CN217238399U - Pretreatment device for analyzing carbon-14 activity in high-activity tritium water - Google Patents
Pretreatment device for analyzing carbon-14 activity in high-activity tritium water Download PDFInfo
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- CN217238399U CN217238399U CN202122560456.1U CN202122560456U CN217238399U CN 217238399 U CN217238399 U CN 217238399U CN 202122560456 U CN202122560456 U CN 202122560456U CN 217238399 U CN217238399 U CN 217238399U
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Abstract
The utility model relates to a pretreatment device for analyzing carbon-14 activity in high-activity tritium water, which comprises an ultraviolet lamp, an oxidation reactor, a carrier gas device and a tritium removal and carbon-14 absorption device; an oxidant inlet and a sample inlet are respectively formed in the upper part of one side face of the oxidation reactor, and an oxidant and a high tritium water sample respectively enter the oxidation reactor through the oxidant inlet and the sample inlet; an ultraviolet lamp is arranged in the oxidation reactor, the top of the oxidation reactor is connected with a carrier gas device, a gas outlet is arranged at the upper part of the other side face of the oxidation reactor, and the gas outlet of the oxidation reactor is connected with a tritium removal and carbon-14 absorption device. The utility model discloses a tritium in the sample is got rid of completely to carbon-14 activity analysis preprocessing device in the high activity tritium water, collects carbon-14 in the sample, and the pulse of tritium is piled up the influence to carbon-14 count when avoiding sample analysis.
Description
Technical Field
The utility model relates to a tritium water analysis technical field especially relates to a carbon-14 activity analysis preprocessing device in high activity tritium water.
Background
The heavy water reactor nuclear power plant carbon-14 is mainly generated by a 17O (n, α) → 14C reaction, and due to the difference in chemical characteristics of the systems of the heavy water reactor nuclear power plant, the form of the carbon-14 is different, for example, the moderator system carbon-14 is mainly inorganic carbon, and the coolant system carbon-14 is mainly in the form of low molecular organic compounds such as volatile gas, methanol, formaldehyde and formic acid.
Because heavy water is used as the moderator and the coolant of the heavy water reactor nuclear power plant, tritium activity in the heavy water is several orders of magnitude higher than that of carbon-14. When a liquid scintillation counter is used for analyzing the activity of carbon-14 in high-tritium water, the pulse accumulation of tritium in a sample can enter a carbon-14 counting interval (18.6-156keV), so that the analysis data of the carbon-14 is higher.
SUMMERY OF THE UTILITY MODEL
Based on this, it is necessary to provide a pretreatment device for analyzing carbon-14 activity in high-activity tritiated water, which completely removes tritium in a sample, collects carbon-14 in the sample, and avoids the influence of pulse accumulation of tritium on carbon-14 counting during sample analysis, in order to solve the problem of influence of tritium in the sample on counting of carbon-14 analysis data during analysis of carbon-14 activity in high-activity tritiated water.
In order to achieve the above object, the present invention provides the following technical solutions:
a pretreatment device for analyzing carbon-14 activity in high-activity tritiated water comprises an ultraviolet lamp, an oxidation reactor, a carrier gas device and a tritium removal and carbon-14 absorption device;
an oxidant inlet and a sample inlet are respectively formed in the upper part of one side face of the oxidation reactor, and an oxidant and a high tritium water sample respectively enter the oxidation reactor through the oxidant inlet and the sample inlet;
an ultraviolet lamp is arranged in the oxidation reactor, the top of the oxidation reactor is connected with a carrier gas device, a gas outlet is arranged at the upper part of the other side surface of the oxidation reactor, and the gas outlet of the oxidation reactor is connected with a tritium removal and carbon-14 absorption device;
the high tritium water sample reacts with an oxidant under the irradiation of an ultraviolet lamp, generated gas flows into a tritium removal and carbon-14 absorption device through a gas outlet through carrier gas, tritium in the high tritium water sample is completely removed through the tritium removal and carbon-14 absorption device, and carbon-14 in the high tritium water sample is collected.
The working principle is as follows: an oxidant and a high tritium water sample respectively enter an oxidation reactor through an oxidant inlet and a sample inlet, the high tritium water sample and the oxidant react under the irradiation of an ultraviolet lamp, carbon-14 existing in organic and inorganic forms in the high tritium water sample is converted into CO2 and flows into a tritium removal and carbon-14 absorption device through a gas outlet by carrier gas, the tritium removal and carbon-14 absorption device completely eliminates tritium in the high tritium water sample and collects carbon-14 in the high tritium water sample, and the influence of pulse accumulation of tritium on carbon-14 counting during analysis of the high tritium water sample is avoided.
Furthermore, a waste discharge valve V is arranged at the bottom of the oxidation reactor, the high tritium water sample and the oxidant react under the irradiation of an ultraviolet lamp, and the generated liquid is discharged through the waste discharge valve.
Further, the oxidant passes through the pipeline and gets into oxidation reactor 3 through the oxidant entry, the oxidant sets up the oxidant isolating valve on the pipeline that the oxidant gets into oxidation reactor through the oxidant entry, high tritium water sample passes through the pipeline and gets into oxidation reactor through the sample entry, high tritium water sample sets up the isolation valve of appearance on the pipeline that the sample entry got into oxidation reactor.
Further, the carrier gas device includes diffusion head, carrier gas pipe, flowmeter and carries the air control valve, carrier gas pipe keeps away from oxidation reactor top one end from the bottom up and is equipped with carrier gas air control valve and flowmeter in proper order, carrier gas pipe is close to oxidation reactor top one end and gets into oxidation reactor and is connected with the diffusion head, the diffusion head sets up inside oxidation reactor, and the carrier gas passes through inside the carrier gas pipe gets into oxidation reactor via the diffusion head.
Further, the carrier gas is N2; the oxidant is H2O2 or H2PO4+ Na2PO 4.
Further, the tritium removal and carbon-14 absorption device comprises a primary acid absorption device, a secondary acid absorption device and an alkali absorption device, and a gas outlet of the oxidation reactor is sequentially connected with the primary acid absorption device, the secondary acid absorption device and the alkali absorption device.
Further, the first-stage acid absorption device is a first glass bubbler filled with an acid absorption liquid, the second-stage acid absorption device is a second glass bubbler filled with the acid absorption liquid, and the alkali absorption device is a glass absorption bottle filled with an alkali absorption liquid.
Further, gas inlets are formed in the tops of the first glass bubbler and the second glass bubbler, and gas outlets are formed in the upper portions of the side surfaces of the first glass bubbler and the second glass bubbler; the gas outlet of the oxidation reactor is connected with the gas inlet of the first glass bubbler through a connecting hose, the gas outlet of the first glass bubbler is connected with the gas inlet of the second glass bubbler through a silicone tube, and the gas outlet of the second glass bubbler is connected with the pipeline of the glass absorption bottle.
Furthermore, a quick connector is arranged on a connecting hose which is connected with the gas outlet of the oxidation reactor and the gas inlet of the first glass bubbler.
Further, the acid absorption liquid of the primary acid absorption device and the acid absorption liquid of the primary acid absorption device are both H2SO 4; and the alkali absorption liquid of the alkali absorption device is NaOH.
Further, the pretreatment device for analyzing the carbon-14 activity in the high-activity tritium water further comprises a waste liquid absorption device, and the waste liquid absorption device is connected with the alkali absorption device through a pipeline.
Further, a gas inlet is formed in the top of the glass absorption bottle, a gas outlet is formed in the upper portion of the side face of the glass absorption bottle, a gas outlet of the second glass bubbler is connected with a gas inlet of the glass absorption bottle through a pipeline, and a gas outlet of the glass absorption bottle is connected with a glass colorimetric tube through a pipeline.
The utility model has the advantages of:
the utility model discloses a carbon-14 activity analysis preprocessing device in high activity tritium water not only can avoid the pulse of high tritium to pile up the influence to carbon-14 count, can also detach the influence of energy beta, gamma nuclide at 18.6-156keV within range in the sample to ensure carbon-14 measuring accuracy.
Drawings
FIG. 1 is a schematic structural diagram of a device for analyzing and pretreating carbon-14 activity in high-activity tritium water.
In the figure, 1, a diffusion head; 2. an ultraviolet lamp; 3. an oxidation reactor, 4, a first glass bubbler; 5. a second glass bubbler; 6. a glass absorber bottle; 7; a glass colorimetric cylinder; 8. a carrier gas pipe; 9. a connecting hose; 10. A silicone tube; 11. an oxidant isolation valve; 12. a sample injection isolation valve; 13. a waste valve; 14. a pneumatic control valve; 15. a quick connector; 16. a flow meter.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Referring to fig. 1, the utility model provides a carbon-14 activity analysis preprocessing device in high activity tritium water, including ultraviolet lamp 2, oxidation reactor 3, the carrier gas device, remove tritium and carbon-14 absorbing device to and waste liquid absorbing device.
And the upper part of one side surface of the oxidation reactor 3 is respectively provided with an oxidant inlet and a sample inlet, and the oxidant and the high tritium water sample respectively enter the oxidation reactor 3 through the oxidant inlet and the sample inlet.
An ultraviolet lamp 2 is arranged inside the oxidation reactor 3, the top of the oxidation reactor 3 is connected with a carrier gas device, a gas outlet is arranged on the upper portion of the other side face of the oxidation reactor 3, and the gas outlet of the oxidation reactor 3 is connected with a tritium removal and carbon-14 absorption device.
The high tritium water sample reacts with an oxidant under the irradiation of an ultraviolet lamp 2, generated gas flows into a tritium removal and carbon-14 absorption device through a gas outlet through carrier gas, tritium in the high tritium water sample is completely removed through the tritium removal and carbon-14 absorption device, and carbon-14 in the high tritium water sample is collected.
The bottom of the oxidation reactor 3 is provided with a waste discharge valve 13, the high tritium water sample and the oxidant react under the irradiation of the ultraviolet lamp 2, and the generated liquid is discharged through the waste discharge valve 13.
The oxidant gets into oxidation reactor 3 through the oxidant entry through the pipeline, set up oxidant isolating valve 11 on the pipeline that the oxidant got into oxidation reactor through the oxidant entry, high tritium water sample gets into oxidation reactor 3 through the sample entry through the pipeline, high tritium water sample sets up on the pipeline that the sample entry got into oxidation reactor and advances a kind isolating valve 12.
The carrier gas device includes diffusion head 1, carrier gas pipe 8, flowmeter 16 and carries air control valve 14, carrier gas pipe 8 is kept away from 3 top one ends from the bottom up of oxidation reactor and is equipped with carrier gas control valve 14 and flowmeter 16 in proper order, carrier gas pipe 8 is close to 3 top one ends of oxidation reactor and gets into oxidation reactor 3 and is connected with diffusion head 1, diffusion head 1 sets up inside oxidation reactor 3, and the carrier gas is through carrier gas pipe 8 inside 3 entering oxidation reactor via diffusion head 1.
The carrier gas is 10mL/min N2; the oxidant is 1 wt% of H2O2 or H2PO4+ Na2PO 4.
The tritium-removing and carbon-14 absorbing device comprises a primary acid absorbing device, a secondary acid absorbing device and an alkali absorbing device, and a gas outlet of the oxidation reactor is sequentially connected with the primary acid absorbing device, the secondary acid absorbing device and the alkali absorbing device.
Carbon-14 existing in organic and inorganic forms in the high tritium water sample is converted into CO2, the CO2 flows into a primary acid absorption device, a secondary acid absorption device and an alkali absorption device through a gas outlet in sequence, most H-3 in the gas is removed by the primary acid absorption device and the secondary acid absorption device, the CO2 in the gas absorbed by acid liquor is absorbed by alkali liquor, and finally the carbon-14 activity in the sample is calculated by measuring the carbon-14 activity in the alkali absorption liquid.
The first-stage acid absorption device is a first glass bubbler 4 filled with acid absorption liquid, the second-stage acid absorption device is a second glass bubbler 5 filled with acid absorption liquid, and the alkali absorption device is a glass absorption bottle 6 filled with alkali absorption liquid.
Carbon-14 existing in organic and inorganic forms in the high tritium water sample is converted into CO2, the CO2 flows into a primary acid absorption device, a secondary acid absorption device and an alkali absorption device through a gas outlet in sequence, most H-3 in the gas is removed by acid absorption liquid of the primary acid absorption device and the secondary acid absorption device, the gas absorbed by the acid absorption liquid absorbs CO2 in the gas by the alkali absorption liquid of the alkali absorption device, and finally the carbon-14 activity in the high tritium water sample is calculated by measuring the carbon-14 activity in the alkali absorption liquid.
The top parts of the first glass bubbler 4 and the second glass bubbler 5 are respectively provided with a gas inlet, and the upper parts of the side surfaces of the first glass bubbler 4 and the second glass bubbler 5 are respectively provided with a gas outlet; the gas outlet of the oxidation reactor 3 is connected with the gas inlet of the first glass bubbler 4 through a connecting hose 9, the gas outlet of the first glass bubbler 4 is connected with the gas inlet of the second glass bubbler 5 through a silicone tube 10, and the gas outlet of the second glass bubbler 5 is connected with the glass absorption bottle 6 through a pipeline.
A quick connector 15 is arranged on a connecting hose 9 which is connected with the gas outlet of the oxidation reactor 3 and the gas inlet of the first glass bubbler 4.
The acid absorption liquid of the primary acid absorption device and the acid absorption liquid of the primary acid absorption device are both 0.4mol/L H2SO 4; and the alkali absorption liquid of the alkali absorption device is 0.2mol/L NaOH.
The waste liquid absorption device is connected with the alkali absorption device through a pipeline, and the waste liquid absorption device is a glass colorimetric tube 7 filled with water.
The first glass bubbler 4 and the second glass bubbler 5 are both 50mL glass bubblers, the glass colorimetric tube is 50mL, the gas carrying tube 8 is a 3/8-inch stainless steel tube, the oxidant isolation valve 11 and the sample injection isolation valve 12 are both 3/8-inch check valves, the connecting hose 9 is a hose with an outer diameter of 4mm, and the quick connector 15 is a PU-4mm gas path quick-plug quick connector; the glass connectors of the oxidation reactor 3, the first glass bubbler 4, the second glass bubbler 5, the glass absorption bottle 6 and the glass colorimetric tube 7 are all connected by 10mm diameter silicone tubes, the flow meter 16 is a DFG-6T gas flow meter, and the gas-carrying control valve 14 is a Lanto-R01316L stainless steel pressure reducing valve.
The gas outlet of the first glass bubbler 4 is connected with the gas inlet of the second glass bubbler 5 through a 10mm diameter silicone tube, the gas outlet of the second glass bubbler 5 is connected with the gas inlet of the glass absorption bottle 6 through a 10mm diameter silicone tube, the gas outlet of the glass absorption bottle 6 is connected with the glass colorimetric tube 7 through a 10mm diameter silicone tube, the oxidant enters the oxidation reactor 3 through the oxidant inlet through the 10mm diameter silicone tube, and the high tritium water sample enters the oxidation reactor 3 through the sample inlet through the 10mm diameter silicone tube.
Use the utility model discloses a carbon-14 activity assay preprocessing device in high activity tritium water, include following step:
1. high-purity nitrogen cylinder adopts 1/4 inches stainless steel park to connect relief pressure valve and floater flowmeter, with 4mm external diameter hose and 4mm quick connector gas circuit insert the mode soon according to figure 1 with the utility model discloses a carbon-14 activity analysis preprocessing device connects in high activity tritium water.
2. 50mL of a 0.4mol/L sulfuric acid solution was added to each of the 50mL first glass bubbler 4 and the second glass bubbler 5.
3. 50mL of 0.2mol/L sodium hydroxide solution was added to a 50mL glass absorption flask 6.
4. 50mL of demineralized water was added to 50mL of glass cuvette 7.
5. 50mL of the first glass bubbler 4, the second glass bubbler 5, the glass absorption flask 6, and the glass colorimetric tube 7 were connected to each glass device by a 10mm diameter silicone tube in the manner shown in FIG. 1.
6. Quantitatively loading a high tritium water sample and an oxidant into the oxidation reactor 3, closing the oxidant isolation valve 11 and the sample injection isolation valve 12, checking the connection and sealing of each glass device, and confirming that no leakage point exists.
7. Turning on the power supply of the ultraviolet lamp 2 and the air-carrying control valve 14, adjusting the flow meter 16, controlling the bubbling flow to be 8-9mL/min, continuously bubbling slowly for 10 minutes, and then turning off the ultraviolet lamp 2 and the air-carrying control valve 14.
8. The 50mL glass vial 6 was taken out, and the alkali-absorbed solution was taken out.
9. The same method is used to treat desalted water as comparison blank.
10. Taking the alkali absorption liquid as a sample, and measuring the carbon-14 activity in the alkali absorption liquid by using a liquid scintillation counter.
11. The carbon-14 activity in the high tritium sample was calculated according to the formula.
The utility model discloses a carbon-14 activity analysis preprocessing device in high activity tritium water not only can avoid the pulse of high tritium to pile up the influence to carbon-14 count, can also detach the influence of energy beta, gamma nuclide at 18.6-156keV within range in the sample to ensure carbon-14 measuring accuracy.
The above-mentioned embodiments only represent several embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (12)
1. A pretreatment device for analyzing carbon-14 activity in high-activity tritiated water is characterized by comprising an ultraviolet lamp (2), an oxidation reactor (3), a carrier gas device and a tritium removal and carbon-14 absorption device; an oxidant inlet and a sample inlet are respectively formed in the upper part of one side face of the oxidation reactor (3), and an oxidant and a high tritium water sample respectively enter the oxidation reactor (3) through the oxidant inlet and the sample inlet; an ultraviolet lamp (2) is arranged inside the oxidation reactor (3), the top of the oxidation reactor (3) is connected with a carrier gas device, a gas outlet is formed in the upper part of the other side face of the oxidation reactor (3), and the gas outlet of the oxidation reactor (3) is connected with a tritium removal and carbon-14 absorption device; the high tritium water sample and an oxidant react under the irradiation of an ultraviolet lamp (2), generated gas flows into a tritium and carbon-14 removing absorption device through a gas outlet by carrier gas, tritium in the high tritium water sample is completely removed by the tritium removing and carbon-14 absorbing device, and carbon-14 in the high tritium water sample is collected.
2. The pretreatment device for analyzing the carbon-14 activity in high-activity tritium water according to claim 1, wherein a waste discharge valve (13) is arranged at the bottom of the oxidation reactor (3), the high-activity tritium water sample and the oxidant react under the irradiation of the ultraviolet lamp (2), and the generated liquid is discharged through the waste discharge valve (13).
3. The pretreatment device for analyzing the carbon-14 activity in the high-activity tritium water according to claim 1, wherein the oxidant enters the oxidation reactor (3) through a pipeline through an oxidant inlet, the pipeline through which the oxidant enters the oxidation reactor is provided with an oxidant isolation valve (11), the high-tritium water sample enters the oxidation reactor (3) through a pipeline through a sample inlet, and the pipeline through which the high-tritium water sample enters the oxidation reactor through the sample inlet is provided with a sample injection isolation valve (12).
4. The pretreatment device for analyzing the carbon-14 activity in high-activity tritiated water, according to claim 1, wherein the carrier gas device comprises a diffusion head (1), a carrier gas pipe (8), a flow meter (16) and a carrier gas control valve (14), the carrier gas pipe (8) is provided with the carrier gas control valve (14) and the flow meter (16) in sequence from bottom to top at the end far away from the top of the oxidation reactor (3), the carrier gas pipe (8) enters the oxidation reactor (3) and is connected with the diffusion head (1) at the end close to the top of the oxidation reactor (3), the diffusion head (1) is arranged inside the oxidation reactor (3), and the carrier gas enters the oxidation reactor (3) through the diffusion head (1) through the carrier gas pipe (8).
5. The apparatus for analysis and pretreatment of carbon-14 activity in high-activity tritiated water according to any one of claims 1 to 4, wherein the tritium removal and carbon-14 absorption apparatus comprises a primary acid absorption apparatus, a secondary acid absorption apparatus and a base absorption apparatus, and the gas outlet of the oxidation reactor is connected with the primary acid absorption apparatus, the secondary acid absorption apparatus and the base absorption apparatus in sequence.
6. The apparatus for analysis and pretreatment of carbon-14 activity in high-activity tritiated water according to claim 5, characterized in that the primary acid absorption device is a first glass bubbler (4) filled with acid absorption liquid, the secondary acid absorption device is a second glass bubbler (5) filled with acid absorption liquid, and the alkali absorption device is a glass absorption bottle (6) filled with alkali absorption liquid.
7. The pretreatment device for analysis of carbon-14 activity in high-activity tritiated water according to claim 6, characterized in that the top of the first glass bubbler (4) and the top of the second glass bubbler (5) are both provided with gas inlets, and the upper side of the first glass bubbler (4) and the upper side of the second glass bubbler (5) are both provided with gas outlets; the gas outlet of the oxidation reactor (3) is connected with the gas inlet of the first glass bubbler (4) through a connecting hose (9), the gas outlet of the first glass bubbler (4) is connected with the gas inlet of the second glass bubbler (5) through a silicone tube (10), and the gas outlet of the second glass bubbler (5) is connected with a glass absorption bottle (6) through a pipeline.
8. The pretreatment device for analysis of carbon-14 activity in high-activity tritiated water according to claim 7, characterized in that a quick connector (15) is arranged on the connection hose (9) connecting the gas outlet of the oxidation reactor (3) and the gas inlet of the first glass bubbler (4).
9. The apparatus for analysis and pretreatment of carbon-14 activity in high-activity tritiated water according to any one of claims 6-8, characterized in that the acid absorption liquid of the primary acid absorption apparatus and the acid absorption liquid of the primary acid absorption apparatus are both H2SO 4; and the alkali absorption liquid of the alkali absorption device is NaOH.
10. The apparatus for analysis and pretreatment of carbon-14 activity in high-activity tritium water according to claim 9, further comprising a waste liquid absorption apparatus, wherein the waste liquid absorption apparatus is connected with the alkali absorption apparatus through a pipeline.
11. The pretreatment device for analyzing carbon-14 activity in high-activity tritiated water according to claim 10, wherein the waste liquid absorption device is a glass colorimetric tube (7) filled with water.
12. The pretreatment device for analysis of carbon-14 activity in high-activity tritiated water according to claim 11, wherein a gas inlet is arranged at the top of the glass absorption bottle (6), a gas outlet is arranged at the upper side of the glass absorption bottle (6), a gas outlet of the second glass bubbler (5) is connected with a gas inlet pipeline of the glass absorption bottle (6), and a gas outlet of the glass absorption bottle (6) is connected with a glass colorimetric tube (7) through a pipeline.
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| CN202122560456.1U CN217238399U (en) | 2021-10-22 | 2021-10-22 | Pretreatment device for analyzing carbon-14 activity in high-activity tritium water |
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