gas chromatograph specifically, and then form a complete connectivity structure.
Adopt in the present embodiment preferred version, on described sample channel 8, be also provided with dring silicon sebific duct 5.
Further, also preferably have in the present embodiment scheme, on described sample channel 8, be also provided with peristaltic pump 6.
During use, will in the water-storing bottle shown in figure 1, be full of water.Then bottom water delivering orifice is connected with the air intake opening of sample bottle, and fills water completely in junction and pipeline, without any gas.The sample channel 8 of gas bottle 4 is directly connected with the sample feeding pipe of gas chromatography 9 by dring silicon sebific duct 7.Wherein, the moisture content of dry silica gel glass-tube 5 in order to retain in suction line, peristaltic pump 6 guarantees that gaseous samples are stable, one direction is to the Flow Sampling of gas chromatography.While starting sample detection, press shown in Fig. 1, water-storing bottle 1 and the water inlet pipe 2 of gas bottle 4 are connected, adjust the rotating speed of peristaltic pump 6, then open successively water intaking valve 3, peristaltic pump 6, gaseous sample will enter chromatographic analysis systems along sample channel 8 drying silicone tubes 5 and peristaltic pump 6.After gas chromatographic sample introduction finishes, close successively water intaking valve 3 and peristaltic pump 6, sample introduction finishes.
Explanation as a supplement, while gathering gas, gas bottle 4 is inverted, as shown in Figure 2, wherein, for the time being using sample channel 8 as drainpipe, using water inlet pipe 2 as sampling pipe, gas enters into gas bottle 4 by water inlet pipe 2, and the water in gas bottle 4 is discharged by sample channel 8, thereby realize the collection that water body discharges gas.
Embodiment 2
First sample bottle is filled to pure water, choose arbitrarily a kind of normal mixture body, in the normal mixture body of selecting in the present embodiment, contain N 2be 15.5%, carbon dioxide 2.1%, methane 43.3%, is stored in the normal mixture body of equivalent in vacuum bag, Dewar bottle and gas bottle respectively, for follow-up accuracy, detects.
Normal mixture body for vacuum bag and Dewar bottle storage adopts traditional sample detection method,
(1) regular injection formula input mode: respectively with vacuum bag and Dewar bottle storage standards mixed gas, do to contrast with airtight pin gas production and to the mode of gas chromatography sample injection and analyze.Sampling time is the 0th, 1,2,3,5,7 day.Same standard concentration mixed gas will be stored in vacuum bag and Dewar bottle.While starting sample introduction, adopt airtight pin from the rubber stopper of vacuum bag and Dewar bottle, to prick in vacuum bag/Dewar bottle and get gas respectively, then got gas is injected into stratographic analysis post from the analytical column mouth of chromatogram, from control software or the control panel of gas chromatography, selects to start to analyze at once afterwards.According to the integration situation on gas chromatography software, the peak area at each sample peak is carried out to integral and calculating.
Normal mixture body for gas bottle storage adopts disclosed sample detection method in the present invention,
(2) according to the mode in embodiment 1, carry out sample detection: utilize gas bottle collected specimens, and carry out pipeline connection according to Fig. 1, open water intaking valve 3 and peristaltic pump 6 beginning sample introductions.Sampling time is the 0th, 1,2,3,5,7 day.When sample introduction finishes, from control software or the control panel of gas chromatography, select to start sample introduction analysis at once.According to the integration situation on gas chromatography software, the peak area at each sample peak is carried out to integral and calculating.
The related data of aforementioned gas chromatographicanalyzer device is as follows: the gaseous sample gathering in this embodiment adopts Shimadzu GC2000 gas chromatograph to analyze, and sampling system is joined quantity tube and the ten logical sampling valve auto injections of 1ml, 70 ℃ of column temperatures, N 2, CH 4, CO 2detecting the detecting device adopting is thermal conductivity detector (TCD) (TCD), and electric current is 70mA, 200 ℃ of detector temperatures, and high-purity hydrogen is as carrier gas, and flow velocity is 8ml/min.
After the analysis of each time point finishes, according to calculated by peak area average relative peak area, respectively the nitrogen peak area of each time point of gas bottle input mode and regular injection formula input mode and the sampling time nitrogen peak area of the 0th are separately compared.Shown in result Fig. 3, as seen from Figure 3, the nitrogen average relative peak area of gas bottle input mode in 7 days remains between 99.5-108.5%, kept stable.And the nitrogen average relative peak area of injecting type input mode (comprising two kinds of modes of vacuum bag and Dewar bottle) is along with the prolongation in storage time constantly increases, be up to sampling 161.1% and the 217.7%(Dewar bottle at zero point).This may be entry needle sample sack/Dewar bottle rubber stopper that repeatedly punctures, and airborne nitrogen is infiltrated through in sample sack/Dewar bottle and caused nitrogen gas concn in sample to continue to raise by penetration damage face.
Visible, the inventive method can continue for sample analysis, the possibility of not damaged face and air penetration contaminated samples.

Claims (5)

1. for water body, discharge the sampling device that gas gas phase is measured, comprise gas chromatograph injection port, it is characterized in that: also comprise and collect the gas bottle that has water body to discharge gas, the bottle stopper that described gas bottle bottleneck is offered two patchholes seals; Also include water tank, the bottom of described water tank offers water delivering orifice, and is communicated with gas bottle by water inlet pipe, and described water inlet pipe is inserted into gas bottle bottom by the patchhole on bottle stopper, is also provided with water valve on described water inlet pipe; Also include sample channel, described sample channel one end is arranged at gas bottle bottle mouth position by the patchhole on bottle stopper, and the other end is communicated with gas chromatograph injection port.
2. the sampling device that discharges gas gas phase mensuration for water body according to claim 1, is characterized in that: on described sample channel, be also provided with dring silicon sebific duct.
3. the sampling device that discharges gas gas phase mensuration for water body according to claim 1 and 2, is characterized in that: on described sample channel, be also provided with peristaltic pump.
4. the sampling device that discharges gas gas phase mensuration for water body according to claim 1, is characterized in that: 0.5 ~ 1.5 centimetre of the distance set gas cylinder bottom, termination of described water inlet pipe.
5. the sampling device that discharges gas gas phase mensuration for water body according to claim 1, is characterized in that: the distance between the termination of described sample channel and gas bottle bottle stopper bottom is less than 0.5 centimetre.
CN201420051407.2U 2014-01-27 2014-01-27 Sample feeding device for measuring gas phase of water body release gas Withdrawn - After Issue CN203720155U (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103792310A (en) * 2014-01-27 2014-05-14 江苏省农业科学院 Sampling device for measuring water body release gas phase
CN111948310A (en) * 2020-08-10 2020-11-17 华东师范大学 Nitrous oxide sample introduction analysis method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103792310A (en) * 2014-01-27 2014-05-14 江苏省农业科学院 Sampling device for measuring water body release gas phase
CN111948310A (en) * 2020-08-10 2020-11-17 华东师范大学 Nitrous oxide sample introduction analysis method and application thereof

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Granted publication date: 20140716

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AV01 Patent right actively abandoned

Granted publication date: 20140716

Effective date of abandoning: 20160217