CN112629998A - Device and method for analyzing and preprocessing total alpha and beta in primary loop medium of nuclear power plant - Google Patents

Device and method for analyzing and preprocessing total alpha and beta in primary loop medium of nuclear power plant Download PDF

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Publication number
CN112629998A
CN112629998A CN202110013773.3A CN202110013773A CN112629998A CN 112629998 A CN112629998 A CN 112629998A CN 202110013773 A CN202110013773 A CN 202110013773A CN 112629998 A CN112629998 A CN 112629998A
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sample
power plant
nuclear power
liquid
treatment
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刘高勇
侯涛
陈东
张领
邢胜剑
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Sanmen Nuclear Power Co Ltd
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Sanmen Nuclear Power Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38Diluting, dispersing or mixing samples
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4027Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a device for the pre-treatment of total alpha and beta analysis in a loop medium of a nuclear power plant, which comprises a box body (4), a liquid dripping part (1) arranged on one side of a chamber of the box body (4), an evaporation part (2) arranged on the other side of the chamber of the box body (4) and a box cover (5) hinged with the box body (4) and provided with a heating part (3); the liquid dripping part (1) comprises a dropper (11) and a transfusion pipeline (12) connected with the dropper (11), and the dropper (11) is provided with a flow regulating device (13) for controlling dripping speed. And a method for analyzing and pretreating the total alpha and beta in a primary loop medium of the nuclear power plant by adopting the pretreatment device. The invention improves the working efficiency of pretreatment, ensures the accuracy of pretreatment, reduces the risk of contamination of personnel, improves the automation degree of the total alpha and beta analysis pretreatment in the primary loop medium of the nuclear power plant, and liberates manpower.

Description

Device and method for analyzing and preprocessing total alpha and beta in primary loop medium of nuclear power plant
Technical Field
The invention relates to the field of analysis of radionuclide in a primary circuit medium of a nuclear power plant, in particular to a device and a method for analyzing and preprocessing total alpha and beta in the primary circuit medium of the nuclear power plant.
Background
The nuclear power plant estimates the total amount of non-fixed fissile material dispersed in the reactor coolant by analyzing the total alpha in the primary loop medium as one of the ways to evaluate the integrity of the fuel clad; the consistency of the various radioactivity measurements was judged by analyzing the total beta in the loop medium. Therefore, the analysis of the total alpha and beta activities in the primary loop medium of the nuclear power plant plays an important role in the smooth operation of the nuclear power plant. Because the total alpha and beta contents in the primary loop medium of the nuclear power plant are low and are measured in trace amount, a sample to be detected needs to be pretreated before the total alpha and beta contents in the primary loop medium of the nuclear power plant are analyzed. The prior art does not report about pretreatment devices. The operation steps of the pretreatment method comprise: after the sample tray is placed on the heating plate, a small amount of samples to be detected are added into the sample tray for multiple times through personnel operation, the samples to be detected are continuously dripped after the samples in the sample tray are heated and volatilized until no water mark is observed visually, and the cyclic operation is carried out until the treatment of all the samples to be detected is finished. The pretreatment method has the following defects: operators need to be always on duty and cannot deal with other things independently, and the working efficiency is affected; errors caused by manual operation cannot be avoided, and the accuracy of an analysis result is difficult to ensure; the operator is in direct contact with the sample to be tested and, even if relevant protective measures are taken, there is still a risk of contamination.
Disclosure of Invention
The invention aims to solve the problems and provides a device for analyzing and pretreating total alpha and beta in a primary loop medium of a nuclear power plant, which has high working efficiency, ensures the treatment accuracy and can reduce the personnel contamination risk.
The device for the analysis pretreatment of total alpha and beta in a loop medium of a nuclear power plant comprises a box body, a liquid dripping part arranged on one side of a cavity of the box body, an evaporation part arranged on the other side of the cavity of the box body and a box cover which is hinged with the box body and is provided with a heating part; the liquid dripping part comprises a dropper and a transfusion pipeline connected with the dropper, and the dropper is provided with a flow regulating device for controlling the dripping speed.
Preferably, the liquid dripping part, the evaporating part and the heating part are controlled by a PLC control system.
Preferably, the flow regulating device is a peristaltic pump.
Preferably, the evaporation part comprises a sample tray bracket and a weight sensing device arranged below the sample tray bracket; the sample tray bracket comprises a tray for placing a sample tray and a rotary sleeve component which is rotatably connected with the base; the base is arranged on the weight sensing device; the tray is provided with a limiting groove of the sample tray.
Preferably, the infusion pipeline comprises a main pipeline and a branch pipeline, the main pipeline is arranged in the box chamber, and the branch pipeline is arranged outside the box chamber; the main pipeline is connected with the dropper through a rotary joint, and the branch pipelines are respectively connected with a sample bottle A, a sample bottle B, a sample bottle C and a sample bottle D which are filled with a treatment liquid A, a treatment liquid B, a treatment liquid C and a sample to be detected; the main pipeline is serially connected with a liquid transfer pump and a liquid storage bag, and the branch pipeline is provided with a stop valve.
Preferably, the heating part comprises an infrared heating pipe for providing heat, the box cover is provided with a discharge port, and the inner wall of the box cover is provided with a heat reflecting layer.
Another object of the present invention is to provide a method for preprocessing α and β analysis in a primary loop medium by using the preprocessing apparatus.
A method for analysis pretreatment of alpha and beta in a loop medium of a nuclear power plant comprises the following steps:
s1: placing a sample tray in a limiting groove of the sample tray, closing a box cover, and operating a PLC control system to set the dropping sequence and the dropping amount of a liquid dropping part, the weight preset value of a weight sensing device of an evaporation part and the heating temperature of a heating part, wherein the weight preset value comprises a first weight preset value and a second preset value;
s2: the liquid dripping part is used for dripping the treatment liquid A, the treatment liquid B and the sample to be detected into the sample tray in sequence, then the heating part is started, the sample to be detected is evaporated and concentrated at the heating temperature set in the step S1, and the evaporated gas is discharged from the discharge port;
s3: evaporating and concentrating the weight of the sample to be detected to the first weight preset value, dropwise adding the treatment liquid C into the sample tray, evaporating and concentrating to the second weight preset value, stopping heating, and cooling the concentrated sample to be detected to room temperature.
Preferably, the treatment liquid A is a potassium iodide solution of 0.08-0.13 mol/L, the treatment liquid B is a sodium hydroxide solution of 0.05-0.1 mol/L, and the treatment liquid C is a methanol or ethanol solution.
The invention has the following beneficial effects:
1. the device for the analysis pretreatment of the total alpha and the total beta in the primary loop medium of the nuclear power plant comprises the liquid dripping part, the evaporating part and the heating part, so that the automation of the analysis pretreatment of the total alpha and the total beta in the primary loop medium of the nuclear power plant is realized, the operation process is simple, operators do not need to continuously watch and repeatedly add the solution, the manpower is liberated, the error of manual dripping operation is reduced, and the operation accuracy is improved.
2. According to the device for the analysis pretreatment of the total alpha and beta in the loop medium of the nuclear power plant, a closed chamber is formed after the box cover is closed, and when a sample to be detected is subjected to evaporation concentration treatment, an operator does not need to directly contact the sample to be detected, so that the contamination risk of the operator is reduced; the exhaust port arranged on the box cover of the device can be connected with the cooling reflux device, so that the evaporated liquid can be recycled, the consumption of newly added supplementary media due to the loss of the media in a loop is reduced, and the production cost is reduced.
3. The heating part comprises the infrared heating pipe for providing heat, the heat propagation speed is high, the heating rate is high, the heating time is shortened, and the working efficiency is improved; in addition, in the heating process, the diffusion directions of the volatile matters can be ensured to be consistent, and the volatilization treatment effect is further ensured; and the infrared heating device has obvious electricity-saving effect and reduces the production cost. The inner wall of the box cover is provided with a heat reflecting layer which plays a positive role in heat transmission, so that heat is concentrated in the evaporation part, and the heat utilization rate and the heating efficiency are improved.
4. The liquid storage bag is provided with the interfaces respectively connected with the branch pipelines, and the treatment fluid A, the treatment fluid B, the treatment fluid C and the sample to be detected respectively enter the liquid storage bag through pipelines, so that mutual pollution is avoided, and the accuracy of alpha and beta analysis pretreatment in a loop medium of a nuclear power plant is ensured.
Drawings
FIG. 1 is a schematic diagram of a device for pre-treatment of total alpha and beta analysis in a primary loop medium of a nuclear power plant;
FIG. 2 is a schematic view of an evaporation section;
FIG. 3 is a schematic view of a liquid dropping portion;
wherein, 1 is a liquid dropping part, 11 is a dropper, 12 is a transfusion pipeline, 121 is a main pipeline, 1211 is a liquid transfer pump, 1212 is a liquid storage bag, 122 is a branch pipeline, 13 is a flow regulating device, 14 is a rotary interface, 2 is an evaporation part, 21 is a sample tray bracket, 211 is a tray, 212 is a rotary sleeve component, 213 is a base, 22 is a weight sensing device, 3 is a heating part, 4 is a box body, 5 is a box cover, 51 is a discharge port, 6 is a sample bottle A, 7 is a sample bottle B, 8 is a sample bottle C, and 9 is a sample bottle D.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
Fig. 1 is a schematic diagram of a device for total alpha and beta analysis pretreatment in a primary loop medium of a nuclear power plant, and as shown in fig. 1, the device for total alpha and beta analysis pretreatment in the primary loop medium of the nuclear power plant comprises a box body 4, a liquid dripping part 1 arranged on one side of a chamber of the box body 4, an evaporation part 2 arranged on the other side of the chamber of the box body 4, and a box cover 5 hinged to the box body 4 and provided with a heating part 3; the liquid dripping part 1 comprises a dropper 11 and a transfusion pipeline 12 connected with the dropper 11, and the dropper 11 is provided with a flow regulating device 13 for controlling dripping speed. The liquid dripping part 1, the evaporating part 2 and the heating part 3 are controlled by a PLC control system. The flow regulating device 13 is a peristaltic pump.
Heating portion 3 include the infrared heating pipe that is used for providing the heat, case lid 5 on be provided with discharge port 51, the discharge port can be connected with condensing equipment, retrieve volatilizing boric acid, 5 inner walls of case lid be provided with the heat reflection stratum. The box body 4 comprises a protective layer, a heat preservation layer and a shell. The heat reflecting layer is an aluminum foil film layer. The box cover further comprises a temperature sensing device, and the temperature sensing device is controlled by the PLC control system.
Fig. 2 is a schematic view of an evaporation portion, and as shown in fig. 2, the evaporation portion 2 includes a sample tray holder 21 and a weight sensing device 22 disposed below the sample tray holder 21; the sample tray bracket 21 comprises a tray 211 for placing a sample tray and a base 213 rotatably connected with the rotary sleeve assembly 212; the base 213 is disposed on the weight sensing device 22; the tray 211 is provided with a limiting groove of the sample tray. Because the chamber of the pretreatment device is in a constant temperature state in the whole evaporation concentration process, the temperature does not influence the measurement precision of the weight sensing device, and the accuracy of the pretreatment is further ensured.
Tray 211 on be provided with 1~6 spacing recess. In order to meet the use requirements of sample trays with different specifications, the diameter of the limiting groove arranged on the tray 211 is 60, 75, 90, 100, 120 or 150 mm. The sample plate is a stainless steel sample plate convenient to clean.
Fig. 3 is a schematic view of a liquid dropping unit, and as shown in fig. 3, the infusion pipeline 12 includes a main pipeline 121 and a branch pipeline 122, the main pipeline 121 is disposed in the chamber of the box 4, and the branch pipeline 122 is disposed outside the chamber of the box 4; the main pipeline 121 is connected with the dropper 11 through a rotary interface 14, and the branch pipeline 122 is respectively connected with a sample bottle A6, a sample bottle B7, a sample bottle C8 and a sample bottle D9 which are filled with a treatment liquid A, a treatment liquid B, a treatment liquid C and a sample to be detected; a liquid-transfering pump 1211 and a liquid storage bag 1212 are serially connected to the main pipeline 121, the liquid storage bag 1212 is provided with a connector respectively connected with the branch pipeline 122, and the branch pipeline 122 is provided with a flow stopping valve.
A method for analyzing and preprocessing total alpha and beta in a loop medium of a nuclear power plant by adopting the device comprises the following steps:
s1: placing a sample tray in a limiting groove of the sample tray 211, closing the box cover 5, and operating the PLC control system to set the dropping sequence and the dropping amount of the liquid dropping part 1, the preset weight value of the weight sensing device 22 of the evaporation part 2 and the heating temperature of the heating part 3, wherein the preset weight value comprises a first preset weight value and a second preset weight value;
s2: the liquid dripping part 1 is used for dripping the treatment liquid A, the treatment liquid B and a sample to be detected into the sample tray in sequence, then the heating part 3 is started, the sample to be detected is evaporated and concentrated at the temperature of 55-65 ℃, and evaporated gas is discharged from the discharge port;
s3: and evaporating and concentrating the weight of the sample to be detected to the first preset weight value, dropwise adding the treatment liquid C into the sample tray, evaporating and concentrating to the second preset weight value, stopping heating, and cooling the concentrated sample to be detected for 4-4.5 hours at room temperature.
The specific dropping process of the liquid dropping part is as follows: opening a flow stopping valve on a branch pipeline connected with the treatment liquid A, pumping the treatment liquid A into the liquid storage bag by a liquid transfer pump arranged on the main pipeline, closing the flow stopping valve at the moment, controlling the treatment liquid A to slowly drip into the sample tray by the flow regulating device, and dripping the treatment liquid B and the sample to be detected into the sample tray once by adopting the same steps after finishing dripping. When the sample is dripped, the position of the burette is adjusted through the rotary interface, so that the burette can be aligned with the center of the sample plate. Because the stop valve is in a closed state in the dripping process, when the liquid storage bag is dripped, the liquid storage bag is compressed due to the action of vacuum negative pressure, so that the liquid treatment liquid A, the treatment liquid B, the treatment liquid C and the sample to be detected stored in the liquid storage bag can be discharged to the greatest extent without residue, and the accuracy of the pretreatment device is improved. After the end, the burette can be turned to the side far away from the evaporation part.
And determining the number of the sample disks to be used according to the amount of the samples to be detected, wherein the sample disks are symmetrically placed in the limiting grooves of the sample disk bracket.
Through the rotation of the rotary sleeve component 212, the tray 211 is driven to rotate, so that the purpose of dripping the treatment liquid A, the treatment liquid B, the treatment liquid C and a sample to be detected into different sample trays is achieved.
Example 2
In this embodiment, the volume of the sample to be measured is 10mL, the specification of the used sample trays is 90mm, the number of the sample trays is 5, and the volume of the sample to be measured divided in each sample tray is 2 mL.
S1: placing a sample tray in a limiting groove of the sample tray, closing a box cover, and operating a PLC control system to set the dropping sequence and the dropping amount of a liquid dropping part, the weight preset value of a weight sensing device of an evaporation part and the heating temperature of a heating part, wherein the weight preset value comprises a first weight preset value and a second preset value;
s2: the liquid dripping part is used for dripping the treatment liquid A, the treatment liquid B and a sample to be detected into the sample tray in sequence, then the heating part is started, the sample to be detected is evaporated and concentrated at 56 ℃, and evaporated gas is discharged from the discharge port;
s3: evaporating and concentrating the weight of the sample to be detected to the first weight preset value, dropwise adding the treatment liquid C into the sample tray, evaporating and concentrating to the second weight preset value, stopping heating, and cooling the concentrated sample to be detected for 4 hours at room temperature.
The treatment solution A is 0.1mol/L potassium iodide solution, the treatment solution B is 0.1mol/L sodium hydroxide solution, and the treatment solution C is methanol solution.
The above-described preferred embodiments of the present invention are not intended to limit the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the claims of the present invention.

Claims (8)

1. Device of total alpha, beta analysis pretreatment in nuclear power plant's a return circuit medium which characterized in that: comprises a box body (4), a liquid dripping part (1) arranged at one side of a chamber of the box body (4), an evaporation part (2) arranged at the other side of the chamber of the box body (4) and a box cover (5) which is hinged with the box body (4) and is provided with a heating part (3); the liquid dripping part (1) comprises a dropper (11) and a transfusion pipeline (12) connected with the dropper (11), and the dropper (11) is provided with a flow regulating device (13) for controlling dripping speed.
2. The device for the pre-treatment of total alpha and beta analysis in a nuclear power plant primary loop medium as recited in claim 1, wherein: the liquid dripping part (1), the evaporating part (2) and the heating part (3) are controlled by a PLC control system.
3. The device for the pre-treatment of total alpha and beta analysis in a nuclear power plant primary loop medium as recited in claim 1, wherein: the flow regulating device (13) is a peristaltic pump.
4. The device for the pre-treatment of total alpha and beta analysis in a nuclear power plant primary loop medium as recited in claim 1, wherein: the evaporation part (2) comprises a sample disc bracket (21) and a weight sensing device (22) arranged below the sample disc bracket (21); the sample plate bracket (21) comprises a tray (211) for placing a sample plate and a rotary sleeve assembly (212) rotatably connected with the base (213); the base (213) is arranged on the weight sensing device (22); the tray (211) is provided with a limiting groove of the sample tray.
5. The device for the pre-treatment of total alpha and beta analysis in a nuclear power plant primary loop medium as recited in claim 1, wherein: the infusion pipeline (12) comprises a main pipeline (121) and a branch pipeline (122), the main pipeline (121) is arranged in the cavity of the box body (4), and the branch pipeline (122) is arranged outside the cavity of the box body (4); the main pipeline (121) is connected with the dropper (11) through a rotary interface (14), and the branch pipeline (122) is respectively connected with a sample bottle A (6), a sample bottle B (7), a sample bottle C (8) and a sample bottle D (9) which are filled with a treatment liquid A, a treatment liquid B, a treatment liquid C and a sample to be detected; the main pipeline (121) is provided with a liquid transfer pump (1211) and a liquid storage bag (1212) in series, and the branch pipeline (122) is provided with a stop valve.
6. The device for the pre-treatment of total alpha and beta analysis in a nuclear power plant primary loop medium as recited in claim 1, wherein: heating portion (3) including being used for providing the infrared heating pipe of heat, case lid (5) on be provided with discharge port (51), case lid (5) inner wall be provided with the heat reflection stratum.
7. A method for pre-processing a total alpha, beta analysis in a nuclear power plant primary loop medium using the apparatus of claim 1, comprising the steps of:
s1: placing a sample tray in a limiting groove of a sample tray (211), then closing a box cover (5), operating a PLC control system to set the dropping sequence and the dropping amount of a liquid dropping part (1), the weight preset value of a weight sensing device (22) of an evaporation part (2) and the heating temperature of a heating part (3), wherein the weight preset value comprises a first weight preset value and a second preset value;
s2: the liquid dripping part (1) sequentially drips the treatment liquid A, the treatment liquid B and the sample to be detected into the sample tray, then the heating part (3) is started, the sample to be detected is evaporated and concentrated at the heating temperature set in the step S1, and the evaporated gas is discharged from the discharge port;
s3: evaporating and concentrating the weight of the sample to be detected to the first weight preset value, dropwise adding the treatment liquid C into the sample tray, evaporating and concentrating to the second weight preset value, stopping heating, and cooling the concentrated sample to be detected to room temperature.
8. The method for the pre-treatment of the total alpha and beta analysis in the primary loop medium of the nuclear power plant as set forth in claim 9, wherein: the treating fluid A is a potassium iodide solution of 0.08-0.13 mol/L, the treating fluid B is a sodium hydroxide solution of 0.05-0.1 mol/L, and the treating fluid C is a methanol or ethanol solution.
CN202110013773.3A 2021-01-06 2021-01-06 Device and method for analyzing and preprocessing total alpha and beta in primary loop medium of nuclear power plant Pending CN112629998A (en)

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Application publication date: 20210409