CN111474037A - Sample concentration device, use method and application - Google Patents
Sample concentration device, use method and application Download PDFInfo
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- CN111474037A CN111474037A CN202010330243.7A CN202010330243A CN111474037A CN 111474037 A CN111474037 A CN 111474037A CN 202010330243 A CN202010330243 A CN 202010330243A CN 111474037 A CN111474037 A CN 111474037A
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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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
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a sample concentration device, a use method and application thereof, comprising an air drying tank, a sample area, a vacuum pump area and a cold well area which are connected in series in sequence; the air inlet of the air drying tank is connected with an air inlet pipe provided with a one-way air valve a; the sample area is provided with a sample tube bracket, a heating module, a vacuum degree sensor and a volatile organic compound sensor a; the vacuum pump area is provided with a vacuum pump, and the vacuum pump is connected with the sample area through a pipeline provided with a one-way air valve c; set up cold trap, recovery jar, outlet duct and volatile organic compounds sensor b in the cold trap region, the cold trap includes the TEC refrigeration piece in condenser pipe and the condenser pipe outside, and the vacuum pump other end is connected to condenser pipe one end and is retrieved the jar, retrieves jar connection and is provided with one-way pneumatic valve b's outlet duct. The invention has simple structure, convenient operation, real-time monitoring and high automation degree; the system suitable for concentration is wide and has large flux; and inert gas is not required to be additionally configured, so that the mixture solvents are respectively recovered, and cross infection is avoided in the concentration process.
Description
Technical Field
The invention belongs to the technical field of sample test pretreatment, and particularly relates to a sample concentrating device convenient to operate, a using method and application.
Background
The method has the advantages of simple and convenient operation, large flux, suitability for concentration of a 5-50m L sample system, particularly simultaneous treatment of a plurality of samples, greatly shortened detection time, wide application in pesticide residue detection, batch treatment of samples in pharmaceutical industry and general research, and the like, wherein the nitrogen blowing instrument is divided into a water bath nitrogen blowing instrument and a metal bath nitrogen blowing instrument, wherein the water bath nitrogen blowing instrument has a heating temperature range from room temperature to 100 ℃, the water bath heating mode has milder heating and more uniform heating, the heating temperature range of the metal bath nitrogen blowing instrument is from room temperature to 150 ℃, the defect that the two nitrogen blowing instruments need inert gas to blow heating sample liquid, are unsuitable for a trace system and a general system of samples, are not suitable for discharge of organic reagents, ensure that the heating temperature range is from room temperature to 150 ℃, the defect that the two nitrogen blowing instruments need inert gas to blow the heating temperature range, and the defect that the samples can not be subjected to vacuum evaporation and concentration by a vacuum evaporation and concentration under the condition that the temperature of the sample is reduced, the temperature of the sample is not suitable for a vacuum evaporation and the concentration of the sample, the sample can be collected by a centrifugal evaporation and the vacuum, the temperature of the sample can not reduced, the sample can be collected by a centrifugal evaporation and the vacuum evaporation and the concentration of the sample can be reduced by a centrifugal evaporation process of a centrifugal vacuum.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a sample concentration device, a use method and application, the structure is simple, the operation is convenient, the system suitable for concentration is wide, no additional inert gas is required to be prepared, the emission of organic waste gas is avoided, the respective recovery of mixture solvents can be realized, and no cross infection exists in the concentration process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a sample concentration device is characterized by comprising an air drying tank, a sample area, a vacuum pump area and a cold well area which are sequentially connected in series; an air inlet of the air drying tank is connected with an air inlet pipe provided with a one-way air valve a; the sample area is provided with a sample tube bracket, a heating module, a vacuum degree sensor and a volatile organic compound sensor a; the vacuum pump area is provided with a vacuum pump, and the vacuum pump is connected with the sample area through a pipeline provided with a one-way air valve c; a cold trap, a recovery tank, an air outlet pipe and a volatile organic compound sensor b are arranged in the cold trap region, the cold trap comprises a condensation pipe and a TEC refrigeration piece outside the condensation pipe, the TEC refrigeration piece is connected with a temperature control system, one end of the condensation pipe is connected with a vacuum pump, the other end of the condensation pipe is connected with the recovery tank, and the recovery tank is connected with the air outlet pipe provided with a one-way air valve b; the air drying tank, the sample area, the vacuum pump area, the cold trap area, the one-way air valve a, the one-way air valve b and the one-way air valve c are connected with an upper computer controller, and the upper computer controller is further connected with a power management board.
In a specific embodiment of the invention, at least one group of cold traps and recovery tanks are arranged, when the number of the groups of the cold traps and the recovery tanks is more than or equal to 2, the cold traps are connected in sequence with a condenser pipe, a recovery tank, a condenser pipe and a recovery tank, the last recovery tank is connected with an air outlet pipe provided with a single-phase air valve b, and a volatile organic compound sensor b is arranged in the last cold trap; for example, the first cold trap comprises a condensation pipe a, a TEC refrigeration piece a and a recovery tank a, the second cold trap comprises a condensation pipe b, a TEC refrigeration piece b, a recovery tank b and a volatile organic compound sensor b, when the two cold traps are connected, one end of the condensation pipe a is connected with an outlet of a vacuum pump, the other end of the condensation pipe a penetrates through the first cold trap and is introduced into the recovery tank a, one end of the condensation pipe b is connected with the recovery tank a, and the other end of the condensation pipe b penetrates through the second cold trap and is introduced into the recovery tank b; the recovery tank b is connected with an air outlet pipe, and a one-way air valve b is arranged on the air outlet pipe; the volatile organic compound sensor b is arranged in the second cold trap.
In a particular embodiment of the invention, the condenser tube is helical or serpentine.
In a specific embodiment of the invention, the heating module is a constant-temperature metal bath, the heating module is matched with the specification of the sample tube in the sample tube bracket, the specification of the sample tube is 0.1 ml-1L, and the outer surface of the sample tube is provided with a polytetrafluoroethylene tube sleeve.
In a specific embodiment of the present invention, the sample tube holder comprises 12 sample tube well locations.
In a specific embodiment of the invention, the upper computer controller is an industrial control screen with an internal android system.
In a specific embodiment of the present invention, the sample concentrating device further includes a bottom plate and a box, the sample region, the vacuum pump region and the cold trap region are disposed on a base in the box, and the sample region, the vacuum pump region and the cold trap region are separated by a partition plate; the upper computer controller is arranged on the box body.
Another aspect of the present invention is to provide a method for using a sample concentrating device, which is characterized by comprising the following steps:
1) setting the temperature of a constant-temperature metal bath and the temperature of a cold trap area according to the type of the recovered sample and the type of the organic reagent in the concentration tube;
2) when the constant temperature metal bath and the cold trap region reach the set temperature, the volatile organic compound sensor a and the volatile organic compound sensor b are monitored;
3) after the numerical values of the volatile organic compound sensor a and the volatile organic compound sensor b are reduced to a certain numerical value, opening a one-way air valve c;
4) after the vacuum degree sensor returns to a certain value, the one-way air valves a, b and c are closed, and the constant-temperature metal bath and the cold trap area are closed;
5) taking out the concentration pipe and the recovery tank.
The invention also aims to provide application of the sample concentrating device in sample pretreatment of food safety detection, forensic material evidence identification and toxicology analysis.
Compared with the prior art, the invention has the beneficial effects that: a sample concentration device, compared to a conventional structure: a one-way air valve a is arranged on an air inlet pipe connected with the air drying tank to ensure that the sucked air has no water vapor; a one-way air valve b is arranged on an air outlet pipe connected with the recovery tank b, and the air outlet pipe extends out of the box body; ensuring the unidirectional flow of the gas; the heating module is set as a constant-temperature metal bath, and the temperature control is reliable; the heating module is matched with the specification of a sample tube in the sample tube bracket; the sample tube bracket can be replaced according to the specification of the sample tube to support the sample tubes with different volumes; a vacuum degree sensor is arranged at the upper end of the front side plate of the sample area; the real-time transmission of air pressure test data to an industrial control screen is realized, and the concentration progress is controlled; the lower end of the right side plate of the sample area is provided with a volatile organic compound sensor a; the real-time transmission of the test data of the gaseous organic matters to an industrial control screen is realized, and the concentration progress is controlled; the vacuum pump is arranged in the vacuum pump area, so that the sample area can be under negative pressure, the boiling point of the solvent is reduced, and the organic solvent is rapidly evaporated at normal temperature; the sample area and the vacuum pump area are provided with one-way air valves c, so that the one-way flow of organic solvent steam is ensured; the cold trap region is provided with a cold trap and a TEC refrigeration piece, one end of the condensation pipe is connected to the outlet of the vacuum pump, and the other end of the condensation pipe penetrates through the cold trap and is inserted into the recovery tank; different kinds of organic solvents can be respectively condensed into different recovery tanks by setting different temperatures for the TEC refrigeration sheets; the lower end of the left side plate of the second cold well region is provided with a volatile organic compound sensor b; the real-time transmission of the test data of the gaseous organic matters to an industrial control screen is realized, and the concentration progress is controlled; the invention has simple structure, reliable connection and convenient operation; the system can be monitored in real time, and has high automation degree; the concentration is suitable for wide system and large flux; no additional inert gas is needed to be configured, and the emission of organic waste gas is avoided; the solvent of the mixture can be respectively recovered; no cross infection is caused in the concentration process; greatly improves the concentration efficiency and reduces the cost.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a perspective view of the external structure of the present invention.
Fig. 2 is a perspective view of the internal structure of the present invention.
FIG. 3 is a simplified schematic of the present invention.
In the figure: 1-android industrial control screen 2-box 3-sample zone 4-vacuum pump zone 5-first cold well zone 6-second cold well zone 7-air drying tank 8-one-way air valve a 9-one-way air valve b 10-one-way air valve c 11-sample tube 12-sample tube support 13-recovery tank a 14-recovery tank b 15-heating module 16-vacuum pump 17-first cold well 18-second cold well 19-volatile organic compound sensor a 20-volatile organic compound sensor b 21-vacuum degree sensor 22-TEC refrigeration piece 24-condenser tube a 25-condenser tube b.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it is obvious that the described embodiments are some, not all embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of describing the invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the invention.
In the description of the invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.
As shown in fig. 1 to 3, a sample concentration device comprises a box body, wherein an android industrial control screen 1 is arranged above the box body 2; four areas, namely a sample area 3, a vacuum pump area 4, a first cold well area 5 and a second cold well area 6 are arranged in the box body 2 through partition plates, the sample area, the vacuum pump area, the first cold well area and the second cold well area are communicated in series, and gas can only flow in one direction; an air drying tank 7 is arranged on the left side of the box body 2, and a one-way air valve a8 is arranged on an air inlet pipe connected with the air drying tank 7; the sample area 3 is provided with a heating module 15, and a sample tube bracket 12 is arranged on the heating module 15; a vacuum degree sensor 21 is arranged at the upper end of the front side plate of the sample area 3; the lower end of the right side plate of the sample area 3 is provided with a volatile organic compound sensor a 19; the vacuum pump area 4 is provided with a vacuum pump 16, and the vacuum pump 16 is connected with the first cold well area 5 and the second cold well area 6 through pipelines; a one-way air valve c10 is arranged between the sample area 3 and the vacuum pump area 4; the first cold trap region 5 is provided with a first cold trap 17 and a recovery tank a13, the second cold trap region 6 is provided with a second cold trap 18 and a recovery tank b14, and the lower end of the left side plate of the second cold trap region 6 is provided with a volatile organic compound sensor b 20; the air outlet pipe connected with the recovery tank b14 is provided with a one-way air valve b9, and the air outlet pipe extends out of the box body 2. The air drying tank, the sample area, the vacuum pump area, the cold well area, the one-way air valve a, the one-way air valve b and the one-way air valve c are connected with the industrial control screen, and the industrial control screen is further connected with the power management board.
The TEC refrigeration pieces 22 are arranged outside the first cold trap 17 and the second cold trap 18, one end of a condensation pipe a24 is connected with an outlet of the vacuum pump 16, the other end of the condensation pipe a24 penetrates through the first cold trap 17 and is led into the recovery tank a13, one end of a condensation pipe b25 is connected with the recovery tank a13, the other end of the condensation pipe b25 penetrates through the second cold trap 18 and is led into the recovery tank b14, the condensation pipe a24 and the condensation pipe b25 which are arranged inside the first cold trap 17 and the second cold trap 18 are both arranged in a spiral shape, the sample area 3, the vacuum pump area 4, the first cold trap area 5 and the second cold trap area 6 are arranged in series, the sample pipe support 12 comprises 12 sample pipe hole positions, the constant-temperature metal bath is arranged, the heating module is matched with the specifications of the sample pipes in the sample pipe support, the specification of the sample pipes 11 is set to be 0.1 ml-1L, and.
In the specific implementation, a one-way air valve a and a one-way valve b are installed outside an instrument box body, the one-way air valves can guarantee one-way flow of air, the one-way air valve a is installed on an air inlet pipe connected with an air drying tank and guarantees that water vapor does not exist in air sucked into a sample area, the one-way air valve b is installed at an air outlet, opening and closing of the one-way air valve a and the one-way air valve b are controlled by an industrial control screen, a constant-temperature metal bath is placed in the sample area, the temperature of the constant-temperature metal bath is controlled by a power management board, a sample tube support is installed in the constant-temperature metal bath and can be replaced according to the specification of the sample tube, the sample tube support supports 1.5m L, 5m L, 10m L and 50m L and other sample tubes with different volumes, a set of vacuum degree sensors is installed in the sample area, air pressure test data are transmitted into the industrial control screen in real time to control the concentration progress, a volatile organic matter concentration detection device of the sample area, gaseous organic matter test data are transmitted into the industrial control screen in real time, a set of a high-power vacuum pump, a set of high-power vacuum pump is installed, the high-power vacuum pump can enable the sample area to be under-pressure test, the sample area to enable the ready negative pressure test data to be rapidly transmitted to be transmitted to enable the sample area, the organic matter to be rapidly transmitted to be transmitted into a refrigeration trap, two sets of a refrigeration trap, the refrigeration system, the refrigeration trap, the refrigeration system, the refrigeration trap is connected with a TEC, the refrigeration system, the refrigeration trap, the refrigeration system, the refrigeration trap is connected with two sets of.
The using method comprises the following steps: firstly, setting the temperatures of a constant-temperature metal bath, a first cold well region and a second cold well region according to the types of sample recovery and the types of organic reagents in a concentration tube; when the constant temperature metal bath, the first cold trap region and the second cold trap region reach the set temperature, the volatile organic compound sensor a and the volatile organic compound sensor b are monitored; after the numerical values of the two groups of TVOC sensors are reduced to a certain numerical value, opening a one-way air valve c; after the vacuum degree sensor returns to a certain numerical value, closing the one-way air valve a, the one-way air valve b and the one-way air valve c, and closing the constant-temperature metal bath, the TEC refrigeration sheets of the first cold well region and the second cold well region; and taking out the concentration pipe and the recovery tank to finish the operation of sample concentration.
The sample concentration device has high flux and can accommodate 1 to 12 samples for simultaneous concentration; the automation degree is high, and the concentration process can be monitored; no additional inert gas is needed to be configured; the sample does not need to be transferred after the concentration is finished; the device has no organic waste gas emission, is suitable for various laboratory environments, and is particularly suitable for laboratories without a fume hood; the mixture solvent can not be recovered respectively; the concentration process has no cross contamination; simple operation, and is provided with a plurality of sample processing methods and one-key operated sample concentration equipment.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A sample concentration device, characterized by: comprises an air drying tank, a sample area, a vacuum pump area and a cold well area which are connected in series in sequence; an air inlet of the air drying tank is connected with an air inlet pipe provided with a one-way air valve a; the sample area is provided with a sample tube bracket, a heating module, a vacuum degree sensor and a volatile organic compound sensor a; the vacuum pump area is provided with a vacuum pump, and the vacuum pump is connected with the sample area through a pipeline provided with a one-way air valve c; a cold trap, a recovery tank, an air outlet pipe and a volatile organic compound sensor b are arranged in the cold trap region, the cold trap comprises a condensation pipe and a TEC refrigeration piece outside the condensation pipe, the TEC refrigeration piece is connected with a temperature control system, one end of the condensation pipe is connected with a vacuum pump, the other end of the condensation pipe is connected with the recovery tank, and the recovery tank is connected with the air outlet pipe provided with a one-way air valve b; the air drying tank, the sample area, the vacuum pump area, the cold trap area, the one-way air valve a, the one-way air valve b and the one-way air valve c are connected with an upper computer controller, and the upper computer controller is further connected with a power management board.
2. The sample concentrating device according to claim 1, wherein: the cold traps and the recovery tanks are at least provided with one group, when the number of the cold traps and the recovery tanks is more than or equal to 2, the cold traps are connected with each other according to the sequence of the condenser pipe, the recovery tanks, the condenser pipe and the recovery tanks, the last recovery tank is connected with the air outlet pipe provided with the single-phase air valve b, and the last cold trap is internally provided with the volatile organic compound sensor b.
3. A sample concentrating device according to claim 1 or 2, wherein: the condensation pipe is spiral or serpentine.
4. The sample concentrating device according to claim 1, wherein the heating module is a constant temperature metal bath, the heating module is matched with the specification of the sample tube in the sample tube bracket, the specification of the sample tube is 0.1 ml-1L, and the outer surface of the sample tube is provided with a polytetrafluoroethylene tube sleeve.
5. The sample concentrating device according to claim 1, wherein: the sample tube support comprises 12 sample tube hole sites.
6. The sample concentrating device according to claim 1, wherein: the upper computer controller is an industrial control screen with an internal android system.
7. The sample concentrating device according to claim 1, wherein: the sample concentrating device also comprises a bottom plate and a box body, wherein the sample area, the vacuum pump area and the cold trap area are arranged on the base in the box body, and are separated by a partition plate; the upper computer controller is arranged on the box body.
8. A method of using a sample concentration device, comprising the steps of:
1) setting the temperature of a constant-temperature metal bath and the temperature of a cold trap area according to the type of the recovered sample and the type of the organic reagent in the concentration tube;
2) when the constant temperature metal bath and the cold trap region reach the set temperature, the volatile organic compound sensor a and the volatile organic compound sensor b are monitored;
3) after the numerical values of the volatile organic compound sensor a and the volatile organic compound sensor b are reduced to a certain numerical value, opening a one-way air valve c;
4) after the vacuum degree sensor returns to a certain value, the one-way air valves a, b and c are closed, and the constant-temperature metal bath and the cold trap area are closed;
5) taking out the concentration pipe and the recovery tank.
9. Use of a sample concentration device according to any one of claims 1 to 7 for sample pre-treatment in food safety testing, forensic physical evidence identification, toxicology analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010330243.7A CN111474037A (en) | 2020-04-24 | 2020-04-24 | Sample concentration device, use method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010330243.7A CN111474037A (en) | 2020-04-24 | 2020-04-24 | Sample concentration device, use method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111474037A true CN111474037A (en) | 2020-07-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010330243.7A Pending CN111474037A (en) | 2020-04-24 | 2020-04-24 | Sample concentration device, use method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111474037A (en) |
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2020
- 2020-04-24 CN CN202010330243.7A patent/CN111474037A/en active Pending
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