CN106289920B - A kind of hydrogen deuterium analysis water-like preparation system and its implementation - Google Patents
A kind of hydrogen deuterium analysis water-like preparation system and its implementation Download PDFInfo
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- CN106289920B CN106289920B CN201611015096.4A CN201611015096A CN106289920B CN 106289920 B CN106289920 B CN 106289920B CN 201611015096 A CN201611015096 A CN 201611015096A CN 106289920 B CN106289920 B CN 106289920B
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Abstract
The invention discloses a kind of hydrogen deuterium analysis water-like preparation systems, including the online gas inlet of hydrogen and inert gas air inlet, the flowmeter being connected to simultaneously with the online gas inlet of hydrogen and inert gas air inlet, air inlet is connect with flowmeter, gas outlet connects the oxidation reaction bed of condenser pipe, the sample tap being connected to condenser pipe, and the exhaust emissions channel being arranged between flowmeter and oxidation reaction bed；The pipeline that the online gas inlet of hydrogen is connected to flowmeter is equipped with the first valve；The pipeline that inert gas air inlet is connected to flowmeter is equipped with the second valve；The pipeline that flowmeter is connected to oxidation reaction bed is equipped with the 6th valve；The pipeline that oxidation reaction bed is connected to condenser pipe is equipped with the 8th valve, and the oxidation reaction bed is placed in a tubular heater.The present invention realizes the purpose that hydrogen isotope gas in hydrogen isotope separation system is oxidized to water sample, and isotope mass spectrometer is facilitated to be sampled analysis, improves hydrogen isotope analysis detection efficiency.
Description
Technical field
The present invention relates to a kind of hydrogen deuterium analysis water-like preparation system and its implementation.
Background technique
Go the hydrogen isotope separations technologies such as tritiated research platform, hydrogen isotope separation and cleaning test system flat for water
Platform, a set of efficient, accurate hydrogen isotope analysis method is very necessary.Currently, in the analysis method of hydrogen isotope,
Isotope mass spectrometer all has very big advantage no matter in terms of accuracy or measurement range.Isotope mass spectrometer, which utilizes, matches
The automatic sample handling system set, is arranged by sequence, can automatically analyze to most 100 water samples.
Existing technology is to carry out gas sample analysis by isotope mass spectrometer mostly, manual operation is not only needed to vary,
Detection, interpretation of result, and gaseous sample is also easy to maintain.And compared to gaseous sample, the use method letter of water sample
Single, storage is convenient, and sample is also not easy to be contaminated in Sampling analysis process, so will have for hydrogen isotope analysis work
Very big help, but the design about hydrogen isotope water sample conversion processing apparatus is at present substantially also in blank stage.
Summary of the invention
The purpose of the present invention is to provide a kind of hydrogen deuterium analysis water-like preparation system and its implementation, realize hydrogen isotope
Hydrogen isotope gas in separation system is oxidized to the purpose of water sample, so that isotope mass spectrometer is sampled analysis, improves hydrogen
Isotope analysis detection efficiency.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of hydrogen deuterium analysis water-like preparation system, including the online gas inlet of hydrogen and inert gas air inlet, simultaneously
The flowmeter being connected to the online gas inlet of hydrogen and inert gas air inlet, air inlet is connect with the flowmeter and inside
Oxidation reaction bed filled with metal oxide, the condenser pipe connecting with the oxidation reaction bed gas outlet, is connected to the condenser pipe
Sample tap, and be arranged between flowmeter and oxidation reaction bed and which is provided with the exhaust emissions channel of the 7th valve；
The pipeline that the online gas inlet of hydrogen is connected to flowmeter is equipped with the first valve；The inert gas air inlet and stream
The pipeline of meter connection is equipped with the second valve；The pipeline that the flowmeter is connected to oxidation reaction bed is equipped with the 6th valve；
The pipeline that the oxidation reaction bed is connected to condenser pipe is equipped with the 8th valve, and the oxidation bed is placed in a tubular heater
In.
Further, the invention also includes be arranged between flowmeter and exhaust emissions channel, the aluminium for loading hydrogen
Foil sampling bag；The aluminium foil sampling bag inlet end is connected to flowmeter, outlet side simultaneously with exhaust emissions channel and oxidation reaction
Bed connection, and the pipeline that aluminium foil sampling bag inlet end is connected to flowmeter is equipped with the 4th valve, outlet side while and tail gas
The pipeline that discharge-channel is connected to oxidation reaction bed is equipped with the 5th valve.
Still further, on the pipeline that the flowmeter is connected to oxidation reaction bed and be located at aluminium foil sampling bag inlet end with
Third valve is additionally provided between outlet side.
Preferably, the inert gas air inlet is nitrogen inlet.
For the safety for guaranteeing system operatio, pressure gauge is also connected at the air inlet of the oxidation reaction bed.
Preferably, the oxidation reaction bed is made of stainless steel.
According to above system structure, the present invention is based under same inventive concept, additionally provide two kinds of realities of the preparation system
Existing scheme is as follows respectively:
Scheme one
Itself the following steps are included:
(1) the online gas inlet of hydrogen is connected to the gas outlet of hydrogen isotope separation system, while by inert gas
Air inlet is connected to inertia gas cylinder；
(2) first, the four, the 5th valves are closed respectively, and are adjusted to the temperature of oxidation reaction bed using tubular heater
350 DEG C or more；
(3) open flowmeter and second, third, the six, the seven, the 8th valves, inert gas is passed through to system and is blown
Sweep 5min or more；
(4) the second, the 7th valve is closed respectively, and stopping is passed through inert gas, and then the flow parameter of preset flow meter, beats
The first valve is opened, hydrogen to be measured is passed through by the online gas inlet of hydrogen；
(5) hydrogen to be measured via oxidation reaction bed aoxidize and condensing tube condensation at liquid water after, in sample tap be discharged, this
When, water sample extraction is carried out using sampling bottle；
(6) the six, the 8th valves are closed respectively, open the 7th valve, and exhaust emissions is carried out by exhaust emissions channel；
(7) the first valve is closed, opens second, the six, the 8th valves respectively, and stop heated oxide reaction bed, then
Be loaded into inert gas to system purge 5min after, close flowmeter and second, third, the six, the seven, the 8th valves.
Scheme two
Itself the following steps are included:
(1) first, the four, the 5th valves are closed respectively, and are adjusted to the temperature of oxidation reaction bed using tubular heater
350 DEG C or more；
(2) open flowmeter and second, third, the six, the seven, the 8th valves, inert gas is passed through to system and is blown
Sweep 5min or more；
(3) third, the 7th valve are closed, then the flow parameter of preset flow meter, the four, the 5th valves is opened, by lazy
Property gas is as system carrier gas, by the hydrogen loading system to be measured in aluminium foil sampling bag；
(4) hydrogen to be measured via oxidation reaction bed aoxidize and condensing tube condensation at liquid water after, in sample tap be discharged, this
When, water sample extraction is carried out using sampling bottle；
(5) respectively close the four, the five, the six, the 8th valves, open third, the 7th valve, by exhaust emissions channel into
Row exhaust emissions；
(6) the six, the 8th valves are opened respectively, and stop heated oxide reaction bed, are then loaded into inert gas to system
Purge 5min after, close flowmeter and second, third, the six, the seven, the 8th valves.
Compared with prior art, the invention has the following advantages:
The configuration of the present invention is simple, process are reasonable, using metal oxide as filler, by hydrogen by way of heating
Gas is oxidized to water, so that under test gas sample is converted to water sample.Present invention hydrogen deuterium-oxide sample obtained can be supplied to equipped with certainly
The low resolution isotope mass spectrometer of dynamic water sample sample injector is analyzed.Also, compared to hydrogen deuterium sample, the use method letter of water sample
Conveniently, sample is also not easy to be contaminated in Sampling analysis process for single, storage, thus improves the analysis inspection of hydrogen isotope well
Survey efficiency.The present invention establishes a set of effective hydrogen isotope water sample conversion processing apparatus, has filled up industry blank, is the same position of hydrogen
The analysis work of element provides guarantee, and therefore, the present invention has substantive distinguishing features outstanding and significant progress.
Detailed description of the invention
Fig. 1 is system block diagram of the invention.
Fig. 2 is the flow diagram of online air inlet oxidation model.
Fig. 3 is the flow diagram of offline air inlet oxidation model.
Wherein, the corresponding title of appended drawing reference are as follows:
The online gas inlet of 1- hydrogen, the first valve of 2-, 3- inert gas air inlet, the second valve of 4-, 5- flowmeter,
6- third valve, the 4th valve of 7-, 8- aluminium foil sampling bag, the 5th valve of 9-, the 6th valve of 10-, the 7th valve of 11-, 12- pressure
Table, 13- oxidation reaction bed, the 8th valve of 14-, 15- condenser pipe, 16- sample tap, 17- exhaust emissions channel.
Specific embodiment
The invention will be further described with embodiment for explanation with reference to the accompanying drawing, and mode of the invention includes but not only limits
In following embodiment.
As shown in Figure 1, the present invention provides a kind of hydrogen deuterium analysis water-like preparation system, for by VPCE, LPCE and its
Hydrogen isotope gas in his hydrogen isotope separation system is oxidized to water sample, so that isotope mass spectrometer is sampled analysis.This
Invention include the online gas inlet 1 of hydrogen, inert gas air inlet 3, flowmeter 5, aluminium foil sampling bag 8, oxidation reaction bed 13,
Condenser pipe 15, sample tap 16 and exhaust emissions channel 17.The online gas inlet 1 of hydrogen be used for for system be passed through online to
Survey hydrogen, the inert gas air inlet 3 be used for for system be passed through inert gas (in the present embodiment, the inert gas air inlet
For nitrogen inlet), the flowmeter 5 is then connected to the online gas inlet 1 of hydrogen and inert gas air inlet 3 simultaneously,
And the pipeline that the online gas inlet 1 of hydrogen is connected to flowmeter 5 is equipped with the first valve 2；And inert gas air inlet 1 with
The second valve 4 is then equipped on the pipeline that flowmeter 5 is connected to.
13 air inlet of oxidation reaction bed is connect with flowmeter 5, and gas outlet connects condenser pipe 15.Oxidation reaction bed 13 is used
It in the oxidation for realizing hydrogen to be measured, is made of stainless steel, inside is filled with metal oxide, and entire oxidation reaction bed is put
It sets in a tubular heater, the heating of oxidation reaction bed is realized by heating furnace.Meanwhile in flowmeter 5 and oxidation reaction bed
Third valve 6, the 6th valve 10 and pressure gauge 12, oxidation reaction bed 13 and condenser pipe 15 are also successively arranged on the pipeline of 13 connections
Between pipeline on then be equipped with the 8th valve 14.
The exhaust emissions channel 17 is arranged between flowmeter 5 and oxidation reaction bed 13, by be arranged on pipeline the
The exhaust emissions in two sub-sampling gaps is realized in the control of seven valves 11.
It is mounted with hydrogen in the aluminium foil sampling bag 8, is arranged between flowmeter 5 and exhaust emissions channel 17, the aluminium
8 inlet end of foil sampling bag is connected to flowmeter 5, and outlet side is connected to exhaust emissions channel 17 and oxidation reaction bed 13 simultaneously.And
And the pipeline that 8 inlet end of aluminium foil sampling bag is connected to flowmeter 5 is equipped with the 4th valve 7, outlet side is logical with exhaust emissions simultaneously
The pipeline that road 17 is connected to oxidation reaction bed 13 is equipped with the 5th valve 9.
The present invention realizes that hydrogen isotope gas is oxidized to there are two types of the modes of water sample, respectively online air inlet oxidation and offline
Air inlet oxidation model controls gas oxidation by the temperature control device of observation pressure gauge, flowmeter and oxidation reaction bed heating furnace
Vaporous water in high-temperature gas is finally cooled to liquid water using condenser pipe by rate, achievees the purpose that collect liquid water sample.Under
Introduce the process of both mode of oxidizing in face.
Online air inlet oxidation model
Firstly, the online gas inlet 1 of hydrogen to be connected to the gas outlet of hydrogen isotope separation system, while by indifferent gas
Body air inlet 3 is connected to inertia gas cylinder (selecting nitrogen cylinder).System integrity and leakproofness are gone through, and ensures sealing joint
Property, while guaranteeing that condenser pipe can normally cool down.
First, the four, the 5th valves are closed respectively, and are adjusted to the temperature of oxidation reaction bed 13 using tubular heater
350 DEG C or more, in the present embodiment, 13 length of oxidation reaction bed is 30cm, and diameter 10cm, internal capacity about 2.35L, single can
To aoxidize 5mol hydrogen, oxidation reaction bed 13 can be reactivated by way of logical oxygen heating, be reused.
Open flowmeter and second, third, the six, the seven, the 8th valves, by nitrogen be passed through to system purge 5min with
On, then, the second, the 7th valve is closed respectively, stopping is passed through nitrogen, and the flow parameter of preset flow meter 5, opens the first valve
Door 2, is passed through hydrogen to be measured by the online gas inlet 1 of hydrogen.
After hydrogen to be measured enters, under the control of flowmeter 5, via the oxidation of oxidation reaction bed and condensing tube condensation at liquid
It after water, is discharged in sample tap, at this point, carrying out water sample extraction using sampling bottle.During sampling twice, the 6th, the is closed respectively
Eight valves open the 7th valve, carry out exhaust emissions by exhaust emissions channel 17.
After sampling, the first valve 2 is closed, opens second, the six, the 8th valves respectively, and it is anti-to stop heated oxide
Answer bed 13, then be loaded into nitrogen to system purge 5min after, close flowmeter and second, third, the six, the seven, the 8th valves
Door.Finally, cleaning work is live, security risk is excluded.The process of the online air inlet oxidation model such as arrow in Fig. 2 is directed toward institute
Show.
Offline air inlet oxidation model
First, the four, the 5th valves are closed respectively, and the temperature of oxidation reaction bed is adjusted to 350 using tubular heater
DEG C or more.Then, open flowmeter and second, third, the six, the seven, the 8th valves, nitrogen is passed through to system purge
5min or more (consistent with online air inlet oxidation model).
Then, third, the 7th valve are closed, then the flow parameter of preset flow meter 5, opens the four, the 5th valves, by
The above-mentioned nitrogen being passed through is as system carrier gas, by the hydrogen loading system to be measured in aluminium foil sampling bag 8.
Hydrogen to be measured under the control of flowmeter 5, via oxidation reaction bed oxidation and condensing tube condensation at liquid water after, in
Sample tap discharge, at this point, carrying out water sample extraction also with sampling bottle.Twice sample during, respectively close the four, the 5th,
Six, the 8th valves open third, the 7th valve, carry out exhaust emissions by exhaust emissions channel 17.
After sampling, the six, the 8th valves are opened respectively, and stop heated oxide reaction bed 13, be then loaded into nitrogen
After system purge 5min, close flowmeter and second, third, the six, the seven, the 8th valves.Finally, cleaning work is existing
, exclude security risk.The process of offline air inlet oxidation model is as shown in the arrow direction in Fig. 3.
The present invention realizes the purpose that hydrogen isotope gas in hydrogen isotope separation system is oxidized to water sample well, convenient
The sampling analysis of isotope mass spectrometer.And in above two air inlet oxidation model, for the analysis that needs to run continuous samples
For experiment, the mode of online air inlet oxidation is more convenient, meanwhile, sample, which is saved, in the form of water sample also ensures safety.And
It is some be inconvenient to carry out the operating condition of online air inlet mode of oxidizing under, then can use gas sample bottle or sampling bag will be to be measured
Then sample collection is analyzed in such a way that offline air inlet aoxidizes.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
Enclose, it is all in body design thought of the invention and mentally make have no the change of essential meaning or polishing, solved
Technical problem is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (8)
1. a kind of hydrogen deuterium analysis water-like preparation system, which is characterized in that including the online gas inlet of hydrogen (1) and inert gas
Air inlet (3), while the flowmeter (5) being connected to the online gas inlet of hydrogen (1) and inert gas air inlet (3), air inlet
Mouth is connect with the flowmeter (5) and the internal oxidation reaction bed (13) for being filled with metal oxide, with the oxidation reaction bed
(13) condenser pipe (15) of gas outlet connection, the sample tap (16) being connected to the condenser pipe (15), and be arranged in flowmeter (5)
Between oxidation reaction bed (13) and it which is provided with the exhaust emissions channel (17) of the 7th valve (11)；The online gas of hydrogen
The pipeline that body air inlet (1) is connected to flowmeter (5) is equipped with the first valve (2)；The inert gas air inlet (1) and flow
The pipeline for counting (5) connection is equipped with the second valve (4)；It is set on the pipeline that the flowmeter (5) is connected to oxidation reaction bed (13)
There is the 6th valve (10)；The pipeline that the oxidation reaction bed (13) is connected to condenser pipe (15) is equipped with the 8th valve (14), and
The oxidation bed (13) is placed in a tubular heater.
2. a kind of hydrogen deuterium analysis water-like preparation system according to claim 1, which is characterized in that further include being arranged in flow
It counts between (5) and exhaust emissions channel (17), the aluminium foil sampling bag (8) for loading hydrogen；Aluminium foil sampling bag (8) air inlet
End is connected to flowmeter (5), and outlet side is connected to exhaust emissions channel (17) and oxidation reaction bed (13) simultaneously, and；Aluminium foil
The pipeline that sampling bag (8) inlet end is connected to flowmeter (5) is equipped with the 4th valve (7), and outlet side is logical with exhaust emissions simultaneously
The pipeline that road (17) is connected to oxidation reaction bed (13) is equipped with the 5th valve (9).
3. a kind of hydrogen deuterium analysis water-like preparation system according to claim 2, which is characterized in that the flowmeter (5) with
Third valve is additionally provided between inlet end and outlet side on the pipeline of oxidation reaction bed (13) connection and positioned at aluminium foil sampling bag (8)
(6)。
4. a kind of hydrogen deuterium analysis water-like preparation system according to any one of claims 1 to 3, which is characterized in that described
Inert gas air inlet (3) is nitrogen inlet.
5. a kind of hydrogen deuterium analysis water-like preparation system according to claim 4, which is characterized in that the oxidation reaction bed
(13) pressure gauge (12) are also connected at air inlet.
6. a kind of hydrogen deuterium analysis water-like preparation system according to claim 5, which is characterized in that the oxidation reaction bed
(13) it is made of stainless steel.
7. a kind of implementation method of hydrogen deuterium analysis water-like preparation system, which comprises the following steps:
(1) the online gas inlet of hydrogen is connected to the gas outlet of hydrogen isotope separation system, while by inert gas air inlet
Mouth is connected to inertia gas cylinder；
(2) first, the four, the 5th valves are closed respectively, and the temperature of oxidation reaction bed is adjusted to 350 DEG C using tubular heater
More than；
(3) open flowmeter and second, third, the six, the seven, the 8th valves, inert gas is passed through to system purge
5min or more；
(4) the second, the 7th valve is closed respectively, and stopping is passed through inert gas, the then flow parameter of preset flow meter, opens the
One valve is passed through hydrogen to be measured by the online gas inlet of hydrogen；
(5) hydrogen to be measured via oxidation reaction bed aoxidize and condensing tube condensation at liquid water after, in sample tap be discharged, at this point, sharp
Water sample extraction is carried out with sampling bottle；
(6) the six, the 8th valves are closed respectively, open the 7th valve, and exhaust emissions is carried out by exhaust emissions channel；
(7) the first valve is closed, second, the six, the 8th valves is opened respectively, and stop heated oxide reaction bed, is then loaded into
After inert gas is to system purge 5min, close flowmeter and second, third, the six, the seven, the 8th valves.
8. a kind of implementation method of hydrogen deuterium analysis water-like preparation system, which comprises the following steps:
(1) first, the four, the 5th valves are closed respectively, and the temperature of oxidation reaction bed is adjusted to 350 DEG C using tubular heater
More than；
(2) open flowmeter and second, third, the six, the seven, the 8th valves, inert gas is passed through to system purge
5min or more；
(3) third, the 7th valve are closed, then the flow parameter of preset flow meter, the four, the 5th valves is opened, by indifferent gas
Body is as system carrier gas, by the hydrogen loading system to be measured in aluminium foil sampling bag；
(4) hydrogen to be measured via oxidation reaction bed aoxidize and condensing tube condensation at liquid water after, in sample tap be discharged, at this point, sharp
Water sample extraction is carried out with sampling bottle；
(5) the four, the five, the six, the 8th valves are closed respectively, open third, the 7th valve, and tail is carried out by exhaust emissions channel
Gas discharge；
(6) the six, the 8th valves are opened respectively, and stop heated oxide reaction bed, are then loaded into inert gas to system purge
After 5min, close flowmeter and second, third, the six, the seven, the 8th valves.
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| CN111739673B (en) * | 2020-05-12 | 2022-11-25 | 中国原子能科学研究院 | Oxidation adsorption experiment system and method for trace hydrogen in oxygen atmosphere |
| CN115359941B (en) * | 2022-08-23 | 2023-08-18 | 中国原子能科学研究院 | Gas environment control method and system |
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