CN105842725A - Method for detecting specific activity of tritiated steam in air - Google Patents
Method for detecting specific activity of tritiated steam in air Download PDFInfo
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- CN105842725A CN105842725A CN201610172939.5A CN201610172939A CN105842725A CN 105842725 A CN105842725 A CN 105842725A CN 201610172939 A CN201610172939 A CN 201610172939A CN 105842725 A CN105842725 A CN 105842725A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/17—Circuit arrangements not adapted to a particular type of detector
- G01T1/178—Circuit arrangements not adapted to a particular type of detector for measuring specific activity in the presence of other radioactive substances, e.g. natural, in the air or in liquids such as rain water
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Abstract
The invention discloses a method for detecting specific activity of tritiated steam in air. The method particularly comprises the steps of absorbing the tritium steam in air by means of a 3A molecular sieve, collecting tritiated water absorbed in the 3A molecular sieve through freezing and sublimating in a freeze drying device, performing absorption and micro-filtering on the collected tritiated water after collection, and detecting the specific activity of the tritiated water. Because the method of the invention realizes relatively high collecting efficiency on the tritiated water and small residual amount of sampling medium, the method can be used for collecting the tritiated water in the air. Furthermore the specific activity of the tritiated water can be detected on condition of relatively low specific activity and furthermore relatively high data precision is realized. The collecting efficiency of the method can reach 99%, and the residual amount of the sampling medium is lower than 1%.
Description
Technical field
The present invention relates to the activity measurement method of radgas, in a kind of air, the ratio of tritiated water steam is lived
The assay method of degree.
Background technology
Tritium runs the important radioactive gas nuclide of heap discharge as fission power, and various nuclear facilities are released into surrounding
Tritium can cause the rising of ambient atmosphere tritium activity, and be operated in nuclear power plant reactor Factory Building and the work about auxiliary plant
Make personnel and can take in tritium by all means, thus cause a certain degree of internal radiation, therefore, the tritium activity in raising air
Accuracy of detection is the key issue that gaseous state tritium measures.
Tritium activity method for measuring at present mainly includes direct method and indirect method, and direct method is to use detection of gas
Device such as ionization chamber, proportional counter carries out the measurement of gas, and indirect method is that after tritium is catalytically oxidized to tritiated water, utilization is dodged
Bright bulk detector measures, and the former sensitivity is low, and when the specific activity of tritium is relatively low, instrument inspection does not measures accurate numerical value,
It is not suitable for the detection of tritium in regular air, may be only available for Tritium measurement in radiation work place, although the latter's sensitivity
Higher, simple, can process a large amount of sample, but the existing method of sampling cannot realize under north low temperature environment in the winter time accurate
Sampling.
Summary of the invention
For solving the problems referred to above, it is an object of the invention to provide the mensuration side of the specific activity of tritiated water steam in a kind of air
Method.
The present invention for achieving the above object, is achieved through the following technical solutions:
The assay method of the specific activity of tritiated water steam in a kind of air, comprises the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 0.9 ~ 1.1m, starts air pump, regulation
Flow control valve makes the flow of effusion meter be positioned between 0.5 ~ 5.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe
Become closing successively after pink air pump, flow control valve from blueness, record integrated flux, take off absorption bottle A and absorption bottle B
After will gather the molecular sieve after tritiated water and pour out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain for 48 ~ 50 hours
Tritiated water；
3. step 2. gained tritiated water adds ion exchange resin, and stirring to tritiated electrical conductivity of water is down to 5 μ S/cm, then
Obtaining tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water is 4 ~ 5:1 with the mass ratio of ion exchange resin；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
Preferably, described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes.
Preferably, described ion exchange resin is EC20MB electron level mixture iron exchange resin.
The assay method of the specific activity of tritiated water steam in further preferred air, comprises the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 1m, starts air pump, and regulation flow is adjusted
Joint valve makes the flow of effusion meter between 1.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe is become from blueness
Close air pump, flow control valve after pink successively, record integrated flux, after taking off absorption bottle A and absorption bottle B, tritium will be gathered
Change the molecular sieve after water and pour out standby；Described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain tritium in 48 hours
Change water；
3. step 2. gained tritiated water is added EC20MB electron level mixture iron exchange resin, stirring to tritiated electrical conductivity of water
Be down to 5 μ S/cm, then obtain tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water mix with EC20MB electron level from
The mass ratio of sub-exchange resin is 4:1；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
The present invention has the advantage that compared to existing technology
The present invention uses the tritiated water steam in 3A molecular sieve adsorption air, and the tritiated water in 3A molecular sieve after water suction is in freezing
Being collected after freezing, distilling in drying device, the tritiated water after collecting removes after ion exchange resin absorption and microfiltration
The miscellaneous specific activity carrying out detecting tritiated water, the method for the present invention due to higher to the collecting efficiency of tritiated water, sampling media residual
Stay few, thus can be collected by tritiated water in atmosphere, and the specific activity of tritiated water can be detected when specific activity is less,
The degree of accuracy of data is higher；Equipment investment used by the method for the present invention is few, connects simple to operation, low to environmental requirement,
Also the tritiated water in air can be collected detection under general environment, be particularly suited under northern China winter low temperature environment adopting
It is difficult to collect sample with additive method, or instrument precision is relatively low cannot accurately survey the low-activity tritiated water in air
During amount；The method design of the present invention is exquisite, and before the tritiated water in 3A molecular sieve adsorption air, air first passes through particulate filter
The filtration of device, removes the dust granules in air, can improve the efficiency of 3A molecular sieve adsorption tritiated water, and utilize 3A molecular sieve
The molecule that only absorption steam not absorbing carbon dioxide, amino molecule etc. is bigger, separates steam and other molecules, thus improves
The precision of sampling；Post processing uses other impurity in ion exchange resin absorption tritiated water, so that tritiated water activity is relatively low
Time detect its numerical value；The method collecting efficiency using the present invention can reach 99%, sampling media residual quantity ＜ 1%.
Accompanying drawing explanation
Fig. 1 is tritiated water sampling apparatus schematic diagram in air.
Detailed description of the invention
It is an object of the invention to provide the assay method of the specific activity of tritiated water steam in a kind of air, pass through techniques below
Scheme realizes:
The assay method of the specific activity of tritiated water steam in a kind of air, comprises the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 0.9 ~ 1.1m, starts air pump, regulation
Flow control valve makes the flow of effusion meter be positioned between 0.5 ~ 5.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe
Become closing successively after pink air pump, flow control valve from blueness, record integrated flux, take off absorption bottle A and absorption bottle B
After will gather the molecular sieve after tritiated water and pour out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain for 48 ~ 50 hours
Tritiated water；
3. step 2. gained tritiated water adds ion exchange resin, and stirring to tritiated electrical conductivity of water is down to 5 μ S/cm, then
Obtaining tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water is 4 ~ 5:1 with the mass ratio of ion exchange resin；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
Preferably, described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes.
Preferably, described ion exchange resin is EC20MB electron level mixture iron exchange resin.
The assay method of the specific activity of tritiated water steam in further preferred air, comprises the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 1m, starts air pump, and regulation flow is adjusted
Joint valve makes the flow of effusion meter between 1.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe is become from blueness
Close air pump, flow control valve after pink successively, record integrated flux, after taking off absorption bottle A and absorption bottle B, tritium will be gathered
Change the molecular sieve after water and pour out standby；Described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain tritium in 48 hours
Change water；
3. step 2. gained tritiated water is added EC20MB electron level mixture iron exchange resin, stirring to tritiated electrical conductivity of water
Be down to 5 μ S/cm, then obtain tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water mix with EC20MB electron level from
The mass ratio of sub-exchange resin is 4:1；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
Below in conjunction with specific embodiment, the invention will be further described.
At the beginning of 2016, Korea has carried out the 4th nuclear test, and China is for responding Korea's nuclear test, to ground, four, border area
The radiation of point has carried out emergent test, has carried out the tritiated water in the gas of overhead, border the most respectively collecting and detecting, concrete steps
And data processed result is as follows:
Embodiment 1
Place 1(test temperature is about 278K) air in the assay method of specific activity of tritiated water steam, including following step
Rapid:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, as it is shown in figure 1, equipped with work in described absorption bottle A and absorption bottle B
3A molecular sieve after change, the volume of 3A molecular sieve accounts for absorption bottle A and more than 2/3rds of absorption bottle B, needed for sample collecting
The device wanted is arranged on the position that distance ground 1.0m is high, starts air pump, and regulation flow control valve makes the flow of effusion meter
Be positioned at 2.0L/min, start sampling, when variable color silica gel instruction pipe silica gel from blueness become closing successively after pink air pump,
Flow control valve, record cumulative flow value is 6.135m3, take off and will gather the molecule after tritiated water after absorption bottle A and absorption bottle B
Sieve is poured out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain for 48 ~ 50 hours
Tritiated water 10.44 grams；
3. step 2. gained tritiated water adds 2.00 grams of ion exchange resin, and 5 μ S/ are down in stirring to tritiated electrical conductivity of water
Cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air；Concrete grammar is as follows: pipette the liquid to be measured of m=8.0g
Sample, to politef counting vial, adds 12.0mL Hisafe III scintillation solution, seals, use wine after concussion mix homogeneously
Soaking wet cotton balls wiping sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, lucifuge is after 2 hours
Measure 1000min.From Low background liquid scintillation energy disperse spectroscopy, take out test specimens and add the tritium mark that 0.1g activity is 8.72Bq/g
Quasi-solution, shakes mix homogeneously, tests 1000min with Low background liquid scintillation energy disperse spectroscopy again after wiping, lucifuge.Record standard
Sample counting rate is 12.528cpm, and sample to be tested counting rate is 0.961cpm, and this bottom sample counting rate is 0.872cpm.
Embodiment 2
Place 2(test temperature is about 273K) air in the assay method of specific activity of tritiated water steam, including following step
Rapid:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, as it is shown in figure 1, equipped with work in described absorption bottle A and absorption bottle B
3A molecular sieve after change, the volume of 3A molecular sieve accounts for absorption bottle A and more than 2/3rds of absorption bottle B, needed for sample collecting
The device wanted is arranged on the position that distance ground 1.0m is high, starts air pump, and regulation flow control valve makes the flow of effusion meter
Be positioned at 2.0L/min, start sampling, when variable color silica gel instruction pipe silica gel from blueness become closing successively after pink air pump,
Flow control valve, record cumulative flow value is 6.135m3, take off and will gather the molecule after tritiated water after absorption bottle A and absorption bottle B
Sieve is poured out standby；Described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain tritium in 48 hours
Change 9.49 grams of water；
3. step 2. gained tritiated water being added EC20MB electron level mixture iron exchange resin 2.10 grams, stirring is to tritiated water
Electrical conductivity is down to 5 μ S/cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air；Concrete grammar is as follows: pipette the liquid to be measured of m=8.0g
Sample, to politef counting vial, adds 12.0mL Hisafe III scintillation solution, seals, use wine after concussion mix homogeneously
Soaking wet cotton balls wiping sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, lucifuge 2.5 hours
Rear measurement 1000min.From Low background liquid scintillation energy disperse spectroscopy, take out test specimens and add the tritium that 0.1g activity is 8.72Bq/g
Standard solution, shakes mix homogeneously, tests 1000min with Low background liquid scintillation energy disperse spectroscopy again after wiping, lucifuge.Record mark
Quasi-sample counting rate is 13.008cpm, and sample to be tested counting rate is 1.008cpm, and this bottom sample counting rate is 0.872cpm.
Embodiment 3
Be 263K to place 3(test temperature) air in the assay method of specific activity of tritiated water steam, comprise the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, as it is shown in figure 1, equipped with work in described absorption bottle A and absorption bottle B
3A molecular sieve after change, the volume of 3A molecular sieve accounts for absorption bottle A and more than 2/3rds of absorption bottle B, needed for sample collecting
The device wanted is arranged on the position that distance ground 0.9m is high, starts air pump, and regulation flow control valve makes the flow of effusion meter
Be positioned at 3.0L/min, start sampling, when variable color silica gel instruction pipe silica gel from blueness become closing successively after pink air pump,
Flow control valve, record cumulative flow value is 10.214m3, dividing after gathering tritiated water after taking off absorption bottle A and absorption bottle B
Son sieve is poured out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain for 48 ~ 50 hours
Tritiated water 8.85 grams；
3. step 2. gained tritiated water adds 2.09 grams of ion exchange resin, and 5 μ S/ are down in stirring to tritiated electrical conductivity of water
Cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air；Concrete grammar is as follows: pipette the liquid to be measured of m=8.0g
Sample, to politef counting vial, adds 12.0mL Hisafe III scintillation solution, seals, use wine after concussion mix homogeneously
Soaking wet cotton balls wiping sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, lucifuge is after 3 hours
Measure 1000min.From Low background liquid scintillation energy disperse spectroscopy, take out test specimens and add the tritium mark that 0.1g activity is 8.72Bq/g
Quasi-solution, shakes mix homogeneously, tests 1000min with Low background liquid scintillation energy disperse spectroscopy again after wiping, lucifuge.Record standard
Sample counting rate is 14.024cpm, and sample to be tested counting rate is 1.012cpm, and this bottom sample counting rate is 0.872cpm.
Embodiment 4
Be 258K to place 4(test temperature) air in the assay method of specific activity of tritiated water steam, comprise the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, as it is shown in figure 1, equipped with work in described absorption bottle A and absorption bottle B
3A molecular sieve after change, the volume of 3A molecular sieve accounts for absorption bottle A and more than 2/3rds of absorption bottle B, needed for sample collecting
The device wanted is arranged on the position that distance ground 0.9m is high, starts air pump, and regulation flow control valve makes the flow of effusion meter
It is positioned at 3L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe is become closing successively after pink air pump, stream from blueness
Adjustable valve, record cumulative flow value is 12.245m3, take off and will gather the molecule after tritiated water after absorption bottle A and absorption bottle B
Sieve is poured out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain tritium in 50 hours
Change 9.68 grams of water；
3. step 2. gained tritiated water adds 1.80 grams of ion exchange resin, and 5 μ S/ are down in stirring to tritiated electrical conductivity of water
Cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air；Concrete grammar is as follows: pipette the liquid to be measured of m=8.0g
Sample, to politef counting vial, adds 12.0mL Hisafe III scintillation solution, seals, use wine after concussion mix homogeneously
Soaking wet cotton balls wiping sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, lucifuge is after 3 hours
Measure 1000min.From Low background liquid scintillation energy disperse spectroscopy, take out test specimens and add the tritium mark that 0.1g activity is 8.72Bq/g
Quasi-solution, shakes mix homogeneously, tests 1000min with Low background liquid scintillation energy disperse spectroscopy again after wiping, lucifuge.Record standard
Sample counting rate is 13.254cpm, and sample to be tested counting rate is 0.989cpm, and this bottom sample counting rate is 0.872cpm.
Comparative example
Tritium sampler in MARC7000 type air is used the steam in the air of place 2 to be acquired, then in steam
The activity of tritium detect, do not detect that the steam in the air of place 2 contains tritiated water.
Result treatment
Processing the data of embodiment 1 ~ 4 according to below equation, the ratio obtaining tritiated water steam in each place air is lived
The data of degree are as shown in table 1.
1. instrument efficiency calculation formula:
×100%
In formula, E instrument efficiency, %；
N2Standard specimen counting rate, cpm；
N1————Sample to be tested counting rate, cpm；
A1Tritium standard solution activity, Bq/g；
m1Add tritium standard solution quality, g.
2. tritiated water sample activity concentration computing formula:
In formula, A2Tritiated water sample activity, Bq/g；
N1Sample to be tested counting rate, cpm；
N0————This bottom sample counting rate, cpm；
E instrument efficiency, %；
M tritiated water volume of sample, g.
3. cumulative sample volume be modified to mark condition volume computing formula:
In formula, V gathers air mark condition volume, m3；
V0Gather sample cumulative volume, m3；
P0Atmospheric pressure during sample collecting, Pa；
Atmospheric pressure under P standard state, 101.3kPa；
Temperature under T standard state, K；
T0Temperature during sample collecting, K.
4. tritium raito (T.R) Activity Calculation formula in air:
In formula, tritiated water vapor ratio activity, Bq/m in A air3；
A2Tritiated water sample activity, Bq/mL；
M tritiated water volume of sample, mL；
V gathers volume of air (mark condition), m3；
m1Gather tritiated water population of samples to amass, mL.
The specific activity result table of tritiated water steam in the air of table 1 embodiment 1 ~ 4
| Instrument efficiency/% | Tritiated water sample activity concentration/Bq/g | Mark condition volume/m3 | Tritium raito (T.R) activity/mBq/m in air3 | |
| Embodiment 1 | 22.1 | 8.4×10-4 | 5.81 | 15.7 |
| Embodiment 2 | 22.9 | 1.2×10-3 | 5.85 | 19.0 |
| Embodiment 3 | 22.7 | 1.3×10-3 | 9.15 | 11.0 |
| Embodiment 4 | 23.4 | 1.0×10-3 | 10.76 | 9.1 |
Shown by the Data Comparison of embodiment 2 and comparative example, in existing air tritium sampler cannot realize tritium concentration relatively
Accurate sampling time low, thus can not accurately detect the specific activity of the tritiated water steam in air, the method for sampling of the present invention
Can realize at low ambient temperatures to the accurate sampling of tritiated water in air, tritiated water concentration realizes time relatively low the most in atmosphere
Accurate measurements to radiation environment.
Claims (4)
1. the assay method of the specific activity of tritiated water steam in an air, it is characterised in that: comprise the following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 0.9 ~ 1.1m, starts air pump, regulation
Flow control valve makes the flow of effusion meter be positioned between 0.5 ~ 5.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe
Become closing successively after pink air pump, flow control valve from blueness, record integrated flux, take off absorption bottle A and absorption bottle B
After will gather the molecular sieve after tritiated water and pour out standby；In described particle filter equipped with microfiltration membrane；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain for 48 ~ 50 hours
Tritiated water；
3. step 2. gained tritiated water adds ion exchange resin, and stirring to tritiated electrical conductivity of water is down to 5 μ S/cm, then
Obtaining tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water is 4 ~ 5:1 with the mass ratio of ion exchange resin；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
The assay method of the specific activity of tritiated water steam in a kind of air the most according to claim 1, it is characterised in that: institute
The particle filter stated built with filter membrane be PTFE micron order hydrophylic filter membranes.
The assay method of the specific activity of tritiated water steam in a kind of air the most according to claim 1, it is characterised in that: institute
The ion exchange resin stated is EC20MB electron level mixture iron exchange resin.
The assay method of the specific activity of tritiated water steam in a kind of air the most according to claim 1, it is characterised in that: bag
Include following steps:
1. the collection of sample: the device required for the collection of sample is by particle filter, flow control valve, effusion meter, absorption bottle
A, absorption bottle B, variable color silica gel instruction pipe and air pump composition, divide equipped with the 3A after activation in described absorption bottle A and absorption bottle B
Son sieve, is arranged on the device required for the collection of sample on the high position of distance ground 1m, starts air pump, and regulation flow is adjusted
Joint valve makes the flow of effusion meter between 1.0L/min, starts sampling, when the silica gel of variable color silica gel instruction pipe is become from blueness
Close air pump, flow control valve after pink successively, record integrated flux, after taking off absorption bottle A and absorption bottle B, tritium will be gathered
Change the molecular sieve after water and pour out standby；Described particle filter built with filter membrane be PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained being gathered tritiated water loads in the specimen disc of vacuum freezing device, be refrigerated to-
20 DEG C, then specimen disc is put on the specimen holder of vacuum freezing device, starts vacuum pump collection tritiated water and obtain tritium in 48 hours
Change water；
3. step 2. gained tritiated water is added EC20MB electron level mixture iron exchange resin, stirring to tritiated electrical conductivity of water
Be down to 5 μ S/cm, then obtain tritiated water to be measured with aqueous micro-filtrate membrane filtration, described tritiated water mix with EC20MB electron level from
The mass ratio of sub-exchange resin is 4:1；
4. step 3. gained tritiated water to be measured Low background liquid scintillation energy disperse spectroscopy is measured the activity of tritium in tritiated water, according to tritium
Change the activity meter of tritium in water and calculate the specific activity of tritiated water steam in air.
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| CN108168955A (en) * | 2018-03-21 | 2018-06-15 | 阳江核电有限公司 | The accumulation sampling system and method for tritiated vapor in a kind of air |
| CN109444944A (en) * | 2018-12-21 | 2019-03-08 | 清华大学 | The fast automatic analysis method and device of tritium in water |
| CN110780332A (en) * | 2019-11-08 | 2020-02-11 | 中国原子能科学研究院 | System and method for measuring transformation rate of element state T and oxidation state T in environment |
| CN113270215A (en) * | 2021-05-18 | 2021-08-17 | 清华大学 | Liquid effluent from nuclear power plants14C automatic pretreatment device and treatment method |
| CN113654841A (en) * | 2021-09-18 | 2021-11-16 | 中国工程物理研究院核物理与化学研究所 | Device for quickly sampling tritiated water in air and method for measuring concentration of tritium in air |
| CN113960650A (en) * | 2021-10-22 | 2022-01-21 | 中核核电运行管理有限公司 | A pretreatment device for carbon-14 activity analysis in high activity tritium water |
| CN114210375A (en) * | 2021-10-23 | 2022-03-22 | 苏州思萃同位素技术研究所有限公司 | Preparation method of hydrogen isotope substituted acid |
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| CN109444944B (en) * | 2018-12-21 | 2024-05-28 | 清华大学 | Method and device for rapidly and automatically analyzing tritium in water |
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| CN110780332B (en) * | 2019-11-08 | 2021-06-29 | 中国原子能科学研究院 | System and method for measuring conversion rate of elemental T and oxidized T in the environment |
| CN113270215A (en) * | 2021-05-18 | 2021-08-17 | 清华大学 | Liquid effluent from nuclear power plants14C automatic pretreatment device and treatment method |
| CN113270215B (en) * | 2021-05-18 | 2022-12-09 | 清华大学 | Liquid effluents from nuclear power plants 14 C automatic pretreatment device and treatment method |
| CN113654841A (en) * | 2021-09-18 | 2021-11-16 | 中国工程物理研究院核物理与化学研究所 | Device for quickly sampling tritiated water in air and method for measuring concentration of tritium in air |
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