CN214503073U

CN214503073U - On-site rapid enrichment, purification and blow-drying device for target pollutants in water environment

Info

Publication number: CN214503073U
Application number: CN202120089610.9U
Authority: CN
Inventors: 文大为; 田林; 杨定忠; 张博
Original assignee: Beijing Chengda Instrument Co ltd
Current assignee: Beijing Chengda Instrument Co ltd
Priority date: 2021-01-14
Filing date: 2021-01-14
Publication date: 2021-10-26
Anticipated expiration: 2031-01-14

Abstract

The utility model belongs to the technical field of the water quality testing technique and specifically relates to a device for quickly enriching, purifying and drying target pollutants in water environment on site, which comprises a sample solid-phase extraction module, a temperature-controllable and drying sample support module, wherein the sample solid-phase extraction module comprises a six-way selector valve, an injection pump, a receiving valve, a first filter, a second filter, a water sample storage tank, an activation liquid bottle, a flushing liquid bottle, a leaching liquid bottle, a container and an adsorption trap; but the temperature control and weather sample support module includes metal bath piece, air pump, temperature control device, and it has the hole site of three adaptation receiving vessel to open on the metal bath piece, and three hole site is in proper order for receiving the position, weather the position, derive the position, receives under the position department receiving tube line, weathers under the position is in the trachea that the air pump connects out, is provided with heating device in the metal bath piece, and heating device electric connection has temperature control device. The utility model has the advantages of simple device, low cost, small weight, easy maintenance and maintenance, and being capable of backflushing the water sample filtering path.

Description

On-site rapid enrichment, purification and blow-drying device for target pollutants in water environment

Technical Field

The utility model relates to a water quality testing technical field especially relates to a device that weathers is purified to on-spot quick enrichment of target pollutant in water environment.

Background

In the water quality detection technology, solid phase extraction is a common water sample pretreatment scheme, and can effectively separate analytes from interfering components. The method can be used as a sample pretreatment scheme of technologies such as atomic absorption, ICP-MS, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry and the like, and can realize the detection of pollutants in water in various aspects such as heavy metal ions, pesticide residues, organic pollutants and the like. Meanwhile, based on the application of forensic medicine and law chemistry, for example, in recent years, a new method, sewage epidemiology, is widely used for evaluating and monitoring the abuse of mental active substances, namely, the per-capita consumption of the drugs is back-calculated by measuring the content of the drugs or metabolites thereof in sewage in a certain area. The method for researching and evaluating the abuse of the mental active substances through environmental detection has the advantages of objectivity, high efficiency, quantifiability and the like.

The method comprises the steps of performing solid-phase extraction pretreatment on a water sample, namely using an adsorption trap (a solid-phase extraction column) filled with adsorbable substances as a material for enriching target substances, generally performing five steps of activation (washing the adsorption trap by using an activation liquid), sample loading (using positive pressure injection or negative pressure suction to enable a large-volume water sample to pass through the adsorption trap), washing (using a cleaning liquid to wash the adsorption trap to remove interferents), blow-drying (draining the adsorption trap), and leaching (using a leaching liquid to wash the adsorption trap), completing a standard working procedure, and collecting the leaching liquid in the last step, wherein the leaching liquid contains the enriched and purified target substances.

Meanwhile, the method and the solid-phase extraction are often combined in a pretreatment process, and are used for blow-drying and derivatization of a sample. The sample drying step is generally carried out under heating conditions (usually 50-100 ℃), and the liquid level is purged by using air flow assistance, so that the eluent obtained in the solid phase extraction process is partially or completely evaporated for concentrating or replacing the solvent.

Another common combining step is derivatization of the sample. In the sample pretreatment of gas chromatography or gas chromatography mass spectrometry, the target substance which is subjected to blow-drying replacement of a solvent needs to react for 10-60 minutes under a heating environment.

Traditionally, the technical methods for detecting mental active substances in water environment at home and abroad are field sampling, and the sampling is sent back to a laboratory for treatment and instrument analysis. The method has some defects, firstly, the acquisition and transportation process needs to occupy considerable manpower and material resources, and the cost is high; secondly, when the number of field sampling points is large and the distance from the laboratory is long, a large number of samples cannot be immediately transported back to the laboratory, and the analysis has hysteresis; thirdly, sample storage conditions such as freezing, acidification and the like are not provided in the field, and the improper storage of the sample can cause great influence on experimental results. Therefore, from the aspect of methodology, a technology capable of performing rapid pretreatment of samples in the field is urgently needed, and the samples are purified, enriched and then stored.

The utility model with publication (publication) number CN210533834U discloses a device for rapidly enriching and purifying mental active substances in water environment on site, but it has the following disadvantages:

(1) the device is complicated, the price is high, and weight is big, difficult maintenance: in the scheme, the whole solid phase extraction process is executed by using two injection pumps and seven valves, so that the weight and the volume are large, and the portability of the device is not facilitated. Meanwhile, the valve switching and the pipeline connection are too complicated, and the diagnosis and the maintenance are inconvenient after the fault occurs;

(2) one-way positive pressure filtration easily blocks up the filter: the positive pressure filtering part of the device has the advantages that the water sample is pressed into the filter from the lower part of the water sample storage tank and the back flushing function is not realized. When a sewage sample is treated, once solid matters in the sewage block a filter, the flow rate of the sample loading step is greatly influenced, and the total treatment speed of the sample is seriously slowed down;

(3) and sample blow-drying and derivatization processing functions cannot be provided on the same device.

SUMMERY OF THE UTILITY MODEL

The utility model aims at solving the problem that the existing device in the prior art is complex, high in price, heavy, difficult maintenance and maintenance, one-way positive pressure filtration plug up the filter easily, can not provide the sample on same device and weather and the shortcoming of derivatization processing function, and the on-the-spot quick enrichment of target pollutant purifies and weathers the device in water environment that proposes.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

designing a field rapid enrichment, purification and blow-drying device for target pollutants in a water environment, comprising a sample solid-phase extraction module and a temperature-controllable and blow-drying sample support module, wherein the sample solid-phase extraction module comprises a six-way selector valve, an injection pump, a receiving valve, a first filter, a second filter, a water sample storage tank, an activation liquid bottle, a flushing liquid bottle, a washing liquid bottle, a container and an adsorption trap, seven interfaces are arranged on the six-way selector valve, a public end interface is arranged in the middle of the seven interfaces, the rest six interfaces are respectively marked as No. 1-6 interfaces, the interfaces are not communicated in pairs, the injection pump is connected with the public end interface of the six-way selector valve through a pipeline, the water sample storage tank is connected with the No. 1 interface of the six-way selector valve through a pipeline, and the tail end of the pipeline arranged in the water sample storage tank is provided with the first filter, a second filter is arranged on a pipeline between the water sample storage tank and the six-way selector valve, the activation liquid bottle is connected with a No. 4 interface of the six-way selector valve through a pipeline, the flushing liquid bottle is connected with a No. 5 interface of the six-way selector valve through a pipeline, and the rinsing liquid bottle is connected with a No. 6 interface of the six-way selector valve through a pipeline;

an emptying pipeline is connected to the No. 2 interface of the six-way selector valve, the other end of the emptying pipeline is not connected with any device and is placed in the air, and the inlet of the adsorption trap is connected with the No. 3 interface of the six-way selector valve through a pipeline;

the receiving valve is a two-position three-way electromagnetic valve, three ports of a common end, an NC end and an NO end are arranged on the receiving valve, an outlet of the adsorption trap is connected with the common end of the receiving valve through a pipeline, the NO end of the receiving valve is connected with a waste liquid discharge pipeline, the other end of the waste liquid discharge pipeline is connected with a waste liquid collecting device, the NC end of the receiving valve is connected with a receiving pipeline, and the tail end of the receiving pipeline is arranged in a receiving container;

but controllable temperature and weather sample support module include metal bath piece, air pump, temperature control device, it has the hole site that three adaptation received the container to open on the metal bath piece, and is three the hole site is in proper order for receiving the position, weathers the position, derives the position, receive under the position department receiving pipeline, weathers under the position is in the trachea that the air pump connects out, be provided with heating device in the metal bath piece, heating device electric connection has temperature control device.

Preferably, the water sample storage tank is a 1L or 2L high-density polyethylene bottle.

Preferably, the first filter is a sintered metal filter with a pore size of 10 microns.

Preferably, the second filter is a 0.46 micron pore size cellulose pin filter.

Preferably, the heating device is a polyimide substrate electric heating sheet.

The utility model provides a device weathers is purified in on-spot quick enrichment of target pollutant in water environment, beneficial effect lies in:

(1) the device is simple, and is with low costs, weight is small, easy maintenance: the whole solid phase extraction process is executed by using a syringe pump, a six-way selector valve and a two-position three-way valve, so that the cost of the device is greatly reduced and the portability is improved. The flow path is simple and clear, and is easy to maintain and repair.

(2) The water sample filtering path can be backflushed: when the sewage sample is treated, once solid matters in the sewage block the filter, the blockage can be eliminated through a back flushing step, and good usability of the sewage sample is ensured.

(3) The device has the advantages that the functions of blow-drying and derivatization treatment of the sample are provided on the same device, the device is convenient to be combined with field analysis technologies such as solvent replacement (such as portable immunofluorescence detection) and derivatization (such as portable gas chromatography detection), and a complete solution is provided for the pretreatment of the sample.

Drawings

Fig. 1 is a schematic structural diagram of the on-site rapid enrichment, purification and blow-drying device for target pollutants in water environment provided by the utility model.

In the figure: the device comprises a six-way selector valve 11, an injection pump 2, a receiving valve 3, a first filter 4, a second filter 5, a water sample storage tank 6, an activation liquid bottle 7, a washing liquid bottle 8, a leacheate bottle 9, a receiving container 10, a metal bath block 11, an air pump 12, a temperature control device 13 and an adsorption trap 14.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.

Example 1

Referring to fig. 1, the on-site rapid enrichment, purification and blow-drying device for target pollutants in water environment comprises a sample solid phase extraction module and a temperature-controllable and blow-drying sample support module, wherein the two parts are uniformly controlled by a circuit system and powered by a battery or an external power supply. The present embodiment is specially provided with a single chip as a controller, and the controller can control functions of valve switching, operation of the injection pump 2, operation of the air pump 12 and the like in the following by programming.

The sample solid phase extraction module comprises a six-way selector valve 1, an injection pump 2, a receiving valve 3, a first filter 4, a second filter 5, a water sample storage tank 6, an activation liquid bottle 7, a washing liquid bottle 8, a washing liquid bottle 9, a container 10 and an adsorption trap 14, wherein seven interfaces are arranged on the six-way selector valve 1, a public end interface is arranged in the middle of the seven interfaces, the rest six interfaces are respectively marked as No. 1-6 interfaces, the interfaces are not communicated pairwise, the six-way selector valve 1 is used as a core component of the sample solid phase extraction module and provides a flow path selection function, the switching of the valves is driven by a motor and is controlled by a circuit part, the six-way selector valve 1 can only select one switching position at the same time, and the public end interface can only be communicated with the currently selected interface and is disconnected with other five unselected interfaces. The six-way selection valve in the device can be replaced by a multi-channel switching valve with more channels, such as eight-way or ten-way valves, and the selectable eluent types are increased.

The injection pump 2 is connected with a public end interface of the six-way selector valve 1 through a pipeline, the injection pump 2 comprises a stepping motor and a driver thereof, a screw rod, a bracket, an injector and the like, and the pushing and the sucking of liquid are realized through the pushing and the pumping of an injector piston. In an application example of the present invention, a syringe pump equipped with a 25mL glass syringe was used to construct the system.

The water sample storage tank 6 is connected with the No. 1 interface of the six-way selector valve 1 through a pipeline, a first filter 4 is arranged at the tail end of the pipeline in the water sample storage tank 6, and a second filter 5 is arranged on the pipeline between the water sample storage tank 6 and the six-way selector valve 1. The water sample storage tank 6 is used for loading water samples needing enrichment treatment. The first filter 4 pre-filters the water sample to remove large-particle solid impurities; in the middle of the pipeline, a second filter 5 is added to further filter fine particle solid impurities in the water sample. In the application example of the present invention, 1L or 2L High Density Polyethylene (HDPE) bottles were used as the water sample storage tanks, sintered metal filters with 10 μm pore size were used as the first filter (4), and cellulose needle filters with 25 mm diameter and 0.46 μm pore size were used as the second filter 5. Can be replaced by other applicable specifications and materials according to the needs.

The activation liquid bottle 7 is connected with the No. 4 interface of the six-way selector valve 1 through a pipeline, the washing liquid bottle 8 is connected with the No. 5 interface of the six-way selector valve 1 through a pipeline, and the leacheate bottle 9 is connected with the No. 6 interface of the six-way selector valve 1 through a pipeline;

the No. 2 interface of the six-way selector valve 1 is connected with an emptying pipeline, the other end of the emptying pipeline is not connected with any device and is placed in the air, and the inlet of the adsorption trap 14 is connected with the No. 3 interface of the six-way selector valve 1 through a pipeline;

the receiving valve 3 is a two-position three-way electromagnetic valve, three ports of a common end, an NC end and an NO end are arranged on the receiving valve 3, an outlet of the adsorption trap 14 is connected with the common end of the receiving valve 3 through a pipeline, the NO end of the receiving valve 3 is connected with a waste liquid discharge pipeline, the other end of the waste liquid discharge pipeline is connected with a waste liquid collecting device, the NC end of the receiving valve 3 is connected with a receiving pipeline, and the tail end of the receiving pipeline is arranged in the receiving container 10; the two-position three-way electromagnetic valve is controlled by double coils, one coil is powered on instantly, the power supply is closed, the valve is opened, and the other coil is powered on instantly, the power supply is closed, and the valve is closed. The mode is one-inlet two-outlet, when the solenoid valve coil is electrified, the NC end is connected with the common end, and the NO end is disconnected; when the solenoid valve coil is powered off, the NO end is connected with the common end, and the NC end is disconnected. In an application example of the invention, the electromagnetic valve is controlled by using 24V power supply. The receiving container 10 is used to receive the eluate containing the enriched and purified target substances in the elution step. In an embodiment of the present invention, a 1.5mL conical centrifuge tube is used as the receiving container.

The connecting pipeline is suitable for medium-pressure chromatographic pipelines and joints. Typically 1/16 inches or 1/8 inches in outside diameter, 0.25-2mm inside diameter, teflon, polyetheretherketone or stainless steel tubing, and a mating threaded connection. In an example of the application of the present invention, stainless steel and teflon tubing of 1/16 inches outside diameter, 0.25, 0.5, or 0.75mm inside diameter, and 10-32 thread fittings, 1/4-28 thread fittings, and luer fittings.

The temperature-controllable and blow-drying sample support module comprises a metal bath block 11, an air pump 12 and a temperature control device 13, wherein three hole sites adaptive to a receiving container 10 are formed in the metal bath block 11, the three hole sites are a receiving position, a blow-drying position and a derivative position in sequence, the receiving position is positioned under a receiving pipeline, the blow-drying position is positioned under an air pipe connected out by the air pump 12, a heating device is arranged in the metal bath block 11, and the heating device is electrically connected with the temperature control device 13. The receiving station is for receiving the container 10 to receive the rinse solution. The blow-drying position is used for blow-drying, the self-receiving position is transferred, and the sample obtained in the solid phase extraction step is leached. The derivatization site is a separate location for storing the sample to be derivatized by heating.

An air pump 12 is used to provide the air flow required to blow the sample dry. In the application example of the invention, a 24V power supply and 1.1L/min flow path micro diaphragm air pump is used, and a polytetrafluoroethylene tube with 0.8mm inner diameter and 1/16 inches outer diameter is used as the air blowing tube.

The heating device is arranged in the metal bath block 11 or at the bottom of the metal bath block and is used for heating the metal bath block 11. In the application example of the present invention, a polyimide-based electric heating sheet supplied with power at 24V was used as the heating means. The heating device is controlled by a temperature control device, in the application example of the invention, the temperature control device is controlled by PID, wherein PT-100 is used for measuring the temperature, 24V is used for supplying power.

The utility model discloses a concrete operation flow as follows:

scheme 1: the solid phase extraction process of the sample comprises the following steps:

step 1: activation (use of activating solution to rinse the adsorption trap)

The device is realized by the following modes:

when the adsorption trap 14 is activated, the selector valve is switched to position 4, and the syringe pump 2 sucks in a fixed amount of the activation liquid. The selector valve is then switched to position 3 to deliver the activation fluid to the trap 14 at the required flow rate and dosage, and the fluid exiting the trap 14 is pushed out of the waste port through the NO end of the receiver valve 3.

Step 2: sample application (Positive pressure injection or negative pressure suction to pass bulk water sample through the adsorption trap 14)

The device is realized by the following modes:

when the adsorption trap 14 is activated, the selection valve is switched to the No. 1 position, and the injection pump 2 sucks in a water sample quantitatively. Then the selection valve is switched to No. 3, the water sample is delivered to the adsorption trap 14 according to the required flow rate and dosage, and the liquid flowing out of the adsorption trap 14 is pushed out of the waste liquid port through the NO end of the receiving valve 3.

If the water sample needing to be enriched is large in volume, the injection pump 2 repeatedly performs the liquid suction-liquid pushing process until the total amount of the pumped water sample meets the application requirement.

In this process, particulate matter that may be present in the sample water may be removed after the coarse filtration by the first filter 4 and the fine filtration by the second filter 5.

Particularly, along with the filtration, the outside of the filter can be blocked by the particulate matter, and the sucked water sample can be pushed back again through the back flushing and flushed to the water sample storage tank 6 through the public end, so that the particulate matter attached to the outside of the micropores of the filter can be flushed back, and the filter passing performance is improved. The water sample is used for backflushing, so that the water sample cannot be polluted by other reagents.

And step 3: flushing (cleaning solution is used to flush the adsorption trap 14 to remove interferents)

The device is realized by the following modes:

when the adsorption trap 14 is activated, the selector valve is switched to the 5 th position, and the syringe pump 2 sucks the washing liquid in a fixed amount. The selector valve is then switched to position 3 to deliver the rinse solution to the trap 14 at the desired flow rate and dosage, and the effluent from the trap 14 is pushed out of the waste port through the NO port of the receiver valve 3.

And 4, step 4: blow-dry (draining the cleaning liquid in the adsorption well 14)

The device is realized by the following modes:

upon activation of the trap 14, the selector valve is switched to position 2 and the syringe pump 2 draws air in a full range. Then the selection valve is switched to the No. 3 position, the air is conveyed to the adsorption trap 14 at the required flow rate, and residual liquid in the adsorption trap 14 is drained. The liquid flowing out of the adsorption trap 14 is pushed out of the waste liquid port through the NO end of the receiving valve 3. The syringe pump 2 will repeat the above-described suction-push process if necessary until the adsorption trap 14 is completely drained.

And 5: rinsing (flushing the adsorption trap 14 with a rinse) and receiving the rinse

The device is realized by the following modes:

when the adsorption trap 14 is activated, the selector valve is switched to position 6, and the syringe pump 2 sucks the eluent in a fixed amount. Then the selection valve is switched to the No. 3 position, the eluent is conveyed to the adsorption trap 14 according to the required flow rate and dosage, the liquid flowing out of the adsorption trap 14 flows through the receiving branch pipe through the NC end of the receiving valve 3 and is injected into the receiving container 10 arranged above the receiving position of the temperature-controllable and blow-drying sample support module.

And (2) a flow scheme: sample blow-drying process

After the solid phase extraction process is finished, the receiving container 10 can be moved to a blow-drying position to start the blow-drying process. At this time, the receiving site is left vacant, and the solid phase extraction process of the next sample can be performed.

During the drying process, the air pump 12 is continuously operated to provide an air flow for drying. The temperature control device 13 is used for setting a proper temperature to accelerate the drying speed.

And (3) a flow path: derivatization process of sample

After the blow-drying process is complete, the derivatization process is initiated by moving the receiving vessel 10 to the derivatization site by adding the appropriate derivatization reagent to the sample vessel and closing the vessel lid. The derivatization temperature can be set by temperature control. Considering that the derivatization temperature and the blow-drying temperature are close to each other in most cases, the device combines temperature control and metal bath heating in the same part, and the temperature setting is based on the derivatization requirement.

Under the maximum efficiency, the sample is subjected to solid phase extraction, blow-drying and derivatization in sequence. At most three samples can be accommodated in one device, and the pretreatment operations in different stages are respectively carried out.

The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.

Claims

1. The on-site rapid enrichment, purification and blow-drying device for the target pollutants in the water environment comprises a sample solid-phase extraction module and a temperature-controllable and blow-drying sample support module, and is characterized in that the sample solid-phase extraction module comprises a six-way selector valve (1), an injection pump (2), a receiving valve (3), a first filter (4), a second filter (5), a water sample storage tank (6), an activation liquid bottle (7), a washing liquid bottle (8), a leacheate bottle (9), a container (10) and an adsorption trap (14), seven interfaces are arranged on the six-way selector valve (1), a public end interface is arranged in the middle of the seven interfaces, the rest six interfaces are respectively marked as No. 1-6 interfaces, the interfaces are not communicated with one another, the injection pump (2) is connected with the public end interface of the six-way selector valve (1) through a pipeline, the device comprises a water sample storage tank (6), a first filter (4), a second filter (5), an activation liquid bottle (7), a flushing liquid bottle (8), a washing liquid bottle (9) and a six-way selector valve (1), wherein the water sample storage tank (6) is connected with a No. 1 interface of the six-way selector valve (1) through a pipeline, the first filter (4) is arranged at the tail end of the pipeline arranged in the water sample storage tank (6), the second filter (5) is arranged on the pipeline between the water sample storage tank (6) and the six-way selector valve (1), the activation liquid bottle (7) is connected with the No. 4 interface of the six-way selector valve (1) through a pipeline, the flushing liquid bottle (8) is connected with a No. 5 interface of the six-way selector valve (1) through a pipeline, and the washing liquid bottle (9) is connected with the No. 6 interface of the six-way selector valve (1) through a pipeline;

an emptying pipeline is connected to the No. 2 interface of the six-way selector valve (1), the other end of the emptying pipeline is not connected with any device and is placed in the air, and the inlet of the adsorption trap (14) is connected with the No. 3 interface of the six-way selector valve (1) through a pipeline;

the receiving valve (3) is a two-position three-way electromagnetic valve, three ports of a common end, an NC end and an NO end are arranged on the receiving valve (3), an outlet of the adsorption trap (14) is connected with the common end of the receiving valve (3) through a pipeline, the NO end of the receiving valve (3) is connected with a waste liquid discharge pipeline, the other end of the waste liquid discharge pipeline is connected with a waste liquid collecting device, the NC end of the receiving valve (3) is connected with a receiving pipeline, and the tail end of the receiving pipeline is arranged in the receiving container (10);

but controllable temperature and weather sample support module include metal bath piece (11), air pump (12), temperature control device (13), it has the hole site of three adaptation receiving vessel (10) to open on metal bath piece (11), and is three the hole site is in proper order for receiving the position, weathers the position, derives the position, receive under the position department receiving pipeline, weathers under the trachea that the position is in air pump (12) and connects out, be provided with heating device in metal bath piece (11), heating device electric connection has temperature control device (13).

2. The on-site rapid enrichment, purification and blow-drying device for the target pollutants in the water environment according to claim 1, wherein the water sample storage tank (6) is a 1L or 2L high-density polyethylene bottle.

3. The on-site rapid enrichment, purification and blow-drying device for the target pollutants in the water environment as claimed in claim 1, wherein the first filter (4) is a sintered metal filter with a pore size of 10 microns.

4. The on-site rapid enrichment, purification and blow-drying device for the target pollutants in the water environment as claimed in claim 1, wherein the second filter (5) is a cellulose needle filter with a pore size of 0.46 μm.

5. The on-site rapid enrichment, purification and blow-drying device for the target pollutants in the aquatic environment as claimed in claim 1, wherein the heating device is a polyimide substrate electric heating sheet.