CN218098575U

CN218098575U - Water sample accelerated evaporation-acidification-concentration device

Info

Publication number: CN218098575U
Application number: CN202122704110.4U
Authority: CN
Inventors: 杨宝华
Original assignee: Beijing Kaiyuan Technology Co ltd
Current assignee: Beijing Zhizhi Heyi Technology Co ltd
Priority date: 2021-11-08
Filing date: 2021-11-08
Publication date: 2022-12-20
Anticipated expiration: 2031-11-08

Abstract

The patent of the utility model relates to an intelligence sample preparation field specifically discloses a water sample evaporation-acidification-enrichment facility with higher speed, adopt weighing transducer real time monitoring water sample to add, the quality change of process is cleared up with acidification to the heating evaporation, possess the automatic function of adding of ration, still possess the trace simultaneously and blow and accelerate evaporation function, the full automatization rapid preparation of bulky water sample has been realized, manual operation has been reduced, to heating temperature, add the water yield, the accurate control of add sour volume and blowing gas flow, to realize unmanned on duty automation mechanized operation in loaded down with trivial details experimentation in the past, make experiment precision and repeatability all improve greatly.

Description

Water sample accelerated evaporation-acidification-concentration device

Technical Field

The utility model belongs to intelligence sample preparation field, concretely relates to water sample evaporates with higher speed-acidification-enrichment facility.

Background

The water quality monitoring process usually involves a large volume of evaporation concentration process, in order to achieve the purpose of removing organic matters and sulfation in water, the concentrated water sample needs to be digested by adding sulfuric acid or nitric acid. The process requires that an operator needs to replace different vessels in the concentration process, the heating plate needs to accurately control the temperature and keep micro-boiling, water needs to be added manually for multiple times, and concentrated sulfuric acid or concentrated nitric acid needs to be added manually. For example, in the detection process of environmental industry standards HJ898-2017 and HJ899-2017 and a domestic drinking water detection standard GB 5750.13 on radioactive indexes in water, 1-5L of water sample needs to be kept slightly boiling and concentrated to 100mL, 1mL of concentrated sulfuric acid needs to be manually added for mild heating and digestion and acid dispelling, the whole process needs a laboratory technician to accurately adjust the temperature of a heating plate, wash a plurality of glassware, and finally concentrate the water sample into a 150mL porcelain evaporation dish. The sample preparation process consumes a large amount of labor and takes long time, evaporation capacity and residual water samples cannot be known in real time, once temperature control is inaccurate, bumping phenomenon is easy to occur, the sample preparation process is not accurate enough, and the accuracy of an experimental result is greatly reduced, so that sample preparation flux and efficiency of a large-volume water sample are severely restricted.

SUMMERY OF THE UTILITY MODEL

The utility model relates to a solve present evaporation process speed slow, do not have a great deal of weak points such as automatic acidification function, for the laboratory provides to have to accelerate evaporation, automatic acidification catch up with sour and accord with the evaporation concentration device that standard method required, for surface water, groundwater, industrial waste water, life drinking water in the radioactivity index, like total alpha, total beta's detection provides full automatization sample pretreatment equipment and method.

The technical scheme of the utility model as follows:

the device is characterized by comprising an automatic sample adding module, an automatic acid adding module, a heating weighing module and a blowing module, is used for the processes of automatic accelerated evaporation, acid adding, acid dispelling, concentration and the like of a large volume of water samples, and realizes the automation of the preparation process of radioactive index samples in the water samples.

The automatic sample adding module is composed of a water sample bottle (101), a sample introduction pump (102), a sample liquid level switch (103) and a sample tube end (104), all the components are connected through pipelines, and the sample liquid level switch (103) is close to the sample tube end (104).

The automatic acid adding module is composed of a reagent pump (201), an upper liquid level sensor (202), a coil pipe (203), a lower liquid level sensor (204), a three-way electromagnetic valve (205), a reagent bottle (206), a discharge valve (207), a reagent liquid level switch (208) and a reagent pipe end (209), all the components are connected in a sealing mode through acid and alkali resistant pipelines, and the reagent liquid level switch (103) is close to the sample pipe end (104).

The heating and weighing module consists of a weight sensor (301), a heat insulation layer (302), a heat transfer block (303), a heating and temperature sensing module (304), a ceramic evaporation dish (305), a straight arm (306) and a vertical column (307). The weight sensor (301) can measure the accurate mass of the added water sample and acid liquor, and can also measure the mass of the residual water sample in the evaporation process; the heat transfer block (303) is in close contact with the ceramic evaporation vessel (305), and the heating temperature sensing module provides a stable heat source to ensure the accurate control of the evaporation process.

The upright column (307) supports the straight arm (306), and each liquid pipeline and each gas pipeline are connected into the straight arm (306) through the upright column and are connected with each end head; the straight arm (306) is arranged above the porcelain evaporation dish (305), and the sample tube end (104), the reagent tube end (209) and the air passage end (403) are connected below the straight arm (306) through threads.

The air blowing module consists of a miniature air pump (401), a steady flow voltage stabilizer (402) and an air circuit end (403), all the components are connected by air circuit pipes, and the air blowing module provides 0.1-100mL/min of air flow for an evaporated water sample and can accelerate the evaporation speed of the water sample.

The water sample accelerated evaporation-acid addition-concentration device is characterized in that: the sample injection pump (102) can be a peristaltic pump, an injection pump or a diaphragm pump, and the outer diameter of a pipeline is 0.1-10mm; the sample level switch (103) may be capacitive or photorefractive, indicating the presence of liquid in the tube.

The reagent pump (201) can be an injection pump, a peristaltic pump or a diaphragm pump, and the outer diameter of the pipeline is 0.1-10mm; the upper level sensor (202) and the lower level sensor (204) may be capacitive or photorefractive, and may indicate the presence of liquid in the tube and whether the liquid level in the reagent bottle (206) has crossed the tubing. The volume in the tube between the two sensors is the volume of acid added each time, which is generally 1-5mL. The discharge valve (207) is a 1-12 unit discharge valve, and can be respectively used for adding acid into a 1-12 position ceramic evaporation pan. The reagent liquid level switch (208) can be of a capacitance induction type or a light refraction type, can indicate the existence of liquid in the pipe and judge whether the acid liquid enters the pipeline behind the valve. The end (209) of the reagent tube is in contact with the inner wall of the ceramic evaporation dish.

When the reagent pump (201) sucks and discharges acid, the acid solution only rises to the upper liquid level sensor (202), and the acid adding process only contacts with the acid and alkali resistant pipeline, the acid and alkali resistant three-way valve and the discharge valve and does not contact with the pump body. The flow rate of the reagent pump (201) during acid suction and discharge is 0.1-100ml/min.

The weight sensor (301) is positioned below the heat insulation layer (302) and is fixed by a non-heat-conducting screw; the heat transfer block (303) is also provided with a heat insulation layer; the heating temperature sensing module (304) can be controlled at 30-350 ℃, and the temperature can be accurately controlled in different heating stages through PID. The volume of the porcelain evaporation dish (305) is 100-300mL.

The distance between the end (403) of the gas path in the blowing module and the liquid level of the solution in the porcelain evaporation dish is 1-30mm.

The sample tube end (104), the reagent tube end (209), the gas circuit end (403), the straight arm (306) and the upright post (307) are all made of acid and alkali resistant materials, and can be but not limited to polytetrafluoroethylene, polyperfluoroethylene propylene and polypropylene.

The device can expand to 1-30 channels by adding the drain valve, can independently control temperature and measure weight of up to 30 ceramic evaporation vessels, has up to 30 air blowing paths, and realizes high-flux water sample rapid parallel evaporation acidification and concentration.

An air suction cover (501) is arranged above the whole device, so that water vapor and acid mist can be discharged in time, and the influence of the acid mist on equipment is reduced.

The automatic evaporation-concentration instrument sold on the market at present has no automatic acid adding function and no blowing function. The utility model discloses a show the effect and lie in:

(1) The utility model discloses a combination of pump, level sensor and many row valves can be for the automatic acidification of the porcelain evaporation ware of every passageway need not manual operation.

(2) The utility model discloses a miniature air pump to set up the air current port above the porcelain evaporation ware, for the porcelain evaporation ware of every passageway provides stable and suitable air current, the gas disturbance of water sample top among the evaporation process has accelerated the evaporation rate, has improved efficiency.

(3) The utility model takes the weight sensor as the core sensitive element, and can monitor the addition amount of the water sample and the evaporation capacity of the water sample in real time; meanwhile, the heating module can accurately control the temperature, realize the accurate control of the evaporation process of the large-volume water sample, automatically add the water sample, avoid the phenomena of bumping and the like, and save a large amount of labor.

(4) The utility model provides an every passageway all is independent accuse temperature and water sample addition system, does not interfere with each other between the passageway, avoids the cross contamination who produces with arm sharing water sample passageway, and the metal element who has also stopped the arm exposes in acid mist and the equipment that produces is fragile, not durable phenomenon.

Drawings

FIG. 1 is a schematic diagram of an intelligent water sample accelerated evaporation-acidification-concentration device

In the figure, 101-a water sample bottle, 102-a sample pump, 103-a sample liquid level switch and 104-a sample tube end, 201-a reagent pump, 202-an upper liquid level sensor, 203-a coil, 204-a lower liquid level sensor, 205-a three-way electromagnetic valve, 206-a reagent bottle, 207-a discharge valve, 208-a reagent liquid level switch and 209-a reagent tube end, 301-a weight sensor, 302-a heat insulation layer, 303-a heat transfer block, 304-a heating temperature sensing module, 305-a ceramic evaporation vessel, 306-a straight arm and 307-an upright post, 401-a micro air pump, 402-a steady flow voltage stabilizer, 403-an air path end and 501-an air suction cover.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.

A water sample accelerated evaporation-acid adding-concentration device comprises an automatic sample adding module, an automatic acid adding module, a heating and weighing module and an air blowing module. The automatic sample adding module adds a water sample into the ceramic evaporation vessel through the sample feeding pump, wherein the liquid level switch of the sample can sense the liquid level in the sample tube and indicate whether the water sample is correctly added into the sample tube. The automatic acid adding module is resistant to concentrated sulfuric acid and concentrated nitric acid integrally and is a control unit of acid liquor. The reagent pump can suck and discharge acid, the upper and lower liquid level sensors indicate liquid level change, the volume of acid liquid sucked into the pipe at each time can be determined, the three-way valve controls the directions of liquid suction and liquid discharge, and the discharge valve can control the corresponding channel added at each time. The heating and weighing module adopts a weight sensor as a weight sensing sensitive device in the steps of adding a water sample and evaporating in the experimental process, and monitors the quality of the water sample in the ceramic evaporating dish in real time; the weight sensor is positioned below the heat insulation layer and is fixed by a non-heat-conducting screw; a heat transfer block with a heat insulation layer is fixed above the heat insulation layer; the heating temperature sensing module accurately controls the temperature at different heating stages through PID. The air blowing module provides proper and stable air flow for the water sample in the ceramic evaporation vessel, so that the water sample is not blown, the air flow disturbance on the upper part during the evaporation of the water sample can be effectively improved, and the evaporation speed is accelerated.

When the automatic acid adding module absorbs acid liquor, the reagent pump and the middle pipeline are communicated to the reagent bottle through the three-way valve, the reagent pump extracts the acid liquor, the lower liquid level sensor indicates whether the acid liquor enters the coil pipe, and the upper liquid level sensor stops the reagent pump when the upper liquid level sensor measures the liquid level change of the acid liquor. When acid liquor is output, the three-way valve enables the pipeline and a common end (207-0) of the discharge valve to be connected, an output port of the discharge valve can be controlled to a corresponding ceramic evaporation pan (for example, the output port 207-1 is connected to the end of a reagent tube above the 1-channel ceramic evaporation pan), the reagent pump is started, the reagent pump is stopped until the lower liquid level sensor indicates that the liquid level in the tube changes, and the step of discharging the acid liquor between the upper liquid level sensor and the lower liquid level sensor into the evaporation pan is completed. The above process can be repeated for a plurality of times, and the addition of acid liquor with larger volume is realized. Because the acid solution only rises to the upper liquid level sensor and only contacts with the acid and alkali resistant pipeline, the acid and alkali resistant three-way valve and the drain valve, the contact of concentrated acid and the pump head is avoided, and the service life of the pump is prolonged. Wherein the reagent pump may be, but is not limited to, a syringe pump, a peristaltic pump, or a diaphragm pump.

Each functional module is controlled by a single chip microcomputer or a PLC or other MCUs, and different experimental operation steps are realized in the evaporation process in the sample preparation process. The specific operation process of the present patent is shown below by taking the sample preparation process in the radioactivity index total alpha and total beta detection process as an example.

1-preparation before operation of intelligent water sample accelerated evaporation-acid addition-concentration device

The sample tube is inserted under the liquid level of the water sample bottle, the sample tube is kept at the bottom, and the water sample in the water sample bottle is larger than the total volume to be evaporated. The sampling pump is started, the flow rate is 20ml/min, a water sample is pumped into the sample tube, the liquid level in the sample tube is monitored by the sample liquid level switch in real time, and the sampling pump is stopped when liquid is sensed.

The reagent pump is started to be in a liquid absorption state, concentrated sulfuric acid is sucked into the coil pipe at the flow rate of 0.5ml/min, and the reagent pump is stopped when the upper liquid level sensor indicates that the concentrated sulfuric acid exists. Then the reagent pump is changed into a liquid discharge mode, and concentrated sulfuric acid is pumped into the first channel pipeline at the flow rate of 1 ml/min. The above process is repeated for many times until the liquid level switch at the end of the reagent tube senses the liquid level change, and the reagent pump is stopped. The operation is repeated by switching the discharge valve to the reagent pipeline of a different channel.

The ceramic evaporation dish which is subjected to constant weight at 450 ℃ is placed in the heat transfer block, and the weight sensor measures the initial mass m0 and records the initial mass m0 by the single chip microcomputer.

At which point the device reaches a ready state.

2-Water sample addition

The sample pump was turned on and held at 5ml/min for T0 min, at which time the mass of the added water sample was measured by a weight sensor and was ml (m 0 was about 100 g). And (4) starting the blowing module, and stirring the water sample liquid level slightly by the air flow from the end of the air path to accelerate evaporation. The heating and temperature control system was turned on and the temperature was set at 105 ℃. The water sample keeps a micro-boiling state under the condition, the weight sensor measures the mass m2 of the water sample every 30s, when m1 is less than 50g, the sample injection pump is started again, T1 min is kept, the mass is measured every 1s by the weight sensor, and when the mass of the added water sample is more than 50g, the sample injection pump is stopped. The singlechip accumulatively records the mass of the added water sample and the mass of the evaporated water sample. This was repeated until the water sample mass had reached 1000g.

3-sulfation

When the concentrated water sample reaches the last 100g, the heating is stopped and the temperature sensor output temperature is waited to be less than 40 ℃. Then, the liquid was sucked and discharged by a reagent pump, and about 1mL of sulfuric acid was pumped into the ceramic evaporation dishes of the respective channels at a flow rate of 1 mL/min. The weight sensor can record the mass of the added concentrated sulfuric acid, so that the accurate volume of the added concentrated sulfuric acid is obtained. After waiting for 5min, the sulfuric acid is uniformly dispersed.

4-acidification heating

The sample was slowly heated and evaporated to dryness by setting the heating module at 120 ℃. And when the change rate of the measurement of the weight sensor is low, increasing the temperature of the heating module to 230 ℃, enabling the sulfuric acid to smoke, keeping for 5 minutes, changing the temperature of the heating module to 380 ℃, and performing final acid removal until the measurement value of the weight sensor is basically unchanged and the smoke is basically removed.

The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art without departing from the spirit of the present invention should fall within the scope of the present invention defined by the appended claims.

Claims

1. A water sample accelerated evaporation-acid adding-concentration device is characterized by comprising an automatic sample adding module, an automatic acid adding module, a heating weighing module and a blowing module, and is used for automatically accelerating evaporation, acid adding, acid removing and concentration processes of a large volume of water sample, so that automation of a preparation process of a radioactive index sample in the water sample is realized;

the automatic sample adding module consists of a water sample bottle (101), a sample feeding pump (102), a sample liquid level switch (103) and a sample tube end (104), all the components are connected by pipelines, and the sample liquid level switch (103) is close to the sample tube end (104);

the automatic acid adding module consists of a reagent pump (201), an upper liquid level sensor (202), a coil pipe (203), a lower liquid level sensor (204), a three-way electromagnetic valve (205), a reagent bottle (206), a discharge valve (207), a reagent liquid level switch (208) and a reagent pipe end (209), and all the components are hermetically connected by acid and alkali resistant pipelines;

the heating and weighing module consists of a weight sensor (301), a heat insulation layer (302), a heat transfer block (303), a heating and temperature sensing module (304), a ceramic evaporation vessel (305), a straight arm (306) and a vertical column (307); the weight sensor (301) can measure the accurate mass of the added water sample and acid liquor, and can also measure the mass of the residual water sample in the evaporation process; the heat transfer block (303) is in close contact with the ceramic evaporation vessel (305), and the heating temperature sensing module provides a stable heat source to ensure the accurate control of the evaporation process;

the upright column (307) supports the straight arm (306), and each liquid pipeline and each gas pipeline are connected into the straight arm (306) through the upright column and are connected with each end head; the straight arm (306) is arranged above the ceramic evaporation dish (305), and the sample tube end (104), the reagent tube end (209) and the air circuit end (403) are connected below the straight arm (306);

the air blowing module consists of a miniature air pump (401), a steady flow voltage stabilizer (402) and an air circuit end (403), and all the parts are connected by air circuit pipes to provide 0.1-100mL/min of air flow for an evaporated water sample.

2. The water sample accelerated evaporation-acidification-concentration device as claimed in claim 1, wherein: the sample feeding pump (102) can be a peristaltic pump, an injection pump or a diaphragm pump, and the outer diameter of the pipeline is 0.1-10mm; the sample level switch (103) may be capacitive or photorefractive, indicating the presence of liquid in the tube.

3. The water sample accelerated evaporation-acidification-concentration device as claimed in claim 1, wherein: the reagent pump (201) can be an injection pump, a peristaltic pump or a diaphragm pump, and the outer diameter of the pipeline is 0.1-10mm; the upper liquid level sensor (202) and the lower liquid level sensor (204) can be of a capacitance induction type or a light refraction type and can indicate the existence of liquid in the pipe and whether the reagent pump sucks acid liquid or not; the volume in the tube between the two sensors is the volume of acid liquor added each time, and is generally 1-5mL; the discharge valve (207) is a 1-12 unit discharge valve, and can be used for adding acid into a 1-12 position ceramic evaporation pan respectively; the reagent liquid level switch (208) can be of a capacitance induction type or a light refraction type, can indicate the existence of liquid in the pipe and judge whether acid liquor enters the pipeline behind the valve; the end (209) of the reagent tube is contacted with the inner wall of the ceramic evaporation dish; the flow rate of the reagent pump (201) during acid suction and discharge is 0.1-100ml/min.

4. An accelerated evaporation-acidification-concentration device for water sample as claimed in claim 1, wherein: the weight sensor (301) is positioned below the heat insulation layer (302) and is fixed through a non-heat-conducting screw; a heat transfer block with a heat insulation layer is fixed above the heat insulation layer; the temperature of the heating temperature sensing module (304) can be controlled to be 30-400 ℃, and the temperature can be accurately controlled in different heating stages through PID; the volume of the porcelain evaporation dish (305) is 100-300mL.

5. The water sample accelerated evaporation-acidification-concentration device as claimed in claim 1, wherein: the distance between the end (403) of the gas path in the blowing module and the liquid level of the solution in the porcelain evaporation dish is 1-30mm.

6. The water sample evaporation-acidification-concentration device as claimed in claim 1, wherein the sample tube end (104), the reagent tube end (209), the gas path end (403), the straight arm (306) and the upright column (307) are made of acid and alkali resistant materials.

7. The water sample accelerated evaporation-acidification-concentration device as claimed in claim 1, wherein the device can be expanded to 1-30 channels, can control temperature and measure weight independently for up to 30 ceramic evaporation vessels, and has up to 30 air blowing paths to realize high-flux water sample rapid parallel evaporation acidification concentration.

8. An apparatus for accelerating evaporation-acidification-concentration of water sample according to claim 1, wherein the whole apparatus has a suction hood (501) above it.