CN211527975U - Equipment for collecting nickel-63 in particle state and dissolved state in water body - Google Patents
Equipment for collecting nickel-63 in particle state and dissolved state in water body Download PDFInfo
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- CN211527975U CN211527975U CN201921927697.1U CN201921927697U CN211527975U CN 211527975 U CN211527975 U CN 211527975U CN 201921927697 U CN201921927697 U CN 201921927697U CN 211527975 U CN211527975 U CN 211527975U
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Abstract
The utility model discloses a particulate state and dissolved state nickel-63's collecting device in water, including sample water tank, first pipeline, collector, second pipeline, the collection water tank that communicates in proper order, the collector includes the first collector that is used for collecting particulate state nickel-63 and is used for collecting dissolved state nickel-63's second collector of establishing ties each other, it strains a section of thick bamboo to be provided with first non-woven fabrics in the first collector, it strains a section of thick bamboo to be provided with the second non-woven fabrics in the second collector, the section of thick bamboo flooding of second non-woven fabrics is strained has dimethylglyoxime, the sample water tank is connected with charge device. The utility model discloses a collecting device strains a section of thick bamboo through the non-woven fabrics that adopts non-woven fabrics to strain a section of thick bamboo and flooding dimethylglyoxime and realizes the collection of nickel-63 of particulate state and dissolved state respectively, and recovery efficiency is high and stable, can shorten processing time and flow greatly in the more sample of short time in-process, and measurement of efficiency is high, is applicable to the survey of nickel-63 in various environment aquatic, including rainwater, drinking water, surface water, groundwater and sea water etc..
Description
Technical Field
The utility model relates to an environmental monitoring technical field, concretely relates to can collect granule attitude in water and dissolve attitude nickel-63's collecting device simultaneously.
Background
Nickel-63 (i.e.63Ni) is an important activation product, mainly derived from the operation of nuclear reactors. Because of good heat transfer performance of nickel, the nickel is widely applied to components such as stainless steel materials, aluminum alloys, concrete and the like of reactors and is dissolved and released under the corrosion action of main loop waterInto the cooling water of the nuclear reactor by neutron activation62Ni(n，γ)63Ni、63Cu(n，p)63Ni producing radionuclides63Ni, minor leakage of main loop coolant and shutdown refueling are released to the environment nickel-63 is a pure β radioactive radionuclide with high activation yield and long life (T)1/2100.1a), which is a toxic nuclide.
Monitoring of nickel-63 in liquid effluents has received increasing attention in recent years due to the greater amount of nickel-63 emitted in liquid effluents from nuclear power plants. The nickel-63 exists in a dissolved state and a particle state in the water body, the activity concentration of the nickel-63 in the environment around the nuclear facility and the liquid radioactive effluent is monitored to confirm whether the nuclear facility has abnormal emission in operation, and the method can be used for accurately evaluating the radiation effect of the nickel-63 emitted by the nuclear facility on the public.
The existing methods only focus on the analysis of dissolved nickel-63, and the analysis time is long. In the prior art, nickel-63 is generally separated and purified by a method of tri-n-octylamine extraction and dimethylglyoxime complexation (GB/T14502-1993), and the measurement is carried out by a liquid scintillation spectrometer. The method has long separation process and much time consumption. A handbook of protocols by the U.S. department of energy (DOE) (DOE, 1993) uses nickel specific resins to separate and purify nickel-63 from water. The method separates and purifies the nickel-63 through a cation exchange resin column and a nickel specific resin extraction chromatographic column, has short separation flow, can not realize automatic collection and still has high analysis cost.
Disclosure of Invention
In view of the above, in order to overcome the defects of the prior art and achieve the above object, the present invention provides a device for collecting nickel-63 in a water body, which can simultaneously collect nickel-63 in a particle state and a dissolved state.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides a collection equipment of particulate state and dissolved state nickel-63 in water, is including sample water tank, first pipeline, collector, second pipeline, the collection water tank that communicates in proper order, the collector includes the first collector that is used for collecting particulate state nickel-63 and is used for collecting dissolved state nickel-63 of establishing ties each other, it strains a section of thick bamboo to be provided with first non-woven fabrics in the first collector, it strains a section of thick bamboo to be provided with the second non-woven fabrics in the second collector, the section of thick bamboo that strains of second non-woven fabrics is soaked with dimethylglyoxime, the sample water tank is connected with charge device. The method for quantitatively collecting the granular nickel-63 by adopting the non-woven fabric filter cylinder and then quantitatively collecting the dissolved nickel-63 by adopting the non-woven fabric filter cylinder impregnated with the dimethylglyoxime develops and establishes a method which can accurately, stably and efficiently collect the granular nickel-63 and the dissolved nickel-63 in the water body and perform efficient measurement, and is suitable for preparing and measuring the nickel-63 in the low-salinity water body sample and the liquid effluent sample of the nuclear facility.
Preferably, the collecting apparatus further comprises a backwashing device including a first three-way valve disposed on the first pipe, a second three-way valve disposed on the second pipe, a backwashing pipe communicating the first three-way valve and the second three-way valve, and a third three-way valve disposed between the first three-way valve and the collector. The provision of the backwash device allows the collector to be cleaned prior to the next measurement so that the measurement results remain accurate.
More preferably, a booster pump is further provided between the first three-way valve and the sample water tank, so that the processing speed can be further controlled.
More preferably, a flow meter is further provided between the second three-way valve and the collection water tank, and the flow meter is used for observing and adjusting the flow rate.
Preferably, an agitator and a filter connected to one end of the first pipe close to the sample water tank are arranged in the sample water tank, and the cross-sectional area of a water inlet of the filter is larger than that of a water outlet of the filter, so that the flow rate of fluid in the pipe can be increased, and the processing speed of the collector can be further increased.
Preferably, the dosing device comprises a doser and a peristaltic pump, and the medicament in the doser is added into the sample water tank through the peristaltic pump to be used for adjusting the pH value of the water body. The agent is ammonia water, and the ammonia water is added into the sample water body, so that on one hand, the granular nickel-63 can be stabilized, and on the other hand, the dissolved nickel-63 can be adsorbed on the butanedione waste under the alkaline condition, and the collection is convenient.
Preferably, the effective filter pore size in the first and second nonwoven fabric cartridges is 0.5 to 2 μm.
Preferably, the first collector is connected in series between the sample water tank and the second collector. Namely, the collection of the nickel-63 in the particle state is firstly carried out, and then the collection of the nickel-63 in the dissolved state is carried out. The granular nickel-63 and the dissolved nickel-63 have different influences on the environment and need to be detected separately.
Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages: the utility model discloses a particulate state and dissolved state nickel-63's collection equipment in water strains a section of thick bamboo and soaks nickel-63's collection that a section of thick bamboo realized particulate state and dissolved state respectively through the non-woven fabrics that adopts non-woven fabrics to strain a section of thick bamboo and flooding dimethylglyoxime, and recovery efficiency is high and stable, can shorten processing time and flow greatly in the more sample of short in-time in-process.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram of a device for collecting nickel-63 in a particle state and a dissolved state in a water body according to a preferred embodiment of the present invention;
in the drawing, a sample water tank 1, a filter 2, a stirrer 3, a doser 4, a peristaltic pump 5, a booster pump 6, a first three-way valve 71, a second three-way valve 72, a third three-way valve 73, a first collector 8, a second collector 9, a flow meter 10, a collection water tank 11, a first pipeline 12, a second pipeline 13, a backwashing pipeline 14 and a drainage pipeline 15.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts shall belong to the protection scope of the present invention.
Example 1 apparatus for collecting nickel-63 in particulate and dissolved form in a body of water
As shown in fig. 1, the collecting apparatus for nickel-63 in particle state and dissolved state in water body of this embodiment includes a backwashing device, and a sample water tank 1, a first pipeline 12, a collector, a second pipeline 13, and a collecting water tank 11 which are connected in sequence. The stirrer 3 and the filter 2 connected to one end of the first pipeline 12 close to the sample water tank 1 are arranged in the sample water tank 1, the cross section of the water inlet of the filter 2 is larger than that of the water outlet, and the arrangement can increase the flow velocity of fluid in the pipeline and further increase the processing speed of the collector. When in use, the rotating speed of the stirrer 3 can be adjusted at 50-2000r/min according to actual needs. The sample water tank 1 and the collection water tank 11 in this embodiment are both 5L in volume and can be adjusted according to the detection limit needs.
Specifically, the relationship between capacity and detection limit can be calculated according to the following formula:
in the formula:
MDC-detection limit, Bq/L;
nb-background count rate, CPM;
tbbackground measurement time, min;
tcbackground sample measurement time, min;
v is the sample volume, L;
recovery of Y-Nickel-63,%;
Effcount efficiency,%.
The nickel-63 collection device in the embodiment can process a large amount of samples according to the detection limit, so that a very low detection lower limit (0.1mBq/L) can be obtained, and the processing speed is high.
The backwashing means includes a first three-way valve 71 provided on the first pipe 12, a second three-way valve 72 provided on the second pipe 13, a backwashing pipe 14 communicating the first three-way valve 71 and the second three-way valve 72, and a third three-way valve 73 provided between the first three-way valve 71 and the collector. The provision of the backwash device allows the collector to be cleaned prior to the next measurement so that the measurement results remain accurate.
A booster pump 6 is further provided between the first three-way valve 71 and the sample water tank 1, and the processing speed can be further controlled. A flow meter 10 is also provided between the second three-way valve 72 and the collection tank 11, the flow meter 10 being used to observe and regulate the flow rate. The flowmeter 10 in this embodiment is a liquid flowmeter 10 having a range of 0.15L/min to 1.5L/min.
The collector comprises a first collector 8 for collecting nickel-63 in particulate form and a second collector 9 for collecting nickel-63 in dissolved form, connected in series. The first collector 8 is connected in series between the sample water tank 1 and the second collector 9. Namely, the collection of the nickel-63 in the particle state is firstly carried out, and then the collection of the nickel-63 in the dissolved state is carried out. Since the granular nickel-63 and the dissolved nickel-63 have different influences on the environment, the detection needs to be carried out separately.
A first nonwoven fabric filter cartridge is arranged in the first collector 8, and a second nonwoven fabric filter cartridge impregnated with dimethylglyoxime is arranged in the second collector 9. The effective filter pore size in the first nonwoven fabric filter cartridge and the second nonwoven fabric filter cartridge is 0.5 to 2 μm, preferably 1 μm. The effective filter pore size is the actual filter pore size of the non-woven fabric filter cylinder.
In this example, the steps for preparing the second nonwoven fabric filter cartridge impregnated with dimethylglyoxime were as follows: firstly, preparing 10g/L dimethylglyoxime solution, then completely soaking the non-woven fabric filter cylinder in the dimethylglyoxime solution, taking out the non-woven fabric filter cylinder for drying after 1h, repeatedly soaking once, taking out and drying. Wherein, the preparation method of the dimethylglyoxime solution comprises the following steps: 10.0g of dimethylglyoxime (C) are weighed out4H8N2O2Not less than97.0%) was dissolved in 100mL of ammonium hydroxide-ethanol solution (pH 8), transferred to a 1L volumetric flask and diluted to the marked line with ammonium hydroxide-ethanol solution (pH 8).
The sample water tank 1 is connected with a dosing device for adjusting the pH value of the water body in the sample water tank 1. The medicine adding device comprises a medicine adding device 4 and a peristaltic pump 5, and medicines in the medicine adding device 4 are added into the sample water tank 1 through the peristaltic pump 5. The agent is ammonia water, and the ammonia water is added into the sample water body, so that on one hand, the granular nickel-63 can be stabilized, and on the other hand, the dissolved nickel-63 can be adsorbed on the butanedione waste under the alkaline condition, and the collection is convenient.
The collection equipment for the granular nickel-63 and the dissolved nickel-63 in the water body is characterized in that the granular nickel-63 is collected quantitatively by adopting the non-woven fabric filter cylinder, and then the dissolved nickel-63 is collected quantitatively by adopting the non-woven fabric filter cylinder impregnated with the dimethylglyoxime, so that the granular nickel-63 and the dissolved nickel-63 in the water body can be collected accurately, stably and efficiently, the recovery efficiency is high and stable, more samples can be processed in a short time, the processing time and the flow are greatly shortened, the measurement efficiency is high, and the equipment is suitable for measuring the nickel-63 in various environmental waters, including rainwater, drinking water, surface water, underground water, seawater and the like.
Example 2 method for detecting Nickel-63 in Water
The method for detecting nickel-63 in the water body in the embodiment uses the collecting device in the embodiment 1, and mainly comprises two steps of collecting and detecting.
Wherein the collecting step comprises: adding ammonia water into the sample water tank 1 under stirring, controlling the pH value of the water body in the sample water tank 1 to reach 8-9, stopping adding the ammonia water, conveying the sample into the collector, allowing the sample to sequentially pass through the first collector 8 and the second collector 9 and then enter the collection water tank 11, and completing nickel-63 collection.
The detection step comprises: and after drying the first non-woven fabric filter cylinder in the first collector 8 and the second non-woven fabric filter cylinder in the second collector 9, putting the first non-woven fabric filter cylinder and the second non-woven fabric filter cylinder into a measuring bottle, adding scintillation liquid into the measuring bottle, and then putting the measuring bottle on a liquid scintillation spectrometer for detection.
The sample was subjected to nickel-63 collection by a nonwoven fabric cartridge and a nonwoven fabric cartridge impregnated with dimethylglyoxime, and the nonwoven fabric cartridge and scintillation liquid were subjected to measurement on a liquid scintillation spectrometer.
Wherein, collecting the granular nickel-63: non-woven fabrics with the aperture of 1 mu m are selected to be placed in the filter cylinder to form a first non-woven fabric filter cylinder, the flow rate is adjusted by the booster pump 6, and the granular nickel-63 in the water body can be effectively and stably extracted and collected. And when the nickel-63 in the granular state is collected, water enters from the middle of the first non-woven fabric filter cylinder and is discharged from the periphery of the first non-woven fabric filter cylinder. The nickel-63 in particle state is collected by filtration, the purpose of water outlet from inside to outside is to better collect the particle state, the particle state can not be fallen off or dissolved again to enter the downstream water body, and the back washing is more facilitated because the inner space is smaller. The recovery efficiency of the granular nickel-63 in the method reaches more than 95 percent.
Collecting dissolved nickel-63: the non-woven fabric is treated into the non-woven fabric impregnated with the dimethylglyoxime by adopting an impregnation technology, 3 second non-woven fabric filter cylinders impregnated with the dimethylglyoxime are connected in series, the flow rate is regulated by the booster pump 6, and the dissolved nickel-63 in the water body can be effectively and stably extracted and collected. When the dissolved nickel-63 is collected, water enters from the periphery of the second non-woven fabric filter cylinder and is discharged from the middle of the second non-woven fabric filter cylinder. The dissolved nickel-63 is absorbed and collected, the purpose from outside to inside is that the external space is large, the pressure is relatively small from inside, thus the liquid from outside to inside has better absorption effect, and the recovery efficiency reaches more than 80%.
Reverse cleaning of the device: and (3) after taking out the first non-woven fabric filter cylinder for collecting nickel-63 and the second non-woven fabric filter cylinder impregnated with dimethylglyoxime, replacing water in the sample water tank 1 with deionized water, switching the three-way valve to a cleaning pipeline, opening the booster pump 6 for cleaning, and carrying out back cleaning on the device to treat the next sample.
Liquid flash measurement: the first non-woven fabric filter cylinder after collecting the nickel-63 and the second non-woven fabric filter cylinder impregnated with the dimethylglyoxime are simply dried and then placed into a measuring bottle, and scintillation liquid is added into the measuring bottle and then placed on a liquid scintillation spectrometer for measurement, so that the sample treatment is easy, and the measuring efficiency can be obviously improved.
The specific implementation process comprises the following steps: adding 5L of an environmental water sample into the sample water tank 1, taking ammonia water out of the chemical feeder 4 through the peristaltic pump 5, adding the ammonia water into the sample water tank 1, stirring and uniformly mixing the sample by using the stirrer 3, and controlling the pH value of the sample to be 8-9. The booster pump 6 is started, the flow rate is adjusted through the flow meter 10, the water sample in the sample water tank 1 enters the first pipeline 12 through the filter 2, at the moment, the first three-way valve 71 and the third three-way valve 73 are communicated with the first pipeline 12 and the collector, the water sample firstly flows through the first collector 8 from the first pipeline 12 to collect the particulate nickel-63, and then the water sample flows through the second collector 9 to collect the dissolved nickel-63. The second three-way valve 72 connects the collector and the collection tank 11, and the water sample enters the collection tank 11 through the second pipe 13. And (3) simply drying the first non-woven fabric filter cylinder after collecting the nickel-63 and the second non-woven fabric filter cylinder impregnated with the dimethylglyoxime, adding scintillation liquid, and then placing the filter cylinder on a liquid scintillation spectrometer for measurement to obtain the content of the nickel-63 in the water body, wherein the scintillation liquid needs to immerse the non-woven fabric filter cylinder.
After processing a sample, the apparatus needs to be backwashed. During backwashing, the first three-way valve 71 communicates the first pipe 12 on the left side thereof with the backwash pipe 14, the second three-way valve 72 communicates the collector with the backwash pipe 14, and the third three-way valve 73 communicates the collector with the drain pipe 15. Deionized water is added into the sample water tank 1, enters the first pipeline 12, enters the backwashing pipeline 14 after passing through the first three-way valve 71, enters the collector after passing through the second three-way valve 72, is backwashed on the collector, and is discharged from the drainage pipeline 15 through the third three-way valve 73, so that backwashing is completed.
The method for detecting nickel-63 in water based on the membrane separation technology is suitable for measuring nickel-63 in particle state and dissolved state in various environmental waters, including rainwater, surface water, drinking water, underground water, seawater and the like. The method comprises the steps of sample mixing, particle state nickel-63 collection, dissolved state nickel-63 collection, device backwashing and liquid flash measurement. Mixing samples: adding a proper amount of ammonia water into a water sample, and simultaneously stirring by using a magnetic stirrer to ensure that the subsequent dissolved nickel-63 is efficiently and stably collected; collecting granular nickel-63: collecting granular nickel-63 by using a first non-woven fabric filter cylinder, adjusting the flow rate by using a booster pump, and recovering the efficiency by more than 95%; collecting dissolved nickel-63: 3 second non-woven fabric filter cylinders impregnated with dimethylglyoxime are connected in series, and the dissolved nickel-63 is efficiently and stably collected; reverse cleaning of the device: taking out the first non-woven fabric filter cylinder for collecting the nickel-63 and the second non-woven fabric filter cylinder for soaking the dimethylglyoxime, and then adopting a deionized water cleaning device for treating the next sample; liquid flash measurement: a liquid scintillation spectrometer was used for the measurement of nickel-63 activity.
The utility model discloses a detection method is strained through the second non-woven fabrics that adopts first non-woven fabrics to strain a section of thick bamboo, flooding dimethylglyoxime respectively and is strained a section of thick bamboo and can be accurate, stable, high-efficient collection water in the particulate state with dissolve attitude nickel-63 and carry out high-efficient measurement, can process more sample like this in short time, shorten processing time and flow greatly.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and to implement the present invention, so as not to limit the protection scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the protection scope of the present invention.
Claims (8)
1. A collection equipment of particle state and dissolved state nickel-63 in water is characterized in that: including sample water tank, first pipeline, collector, second pipeline, the collection water tank that communicates in proper order, the collector includes the first collector that is used for collecting particulate state nickel-63 and is used for collecting the second collector of dissolving state nickel-63 of establishing ties each other, it strains a section of thick bamboo to be provided with first non-woven fabrics in the first collector, it strains a section of thick bamboo to be provided with the second non-woven fabrics in the second collector, the section of thick bamboo is strained to the second non-woven fabrics has dimethylglyoxime, the sample water tank is connected with charge device.
2. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 1, wherein: the collecting equipment further comprises a backwashing device, and the backwashing device comprises a first three-way valve arranged on the first pipeline, a second three-way valve arranged on the second pipeline, a backwashing pipeline communicated with the first three-way valve and the second three-way valve, and a third three-way valve arranged between the first three-way valve and the collector.
3. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 2, wherein: and a booster pump is also arranged between the first three-way valve and the sample water tank.
4. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 2, wherein: and a flowmeter is also arranged between the second three-way valve and the water collection tank.
5. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 1, wherein: the sample water tank is internally provided with a stirrer and a filter connected to one end of the first pipeline close to the sample water tank, and the sectional area of a water inlet of the filter is larger than that of a water outlet.
6. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 1, wherein: the medicine adding device comprises a medicine adding device and a peristaltic pump, and the medicine in the medicine adding device is added into the sample water tank through the peristaltic pump.
7. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 1, wherein: the effective filter pore size in the first non-woven fabric filter cylinder and the second non-woven fabric filter cylinder is 0.5-2 μm.
8. The apparatus for collecting nickel-63 in particulate and dissolved form in a body of water of claim 1, wherein: the first collector is connected in series between the sample water tank and the second collector.
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| CN110745996A (en) * | 2019-11-08 | 2020-02-04 | 苏州热工研究院有限公司 | Collecting device for nickel-63 in water body and detection method for nickel-63 in water body |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110745996A (en) * | 2019-11-08 | 2020-02-04 | 苏州热工研究院有限公司 | Collecting device for nickel-63 in water body and detection method for nickel-63 in water body |
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