CN108982583A - The method and apparatus of Engineering Barrier Materials gas on-line testing under heat effect - Google Patents

The method and apparatus of Engineering Barrier Materials gas on-line testing under heat effect Download PDF

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Publication number
CN108982583A
CN108982583A CN201810634366.2A CN201810634366A CN108982583A CN 108982583 A CN108982583 A CN 108982583A CN 201810634366 A CN201810634366 A CN 201810634366A CN 108982583 A CN108982583 A CN 108982583A
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China
Prior art keywords
canister
flange
heat effect
barrier materials
under heat
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Pending
Application number
CN201810634366.2A
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Chinese (zh)
Inventor
刘伟
杨仲田
梁栋
李洪辉
贾梅兰
赵帅维
毛亮
刘建琴
叶盾毅
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China Institute for Radiation Protection
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China Institute for Radiation Protection
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Priority to CN201810634366.2A priority Critical patent/CN108982583A/en
Publication of CN108982583A publication Critical patent/CN108982583A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006Investigating resistance of materials to the weather, to corrosion, or to light of metals

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Pathology (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Ecology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Environmental Sciences (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)

Abstract

The present invention relates to the method and apparatus of Engineering Barrier Materials gas on-line testing under heat effect.Described device includes canister, baking oven and mass spectrograph;The canister includes valve, and the mass spectrometric air inlet capillary is connected by fast joint with valve;Canister is placed in baking oven.The device of the invention can be simulated in high-level radioactive waste geological disposal, the Evolution of Engineering Barrier Materials gas in the case where waste body nucleic decays heat effect.

Description

The method and apparatus of Engineering Barrier Materials gas on-line testing under heat effect
Technical field
The invention belongs to Radwastes treatment disposal technology fields, and in particular to Engineering Barrier Materials gas under heat effect The method and apparatus of body on-line testing.
Background technique
In the processing disposition of radioactive waste, the decay of itself nucleic of waste body will generate decay heat.For example, high level is put In the deep geological disposal of injectivity waste (HLW), the radionuclide decay in waste body will generate certain heat, and the heat Amount can continue long time, and therefore, Engineering Barrier Materials will be chronically under heat effect.Heat effect may accelerate metal packet Package material corrosion, so that the variation of gas near field can be caused.On the one hand the variation of these gases will affect near field redox Environment, and then will affect the processes such as nuclein migration;If on the other hand assembling a large amount of gas (especially H near field2), this will Seriously affect the safety in entire disposition library.Therefore it needs to carry out phase to the Evolution of Engineering Barrier Materials gas under heat effect The method of gas test and the device of test under the conditions of the heat effect of analog near field are established in the research of pass.
Summary of the invention
In view of the deficiencies in the prior art, the object of the present invention is to provide Engineering Barrier Materials under heat effect gas The method and apparatus of on-line testing, the Evolution of energy research engineering barrier material gas under heat effect.
To achieve the above objectives, the technical solution adopted by the present invention is that: a kind of geological disposal Engineering Barrier Materials are provided and are existed The device of gas on-line testing under heat effect, comprising: canister, baking oven and mass spectrograph;
The canister includes valve, and the mass spectrometric air inlet capillary is connected by fast joint with valve;
The canister is placed in baking oven.
Further, the canister specifically includes: hollow metal cylinder body, first flange and second flange;
First flange and second flange are mating, have a diameter larger than hollow metal cylinder body, press default spacing set at its edge Take the hole of installation bolt;
First flange center setting with hollow metal cylinder body in diameter circular hole of the same size, with second flange interface It is processed close to edge fluted;
Second flange center weld valve is machined with the edge of a knife in position corresponding with first flange groove;
By the welding of hollow metal cylinder body, first flange, second flange assembling, to obtain metal containment unit.
Further, the canister further includes a pair of of lifting lug, and the lifting lug is in second flange and is symmetrically distributed in Valve two sides.
The another technical solution that the present invention uses is: providing a kind of Engineering Barrier Materials gas under heat effect and surveys online The method of examination, which comprises
(1) canister is prepared;
(2) the pre- heat ageing of canister;
(3) prepare sample;
(4) canister is hunted leak;
(5) sample heat ageing;
(6) gas test.
Further, step (2) specifically includes:
Hollow metal cylinder body and remainder are put into heat ageing 7 days in 90 DEG C of baking oven after canister is opened.
Further, step (3) specifically includes:
Prepare 3 same metal containers, the first canister is empty container, i.e., only sealing assembles the air under environment;The Two canisters are put into the sample of metal material and bentonite mixing;Third canister is put into the second canister moderate Swelling earth sample.
Further, the bentonitic moisture content is to adjust by preset ratio.
Further, the second canister metal material and the mass ratio of bentonite mixing are 15/85.
Further, the step (5) specifically includes:
Interval carries out the gas test of sample at preset timed intervals.
Effect of the invention is that: method and apparatus provided by the present invention have the advantage that
1) present apparatus can be simulated in deep geological disposal, heat effect suffered by the Engineering Barrier Materials of near field;
2) gas on-line checking may be implemented in this test method;
3) present invention can measure under heat effect, and gas, which is generated, in bentonite generates and disappear with Expenditure Levels and metal erosion The gas station of consumption, and then it can be inferred that the substance of gas and the process machine of metal erosion reaction are generated and consumed in bentonite Reason.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of one embodiment of device of the present invention;
Fig. 2 is the structural schematic diagram of one embodiment of canister of the present invention;
Fig. 3 is the flow diagram of one embodiment of the method for the invention.
Specific embodiment
To keep the technical problems solved, the adopted technical scheme and the technical effect achieved by the invention clearer, below It will the technical scheme of the embodiment of the invention will be described in further detail in conjunction with attached drawing.Obviously, described embodiment is only It is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people Member's every other embodiment obtained without making creative work, belongs to the scope of protection of the invention.
As shown in Figure 1, Fig. 1 is the structural schematic diagram of one embodiment of device of the present invention, described device 100 includes: gold Belong to container 101, baking oven 102 and mass spectrograph 103.
Canister 101 includes valve 1011, the air inlet capillary 1031 of the mass spectrograph 103 by fast joint 104 with Valve 1011 is connected.
Canister 101 is placed in baking oven 102.
Fig. 2 is the structural schematic diagram of one embodiment of canister provided by the invention, referring to Fig.2, canister 101 wraps It includes: hollow metal cylinder body 1014, first flange 1012, second flange 1013.
First flange 1012 and second flange 1013 are mating, have a diameter larger than hollow metal cylinder body 1011, at its edge The mounting hole of installation bolt is extracted by default spacing.
1012 center of first flange setting with the consistent circular hole of 1014 inner diameter size of hollow metal cylinder body, with the second method Blue 1013 interfaces are processed fluted close to edge.
1013 center weld valve 1011 of second flange is machined with knife in position corresponding with 1012 groove of first flange Mouthful.
Hollow metal cylinder body 1014, first flange 1012, second flange 1013 are assembled, to obtain metal sealing appearance Device 101.
Further, in order to more easily move canister 101.Canister 101 further includes a pair of of lifting lug 1015, institute Lifting lug 1015 is stated in second flange 1013 and is symmetrically distributed in 1011 two sides of valve.
Feature, the dress of Engineering Barrier Materials provided by the invention gas on-line testing under heat effect is different from the prior art It sets, the Evolution of energy research engineering barrier material gas under heat effect.
Fig. 3 is the flow diagram of one embodiment of the method for the invention, refering to Fig. 3, engineering barrier provided by the invention The method of material gas on-line testing under heat effect the following steps are included:
Step 101: preparing canister.
Specifically, the device of gas on-line testing prepares canister under heat effect by above-mentioned Engineering Barrier Materials.
Step 102: the pre- heat ageing of canister.
In a specific embodiment, hollow metal cylinder body and remainder are put into 90 after canister being opened DEG C baking oven in heat ageing 7 days.
Step 103: preparing sample.
It is accurate for experimental data, three identical metals are prepared using the method for comparative experiments in the present embodiment and are held Device.First canister is empty container, i.e., only sealing assembles the air under environment;Second canister is put into metal material and swollen The sample of profit soil mixing;Third canister is put into the swelling earth sample of the second canister moderate.
Wherein, bentonitic moisture content is to adjust by preset ratio, metal material and bentonite in the second canister It is also to be mixed by preset ratio.
In a specific embodiment, spare after bentonitic moisture content being adjusted to 17% and is homogenized 3 days, then will The first canister sealing (gas under assembling environment) in ready 3 canisters, gold is added in the second canister Belong to powder/wet soil mass ratio 15/85 sample after mixing and sealing, is added and the second canister in third canister It is sealed after the bentonite of mean quality.
Step 104: canister leak detection.
It must be to container the being sealed property inspection after being put into sample and assembling, it is ensured that the leakproofness of container is good.It checks Method is hunted leak according to QJ3253-2005 " leak detection by bubbles test method ", when irregularities bubble generates during leak detection, depending on To assemble accepted container, follow-up test can be carried out.
Step 105: sample heat ageing.
After ensuring that container tightness is good, it is put into 90 DEG C of baking oven and carries out heat ageing.
Step 106: gas test.
In Heat Ageing, interval carries out the gas test of sample at preset timed intervals.
For metal sample in second canister by taking iron powder as an example, following table gives the result of gas test.The number from table According to can be seen that 1) for slack tank, after 90 DEG C of heat ageing different times, H2、H2O、O2And CO2Content and background Content (when container assembles, each gas componant content in Laboratory air) is quite namely slack tank itself does not generate and also do not consume gas Body.2) for being 17% bentonitic container containing only initial aqueous rate, after 90 DEG C of heat ageing different times, H2Content and this Bottom content is consistent, i.e., simple bentonite does not generate H under heat effect2;Gaseous state H2O increased compared with background, this is because swelling Moisture evaporation in soil makes gaseous state H in container2O content increases;O2Content slightly reduced, and CO2Content is increased slightly, This small amount of O that may be microbial consumption existing for bentonite2And produce CO2And organic matter decomposition produces CO2.3) right When the container containing iron powder and bentonite mixtures, heat ageing 5 days, a large amount of H are produced2, consumed the O of the overwhelming majority2, Gaseous state H2O has also been consumed a part, and CO2It is increased slightly, this is because metal erosion consumes O2And H2O simultaneously produces H2。 With the increase of ageing time, H2Amount continue to increase (at 45 days, H2May be oozed out from bucket wall and reduce content), O2And H2O It is lasting to reduce, and CO2Substantially remain in a comparable level;From the point of view of entire reaction process, O early period is tested2Quickly reduce, And H2It quicklys increase, the later period is substantially without O2When, gaseous state H2O is gradually reduced, H2Amount be slowly increased.
Gas test result is as follows:
From the point of view of entire test result, the slack tank after preparatory heat ageing is substantially at stable state, i.e., does not consume and also do not produce Raw any gas, but due to H2Dialyzing, after a long time placement, H in container2Content will reduce;It is competing in no iron powder It strives under reaction condition, bentonite will consume the oxygen of part and generate a certain amount of CO2, and in the condition for having iron powder competitive reaction Under, the bentonite containing iron powder also has the CO of part2Generate, but its content relatively only have swelling earth sample when it is much smaller, and with The increase in reaction time is basically unchanged, that is to say, that the presence of iron powder inhibits CO2Generation, this may show in bentonite In the presence of happiness oxygen type microorganism;There are following reaction process for iron powder corrosion: it is aerobic have water under conditions of, iron powder and O2Reaction is simultaneously Generate a large amount of H2, and the speed reacted is quickly;Under conditions of having water anaerobic, iron powder will be with H2O reaction will also generate H2, but Reaction speed is slower.This shows O2And H2The presence of O will lead to the corrosion of iron powder, and O2Presence will accelerate its corrosion.
Feature, a kind of Engineering Barrier Materials gas on-line testing under heat effect provided by the invention is different from the prior art Method can measure under heat effect, gas generates in bentonite and Expenditure Levels and metal erosion generate and the gas feelings of consumption Condition, and then it can be inferred that the substance of gas and the process mechanism of metal erosion reaction are generated and consumed in bentonite.
It will be understood by those skilled in the art that method and system of the present invention is not limited to institute in specific embodiment The embodiment stated, specific descriptions above are intended merely to explain the purpose of the present invention, are not intended to limit the present invention.This field skill Art personnel can derive other implementation manners according to the technical scheme of the present invention, and also belong to the scope of the technical innovation of the present invention, this The protection scope of invention is defined by the claims and their equivalents.

Claims (9)

1. the device of Engineering Barrier Materials gas on-line testing under heat effect, which is characterized in that described device includes that metal holds Device, baking oven and mass spectrograph;
The canister includes valve, and the mass spectrometric air inlet capillary is connected by fast joint with valve;
The canister is placed in baking oven.
2. the device of Engineering Barrier Materials gas on-line testing under heat effect according to claim 1, which is characterized in that institute It states canister to specifically include: hollow metal cylinder body, first flange and second flange;
First flange and second flange are mating, have a diameter larger than hollow metal cylinder body, have extracted at its edge by default spacing The hole of bolt is installed;
The setting of first flange center and diameter circular hole of the same size in hollow metal cylinder body, close with second flange interface Edge processing is fluted;
Second flange center weld valve is machined with the edge of a knife in position corresponding with first flange groove;
By the welding of hollow metal cylinder body, first flange, second flange assembling, to obtain metal containment unit.
3. the device of Engineering Barrier Materials gas on-line testing under heat effect according to claim 2, which is characterized in that institute Stating canister further includes a pair of of lifting lug, and the lifting lug is in second flange and is symmetrically distributed in valve two sides.
4. the method for Engineering Barrier Materials gas on-line testing under heat effect, which is characterized in that
(1) canister is prepared;
(2) the pre- heat ageing of canister;
(3) prepare sample;
(4) canister is hunted leak;
(5) sample heat ageing;
(6) gas test.
5. the method for Engineering Barrier Materials gas on-line testing under heat effect according to claim 4, which is characterized in that step Suddenly (2) specifically include:
Hollow metal cylinder body and remainder are put into heat ageing 7 days in 90 DEG C of baking oven after canister is opened.
6. the method for Engineering Barrier Materials gas on-line testing under heat effect according to claim 4, which is characterized in that step Suddenly (3) specifically include:
Prepare 3 same metal containers, the first canister is empty container, i.e., only sealing assembles the air under environment;Second gold medal Belong to the sample that container is put into metal material and bentonite mixing;Third canister is put into the swelling of the second canister moderate Earth sample.
7. the method for Engineering Barrier Materials gas on-line testing under heat effect according to claim 6, which is characterized in that institute Stating bentonitic moisture content is to adjust by preset ratio.
8. the method for Engineering Barrier Materials gas on-line testing under heat effect according to claim 6, which is characterized in that the It is 15/85 that metal material and bentonite, which press mixed mass ratio, in two canisters.
9. the method for Engineering Barrier Materials gas on-line testing under heat effect according to claim 4, which is characterized in that institute Step (6) is stated to specifically include:
Interval carries out the gas test of sample at preset timed intervals.
CN201810634366.2A 2018-06-20 2018-06-20 The method and apparatus of Engineering Barrier Materials gas on-line testing under heat effect Pending CN108982583A (en)

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Publication number Priority date Publication date Assignee Title
DE19853049A1 (en) * 1998-11-17 2000-06-21 Joachim Franzke Leak testing of engineering components comprises use of high pressure test gas, carrier gas, discharge tube detector and laser spectrometer, where both gases are constituents of air
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DE19853049A1 (en) * 1998-11-17 2000-06-21 Joachim Franzke Leak testing of engineering components comprises use of high pressure test gas, carrier gas, discharge tube detector and laser spectrometer, where both gases are constituents of air
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Application publication date: 20181211