U.S. patent application number 17/523486 was filed with the patent office on 2022-04-14 for automatic tritium extraction method for environmental monitoring.
The applicant listed for this patent is Zhejiang Hengda Instrumentation Co., Ltd.. Invention is credited to Shibo Liu, Zhidong Pan, Cheng Wu, Lulu Zheng, Naizheng Zhou.
Application Number | 20220111304 17/523486 |
Document ID | / |
Family ID | 1000006106853 |
Filed Date | 2022-04-14 |
United States Patent
Application |
20220111304 |
Kind Code |
A1 |
Pan; Zhidong ; et
al. |
April 14, 2022 |
AUTOMATIC TRITIUM EXTRACTION METHOD FOR ENVIRONMENTAL
MONITORING
Abstract
An automatic tritium extraction method for environmental
monitoring comprises the following steps: 1) cleaning of a
distillation chamber; 2) distillation rising; 3) distillation; 4)
condensation; 5) discharging samples out of the distillation
chamber. By the adoption of the automatic tritium extraction device
and method for environmental monitoring, fully-automatic
distillation and condensation of environmental tritium samples,
automatic cleaning of the distillation chamber, and automatic and
accurate addition of required agents are realized, and
fully-automatic acquisition, preparation, distillation,
purification, measurement and analysis of environmental tritium can
be completed; and manual intervention is reduced, so that
monitoring results are more accurate, and labor costs are
saved.
Inventors: |
Pan; Zhidong; (Hangzhou
City, CN) ; Liu; Shibo; (Hangzhou City, CN) ;
Zhou; Naizheng; (Hangzhou City, CN) ; Wu; Cheng;
(Hangzhou City, CN) ; Zheng; Lulu; (Hangzhou City,
CN) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Zhejiang Hengda Instrumentation Co., Ltd. |
Hangzhou City |
|
CN |
|
|
Family ID: |
1000006106853 |
Appl. No.: |
17/523486 |
Filed: |
November 10, 2021 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
16896689 |
Jun 9, 2020 |
11202972 |
|
|
17523486 |
|
|
|
|
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
B01D 3/42 20130101; B01D
3/146 20130101 |
International
Class: |
B01D 3/42 20060101
B01D003/42; B01D 3/14 20060101 B01D003/14 |
Foreign Application Data
Date |
Code |
Application Number |
Jun 10, 2019 |
CN |
201910496784.4 |
Claims
1. An automatic tritium extraction method for environmental
monitoring, comprising the following steps: 1) cleaning of a
distillation chamber: a cleaning fluid is used, a first pump is
started to pump a specified quantity of the cleaning fluid into the
distillation chamber, a temperature control unit is started to heat
the distillation chamber to a preset temperature, then a third pump
is started to deliver outside air into the distillation chamber,
and when agitation cleaning of the distillation chamber is
completed, mixed liquor in the distillation chamber is discharged
by the third pump; 2) distillation rinsing: a distilling fluid is
used, a second pump is started to pump a specified quantity of
samples into the distillation chamber, then, the first pump is
started to pump a specified quantity of the distilling fluid into
the distillation chamber, and the temperature control unit is
started to maintain the temperature of an outer wall of the
distillation chamber at the preset temperature, and a collection
tank containing finished products is replaced with an empty
collection tank; 3) distillation: the distilling fluid is used, the
second pump further pumps a specified quantity of samples into the
distillation chamber, the first pump is started to pump a specified
quantity of the distilling fluid into the distillation chamber, and
the temperature control unit is started to maintain the
distillation chamber at a preset temperature and is stopped when
the distillation amount reaches a preset value; 4) carrying out
condensation when Step 2) and Step 3) are performed: an auxiliary
condensation unit is started, and a condensing agent is delivered
into a condensing agent circulation chamber via a lower tube and
flows back into a cavity via an upper tube after being subjected to
heat exchange in the condensing agent circulation chamber; 5)
discharging samples out of the distillation chamber: the second
pump further pumps the rest of samples in a sample tank into the
distillation chamber, and the third pump is started to discharge
all the samples out of the distillation chamber.
2. The automatic tritium extraction method for environmental
monitoring according to claim 1, wherein the preset temperature in
Step 1) and Step 2) is 80-100.degree. C., and the preset value in
Step 3) is 500-700 mL.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a Divisional of co-pending application
Ser. No. 16/896,689, filed on Jun. 9, 2020, for which priority is
claimed under 35 U.S.C. .sctn. 120; and this application claims
priority of Application No. 201910496784.4 filed in China on Jun.
10, 2019 under 35 U.S.C. .sctn. 119; the entire contents of all of
which are hereby incorporated by reference.
BACKGROUND OF THE INVENTION
1. Technical Field
[0002] The invention belongs to the technical fields of
environmental protection and automatic equipment, in particular to
an automatic tritium extraction device and method for environmental
monitoring.
2. Description of Related Art
[0003] Tritium is a radioactive substance with a half-life period
of 12.6 years. Most tritium in the air will eventually turn into
tritium oxide-water steam which, together with ordinary water, is
involved in water circulation, and thus, human beings are likely to
be exposed to tritium radiation. During environmental protection,
monitoring of the content of tritium in water and air has received
extensive international attention. Of all existing tritium
monitoring methods, indirect measurement methods are obviously
superior to other methods and are implemented on the basis of the
following principle: air tritium oxide samples are prepared through
an air condensation method and are taken back to the laboratory,
then tritium sample purification is carried out through a manual
distillation and condensation method, after that, the tritium oxide
samples and a scintillation solution are quantitatively injected
into sample bottles in a certain proportion, and finally, the
sample bottles are placed into an instrument one by one for
analysis. Existing distillation and concentration methods typically
include semi-automatic distillation and manual distillation,
wherein semi-automatic distillation can fulfill automatic
distillation of single samples, and cleaning is performed manually
after distillation; and traditionally, manual distillation is
carried out in the laboratory, and all operations are performed
manually. Both distillation methods have the following drawbacks:
1, sample preparation personnel may be exposed to radiation when
the concentration of tritium samples is high; 2, experimenters
should be highly skilled to complete quantitative sample
preparation, personal operation errors may be caused, the
experimental operation time is long, and manual attendance is
required; and 4, the cleaning process needs to be manually
completed, so that full automation of the process is not available,
and online monitoring of air tritium cannot be realized either.
BRIEF SUMMARY OF THE INVENTION
[0004] The technical issue to be settled by the invention is to
overcome the defects of the prior art by providing an automatic
tritium extraction device and method for environmental monitoring
to fulfill automatic distillation of tritium samples and automatic
cleaning of distillation chambers and to save labor costs.
[0005] The technical solution adopted by the invention to settle
the aforesaid technical issue is as follows: an automatic tritium
extraction device for environmental monitoring comprises a
distillation chamber, a temperature control unit used to heat the
distillation chamber, a condensation unit connected to the
distillation chamber through a delivery pipe, and an auxiliary
condensation unit used to cyclically deliver a condensing agent
into the condensation unit, wherein the distillation chamber is
connected to a first pump for delivering agents into the
distillation chamber, a second pump for delivering samples into the
distillation chamber, and a third pump for communicating the
distillation chamber with the outside; and the delivery pipe
comprises a first vertical pipe connected to the top of the
distillation chamber, a second vertical pipe connected to the top
of the condensation unit, and an oblique pipe obliquely connected
between the first pipe and the second pipe, and the oblique pipe
inclines upwards from the distillation chamber to the condensation
unit.
[0006] Furthermore, a first spherical bulge with a larger inner
diameter is disposed on the first vertical pipe, and a second
spherical bulge with a large inner diameter is disposed on the
second vertical pipe.
[0007] Furthermore, the first pump is connected to an upper part of
the distillation chamber, the second pump is also connected to the
upper part of the distillation chamber, and the third pump is
connected to the bottom of the distillation chamber and is used to
deliver air into the distillation chamber or discharge samples in
the distillation chamber to the outside.
[0008] Furthermore, a main part of the distillation chamber is
cylindrical, the bottom of the distillation chamber is conical, and
the temperature control unit comprises heating elements encircling
the outer wall of the main part of the distillation chamber and a
temperature control switch disposed between the heating elements
and the outer wall of the distillation chamber.
[0009] Furthermore, the agents include a cleaning agent and a
distilling agent.
[0010] Furthermore, the condensation unit comprises a condensing
agent circulation chamber and a spiral heat-exchange tube disposed
in the condensing agent circulation chamber, and the condensing
agent circulation chamber comprises an inlet connected to the
second vertical pipe and an outlet connected to a collection
tank.
[0011] Furthermore, the second pump is connected to a sample tank
for containing the samples.
[0012] Furthermore, the auxiliary condensation unit comprises a
cavity for storing the condensing agent, a power device for
cyclically delivering the condensing agent into the condensing
agent circulation chamber, an upper tube connected to an upper part
of the condensing agent circulation chamber, and a lower tube
connected to a lower part of the condensing agent circulation
chamber.
[0013] The invention further discloses an automatic tritium
extraction method for environmental monitoring, which comprises the
following steps:
[0014] 1) Cleaning of a distillation chamber: a cleaning agent is
used, a first pump is started to pump a specified quantity of the
cleaning agent into the distillation chamber, a temperature control
unit is started to heat the distillation chamber to a preset
temperature, then a third pump is started to deliver outside air
into the distillation chamber, and when agitation cleaning of the
distillation chamber is completed, mixed liquor in the distillation
chamber is discharged by the third pump;
[0015] 2) Distillation rinsing: a distilling agent is used, a
second pump is started to pump a specified quantity of samples into
the distillation chamber, then, the first pump is started to pump a
specified quantity of the distilling agent into the distillation
chamber, and the temperature control unit is started to maintain
the temperature of the outer wall of the distillation chamber at
the preset temperature, and a collection tank containing finished
products is replaced with an empty collection tank;
[0016] 3) Distillation: the distilling agent is used, the second
pump further pumps a specified quantity of samples into the
distillation chamber, the first pump is started to pump a specified
quantity of the distilling agent into the distillation chamber, and
the temperature control unit is started to maintain the
distillation chamber at a preset temperature and is stopped when
the distillation amount reaches a preset value;
[0017] 4) Carrying out condensation when Step 2) and Step 3) are
performed: an auxiliary condensation unit is started, and a
condensing agent is delivered into a condensing agent circulation
chamber via a lower tube and flows back into a cavity via an upper
tube after being subjected to heat exchange in the condensing agent
circulation chamber;
[0018] 5) Discharging samples out of the distillation chamber: the
second pump further pumps the rest of samples in a sample tank into
the distillation chamber, and the third pump is started to
discharge all the samples out of the distillation chamber.
[0019] Preferably, the preset temperature in Step 1) and Step 2) is
80-100.degree. C., and the preset value in Step 3) is 500-700
mL.
[0020] The invention has the following beneficial effects:
fully-automatic distillation and condensation of environmental
tritium samples, automatic cleaning of the distillation chamber,
and automatic and accurate addition of required agents are
realized. The automatic tritium extraction device fills the blank
of fully-automatic distillation and purification of environmental
tritium analysis and can complete fully-automatic acquisition,
preparation, distillation, purification, measurement and analysis
of environmental tritium together with a tritium analysis meter, so
that an environmental tritium analysis system is free of attendance
in the entire process, and fully-automatic monitoring of regions
with severe environmental tritium radiation is realized; and the
automatic tritium extraction device greatly reduces manual
intervention, so that monitoring results are more accurate, labor
costs are saved, and the probability of physical harm to relevant
service personnel is drastically lowered.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0021] FIG. 1 is a flow structural diagram of the invention.
[0022] FIG. 2 is a collaboration diagram of a temperature control
unit and a distillation chamber of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0023] To provide a better understanding of the technical solutions
of the invention for those skilled in the art, the technical
solutions of the embodiments of the invention will be clearly and
completely described below in conjunction with the accompanying
drawings of the embodiments. Obviously, the embodiments in the
following description are merely illustrative ones, and are not all
possible ones of the invention. All other embodiments obtained by
those ordinarily skilled in the art without creative labor should
also fall within the protection scope of the invention.
[0024] As shown in FIG. 1, 2, an automatic tritium extraction
device for environmental monitoring comprises a distillation
chamber 1, a temperature control unit 2, a condensation unit 4 and
an auxiliary condensation unit 5, wherein a main part of the
distillation chamber 1 is cylindrical, and the bottom of the
distillation chamber 1 is conical; the temperature control unit 2
encircles one part of the outer wall of the main part of the
distillation chamber 1 and is used to heat the distillation chamber
1; one end of the condensation unit 4 is connected to the top of
the distillation chamber 1, and the other end of the condensation
unit 4 is connected to a delivery pipe 3 at the top of the
condensation unit 4; and the auxiliary condensation unit 5 is
connected to the condensation unit 4 and is used to cyclically
deliver a condensing agent into the condensation unit 4.
[0025] An upper part of the distillation chamber 1 is connected to
multiple agent bottles through multiple pipes and a first pump 11,
wherein cleaning agents or distilling agents are contained in the
multiple bottles 15, and the first pump 11 may be a WK10
high-precision micro peristaltic pump capable of accurately
regulating and controlling the delivery quantity. The upper part of
the distillation chamber 1 is also connected to a sample tank 7
containing to-be-tested tritium-containing samples through a pipe
and a second pump 12, wherein the second pump 12 is used to
transport the tritium-containing samples into the distillation
chamber 1. A sample outlet 14 is formed in the conical bottom of
the distillation chamber 1 and is communicated with the outside
through a third pump 13 to discharge the samples in the
distillation chamber 1 to the outside.
[0026] As shown in FIG. 2, the temperature control unit 2 comprises
heating elements 21 encircling the outer wall of the main part of
the distillation chamber 1 and a temperature control switch 22
disposed between the heating elements 21 and the outer wall of the
distillation chamber 1, wherein the heating elements 21 generate
heat for distillation in the distillation chamber 1; and the
temperature control switch 22 is used to sense the temperature of
the outer wall surface of the distillation chamber 1 in real time,
timely and automatically power on the heating elements 21 to heat
the distillation chamber 1 when the temperature of the outer wall
surface of the distillation chamber 1 is lower than a preset value
80-100.degree. C., and timely and automatically power off the
heating elements 21, when the temperature of the outer wall surface
of the distillation chamber 1 is higher than the preset value
80-100.degree. C., to maintain the temperature of the distillation
chamber 1 at the preset value to ensure continuous and efficient
distillation.
[0027] The condensation unit 4 comprises a hollow condensing agent
circulation chamber 41 and a spiral heat-exchange tube 42 disposed
in the condensing agent circulation chamber 41, wherein the spiral
heat-exchange tube 42 allows tritium sample steam to circulate
therein, the condensing agent circulation chamber 41 is filled with
the condensing agent which may be deionized distilled water, the
tritium sample steam in the spiral heat-exchange tube 42 is cooled
and condensed into liquid by the condensing agent, an inlet 411
communicated with the delivery pipe 3 is formed in the top of the
condensing agent circulation chamber 41, an outlet 412 communicated
with an environmental tritium sample collection tank 6 may be
formed in the bottom of the condensing agent circulation chamber
41, and an airtight container is formed by other parts of the
condensing agent circulation chamber 41 to allow the condensing
agent to circulate therein.
[0028] The auxiliary condensation unit 5 is used to control the
condensing process of the condensation unit 4 and comprises a
cavity 51 for storing the condensing agent, an upper tube 52 for
communicating the cavity 51 with an upper part of the condensing
agent circulation chamber 41, a lower tube 53 for communicating the
cavity 51 with a lower part of the condensing agent circulation
chamber 41, and a power device for driving the condensing agent to
flow into the condensing agent circulation chamber 41 from the
cavity 51 through the lower tube 53 or driving the condensing agent
to flow into the cavity 51 from the condensing agent circulation
chamber 41 through the upper tube 52, wherein the power device is a
peristaltic pump or a diaphragm pump and is used to drive the
condensing agent to cyclically flow between the condensing agent
circulation chamber 41 and the cavity 51.
[0029] The delivery pipe 3 for guiding distillation gas generated
in the distillation chamber 1 into the condensation unit 4
comprises a first vertical pipe 31 connected to the top of the
distillation chamber 1, a second vertical pipe 32 connected to the
top of the condensing agent circulation chamber 41, and an oblique
pipe 33 obliquely connected between the first vertical pipe 31 and
the second vertical pipe 32, wherein the top of the distillation
chamber 1 is located on the same horizontal plane as the top of the
condensing agent circulation chamber 41, and the oblique pipe 33
inclines upwards from the distillation chamber 1 to the
condensation unit 4, that is, the second vertical pipe 32 is longer
than the first vertical pipe 31.
[0030] A first spherical bulge 311 with a larger inner diameter is
formed in the first vertical pipe 31, is close to the top of the
distillation chamber 1 and is spaced from the top of the top of the
distillation chamber 1 by a small distance, so that steam output
from the top of the distillation chamber 1 passes through the first
vertical pipe 31 with the inner diameter sharply decreased to form
a micro positive pressure and then enters the first spherical bulge
311 with the larger inner diameter to form a micro negative
pressure, in this way, sample drops carried by steam are prevented
from entering the condensation unit 4 via the delivery pipe 3, and
the monitoring accuracy of the environmental tritium samples is
guaranteed.
[0031] A second spherical bulge 321 with a larger inner diameter is
formed in the second vertical pipe 32, is close to the top of the
condensing agent circulation chamber 41 and is spaced from the top
of the condensing agent circulation chamber 41 by a small distance,
so that steam entering the condensing agent circulation chamber 41
first passes through the second spherical bulge 321 with the inner
diameter sharply increased to be pre-condensed and then enters the
condensing agent circulation chamber 41 via the second vertical
pipe 32 with a smaller inner diameter, thus improving the
condensation efficiency.
[0032] After the automatic tritium extraction device is started,
the distillation chamber 1 is automatically cleaned at first, then,
the environmental tritium samples and the distilling agent enter
the distillation chamber, the temperature control unit 2 is started
to carry out controllable distillation, and steam enters the steam
delivery pipe 3, wherein one part of the steam is condensed to flow
back into the distillation chamber 1 to be re-distillated under the
effect of the structure of the first spherical bulge 311 at a port
of the first vertical pipe 31 and the oblique upward structure of
the oblique pipe 33, and the other part of the steam enters the
condensation unit 4 via the steam delivery pipe 3 and is mostly
condensed in the spiral heat-exchange tube 42 in the condensing
agent circulation chamber 41 under the effect of the structure and
temperature to flow into the environmental tritium sample
collection tank 6 under the effect of gravity; and the steam and
the condensing agent exchange heat in the spiral heat-exchange tube
42, so that the temperature of the steam drops, the temperature of
the condensing agent rises, the condensing agent with the
temperature increased returns into the cavity 51 via the upper tube
52, and the low-temperature condensing agent in the cavity 51
enters the condensing agent circulation chamber 41 via the lower
tube 53, and thus, the condensing capacity of the condensation unit
4 is guaranteed.
[0033] An automatic tritium extraction method for environmental
monitoring comprises the following steps:
[0034] 1) Cleaning of a distillation chamber: a cleaning agent is
used, a first pump is started to pump the cleaning agent into the
distillation chamber, and the quantity of the cleaning agent pumped
into the distillation chamber is accurately controlled; the
temperature control unit is started to increase the temperature of
the outer wall surface of the distillation chamber 1 to
80-100.degree. C.; a third pump is started to deliver outside air
into the distillation chamber 1 to agitate the cleaning agent to
clean the distillation chamber 1, and at this moment, a second pump
and a condensation unit are stopped; and when agitation cleaning of
the distillation chamber is completed a period of time later, the
third pump is started again to discharge mixed liquor in the
distillation chamber 1 out of the distillation chamber 1 via a
sample outlet 14;
[0035] 2) Distillation rinsing: the cleaning agent is replaced with
a distilling agent, the second pump is started to pump a specified
quantity of samples, namely one third of samples in a sample tank
7, into the distillation chamber 1; then, the first pump is started
to pump a specified quantity of the distilling agent, in proportion
with the one third of the samples, into the distillation chamber 1
from different bottles; the samples and the distilling agent are
mixed; and the temperature control unit is kept in the on-state to
maintain the temperature of the outer wall surface of the
distillation chamber 1 at 80-100.degree. C.;
[0036] 3) Distillation: a collection tank containing environmental
tritium finished products in step 2) is replaced with an empty
collection tank, and the second pump further pumps one third of
samples into the distillation chamber 1 from the sample tank 7; the
first pump is started to pump a specified quantity of the
distilling agent, in proportion with the one third of samples, into
the distillation chamber 1 from different bottles; and temperature
control unit is kept in the on-state to maintain the temperature of
the outer wall surface of the distillation chamber 1 at
80-100.degree. C. and is stopped when the distillation amount
reaches a preset value 500-700 mL;
[0037] 4) Carrying out condensation when Step 2) and Step 3) are
performed: an auxiliary condensation unit is started, a power
device delivers a condensing agent into a condensing agent
circulation chamber 41 from a cavity via a lower tube 53 and
recovers the condensing agent subjected to heat exchange in the
condensing agent circulation chamber 41 back into the cavity 51 via
an upper tube in the direction of arrow;
[0038] 5) Discharging samples out of the distillation chamber: the
second pump further pumps the last one third of samples into the
distillation chamber 1 from the sample tank 7; and the first pump
is stopped, and the third pump is started to discharge all the
samples 1 in the distillation chamber 1 out of the distillation
chamber 1 via the sample outlet 14; and
[0039] 6) Monitoring: liquid environmental tritium finished
products in the collection tank 6 are measured and analyzed by a
tritium analysis meter.
[0040] The above specific embodiments are merely used to explain
the invention, and are not intended to limit the invention. Any
modifications or transformations of the invention made on the basis
of the spirit of the invention and within the protection scope of
the claims should also fall within the protection scope of the
invention.
* * * * *