CN106872225A - A kind of water sample pretreatment device and its application method - Google Patents
A kind of water sample pretreatment device and its application method Download PDFInfo
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- CN106872225A CN106872225A CN201510916238.3A CN201510916238A CN106872225A CN 106872225 A CN106872225 A CN 106872225A CN 201510916238 A CN201510916238 A CN 201510916238A CN 106872225 A CN106872225 A CN 106872225A
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01F23/00—Indicating or measuring liquid level or level of fluent solid material, e.g. indicating in terms of volume or indicating by means of an alarm
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L11/00—Measuring steady or quasi-steady pressure of a fluid or a fluent solid material by means not provided for in group G01L7/00 or G01L9/00
Abstract
The invention provides a kind of water sample pretreatment device and its application method, the device is made up of the part such as lid, sealing ring, collecting pit, liquid level sensor, water outlet on-off valve, drainpipe, two five mouthfuls of switching valves and air pump on water inlet on-off valve, water inlet pipe, tracheae, temperature sensor, pressure sensor, collecting pit.By controlling the folding of valve, an air pump realizes that collecting pit switches circulation between the state of drawing water and hull-borne, and iterative cycles are to complete water sample with bulk mass product pre-treatment, while water sample pre-treatment major parameter is measured, and with functions such as filter membrane replacing promptings.Simple structure of the present invention, technology maturation, a large amount of cumbersome artificial operations are eliminated, be particularly well-suited to ambient water sample filtering enrichment pretreatment process.
Description
Technical field
The invention belongs to target contaminant analysis field in ambient water sample, relate generally to such as river, lake,
The analysis pre-treatment of the environment organic pollutants such as ocean, discharge water, the particularly filtering of laboratory water sample,
A kind of water sample preprocessing system and its application method that enrichment Treatment Analysis process is related to.
Background technology
The organic pollution of trace present in ambient water, especially multiring aromatic hydrocarbon, polychlorinated biphenyl and have
Machine chloro pesticide class etc., although absolute content is very low, but due to its persistence, bioconcentration and it is long away from
From the characteristic of transmission, cause the extensive attention of people.
In order to adapt to various analysis means, such as GC, LC, HPLC-MS, GC/MS etc., often
Need to gather a large amount of water samples and extracted and concentrated to laboratory.So not only workload is big, but also exists
A series of unfavorable factors, the problem for conveying bulk sample is change and the vessel surface that chemistry possible occur
Adsorption loss.Additionally, it is contemplated that the continuous sampling of water system will than obtained by timing sampling with more generation
The sample of table.So analysis worker wishes to try effectively eliminate these unfavorable factors, divided with improving
Analysis quality.
In general, the pretreatment process of sample takes and accounts for more than the 60% of whole analysis process, before sample
Treatment is the emphasis of trace analysis.At present, technology development comparative maturity, extraction efficiency are higher and using more
Trace organic pollutant in water pre-treating method have SPE (solid phase extraction,
SPE), SPME (solid phase micro-extraction, SPM E), membrane extraction (membrane
Extraction), pellicle passive sampling apparatus (semi-permeable membrane devices,
SPMD) etc..General filter water population of samples product is 20L even more than 50L, and water sample is by filtering
Film, extraction column flow rate are relatively low, when filtering water sample using traditional bottle,suction experimental system, every several minutes just
Need artificial operation to outwell waste water or change bottle,suction, prepare a concentrating sample and generally require more than ten or tens
Individual hour, waste time and energy.
Apparatus of the present invention and its application method are proposed for this, is driven in water sample pretreatment device of the invention
Under, the water sample of collection forms filters stream：Water sample is enriched with by membrane filtration or solid-phase extraction column
Afterwards, flow into metering and control device, the present apparatus to the major parameter in water sample filter process carry out metering and
Control, the filtering process of automatic stabilization can be realized by computer controls.
The content of the invention
Technical problem solved by the invention is to provide the side of a kind of water sample pre-treatment parameter metrology and control
Method and device.The invention belongs to target contaminant analysis field in water sample, such as river, lake are related generally to
The analysis pre-treatment of the environment organic pollutants such as pool, ocean, discharge water, particularly laboratory water sample mistake
A kind of water sample pretreatment device and its application method that filter, enrichment Treatment Analysis process are related to.
A kind of water sample pre-treatment parameter metrology proposed by the present invention and the system of control, chief component bag
Include and covered on water on-off valve, water inlet pipe, tracheae, temperature sensor, pressure sensor, collecting pit, sealed
The portions such as ring, collecting pit, liquid level sensor, water outlet on-off valve, drainpipe, two five mouthfuls of switching valves and air pump
Part is constituted；Lid, sealing ring and collecting pit coordinate so that collecting pit is internally formed closing on described collecting pit
Space；Water inlet pipe, tracheae, temperature sensor, pressure sensor are mounted on collecting pit on lid；In
Collecting pit side wall is provided with liquid level sensor；Water outlet on-off valve, drainpipe are installed in collecting pit bottom, are gone out
Normal off status is in when water on-off valve is not powered on；By tracheae by collecting pit Shang Gai and two five mouthfuls of switching valve phases
Connection so that collecting pit inner space gas circuit is communicated with two five mouthfuls the P of switching valve mouthfuls.
Water inlet bottom of the tube is angular cut, is installed on collecting pit on lid, coordinate it is fixed after water inlet pipe otch with
Collecting pit inwall is contacted, and current slowly flow into collecting pit inner space along collecting pit inwall.
Temperature sensor is elongated thermal resistance or thermocouple, is installed on collecting pit on lid, is coordinated after fixing
Bottom extend into collecting pit inner space, is used to detect the temperature of water sample.
Pressure sensor is the pressure sensor with data-signal output, is used to detect collecting pit inner space
Air pressure.
Collecting pit, is processed by materials such as stainless steel, lucite, and inner wall smooth, bottom is tapered,
The water for collecting can smoothly be flowed through along inwall water outlet on-off valve, drainpipe and discharge collecting pit.
Liquid level sensor is affixed to a kind of continuous liquid level sensor of collecting pit side, is used to detect collecting pit
The height of the water sample of interior collection, by the cumulative volume, the mean flow rate that calculate the water sample that can draw filtering
Etc. parameter.
Two five mouthfuls of switching valves have five gas ports of A, B, R, P, S, and A mouthfuls is entered by pipeline with air pump
Gas port is connected；Two five mouthfuls the B of switching valve mouthfuls is connected by pipeline with air pump gas outlet；Two five mouthfuls
P mouthfuls of switching valve is connected by tracheae with the inner space of collecting pit；Two five mouthfuls of switching valves are in acquiescence
Lower two P mouthfuls of the five mouthfuls of switching valve internal ducts of state are communicated with A mouthfuls, and B mouthfuls communicates with S mouthfuls, air pump pair
Collecting pit inner space is evacuated；In the energized state, two P mouthfuls and B mouthfuls of five mouthfuls of switching valve internal ducts
Communicate, A mouthfuls communicates with R mouthfuls, and air pump is to the air-blowing of collecting pit inner space.
The application method of a kind of water sample pre-treatment parameter metrology and the system of control, by controlling air pump and valve
Door state, realizes the water sample filtration parameter metering to slow flow velocity, and realize the water sample in a constant volume
It is automatic to collect and draining, monitor real time temperature, mean flow rate, the filtering cumulative volume of water sample.
The working condition of stream control system is drawn water and 2 kinds of states of draining：Draw water under state, break-make of intaking
Valve internal duct is opened, water outlet on-off valve internal duct is closed, two five mouthfuls of switching valves are closed, internal duct
P mouthfuls communicates with A mouthfuls, and B mouthfuls communicates with S mouthfuls, and air pump is evacuated to collecting pit inner space, forms negative pressure water
Sample is into collecting pit and collects；When the water sample liquid level of liquid level sensor detection reaches the higher limit of setting,
System control switches to hull-borne, and water inlet on-off valve internal duct is closed, water outlet on-off valve internal duct is opened
Open, two five mouthfuls of switching valves are opened, internal duct P mouthfuls communicates with B mouthfuls, and A mouthfuls communicates with R mouthfuls, gas
Pump forms malleation to the air-blowing of collecting pit inner space, and after switching on-off valve, water sample is arranged from collecting pit bottom
Go out；When the water sample liquid level of liquid level sensor detection reaches the lower limit of setting or a period of time by setting
Afterwards, system switches to the state of drawing water, and the water sample cumulative volume of filtering is cumulative 1 time；Iterative cycles are big to complete
Volume of water sample pre-treatments.
Draw water with one cycle period of draining, the collecting pit of system record filtering time and initial alignment
Dischargeable capacity, the average current velocity in the conversion single cycle cycle.
There is filter membrane to block, prompting function is changed for the system, and system rule of thumb sets alarm pressure limiting value,
When the pressure value of pressure sensor exceedes alarm pressure limiting value, system sends signal and reminds user to change filter membrane.
The beneficial effects of the invention are as follows：Water sample pre-treatment parameter metrology proposed by the present invention and the system of control,
Instead of the cumbersome artificial operation that the traditional means concentration such as laboratory bottle,suction prepares water sample；It is easy to program automatic
Control realization current road, complete water sample filtering enrichment after automatic gauge filtering water temperature, average current velocity,
The parameters such as total filtering water volume；By monitoring air pressure in collecting pit, it is capable of achieving filter membrane and blocks the functions such as alarm.
Simple structure of the present invention, technology maturation, are particularly suitable for the analysis pre-treatment of large volume ambient water and prepare sample mistake
Cheng Zhong.
Brief description of the drawings
Fig. 1 be water sample pre-treatment parameter metrology of the invention and control system in water sample preparation process
Connection diagram.The substantially ponding of collection is by after filtering membrane filtration, enrichment unit enrichment, current enter this
The water sample pre-treatment parameter metrology of invention and the system of control；
Fig. 2 is the schematic diagram of the system of water sample pre-treatment parameter metrology of the invention and control；
Wherein, 1 is water inlet on-off valve；2 is water inlet pipe；3 is tracheae, 4 is temperature sensor, 5 is pressure
Force snesor, 6 are to be covered on collecting pit, and 7 is sealing ring, and 8 is collecting pit, and 9 is liquid level sensor, 10
It is water outlet on-off valve, 11 is drainpipe, and 12 is two five mouthfuls of switching valves, and 13 is air pump；
Fig. 3 is water sample preparation process FB(flow block)；
Fig. 4 is view of drawing water；
Fig. 5 is hull-borne schematic diagram.
Specific embodiment
A kind of water sample pretreatment device proposed by the present invention, including water inlet on-off valve, water inlet pipe, tracheae,
Lid, sealing ring, collecting pit, liquid level sensor, water outlet on temperature sensor, pressure sensor, collecting pit
The parts such as on-off valve, drainpipe, two five mouthfuls of switching valves and air pump are constituted；It is described collecting pit Shang Gai, close
Seal ring coordinates the space for collecting pit is internally formed closing with collecting pit；Water inlet pipe, tracheae, TEMP
Device, pressure sensor are mounted on collecting pit on lid；In collecting pit side, wall is provided with liquid level sensor；
Water outlet on-off valve, drainpipe are installed in collecting pit bottom, normal off status is in when water outlet on-off valve is not powered on；
Collecting pit Shang Gai is connected with two five mouthfuls of switching valves by tracheae so that collecting pit inner space gas circuit with
Two five mouthfuls the P of switching valve mouthfuls communicates.
Water inlet bottom of the tube is angular cut, is installed on collecting pit on lid, coordinate it is fixed after water inlet pipe otch with
Collecting pit inwall is contacted, and current slowly flow into collecting pit inner space along collecting pit inwall.
Temperature sensor is elongated thermal resistance or thermocouple, is installed on collecting pit on lid, is coordinated after fixing
Bottom extend into collecting pit inner space, is used to detect the temperature of water sample.
Pressure sensor is the pressure sensor with data-signal output, is used to detect collecting pit inner space
Air pressure.
Collecting pit, is processed by materials such as lucite, and inner wall smooth, bottom is tapered, the water for collecting
Can smoothly be flowed through along inwall water outlet on-off valve, drainpipe and discharge collecting pit.
Liquid level sensor is affixed to a kind of continuous liquid level sensor of collecting pit side, is used to detect collecting pit
The height of the water sample of interior collection, by the cumulative volume, the mean flow rate that calculate the water sample that can draw filtering
Etc. parameter.
Two five mouthfuls of switching valves have five gas ports of A, B, R, P, S, and A mouthfuls is entered by pipeline with air pump
Gas port is connected；Two five mouthfuls the B of switching valve mouthfuls is connected by pipeline with air pump gas outlet；Two five mouthfuls
P mouthfuls of switching valve is connected by tracheae with the inner space of collecting pit；Two five mouthfuls of switching valves are in acquiescence
Lower two P mouthfuls of the five mouthfuls of switching valve internal ducts of state are communicated with A mouthfuls, and B mouthfuls communicates with S mouthfuls, air pump pair
Collecting pit inner space is evacuated；In the energized state, two P mouthfuls and B mouthfuls of five mouthfuls of switching valve internal ducts
Communicate, A mouthfuls communicates with R mouthfuls, and air pump is to the air-blowing of collecting pit inner space.
It is below specific implementation of the patent mode for example, concretely comprising the following steps：
1) the environmental water sample 20L such as collection rivers, lake, after pipeline is connected through into filter membrane and enrichment unit
It is connected with system of the invention.
2) under program, booster air pump, water inlet on-off valve 1 internal duct is opened, water outlet on-off valve 10
Internal duct close, two five mouthfuls of switching valves 12 close, internal duct P mouthful communicates with A mouthfuls, B mouthfuls and
S mouthfuls communicates, and air pump is evacuated to the inner space of collecting pit 8, and negative pressure water sample is into collecting pit and collects for formation.
3) through (such as 20s) after a period of time, the water sample liquid level of the detection of liquid level sensor 9 is reached and set
During fixed higher limit, under program, system control switches to hull-borne, inside water inlet on-off valve 1
Pipeline is closed, the internal duct of water outlet on-off valve 10 is opened, two five mouthfuls of switching valves 12 are opened, internal duct
P mouthfuls is communicated with B mouthfuls, and A mouthfuls communicates with R mouthfuls, and air pump 13 is formed to the inner space air-blowing of collecting pit 8
Malleation, after switching on-off valve, water sample is discharged from the bottom of collecting pit 8.
4) when water drains into liquid level sensor preset lower limit, under program, system switches to the state of drawing water,
The water sample cumulative volume of filtering is cumulative 1 time；
5) iterative cycles above step 2-4, until system monitoring air pressure is less than the pressure of experience setting (such as
- 20Kpa), program provides filter membrane and blocks alarm, points out operating personnel to change filter membrane；
6) change and continue to reach 20L up to total filtering water volume after finishing, collect filter membrane and enrichment unit conduct
The condensed water sample of preparation, delivers to the next step flow of pollutant analysis.
Claims (10)
1. a kind of water sample pretreatment device, it is characterised in that：Part include water inlet on-off valve (1),
On water inlet pipe (2), tracheae (3), temperature sensor (4), pressure sensor (5), collecting pit cover (6),
Sealing ring (7), collecting pit (8), liquid level sensor (9), water outlet on-off valve (10), drainpipe (11),
Two five mouthfuls of switching valves (12) and air pump (13)；
Collecting pit (8) is the container of upper end open, and container open end is provided with lid (6) on collecting pit, receives
(6) are covered on Ji Chi sealing ring (7) is provided with and between container open end；On described collecting pit cover (6),
Sealing ring (7) coordinates the space for collecting pit is internally formed closing with collecting pit (8)；
Water inlet pipe (2), tracheae (3), temperature sensor (4), pressure sensor (5) are installed and fixed
In covered on collecting pit on (6) and respectively with collecting pit (8) intracavity inter-connection, water inlet pipe sets on (2)
Have into water on-off valve (1)；In collecting pit (8) side, wall is provided with for monitoring collecting pit (8) interior liquid
The liquid level sensor (9) of height；Drainpipe (11), drainpipe (11) are installed in collecting pit (8) bottom
Water outlet on-off valve (10) is provided with, normal off status is in when water outlet on-off valve (10) is not powered on；Tracheae
(3) it is connected with a port of two five mouthfuls of switching valves (12) away from one end that (6) are covered on collecting pit
It is logical, collecting pit (8) inner chamber is connected with two five mouthfuls of switching valves (12) by tracheae (3), make
Collecting pit (8) inner space gas circuit is obtained to be communicated with two P mouthfuls of five mouthfuls of switching valves (12).
2. device as claimed in claim 1, it is characterised in that：Water inlet pipe (2) outlet at bottom is wedge
Shape angular cut, is installed on collecting pit and covers on (6), coordinates the otch of water inlet pipe (2) and receipts after fixing
Ji Chi (8) inwall is contacted, and it is internal that current slowly flow into collecting pit (8) along collecting pit (8) inwall
Space.
3. device as claimed in claim 1, it is characterised in that：Temperature sensor (4) is elongated
Thermal resistance or thermocouple, are installed on collecting pit and cover on (6), coordinate fixed rear lower to extend into collection
Pond (8) inner space, is used to detect the temperature of water sample；
Described pressure sensor (5), the pressure sensor with data-signal output, is used to detect receipts
The air pressure of Ji Chi (8) inner space.
4. device as claimed in claim 1, it is characterised in that：Collecting pit (8) is by stainless steel or has
The materials such as machine glass are processed, and inner wall smooth, bottom is tapered, and the water for collecting can be smooth along inwall
Flow through water outlet on-off valve (10), drainpipe (11) and discharge collecting pit.
5. device as claimed in claim 1, it is characterised in that：Liquid level sensor (9) is affixed to
A kind of continuous liquid level sensor of collecting pit (8) side, is used to detect the water collected in collecting pit (8)
The height of sample, by the cumulative volume, the mean flow rate that calculate the water sample that can draw filtering.
6. device as claimed in claim 1, it is characterised in that：Two five mouthfuls of switching valves (12) tools
There are five gas ports of A, B, R, P, S, A mouthfuls is connected by pipeline with air pump (13) air inlet (13a)
It is logical；Two B mouthfuls of five mouthfuls of switching valves (12) passes through pipeline and air pump (13) gas outlet (13b) phase
Connection；Two P mouthfuls of five mouthfuls of switching valves (12) empty with the inside of collecting pit (8) by tracheae (3)
Between be connected；
Two five mouthfuls of switching valves (12), two five mouthfuls of switching valve (12) internal duct P by default
Mouth is communicated with A mouthfuls, and B mouthfuls communicates with S mouthfuls, and air pump (13) is evacuated to collecting pit (8) inner space；
In the energized state, two five mouthfuls of P mouthfuls of switching valve (12) internal ducts are communicated with B mouthfuls, A mouthfuls and R
Mouth is communicated, and air pump (13) is to collecting pit (8) inner space air-blowing.
7. a kind of application method of any water sample pretreatment devices of claim 1-6, it is characterised in that：
By controlling air pump and valve state, realize that the water sample in a constant volume is collected and draining automatically,
And monitor real time temperature, mean flow rate, the filtering cumulative volume of water sample.
8. application method as claimed in claim 7, it is characterised in that：Working state of system draws water
With 2 kinds of states of draining：
Draw water under state, water inlet on-off valve (1) internal duct is opened, water outlet on-off valve (10) is internal
Pipeline is closed, two five mouthfuls of switching valves (12) are closed, and internal duct P mouthful communicates with A mouthfuls, B mouthfuls and
S mouthfuls communicates, and air pump is evacuated to collecting pit (8) inner space, forms negative pressure water sample and enters collecting pit simultaneously
Collect；When the water sample liquid level of liquid level sensor (9) detection reaches the higher limit of setting, system control
System switches to hull-borne, and water inlet on-off valve (1) internal duct is closed, water outlet on-off valve (10) is interior
Portion's pipeline is opened, two five mouthfuls of switching valves (12) are opened, and internal duct P mouthfuls communicates with B mouthfuls, A mouthfuls
Communicated with R mouthfuls, air pump (13) forms malleation to collecting pit (8) inner space air-blowing, and switching is logical
After disconnected valve, water sample is discharged from collecting pit (8) bottom；When the water sample of liquid level sensor (9) detection
Liquid level reaches the lower limit of setting or by after a period of time for setting, system switches to the state of drawing water, mistake
The water sample cumulative volume of filter is cumulative 1 time；Iterative cycles are completing water sample with bulk mass product pre-treatment.
9. water sample pre-treatment parameter metrology as claimed in claim 7 or 8 and the system of control make
With method, it is characterised in that draw water with one cycle period of draining, the system record filtering time and
The dischargeable capacity of the collecting pit of initial alignment, the average current velocity in the conversion single cycle cycle.
10. application method as claimed in claim 7 or 8, it is characterised in that：The system has filter membrane
Block, change prompting function, system rule of thumb sets alarm pressure limiting value, when pressure sensor
Pressure value exceedes alarm pressure limiting value, and system sends signal and reminds user to change filter membrane.
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| CN201510916238.3A CN106872225A (en) | 2015-12-10 | 2015-12-10 | A kind of water sample pretreatment device and its application method |
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| CN201510916238.3A CN106872225A (en) | 2015-12-10 | 2015-12-10 | A kind of water sample pretreatment device and its application method |
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| CN108020628A (en) * | 2018-01-02 | 2018-05-11 | 江苏中宜金大分析检测有限公司 | A kind of method that sulfanilamide (SN) in water is measured using high pressure liquid chromatography tandem mass spectrometry |
| CN108444797A (en) * | 2018-06-06 | 2018-08-24 | 西藏农牧学院 | A kind of water sample preprocessing system |
| CN111982384A (en) * | 2020-08-17 | 2020-11-24 | 诸暨新伏给排水设备有限公司 | Sewage drain valve port water pressure monitoring facilities |
| CN112516798A (en) * | 2020-11-16 | 2021-03-19 | 江苏汉光生物工程有限公司 | Method for purifying erythritol fermentation liquor |
| RU2786650C1 (en) * | 2022-04-14 | 2022-12-23 | Федеральное государственное бюджетное учреждение науки Тихоокеанский океанологический институт им. В.И. Ильичева Дальневосточного отделения Российской академии наук | Water collector sampling system |
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| RU2786650C1 (en) * | 2022-04-14 | 2022-12-23 | Федеральное государственное бюджетное учреждение науки Тихоокеанский океанологический институт им. В.И. Ильичева Дальневосточного отделения Российской академии наук | Water collector sampling system |
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