CN106932228B - Natural hex liquid phase sampling system and method - Google Patents
Natural hex liquid phase sampling system and method Download PDFInfo
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- CN106932228B CN106932228B CN201511025969.5A CN201511025969A CN106932228B CN 106932228 B CN106932228 B CN 106932228B CN 201511025969 A CN201511025969 A CN 201511025969A CN 106932228 B CN106932228 B CN 106932228B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1062—Sampling under constant temperature, pressure, or the like
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
- G01N2001/1418—Depression, aspiration
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Abstract
The invention belongs to natural hex liquid phase sampling technique fields, and in particular to a kind of natural hex liquid phase sampling system and method.First-stage condenser liquid-phase outlet connects sampler A and sampler B, the identical mutual backup of the two connection relationship；Sampler A connection relationship are as follows: first-stage condenser is connected with liquid phase general pipeline, pressure gauge is provided on liquid phase general pipeline, sampling pipe connects liquid phase general pipeline and 740L vessel inlet valve J-07, sampling pipe is equipped with valve J-01, J-02, J-03, J-04, J-05, J-06, and the pipeline between valve J-02 and J-03, J-03 and J-04, J-04 and J-05 is quantity tube；Quantity tube center between valve J-02 and J-03 is connected by angle valve J-08 with 2S sampling bottle A1 imported valve S1, and the quantity tube center between valve J-03 and J-04 is connected by angle valve J-09 with 2S sampling bottle A2 imported valve S2.The present invention in hex production process to after homogenize process product quantitative sampling, analyze determine hex product quality whether qualification provides condition.
Description
Technical field
The invention belongs to natural hex liquid phase sampling technique fields, and in particular to a kind of natural hex liquid phase takes
Sample system and method.
Background technique
It is whether qualified for confirmation product quality in natural hex production process, product must be sampled, analysis.It takes
During sample, the quantitative collection of liquid hex is an important technology.Currently, the U.S. is to the sampling of natural hex
It quantitatively shifts to realize by liquid phase hex, specifically: after natural hex product liquefaction and perfectly homogenousization,
Carrying out pressurising test to sampling system, (test gas is dry inert gas, and test pressure is greater than or equal to the work of hex
Make pressure) and confirm air-tightness qualification, then to sampling system vacuum pumping negative pressure to 3.4 × 103Pa or less.Open sampling
Valve allows liquid hex to flow into and is full of the sampling pipe of fixed volume, is then shut off sampling pipe front and back end valve and cuts
Disconnected hex continues to flow into, and finally opens sampling container valve, the hex of fixed volume is allowed to enter sampling container.Later
Sampling container is immersed into cooling in liquid nitrogen, until the pressure in sampling container is down to 6.89 × 103Pa (5.2cmHg) is hereinafter, close
Close sampling container valve.In entire sampling process, guarantee that (including sampling is held for natural hex product and entire sampling system
Device, pipeline, valve) temperature be kept at (93~113) DEG C.Currently, domestic hex preparation manufacturer passes through foreign
Advanced experience establishes a set of safe and efficient liquid hex quantitative sampling system in conjunction with itself many years knowhow,
And natural hex liquid phase sampling technique is skillfully grasped.
Summary of the invention
The purpose of the present invention is to provide a kind of natural hex liquid phase sampling system and methods, produce for hex
The whether qualified offer condition of hex product quality is determined to the product quantitative sampling after homogenize process, analysis in the process.
In order to achieve the above objectives, the technical solution used in the present invention are as follows:
A kind of natural hex liquid phase sampling system, first-stage condenser liquid-phase outlet connect sampler A and sampling dress
Set B, the identical mutual backup of the two connection relationship；Sampler A connection relationship are as follows: first-stage condenser is connected with liquid phase general pipeline, liquid
Pressure gauge is provided on Xiang general pipeline, sampling pipe connects liquid phase general pipeline and 740L vessel inlet valve J-07, sets on sampling pipe
There are valve J-01, J-02, J-03, J-04, J-05, J-06, between valve J-02 and J-03, J-03 and J-04, J-04 and J-05
Pipeline be quantity tube；Quantity tube center between valve J-02 and J-03 passes through angle valve J-08 and the A1 import of 2S sampling bottle
Valve S1 is connected, and the quantity tube center between valve J-03 and J-04 passes through angle valve J-09 and 2S sampling bottle A2 imported valve
S2 is connected, and the quantity tube center between valve J-04 and J-05 passes through angle valve J-10 and 2S sampling bottle A3 imported valve S3 phase
Even, originally water cooling tank is equipped with below 2S sampling bottle；740L container is placed in inside water bath, is equipped with electronics thereunder
Scale, pipeline transfers from one department to another system and nitrogen system by valve J-11 and external gas between valve J-06 and 740L vessel inlet valve J-07
It is connected, is equipped with pressure gauge on pipeline between valve J-05 and valve J-06.
A kind of natural hex liquid phase sampling method based on natural hex liquid phase sampling system, including walk as follows
It is rapid: to heat up and liquefy to the hex in first-stage condenser, hex is made sufficiently to liquefy and homogenize；Natural hex
Liquid phase sampling is installed 2S sampling bottle and electrical heat tracing box and is heated to its power transmission, checks 740L container and sampling pipe pressure,
Ensure that pressure is -200~-700Pa, the negative pressure of 740L container is transfered from one department to another system by gas by the first-stage condenser with negative pressure and held to 740L
Device carries out evacuation realization, slowly open J-01~J-07 valve, using between first-stage condenser and 740L container pressure difference and
Difference in height enters the hex of liquid in 740L container by liquid phase general pipeline, sampling pipe；When 740L container electronic scale is aobvious
When showing 30~100kg of weight gain, J-05, J-04, J-03, J-02 valve are successively closed, the hex sample of liquid is concentrated to
In three sections of quantity tubes；J-08, J-09, J-10 valve and 2S sampling bottle S1, S2, S3 valve are opened, using pressure difference by quantity tube
In liquid hex acquire into 2S sampling bottle；2S sampling bottle cooling trough is installed, by tap water circulating cooling, by 2S
Liquid hex sample in sampling bottle is condensed into solid-state；After 2S sampling bottle is completely cooling, closing 2S sampling bottle S1, S2,
It is cooling to stop tap water for S3 valve；The evacuation of remaining hex in sampling system, sampling, which finishes, opens J-03, J-04, J-05
Valve, with 740L container by quantity tube and sampling connecting tube in remaining hex evacuate, after evacuation close J-08, J-09,
J-10 valve keeps tiny structure in system, dismantles electrical heat tracing box and 2S sampling bottle, and samples weighing is sent to analysis room and carries out sample
Product analysis；During 740L container production, when accumulative reception reaches specified amount or system shutdown, hot water is led to 740L container water bath and is added
Heat opens J-07, J-11 or J-18, J-22 valve, transfers from one department to another hex, by 740L gas tube road, through gas with gaseous form
System enters in production system, and after gas turns, 740L container Temperature fall is for future use.
During heating liquefaction, temperature is controlled in 55 DEG C of 3~4h of constant temperature, 95 are risen to later with 10~20 DEG C/h gradient~
100 DEG C, constant temperature 15h or more.
The liquid phase sampling of natural hex, checks liquid pipe, sampling system valve state and pipe temperature before sampling,
And positive pressure of nitrogen is carried out to it and is leaked hunting.
It is obtained by the present invention to have the beneficial effect that
The present invention relates in the quantitative collection of natural hex liquid phase sample, sample bottle liquid hex it is cold
The technologies such as solidifying, remaining hex in system pipeline collection and the transfer of 740L container hex gas phase.The present invention passes through certainly
The sampling system of system is realized using the liquid phase sampling technique that long-felt determines to the hex product of homogenize process
Quantitative sampling, to be analyzed to identify hex product quality, whether qualification provides condition.The technical method includes device structure
It is simple and convenient to operate that quick, control condition is easily achieved, sampling amount can quantify to determine, safety coefficient is higher, and considers simultaneously
After sampling in pipeline the advantages that the processing of residual material.Specific advantage is as described below:
(1) system structure is simple.The sampling system mainly includes liquid phase general pipeline, probe tube, 2S sampling bottle, tap water cooling
Slot, 740L container, electronic scale, pressure gauge and heat-preserving equipment etc..
(2) easy to operate.After the completion of hex product liquefies and homogenizes, by controlling a small amount of relevant control
Unlatching/closed state of valve, under negative pressure state, liquid hex is transferred in sampling bottle in liquid form, later
2S sampling bottle and hex product are cooled down using tap water circulating cooling mode, make hex sample with solid
Form is offline.
(3) control condition is easily achieved.The temperature and pressure of sampling system is mainly controlled in this process.Pressure needs to maintain
In negative pressure state, by the way that the cooling of 740L container can be realized；Temperature maintains as (90~120) DEG C, passes through electric heating and steaming
Vapour adjoining pipe form can be realized.
(4) sampling amount can quantify to determine.Quantity tube is provided in the system, according to determining operating process, by opening
Opening/close a small amount of related valve can be realized the quantitative sampling of liquid phase hex, to meet in analytic process to sample size
It is required that.
(5) safety coefficient is higher.By the sampling operation, hex product sample is finally in solid form from this system
Offline, safety coefficient is higher.
(6) consider the processing of residual material in pipeline after sampling.After sampling, band associated with this system can be passed through
The condensing trapping system or 740L negative pressure system of negative pressure will remain hex and carry out safe transfer in pipeline, and straight as product
Receive collection.
Detailed description of the invention
Fig. 1 is natural hex liquid phase sampling system structure chart of the present invention；
In figure: A1~A3, B1~B3 are 2S sampling bottle；740L/1~2 are 740L container；J-01~J-21 valve is liquefaction
Shut-off valve；S1~S6 valve is 2S sampling bottle container valve；Liquid phase general pipeline connection first-stage condenser liquid-phase outlet valve and sampling
Pipeline；Sampling pipe connects liquid phase general pipeline and 740L container；In sampling pipe, J-02~J-03, J-03~J-04, J-04~
Connecting tube between J-05, J-13~J-14, J-14~J-15, J-15~J-16 valve is quantity tube；2S sampling bottle passes through J-
08~J-10, J-19~J-21 valve and short tube are connected on quantity tube；Pressure gauge is equipped on liquid phase general pipeline and sampling pipe.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
UF6 relative molecular weight is 352, and under normal temperature and pressure, UF6 is white crystal, orthorhombic crystalline structure.In 101.325kPa
Under, the sublimation point of UF6 is 56.4 DEG C, and three phase point is 64.02 DEG C.It reads up the literature it is found that in three phase point in 160 DEG C, the density of UF6
Rise with viscosity with temperature and reduce, UF6 feed liquid flows smooth in pipeline when in order to sample, and in conjunction with knowhow, selection is taken
UF6 thermostat temperature is (93 ± 3) DEG C when sample, at this point, hex vapour pressure is about 0.32MPa (gauge pressure).To natural lithium
During uranium product quality testing by the way of liquid phase sampling, specifically: setting two sets of sampling systems of A, B, every set can be simultaneously
Take 3 Duplicate Samples, sampling system by liquid phase general pipeline, sampling pipe, 2S sampling bottle, originally water cooling tank, 740L container etc. are constituted,
The tail end of sampling pipe is arranged in 740L container, and every set system is arranged 1, and bottom is equipped with electronic scale.It is produced using 740L container
After raw negative pressure (- 200~-700) Pa evacuates sampling system, leaks hunting, the inlet valve of 2S sampling bottle is closed, is opened
First-stage condenser liquid-phase outlet valve makes abundant liquid using the pressure difference and difference in height between first-stage condenser and 740L container
Change and the liquid hex product homogenized is entered in 740L container by sampling pipe.When 740L container bottom electronic scale is aobvious
When indicating value weight gain (30~100) kg, valve before and after once closing quantitative pipeline from sampling pipe tail end is closed, hex is cut off
It continues to flow into, makes the hex for being full of liquid in quantity tube.The inlet valve for opening 2S sampling bottle, utilizes 2S sampling bottle itself
The negative pressure having acquires the liquid hex in quantitative pipeline into 2S sampling bottle.It is sampled using tap water circulating cooling 2S
Bottle, makes the hex in 2S sampling bottle be condensed into solid-state.Remaining hex can be directly straight with 740L container in sampling pipe
Tap into capable evacuation, or by 740L gas tube road, using the condensing trapping system with negative pressure associated with sampling system into
Row evacuates.In entire sampling process, using heat preservation and electric heating system, (2S samples bottle valve and uses electric heating, remaining pipes
And valve is heated using steam adjoining pipe) guarantee that the temperature of entire sampling system is kept at (90~120) DEG C, to ensure probe tube
The temperature of hex maintains (93 ± 3) DEG C in road.
As shown in Figure 1, natural hex liquid phase sampling system structure of the present invention is as follows:
First-stage condenser liquid-phase outlet connects sampler A and sampler B, and the two connection relationship is identical, mutual backup.
Below by taking sampler A as an example, its connection relationship is described:
First-stage condenser is connected with liquid phase general pipeline, and pressure gauge is arranged on liquid phase general pipeline.Sampling pipe connect liquid phase general pipeline with
740L vessel inlet valve J-07, sampling pipe are equipped with valve J-01, J-02, J-03, J-04, J-05, J-06, valve J-02
Pipeline between J-03, J-03 and J-04, J-04 and J-05 is quantity tube.Quantitative tube hub between valve J-02 and J-03
Position is connected by angle valve J-08 with 2S sampling bottle A1 imported valve S1, the quantity tube center between valve J-03 and J-04
It is connected by angle valve J-09 with 2S sampling bottle A2 imported valve S2, the quantity tube center between valve J-04 and J-05 passes through
Angle valve J-10 is connected with 2S sampling bottle A3 imported valve S3, is equipped with originally water cooling tank below 2S sampling bottle.740L container is put
It is placed in inside water bath, is equipped with electronic scale thereunder, pipeline passes through between valve J-06 and 740L vessel inlet valve J-07
Valve J-11 transfers from one department to another system with gas and nitrogen system is connected, and is equipped with pressure gauge on pipeline between valve J-05 and valve J-06.
Natural hex liquid phase sampling method based on above system is as follows:
Step 1: hex liquid phase sampler is established.The device by liquid phase general pipeline, sampling pipe, 2S sampling bottle,
The most of composition of 740L container, pressure gauge and heat-preserving equipment etc. five.
Step 2: the constant temperature of natural hex product liquefies and homogenizes.To the hex liter in first-stage condenser
Temperature liquefaction.During heating liquefaction, temperature is controlled in 55 DEG C of constant temperature (3~4) h, rises to (95 later with (10~20) DEG C/h gradient
~100) DEG C, constant temperature 15h or more makes hex product sufficiently liquefy and homogenize.
Step 3: the liquid phase sampling of natural hex (by taking sampler A operation as an example).
(1) liquid pipe, sampling system valve state and pipe temperature are checked before sampling, and it is carried out positive pressure of nitrogen into
Row leaks hunting.
(2) 2S sampling bottle and electrical heat tracing box are installed and its power transmission is heated.
(3) 740L container and sampling pipe pressure are checked, it is ensured that pressure is the negative pressure of (- 200~-700) Pa, 740L container
System can be transfered from one department to another by gas by the first-stage condenser with negative pressure and evacuation realization is carried out to 740L container.
(4) J-01~J-07 valve is slowly opened, the pressure difference and height between first-stage condenser and 740L container are utilized
Difference enters the hex of liquid in 740L/1 container by liquid phase general pipeline, sampling pipe.
(5) when 740L/1 container electronic scale shows weight gain (30~100) kg, J-05, J-04, J-03, J- are successively closed
The hex sample of liquid is concentrated in three sections of quantity tubes by 02 valve.
(6) J-08, J-09, J-10 valve and 2S sampling bottle S1, S2, S3 valve are opened, pressure difference (empty 2S sampling bottle is utilized
Per se with negative pressure) the liquid hex in quantity tube is acquired into 2S sampling bottle.
(7) 2S sampling bottle cooling trough is installed, by tap water circulating cooling, by the liquid hex in 2S sampling bottle
Sample is condensed into solid-state.
(8) after 2S sampling bottle is completely cooling, 2S sampling bottle S1, S2, S3 valve is closed, it is cooling to stop tap water.
Step 4: the evacuation of remaining hex in sampling system
Sampling finishes, and opens J-03, J-04, J-05 valve, will be in quantity tube and sampling connecting tube with 740L/1 container
Remaining hex evacuates.After evacuation, J-08, J-09, J-10 valve are closed, tiny structure is kept in system, disassembly electric heating is protected
Warm box and 2S sampling bottle, samples weighing are sent to analysis room's progress sample analysis.
Step 5: the gas of hex turns in 740L container
During 740L container production, when accumulative reception reaches specified amount or system shutdown, hot water is led to 740L container water bath
J-07, J-11 (or J-18, J-22) valve is opened in heating, makes hex with gaseous form by 740L gas tube road, through gas
Transfer from one department to another system to enter in production system.After gas turns, 740L container Temperature fall is for future use.
Claims (4)
1. a kind of natural hex liquid phase sampling system, it is characterised in that: first-stage condenser liquid-phase outlet connects sampler A
With sampler B, the identical mutual backup of the two connection relationship；Sampler A connection relationship are as follows: first-stage condenser and liquid phase general pipeline
It is connected, pressure gauge is provided on liquid phase general pipeline, sampling pipe connects liquid phase general pipeline and 740L vessel inlet valve J-07, probe tube
Road is equipped with valve J-01, J-02, J-03, J-04, J-05, J-06, valve J-02 and J-03, J-03 and J-04, J-04 and J-
Pipeline between 05 is quantity tube；Quantity tube center between valve J-02 and J-03 passes through angle valve J-08 and 2S sampling bottle
A1 imported valve S1 is connected, quantity tube center between valve J-03 and J-04 by angle valve J-09 and 2S sampling bottle A2 into
Mouth valve S2 is connected, and the quantity tube center between valve J-04 and J-05 passes through angle valve J-10 and 2S sampling bottle A3 inlet valve
Door S3 is connected, and is equipped with originally water cooling tank below 2S sampling bottle；740L container is placed in inside water bath, is equipped with thereunder
Electronic scale, pipeline transfers from one department to another system and nitrogen by valve J-11 and external gas between valve J-06 and 740L vessel inlet valve J-07
System is connected, and is equipped with pressure gauge on pipeline between valve J-05 and valve J-06.
2. a kind of natural hex liquid phase sampling side based on natural hex liquid phase sampling system as described in claim 1
Method, characterized by the following steps: heat up and liquefy to the hex in first-stage condenser, make the abundant liquid of hex
Change and homogenizes；The liquid phase sampling of natural hex is installed 2S sampling bottle and electrical heat tracing box and is heated to its power transmission, inspection
Look into 740L container and sampling pipe pressure, it is ensured that pressure is -200~-700Pa, and the negative pressure of 740L container is by the level-one with negative pressure
Condenser transfers from one department to another system by gas and carries out evacuation realization to 740L container, slowly opens J-01~J-07 valve, is condensed using level-one
Pressure difference and difference in height between device and 740L container enter the hex of liquid by liquid phase general pipeline, sampling pipe
In 740L container；When 740L container electronic scale shows 30~100kg of weight gain, J-05, J-04, J-03, J-02 valve are successively closed
Door, the hex sample of liquid is concentrated in three sections of quantity tubes；Open J-08, J-09, J-10 valve and 2S sampling bottle
S1, S2, S3 valve are acquired the liquid hex in quantity tube into 2S sampling bottle using pressure difference；It is cold that 2S sampling bottle is installed
Liquid hex sample in 2S sampling bottle is condensed into solid-state by tap water circulating cooling by but sink；To 2S sampling bottle
Completely after cooling, 2S sampling bottle S1, S2, S3 valve is closed, it is cooling to stop tap water；The pumping of remaining hex in sampling system
Sky, sampling finish open J-03, J-04, J-05 valve, with 740L container by quantity tube and sampling connecting tube in remaining hexafluoro
Change uranium to evacuate, J-08, J-09, J-10 valve are closed after evacuation, tiny structure is kept in system, dismantles electrical heat tracing box and 2S takes
Sample bottle, samples weighing are sent to analysis room and carry out sample analysis；During 740L container production, accumulative receive is stopped up to specified amount or system
Che Shi leads to hot water heating to 740L container water bath, opens J-07, J-11 valve, pass through hex with gaseous form
740L gas tube road transfers from one department to another system through gas and enters in production system, and after gas turns, 740L container Temperature fall is for future use.
3. natural hex liquid phase sampling method according to claim 2, it is characterised in that: during heating liquefaction,
Temperature is controlled in 55 DEG C of 3~4h of constant temperature, rises to 95~100 DEG C later with 10~20 DEG C/h gradient, constant temperature 15h or more.
4. natural hex liquid phase sampling method according to claim 2, it is characterised in that: the liquid of natural hex
It mutually samples, checks liquid pipe, sampling system valve state and pipe temperature before sampling, and positive pressure of nitrogen is carried out to it and is surveyed
Leakage.
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| CN109424853A (en) * | 2017-09-04 | 2019-03-05 | 中核陕西铀浓缩有限公司 | A kind of packing of uranium enrichment product gaseous state and gaseous state sampling method |
| CN109975078A (en) * | 2017-12-28 | 2019-07-05 | 中核陕西铀浓缩有限公司 | A kind of system and method dividing sample suitable for hex liquefaction |
| CN112414768A (en) * | 2019-08-20 | 2021-02-26 | 中核陕西铀浓缩有限公司 | Subsampling method of uranium concentration plant |
| CN112414763A (en) * | 2019-08-22 | 2021-02-26 | 中核陕西铀浓缩有限公司 | Uranium hexafluoride product container liquefaction and homogenization device and method |
| CN110763813A (en) * | 2019-10-18 | 2020-02-07 | 浙江润土农业科技有限公司 | Portable tea leaf pesticide residue detection equipment |
| CN110836790A (en) * | 2019-11-18 | 2020-02-25 | 核工业北京化工冶金研究院 | Multi-channel automatic measuring device and method for centralized control room of in-situ leaching uranium mining area |
| CN111122249A (en) * | 2019-12-06 | 2020-05-08 | 合肥通用机械研究院有限公司 | High-precision full-automatic sampling device and method for measuring oil content of refrigerant |
| CN112345307B (en) * | 2020-11-01 | 2024-05-28 | 百色学院 | Liquid heavy metal loop sampling device and use method thereof |
| CN114307643A (en) * | 2021-12-17 | 2022-04-12 | 四川红华实业有限公司 | Feeding device for processing bromine trifluoride of unit |
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| GB2432711B (en) * | 2005-10-11 | 2008-04-02 | Gv Instr | Ion source preparation system |
| CN201141736Y (en) * | 2007-11-30 | 2008-10-29 | 核工业第七研究设计院 | Inner-cooling type condenser for uranium hexafluoride gas condensation |
| EP2342719B1 (en) * | 2008-09-25 | 2014-09-03 | Columbiana Hi Tech LLC | Container for transporting and storing uranium hexafluoride |
| CN102478415B (en) * | 2010-11-29 | 2013-10-09 | 中核建中核燃料元件有限公司 | Uranium hexafluoride online monitoring method |
| CN203656205U (en) * | 2013-12-10 | 2014-06-18 | 中核四〇四有限公司 | Novel condensing hydraulic valve for uranium conversion |
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