CN107192786B - The enrichment preparation facilities and its method of gas in a kind of water body - Google Patents
The enrichment preparation facilities and its method of gas in a kind of water body Download PDFInfo
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- CN107192786B CN107192786B CN201710539252.5A CN201710539252A CN107192786B CN 107192786 B CN107192786 B CN 107192786B CN 201710539252 A CN201710539252 A CN 201710539252A CN 107192786 B CN107192786 B CN 107192786B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The present invention relates to the enrichment preparation facilities and its method of gas in a kind of water body, including water sample metering units, de aerated water preparation unit, gas dosing unit, digital supervision and operating system unit；The water sample metering units are used to measure the volume of water sample to be measured for being actually used in degassing；The de aerated water preparation unit is used to be de-gassed saturated salt solution storage；The gas dosing unit is used to carry out quantitative measurment to the volume of water sample to be measured abjection gas.Technical scheme passes through the optimization, improvement and integrative design for vacuum outgas enriching apparatus structure and material, innovate vacuum section valve arrangement, introduce digital automatic control technology, form and gas in natural water is enriched with by vacuum outgas method, with reference to gas chromatographic analysis means, the analysis method and its enriching apparatus of ppt grades of content gas (such as methane) in water body can be measured, is adapted to geological prospecting to be tested with the lab analysis test in environmental monitoring and boat-carrying with the field assay under the conditions of the wild environment of land.
Description
Technical field
The present invention relates to technical field of geological exploration, and in particular to the enrichment preparation facilities of gas and its side in a kind of water body
Method.
Background technology
Methane content is the leading indicator of Environmental Monitoring and Assessment in natural water, and methane content data are marine sites in seawater
Strong sign parameter existing for oil-gas reservoir in oil-gas exploration, meanwhile, it is also that marine site oil gas is opened to monitor methane content change in seawater
The effective technology means of oil gas leakage are taken precautions against in hair.However, methane content is very low in natural water under normal circumstances, it is carried out
Quantitative determine relatively difficult, alternative technology ways and means is limited.Gas chromatography is the micro and trace of quantitative detection
The effective technology method of gas componant is measured, but conventional gas phase chromatographic process can not directly measure the methane content in seawater, need
Using purge and trap-gas-chromatography combination method, but the cold trapping methane gas using liquid nitrogen cooling is needed during measure,
Equipment and technology is complicated, inconvenient, is not particularly suitable for boat-carrying on-the-spot test.Current state-of-the-art technological means is to use infrared spectrum
Technology directly implements seawater methane content test, -5 DEG C of Applicable temperature~30 DEG C, but this method device therefor costliness, and measures
Scope is in 30nmol/L~5000nmol/L, unsuitable trace analysis.
Main stream approach currently used for dissolved methane content in the water bodys such as test surface water, underground water, seawater can be divided into two
Class, first, first pass through vacuum degasser obtains dissolved methane gas from water body, then carries out gas chromatographic analysis；Another
It is directly to be measured by methane transducer.Wherein, the utility model patent of Application No. CN201420224819.1 discloses one
Kind liquid solution gas simple vacuum degasser, but it is the simple glass device for applying mechanically hose connection, and easy gas leakage, uses
In be full manual operations, time-consuming and laborious, effect is extremely low, and needs man-made assembly, glass apparatus used it is frangible, it is necessary to stablize
Operating environment, is not suitable for field in-situ analysis, the field assay being not particularly suitable under the mobile status such as boat-carrying, it is impossible to meets marine
Oil-gas exploration and development requirements of one's work；Most important, its test error is big, and quality is difficult to ensure, be suitable only for methane concentration compared with
The analysis of high water body example, the restricted application in geological prospecting and environmental monitoring.Although and methane transducer operation side
Just, it is easy to carry, or but be not suitable for trace analysis, or it is expensive, it is difficult to promote the use of.
The content of the invention
It is an object of the invention to provide the enrichment preparation facilities and its method of gas in a kind of water body, solves the prior art
Concentration range deficiency, the analysis quality analyzed for gas content in water body be difficult to ensure, be not suitable for field in-situ analysis, cannot
Meet geological prospecting and the technical problem of the field in-situ analysis test needs in environmental monitoring.
To achieve the above object, the technical solution adopted by the present invention is：
The vacuum outgas enriching apparatus of gas in a kind of water body, including water sample metering units, de aerated water preparation unit, gas
Metering units, digital supervision and operating system unit；
The water sample metering units include sample cell and circuit switch, and the water sample metering units are used to preserve to be measured
Water sample, metering are actually used in the volume of water sample of degassing；
The de aerated water preparation unit includes de aerated water and prepares part and de aerated water storage part, and the de aerated water prepares single
Member is used to be de-gassed saturated salt solution, and the saturated salt solution after degassing is stored；
The gas dosing unit includes water sample degassing section to be measured, gas collecting portion and gas metering section, described
Gas dosing unit is used to prepare abjection gas and the volume to deviating from gas carries out quantitative measurment；
The digital supervision includes computer, vacuum pump, gas pressure sensor, two-port valve, three with operating system unit
Port valve, intelligent switch, digital communication component；The intelligent switch refers to controlling corresponding component after computer instruction is received
Open and close or the component for changing component working mode, such as numerical control circuit switch；The digital communication component is to link up to calculate
The component of digital communication between machine and intelligent switch, such as digital communication interface, data cable；
The triple valve includes No.1 triple valve, No. two triple valves, No. three triple valves, and the two-port valve includes No.1 two-way
Valve, No. two two-port valves, No. three two-port valves, No. four two-port valves, No. five two-port valves, the vacuum pump include No.1 vacuum pump, No. two
Vacuum pump, the gas pressure sensor include No.1 gas pressure sensor, No. two gas pressure sensors；
Further, the sample cell is provided with water sample loaded line, and pond is internally provided with float, is provided with and floats outside pond
The circuit switch of son linkage；
Further, the de aerated water, which prepares part, includes cistern, degassing hydroecium, the cistern and the de aerated water
Room is connected by the No.1 two-port valve, is connected between the degassing hydroecium and the No.1 vacuum pump by No. three triple valves
Connect, the degassing hydroecium is directly connected to No. two gas pressure sensors；
The de aerated water storage unit point includes preparing the degassing hydroecium of partial sharing with the de aerated water；
Further, the water sample degassing section to be measured includes degassing room, and the degassing room leads to No. two vacuum pumps
Cross No. two triple valves connection；
The gas collecting portion includes gas volume quantity tube, air hatch, and the No.1 gas pressure sensor is set
Below the sample tap, the gas volume quantity tube is directly connected with the degassing room and No.1 gas pressure sensor；
Further, the gas dosing part includes pressure-equalizing pipe, and the pressure-equalizing pipe passes through described No. two two
Port valve is connected with the degassing hydroecium, is connected by No. three two-port valves with the degassing room, acts on the gas volume
Quantity tube, balances for regulating system integral pressure, ensures to carry out body to water sample to be measured abjection gas under required pressure condition
Product measurement；
Further, the No.1 gas pressure sensor, No. two gas pressure sensors, No.1 vacuum pump, No. two it is true
Empty pump, No.1 triple valve, No. two triple valves, No. three triple valves, No.1 two-port valve, No. two two-port valves, No. three two-port valves, No. four two
Port valve, No. five two-port valves are respectively provided with independent driving part, power supply part, the No.1 gas pressure sensor, No. two gases
Pressure sensor, No.1 vacuum pump, No. two vacuum pumps, No.1 triple valve, No. two triple valves, No. three triple valves, No.1 two-port valve,
No. two two-port valves, No. three two-port valves, No. four two-port valves, the power supply part of No. five two-port valves, driving part are by described
Digital communication component, intelligent switch are connected with the computer；
Further, the two-port valve covered in vitro including pipe valve, needle, magnet, electromagnet, sealing gasket for valve, needle it is close
Seal ring, needle sealing ring cap, valve seal ring, the needle are arranged in the valve body overcoat, and the magnet is fixed on described
On needle, the electromagnet is fixed on the inside of the valve body overcoat, and the needle sealing ring and the needle sealing ring cap are surround
The needle is set, and described needle one end is provided with the sealing gasket for valve, and the valve seal ring is socketed along outside the valve body
Choma is set around valve body；
The triple valve is connected and composed for two two-port valves by threeway bridge joint.
The invention also discloses the analysis method using the vacuum outgas enriching apparatus of gas in above-mentioned water body, including such as
Lower step：
1) the No.1 two-port valve, No. two two-port valves are closed, saturated salt solution is injected into the cistern, opens described one
Number two-port valve, makes saturated salt solution enter the degassing hydroecium from the cistern, closes the No.1 two-port valve, described in connection
Gas circuit between No.1 vacuum pump and the degassing hydroecium, required vacuum is evacuated to the No.1 vacuum pump by the degassing hydroecium
Degree, adjusts No. three triple valves, and the gas circuit for cutting off the No.1 vacuum pump with the degassing hydroecium is connected, the saturation that must deaerate food
Brine；
2) water outlet that the No.1 triple valve cuts off the sample cell is adjusted, water sample to be measured is injected into the sample cell,
No. three two-port valves, No. four two-port valves are closed, the gas circuit between No. two vacuum pumps and the degassing room is connected, uses
The degassing room and the gas volume quantity tube are evacuated to required vacuum by No. two vacuum pumps, adjust No. two threeways
Valve, the gas circuit for cutting off No. two vacuum pumps with the degassing room are connected, adjust the No.1 triple valve, make set amount water to be measured
From the sample cell after the quantity tube slowly enters the degassing room, the quantity tube for closing the No.1 triple valve leads to sample
Road, treats in water sample that gas abjection is completed, must be enriched with needed for gas abjection gas；
3) No. five two-port valves are closed, adjust No. three triple valves, the degassing hydroecium is communicated with ambient air,
No. two two-port valves, No. three two-port valves are opened successively, and the degassing saturated salt solution allowed in the degassing hydroecium enters institute
State in degassing room, abjection gas is pressed in the gasometry pipe, No. three two-port valves is closed, reads the gas volume
The volume of gas, the No.1 gas pressure sensor pressure value and environment temperature in quantity tube, and determine from the gas volume
Gas is extracted in buret to be analyzed；
4) analysis terminates, and adjusting the No.1 triple valve makes the gasometry pipe be communicated with atmospheric environment, described in opening
No. four two-port valves, drain the water in the degassing room；
5) adjust the No.1 triple valve and drain remaining water sample in the sample cell.
Further, the required vacuum described in step 1) is 160Pa, and the required vacuum described in step 2) is
120Pa。
The method of the present invention has the following advantages that：
Technical scheme overcomes the deficiencies in the prior art well, in being analyzed based on hydrocarbon geochemical exploration Acid Hydrolytic Hydrocarbon
Light hydrocarbon gas are enriched with preparation method principle, by the optimization, improvement and integrative design for vacuum outgas enriching apparatus structure,
Vacuum section valve arrangement is innovated, digital automatic control technology is introduced, using integrally curing structure design, forms and taken off by vacuum
The automation equipment that gas method is enriched with the gases such as methane in natural water, and established with reference to gas chromatographic analysis means
The analysis method of methane content in the water bodys such as seawater is measured, has reached the technique effect that can measure ppt grades of methane contents, so that
Solve the prior arts such as existing purge and trap gas chromatography, method of infrared spectrophotometry, liquid solution gas vacuum degasser
Means are for the analytical concentration scope deficiency in methane content analysis in water body, analysis quality is difficult to ensure, are not suitable for field shows
Field analysis, cannot meet the problem of geological prospecting tests needs with the field in-situ analysis in environmental monitoring, be suitable for geology and survey
Visit and tested with the lab analysis test in environmental monitoring and boat-carrying with the field assay under the conditions of the wild environment of land.
1) apparatus structure design science, makes the vacustat of degassing and secure using design is cured, especially presses
The design of dynamic balance pipe, not only solves the gas volume metering problem under the conditions of consolidated structures, also achieves standard state gas
Body volume is directly read；
2) air-tightness of vacuum section valve (two-port valve and triple valve) is good, is the core component of ensuring equipment degasifying effect, and
Easy to digital control, maintain easily；
3) by digital automatic control, human error is avoided, and it is easy to operate, it is easy to spread；
4) method for automatically controlling fixed amount volume sample by float and on-off circuit and loading is provided；
5) method operated by gas pressure automatic identification control device is provided；
6) method that standard state volume metering is directly carried out to abjection gas by pressure control is provided.
Brief description of the drawings
Fig. 1 is the structure diagram of the vacuum outgas enriching apparatus of gas in water body of the invention；
Fig. 2 is the two-way valve structure schematic diagram of the vacuum outgas enriching apparatus of gas in water body of the invention；
Fig. 3 is the triple valve structure diagram of the vacuum outgas enriching apparatus of gas in water body of the invention.
1- sample cells, 2- degassings room, 3- gas volume quantity tubes, 4- sample taps, 5- pressure-equalizing pipes, 6- cisterns, 7-
Deaerate hydroecium, 8- No.1 vacuum pumps, No. bis- vacuum pumps of 9-, 10- No.1 triple valves, No. bis- triple valves of 11-, No. tri- triple valves of 12-,
13- No.1 gas pressure sensors, No. bis- gas pressure sensors of 14-, 15- No.1 two-port valves, No. bis- two-port valves of 16-, 17- tri-
Number two-port valve, No. tetra- two-port valves of 18-, No. five two-port valves of 19-, 20- computers, 21- tube bodies, 22- valve body overcoats, 23- needles,
24- magnet, 25- electromagnet, 26- sealing gasket for valve, 27- needle sealing rings, 28- needle sealing ring caps, 29- valve seal rings,
30- threeways bridge, a- water samples loading minimum altitude line, b- floats, c- circuit switch, c1- liquid level home-position contact, c2- liquid level
Terminate contact.
Embodiment
Following embodiments are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
As shown in Figure 1, in a kind of water body the vacuum outgas enriching apparatus of gas composition：Including water sample metering units, take off
Air water preparation unit, gas dosing unit, and digital supervision and operating system unit.
The water sample metering units are used to preserve water sample to be measured, and metering is actually used in the volume of water sample of degassing, including sample
Product pond 1；The sample cell 1 is provided with water sample loading minimum altitude line a, float b and circuit switch c, circuit switch
Lower part is provided with liquid level home-position contact c1, top be provided with liquid level terminate contact c2；In sample loading procedure, No.1 threeway is opened
The water discharging valve of valve 10, makes the water sample in water sample pool 1 slowly discharge, the contact of circuit switch c decline with float b and
Movement, when c reaches liquid level home-position contact c1When connect circuit, triggering computer closes the water discharging valve of No.1 triple valve 10, together
When open sample introduction valve, make water sample via gas volume quantity tube 3 slowly enter degassing room 2, until c reach liquid level terminate contact
c2When, triggering computer closes the sample introduction valve of No.1 triple valve 10, while opens the water discharging valve of No.1 triple valve 10, discharges
Unnecessary water sample in sample cell 1.
The de aerated water preparation unit be used for saturated salt solution is de-gassed, and to the saturated salt solution after degassing into
Row storage, including cistern 6, degassing hydroecium 7, the two is connected by No.1 two-port valve 15.Further, deaerate hydroecium 7 and one
Connected by No. three triple valves 12 between number vacuum pump 8, be directly connected to No. two gas pressure sensors 14；
The gas dosing unit prepares gas in water sample and the volume to deviating from gas carries out quantitative measurment,
Including water sample degassing section, gas collecting portion and gas metering section；The degassing section includes degassing room 2, and deaerate room 2
It is connected with No. two vacuum pumps 9 by No. two triple valves 11, separately there are No. four two-port valves 18 to be used for the discharge after test and abandon water；
The gas collecting portion is directly connected with degassing room 2, including gas volume quantity tube 3, air hatch 4, No.1 gas pressure
Sensor 13 is arranged at by air hatch 4；The gas dosing part includes the two-way of two-port valve 16, three of pressure-equalizing pipe 5, two
Valve 17 and No. five two-port valves 19, pressure-equalizing pipe 5 are connected by No. two two-port valves 16 with degassing hydroecium 7, pass through No. three two-port valves
17 are connected with degassing room 2, act on gas volume quantity tube 3 and carry out cubing to abjection gas, separately have No. five valves 19 to use
In the unnecessary de aerated water of discharge.
The degassing enrichment process that the digital supervision is used for device with operating system is automatically brought into operation and is controlled, and is wrapped
Include computer 20 and by digital communication component and intelligent switch it is being connected with computer 20, for monitoring and manipulating No.1
8, No. two vacuum pumps 9 of vacuum pump, No.1 triple valve 10, two triple valve 11, three triple valve 12, No.1 gas pressure sensor
13rd, No. two gas pressure sensors 14,17, No. four two-port valves 18 of the two-port valve of two-port valve 16, three of No.1 two-port valve 15, two,
No. five two-port valves 19, the driving part of circuit switch c, power supply part.Computer, driving part, power supply part, number herein
Word communication component, the selection of intelligent switch and connection mode belong to the prior art, and applicant thinks to be described in detail.
The container and pipeline of described device are with surface is smooth, corrosion-resistant material makes.
Embodiment 2
As shown in figures 2-3, the two-port valve and the vacuum section valve that triple valve is special designing, by tube body and valve body two
Part forms, wherein, valve is arranged in tube body 21, and the switch of valve passes through sealing gasket for valve by the Bit andits control of needle 23
26 ensure sealing effect during valve closure；The displacement of needle is driven by magnet 24 and electromagnet 25, and the direction of its displacement passes through
The N poles and S poles matching status for changing electromagnet 25 and magnet 24 control；Needle sealing ring 27 and needle sealing ring cap 28 are needle
23 provide sealing；The integral sealing of valve body is provided by valve seal ring 29 and valve body overcoat 22.
Triple valve bridges 30 by a threeway for two two-port valves and is formed by connecting.
Embodiment 3
The operation principle and working method of gas vacuum degassing enriching apparatus in water body：
Device prepares the gas in water body by following main work links enrichment and measures its volume, for gas-chromatography point
Analysis：
1st, degassing saturated salt solution is prepared
No. two two-port valves 16 are closed, open No.1 two-port valve 15, allow saturated salt solution to enter degassing hydroecium 7 from cistern 6.
No.1 two-port valve 15 is closed, degassing hydroecium 7 is evacuated to vacuum with No.1 vacuum pump 8 reaches 160Pa, obtains degassing saturated common salt
Water.
2nd, the degassing of gas is enriched with water sample
Close 17, No. four two-port valves 18 of No. three two-port valves；Adjust No.1 triple valve 10, cut-out gas volume quantity tube 3 with
The connection in 1 direction of sample cell；No. two triple valves 11 are adjusted at the same time, degassing room 2 is connected with No. two vacuum pumps 9, it is big with environment
Air bound is exhausted；It is evacuated to vacuum with will deaerate room 2 and gas volume quantitative pipe 3 of No. two vacuum pumps 9 and is reached 120Pa.Cut-out two is true
Sky pump 9 is connected with the gas circuit for the room 2 that deaerates.No.1 triple valve 10 is adjusted, makes water sample to be measured from sample cell 1 through gas volume quantity tube
3 slowly enter in degassing room 2；After set amount water sample all enters the room 2 that deaerates from sample cell 1, No.1 three-way valve 10 is adjusted,
Cut off the connection of sample cell 1 and gas volume quantity tube 3.Treat that gas abjection is completed in water sample, must be enriched with the abjection of component to be measured
Gas.
3rd, metering abjection gas volume
No. five two-port valves 19 are closed, adjusting No. three triple valves 12 makes degassing hydroecium 7 be connected with ambient air；Open No. two two
Port valve 16, makes degassing saturated salt solution form water column in pressure-equalizing pipe 5；Open No. three two-port valves 17, allow degassing hydroecium 7 in
Degassing saturated salt solution enter degassing room 2 in, will abjection gas press in gas volume quantity tube 3.Treat in pressure-equalizing pipe 5
Water column forms positive pressure to gas in gas volume quantity tube 3, closes No. two two-port valves 16, adjusts No. five two-port valves 19 and allows pressure to put down
Water column in weighing apparatus pipe 5 slowly declines, and controls when No.1 gas pressure sensor 13 shows that pressure is 1 in gas volume quantity tube 3
A standard atmospheric pressure, or during according to the conversion of prevailing circumstances temperature to pressure corresponding to standard state volume, close No. five two-ways
Valve 19, reads the volume of gas in gasometry pipe 3.
Embodiment 4
The concrete operation step of gas vacuum degassing enriching apparatus in water body：
1) close air hatch 4 is covered.
2) No.1 triple valve 10,17, No. four two-port valves of two-port valve of two-port valve 16, three of No.1 two-port valve 15, two are closed
18th, No. five two-port valves 19；No. three triple valves 12 is connected the gas circuit of degassing hydroeciums 7 and No.1 vacuum pump 8, with atmospheric environment every
Absolutely；No. two triple valves 11 is connected No. two vacuum pumps 9 and the gas circuit of degassing room 2, completely cut off with atmospheric environment.
3) it is 1/2~4/5 full to it that saturated salt solution is filled into cistern 6.
4) water sample to be measured is slowly injected into sample cell 1, exceedes water sample loaded line a to the water surface.
5) water discharging valve of No.1 triple valve 10 is opened, the water sample in sample cell 1 is slowly discharged, until connecting and disconnecting of the circuit is opened
Close c and reach liquid level home-position contact c1, the water discharging valve of triggering computer closing No.1 triple valve 10.
6) No. two vacuum pumps 9 are started, the pressure to No.1 gas pressure sensor 13 reaches setting value P1, adjust No. two three
Port valve 11, makes No. two vacuum pumps 9 completely cut off with degassing room 2, is connected with atmospheric environment.Close No. two vacuum pumps 9.
7) the sample introduction valve of No.1 triple valve 10 is opened, the water sample in sample cell 1 is slowly entered degassing room 2 and deaerates.Treat
Float b drops to setting height, and circuit switch c reaches liquid level and terminates contact c2, triggering computer closing No.1 triple valve
10 sample introduction valve.The water discharging valve of No.1 triple valve 10 is opened at the same time, discharges the unnecessary water sample in sample cell 1.
8) start No.1 vacuum pump 8, drop to setting value P to 14 pressure of gas pressure sensor2, adjust No. three triple valves
12, No.1 vacuum pump 8 is completely cut off with degassing hydroecium 7, connected with atmospheric environment.Close No.1 vacuum pump 8.
9) No.1 two-port valve 15 is opened, the saturated salt solution in cistern is slowly entered degassing hydroecium 7, to No. two gases
14 pressure of pressure sensor rises to setting value P3, close No.1 two-port valve 15.
10) No. three triple valves 12 are adjusted, No.1 vacuum pump 8 is connected with degassing 7 gas circuit of hydroecium, completely cuts off with atmospheric environment；
Start No.1 vacuum pump 8, drop to setting value P to No. two 14 pressure of gas pressure sensor4, No. three triple valves 12 are adjusted, are made
Vacuum pump 8 completely cuts off with degassing hydroecium 7, is connected with atmospheric environment.Close No.1 vacuum pump 8.
11) No. three triple valves 12 are adjusted, degassing hydroecium 7 is connected with atmospheric environment.
12) No. two two-port valves 16 are opened, the degassing saturated salt solution in degassing hydroecium is entered in pressure-equalizing pipe 5, extremely
Pressure balance between the two.
13) water sample degassing is completed in room 2 to be de-gassed, opens No. three two-port valves 17, degassing saturated salt solution is entered degassing
In room 2, the pressure to No.1 gas pressure sensor 13 rises to setting value P5, close No. two two-port valves 16；Open No. five two
Port valve 19, makes saturated salt solution column in pressure-equalizing pipe 5 slowly decline, the pressure to No.1 gas pressure sensor 13 drops to
Current environment atmospheric pressure (or according to current environmental temperature conversion to the pressure corresponding to standard state volume) P0When, close five
Number two-port valve 19, turns off No. three two-port valves 17.
14) read and record gas volume in gasometry pipe 3, the pressure value P of No.1 gas pressure sensor 130, ring
Border temperature.
15) certain volume gas is extracted from gas volume quantity tube 3 by sample tap 4 with quantitative gas syringe, noted
Enter in gas chromatograph and analyze.
16) repeat step 12~15, can sampling analysis again.
17) analysis terminates, and adjusts No.1 triple valve 10, gas volume quantity tube 3 is communicated with atmospheric environment；Open No. four
Two-port valve 18, drains the water in degassing room 2.
Embodiment 5
Methane content analysis example in water body：
1) start gas chromatograph, instrument operating condition and analysis condition are set, it is dense with 5 kinds of differences after instrument stabilizer
The Standard Gas of Methane calibrating instrument of degree, each 200 μ L of sampling volume, determine the value of a and b in formula 1.
G=a A+b (1)
In formula：G is the volume fraction (mL/L) of methane in calibrating gas；
A is the gas-chromatography peak area of methane；
A and b is the constant (mL/L) determined by gas chromatograph and its operating condition.
2) water body example degassing enrichment is carried out according to the step of embodiment 4, and takes 200 μ L abjection gaseous sample injection gas phases
In chromatograph, analysis obtains methane chromatographic peak area A.Methane content in water body is calculated by formula 2.
In formula：C is the content (nmol/L) of methane in water sample；
A and b is the constant (mL/L) determined by gas chromatograph and its operating condition；
A is the gas-chromatography peak area of methane；
G is abjection gas cumulative volume (L)；
W is the volume of water sample (L) for degassing；
P is gas pressure P in gas volume quantity tube 30(Pa)；
T is gas temperature (DEG C) in gas volume quantity tube 3, is considered as ambient air temperature.
3) the actual measurement condition of the specific sample in part and result are as follows：
Sample 1：
Water sample source：Tianjin seismic network, the Bohai Sea, seawater.
Volume of water sample：120mL.
Ambient air temperature：17℃.
Process control pressure：
| P0 | P1 | P2 | P3 | P4 | P5 |
| 101.3kPa | 120Pa | 200Pa | 101.2kPa | 160Pa | 101.5kPa |
Analysis result：Methane content 3.56nmol/L.
Purge and trap gas-chromatography compares analysis result：Methane content 3.48nmol/L.
Sample 2：
Water sample source：Forests in Wanning, Hainan Islands, the South Sea, seawater.
Volume of water sample：120mL.
Ambient air temperature：28℃.
Process control pressure：
| P0 | P1 | P2 | P3 | P4 | P5 |
| 101.5kPa | 120Pa | 200Pa | 101.4kPa | 160Pa | 101.6kPa |
Analysis result：Methane content 2.46nmol/L.
Purge and trap gas-chromatography compares analysis result：Methane content 2.41nmol/L.
Sample 3：
Water sample source：Shandong Yantai, the Huanghai Sea, seawater.
Volume of water sample：120mL.
Ambient air temperature：21℃.
Process control pressure：
| P0 | P1 | P2 | P3 | P4 | P5 |
| 101.1kPa | 120Pa | 200Pa | 101kPa | 160Pa | 101.2kPa |
Analysis result：Methane content 2.16nmol/L.
Purge and trap gas-chromatography compares analysis result：Methane content 2.17nmol/L.
Sample 4：
Water sample source：Beijing Haidian, Yuyuan Lake, river water.
Volume of water sample：120mL.
Ambient air temperature：13℃.
Process control pressure：
| P0 | P1 | P2 | P3 | P4 | P5 |
| 101.3kPa | 120Pa | 200Pa | 101.2kPa | 160Pa | 101.5kPa |
Analysis result：Methane content 2.16nmol/L.
Purge and trap gas-chromatography compares analysis result：Methane content 2.06nmol/L.
Sample 5：
Water sample source：Yanqing County of Beijing, Guanting reservoir, lake water.
Volume of water sample：120mL.
Ambient air temperature：16℃.
Process control pressure：
| P0 | P1 | P2 | P3 | P4 | P5 |
| 101.3kPa | 120Pa | 200Pa | 101.2kPa | 160Pa | 101.5kPa |
Analysis result：Methane content 2.01nmol/L.
Purge and trap gas-chromatography compares analysis result：Methane content 1.97nmol/L.
Although above with general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (7)
1. the vacuum outgas enriching apparatus of gas in a kind of water body, it is characterised in that prepared including water sample metering units, de aerated water
Unit, gas dosing unit, digital supervision and operating system unit；
The water sample metering units include sample cell and circuit switch, and the water sample metering units are used to preserve water to be measured
Sample, metering are actually used in the volume of water sample to be measured of degassing；
The de aerated water preparation unit includes de aerated water and prepares part and de aerated water storage part, and the de aerated water preparation unit is used
It is de-gassed in saturated salt solution, and the saturated salt solution after degassing is stored；
The gas dosing unit includes water sample degassing section to be measured, gas collecting portion and gas metering section, the gas
Metering units are used to prepare abjection gas and the volume to deviating from gas carries out quantitative measurment；
The digital supervision and operating system unit include computer, vacuum pump, gas pressure sensor, two-port valve, triple valve,
Intelligent switch, digital communication component；
The triple valve include No.1 triple valve, No. two triple valves, No. three triple valves, the two-port valve include No.1 two-port valve,
No. two two-port valves, No. three two-port valves, No. four two-port valves, No. five two-port valves, the vacuum pump include No.1 vacuum pump, No. two vacuum
Pump, the gas pressure sensor include No.1 gas pressure sensor, No. two gas pressure sensors；
The water sample degassing section to be measured includes degassing room, and the degassing room and No. two vacuum pumps pass through No. two threeways
Valve connects；
The gas collecting portion includes gas volume quantity tube, air hatch, and the No.1 gas pressure sensor, which is arranged at, to be taken
Below sample mouth, the gas volume quantity tube is directly connected with the degassing room and No.1 gas pressure sensor；
The gas dosing part includes pressure-equalizing pipe, and the pressure-equalizing pipe passes through No. two two-port valves and the degassing
Hydroecium is connected, is connected by No. three two-port valves with the degassing room, the gas volume quantity tube is acted on, for adjusting
System integral pressure balances, and ensures to carry out water sample abjection air volume measurement to be measured under required pressure condition.
2. the vacuum outgas enriching apparatus of gas in a kind of water body as claimed in claim 1, it is characterised in that the sample cell
Water sample loaded line is provided with, the sample cell is internally provided with float, and the electricity with float linkage is provided with outside the sample cell
Road on-off switch.
3. the vacuum outgas enriching apparatus of gas in a kind of water body as claimed in claim 1, it is characterised in that the de aerated water
Preparing part includes cistern, and the de aerated water prepares part and further includes the de aerated water that partial sharing is stored with the de aerated water
Room, the cistern with it is described degassing hydroecium connected by No.1 two-port valve, it is described degassing hydroecium and the No.1 vacuum pump it
Between by No. three triple valves connect, it is described degassing hydroecium be directly connected to No. two gas pressure sensors.
4. the vacuum outgas enriching apparatus of gas in a kind of water body as claimed in claim 1, it is characterised in that the No.1 gas
Pressure sensor, No. two gas pressure sensors, No.1 vacuum pump, No. two vacuum pumps, No.1 triple valve, No. two triple valves,
No. three triple valves, No.1 two-port valve, No. two two-port valves, No. three two-port valves, No. four two-port valves, No. five two-port valves are respectively provided with independent
Driving part, power supply part, the No.1 gas pressure sensor, No. two gas pressure sensors, No.1 vacuum pump, No. two it is true
Empty pump, No.1 triple valve, No. two triple valves, No. three triple valves, No.1 two-port valve, No. two two-port valves, No. three two-port valves, No. four two
Port valve, the power supply part, the driving part of No. five two-port valves pass through the digital communication component, intelligent switch and the meter
Calculation machine is connected.
5. the vacuum outgas enriching apparatus of gas in a kind of water body as claimed in claim 1, it is characterised in that the two-port valve
Covered in vitro including pipe valve, needle, magnet, electromagnet, sealing gasket for valve, needle sealing ring, needle sealing ring cap, valve seal
Ring, the needle are arranged in the valve body overcoat, and the magnet is fixed on the needle, and the electromagnet is fixed on described
On the inside of valve body overcoat, the needle sealing ring and the needle sealing ring cap are set around the needle, and described needle one end is set
The sealing gasket for valve is equipped with, the valve seal ring is set along the valve body overcoat interface rings around valve body；
The triple valve is connected and composed for two two-port valves by threeway bridge joint.
6. a kind of analysis method using the vacuum outgas enriching apparatus of gas in water body as claimed in claim 1, its feature
It is, includes the following steps：
1) the No.1 two-port valve, No. two two-port valves are closed, saturated salt solution is injected into cistern, opens the No.1 two-way
Valve, makes saturated salt solution enter the degassing hydroecium from cistern, closes the No.1 two-port valve, connect the No.1 vacuum pump
With the gas circuit between the degassing hydroecium, the degassing hydroecium is evacuated to required vacuum with the No.1 vacuum pump, adjusts institute
No. three triple valves are stated, the gas circuit for cutting off the No.1 vacuum pump with the degassing hydroecium is connected, and obtains degassing saturated salt solution；
2) water outlet that the No.1 triple valve cuts off the sample cell is adjusted, water sample to be measured is injected into the sample cell, is closed
No. three two-port valves, No. four two-port valves, connect the gas circuit between No. two vacuum pumps and the degassing room, with described
The degassing room and the gas volume quantity tube are evacuated to required vacuum by No. two vacuum pumps, adjust No. two triple valves,
The gas circuit that No. two vacuum pumps are cut off with the degassing room is connected, and is adjusted the No.1 triple valve, is made set amount water sample to be measured
From the sample cell after the quantity tube slowly enters the degassing room, the quantity tube path of the No.1 triple valve is closed,
Treat in water sample that gas abjection is completed, must be enriched with needed for gas abjection gas；
3) No. five two-port valves are closed, adjust No. three triple valves, the degassing hydroecium is communicated with ambient air, successively
No. two two-port valves, No. three two-port valves are opened, the degassing saturated salt solution allowed in the degassing hydroecium enters described take off
In gas chamber, abjection gas is pressed in the gas volume quantity tube, No. three two-port valves is closed, reads the gas volume
The volume of gas, the No.1 gas pressure sensor pressure value and environment temperature in quantity tube, and determine from the gas volume
Gas is extracted in buret to be analyzed；
4) analysis terminates, and adjusting the No.1 triple valve makes the gasometry pipe be communicated with atmospheric environment, opens described No. four
Two-port valve, drains the water in the degassing room；
5) adjust the No.1 triple valve and drain remaining water sample in the sample cell.
7. as claimed in claim 6 using point of the vacuum outgas enriching apparatus of gas in water body as claimed in claim 1
Analysis method, it is characterised in that the required vacuum described in step 1) is 160Pa, and the required vacuum described in step 2) is
120Pa。
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