JP2009098064A - Automatic concentration apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To solve the problem that a sample concentrating operation and a series of related operations necessary for a residual pesticide test and the like remain unautomated. <P>SOLUTION: An automatic concentration apparatus is proposed, in which a column 1, a sample vessel 2 and a solvent vessel 3 are arranged in a one-dimensional direction, and a dispensing needle 5 is configured to be movable above them and movable up and down in the vertical direction, and a waste liquid vessel 8 and a concentration-use warming device 7 to which a concentrating vessel 6 is attached, are configured to be movable below an arrangement including the column, and the connection head 10 of a pressure reduction system, which can contact with the upper aperture of the concentrating vessel, is configured to be movable and to be able to move up and down. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an automatic concentration apparatus for automating a work for concentrating a substance to be examined in a solvent extracted from a sample such as food with a solvent and a series of work related thereto.

  In recent years, the introduction of the so-called positive list system has expanded the scope of inspection of residual agricultural chemicals in foods, and therefore it is desired to perform inspections for a large number of agricultural chemicals efficiently and in a short period of time.

  Residual pesticide residue inspection is conducted according to procedures prescribed in official test methods such as “Simultaneous testing method for agricultural chemicals by GC / MS (agricultural products)” and “Simultaneous testing method for agricultural chemicals by LC / MS (agricultural products)”. Is called. In this test method, in the process of preparing a test solution as a pretreatment for inspection using a gas chromatograph / mass spectrometer (GC-MS), liquid chromatograph / mass spectrometer (LC-MS), etc. Automation is difficult because it requires detailed work. In particular, it is difficult to automate the concentration work and a series of work related to each of the work in the preparation process of the test solution. Conventionally, the work is generally performed manually. .

  On the other hand, as an apparatus for automatically performing the concentration work itself, for example, an automatic concentration apparatus as disclosed in Patent Document 1 and Patent Document 2 has been proposed.

  Patent Document 1 relates to an automatic concentration apparatus that performs a concentration process by introducing a gas into a concentration container. A gas introduction pipe and a gas discharge pipe are provided on an upper part of a concentration container filled with a solution to be concentrated inside, and concentration is performed. A liquid level sensor that detects the amount of solution is provided at the bottom of the container. Based on the amount of solution detected by the liquid level sensor, the solenoid valve is driven and controlled when the amount of solution in the concentration container falls below a predetermined level. And a concentration control device that prohibits the introduction of gas into the concentration container.

In addition, the automatic concentration apparatus of Patent Document 2 supports a concentration container such as a round bottom flask filled with a liquid to be concentrated in a heat medium bath such as a water bath so as to be rotatable by a support tool, and at the opening of the concentration container. A pipe for supplying the liquid to be concentrated is connected, and a supply control means for controlling the supply is provided, and further, a weight measuring means such as a load cell for measuring the total weight including the heat medium bath is provided. When the weight of the liquid to be concentrated in the container is out of a predetermined range, automatically adjusting the amount of liquid to be concentrated to the container so that the weight of the liquid to be concentrated in the container is within the predetermined range. Concentration work.
Japanese Patent Laid-Open No. 6-18512 JP-A-11-156101

  The automatic concentrators of Patent Document 1 and Patent Document 2 listed above are intended to automate the concentration operation after filling the liquid to be concentrated in the concentration container, and a series of operations before and after the concentration operation, for example, Automation of operations such as preparation of the liquid to be concentrated and injection into the concentration container is not envisaged.

  In the present invention, one of the objects is to automate a concentration operation and a series of operations related thereto.

  On the other hand, in order to automate the concentration operation, it is necessary to stop the concentration operation when the remaining amount of the liquid in the concentration container reaches a predetermined amount, which is also shown in Patent Document 1 and Patent Document 2 described above. As described above, a liquid level sensor for detecting the amount of residual liquid in the concentration container is required.

  In general, there are two types of liquid level sensors: contact type and non-contact type. However, the contact type has a problem in handling such as contamination, so the non-contact type is used as the concentration device. Non-contact type general liquid level sensors include electrostatic capacity type and optical type sensors.

  In the residual agricultural chemical inspection as described above, since residual agricultural chemicals are collected from a sample in which food is mixed with a solvent, crystallized salt or the like adheres to the inner wall of the concentration container when the concentration progresses in the concentration operation. In addition, the manner of attachment varies depending on the difference of samples.

  For this reason, in the case of an optical sensor, light is scattered or blocked by adhering salt, etc., and the remaining liquid amount cannot be detected satisfactorily. In the case of a capacitive sensor, the adhering salt, etc. May be erroneously detected as the liquid level of the remaining liquid.

  In the present invention, in the concentration operation, the amount of residual liquid in the concentration container can be detected satisfactorily without being affected by the type of sample, and therefore automatically when the residual liquid amount reaches a predetermined amount. One of the purposes is to make it possible to stop the concentration accurately.

  In the present invention, in order to solve the above-described problem, the column, the sample container, and the solvent container are arranged in a one-dimensional direction, and the dispensing needle can be moved in the one-dimensional direction above the arrangement, In addition, it can be moved up and down in the vertical direction, and below the arrangement including the column, the concentrating heating device for mounting the concentration container and the waste liquid container support device for mounting the waste liquid container can be moved in the one-dimensional direction. Further, an automatic concentrator configured to be able to move in the one-dimensional direction and move up and down the connection head of the decompression system capable of contacting the upper opening of the concentrating container above the concentrating heating device. Propose.

  Further, the present invention proposes a configuration in which the condenser and the condensate container are provided in the decompression system, and the liquid level sensor is provided in the condensate container in the automatic concentrator.

  Further, the present invention proposes a configuration in which vibration generating means is provided in the concentrating warming device in the automatic concentrating device. In addition, it is proposed that this vibration generating means is configured as a moving means of the concentrating warming device.

  Further, the present invention proposes a configuration in which in the automatic concentrator, the connection head is connected to a purge gas supply system that can be branched and switched from the decompression system.

  Further, the present invention proposes a configuration in which a needle cleaning / drying unit is provided in an arrangement including a column in the automatic concentrator.

  The present invention also proposes a configuration in which a plurality of columns are arranged in the automatic concentrator, and include a dehydration column and a deoiling column.

  In the present invention, it is proposed that the automatic concentrating device has a configuration in which the dispensing needle includes a plurality of needles, and a part of the needle has a shower hole.

  Further, the present invention proposes a configuration in which a plurality of heating devices for concentration are arranged in the automatic concentrator.

  In the present invention, the dispensing needle is configured to be movable in the one-dimensional direction above and below the column, sample container, and solvent container arranged in the one-dimensional direction, and can be moved up and down. Since the concentrating heating device and the waste liquid container support device to which the waste liquid container is mounted are configured to be movable in the one-dimensional direction, the work of feeding the sample in the sample container and the solvent in the solvent container to the column Automating a series of operations such as sending the liquid that has passed through the column to a predetermined concentration container or waste liquid container, and related column conditioning, washing of the dispensing needle by the needle washing and drying unit, and drying be able to.

  After the liquid passing through the column is sent to the concentration container in this way, the connection head is brought into contact with the concentration container, and the concentration heating operation and the decompression system are operated to automatically perform the concentration operation.

  Therefore, even when the test solution preparation method in pesticide residue inspection is executed, there are a lot of fine work and when it is necessary to use a solvent that affects the human body, such as acetonitrile or toluene. Thus, the concentration operation and a series of operations related thereto can be performed safely.

  In the present invention, with respect to the column, sample container, and solvent container arranged in a one-dimensional direction, the concentrating heating device for mounting the concentration container below and the waste liquid container support device for mounting the waste liquid container are the above-mentioned one-dimensional direction. Therefore, an appropriate number of columns, concentration containers, and the like can be arranged, and an efficient concentration operation can be performed.

  If a condenser and a condensate container are provided in the decompression system, and a liquid level sensor is provided in the condensate container, the residual liquid amount in the concentration container can be obtained from the liquid level of the condensate container detected by the liquid level sensor. it can. Since no sample or salt adheres to the inner wall of the condensate container, the liquid level can be accurately detected by an appropriate liquid level sensor.

  Therefore, it is possible to detect that the amount of the remaining liquid in the concentrating container has reached a predetermined amount from the liquid level of the condensate container detected by the liquid level sensor, and to automatically stop the concentration operation.

  As in the case of the column and the concentration container, an efficient concentration operation can be performed by configuring a plurality of elements of the decompression system including the connection head.

  By providing vibration generating means in the concentrating warming device and applying vibration to the concentration container, evaporation of the solvent can be promoted to perform the concentration operation efficiently. This vibration generating means can be provided in the concentrating warmer or in the moving means.

  By connecting the connecting head to a switchable purge gas supply system that branches off from the decompression system, the purge operation is performed from the decompression system concentration in a state where the decompression system is operated. It is possible to switch to the gas purge method concentration in the above state.

  As a method for evaporating the solvent quickly in the concentration, a decompression method, a heating method, a stirring method, and a gas purge method are generally used. Of these, a decompression method having the highest speed is often used in the concentrator.

  However, since a very small amount of pesticide must be detected from the sample in the residual pesticide test, if the evaporation rate is too fast in all the concentration steps, the pesticide itself may be evaporated together.

  On the other hand, as described above, the pressure reduction method is initially concentrated in a state where the pressure reduction system is operated, and then the gas purge method in the state where the purge gas supply system is operated when the remaining liquid amount reaches a predetermined amount. By performing concentration by switching, the time required for concentration can be shortened without evaporating a trace amount of substance to be detected.

Next, embodiments of the present invention will be described with reference to the accompanying drawings.
FIG. 1 shows the overall configuration of an automatic concentrator according to the present invention. Reference numeral 1 denotes a column, 2 denotes a sample container, 3 denotes a solvent container, and 4 denotes a needle washing / drying unit. They are arranged in a one-dimensional direction L indicated by a chain line.

  This embodiment corresponds to the test solution adjustment method in the residual agricultural chemical inspection described above, and the column 1 is for deoiling in which a dehydrating column 1a containing anhydrous sodium sulfate and graphite carbon and aminopropyl silica gel are laminated. Column 1b. The solvent container 3 is composed of a solvent container 3a containing acetonitrile and a solvent container 3b containing a solvent in which acetonitrile and toluene are mixed at a ratio of 3: 1. Furthermore, the needle cleaning / drying unit includes a needle cleaning unit 4a using a cleaning liquid and a needle drying unit 4b using an air blow.

  The dispensing needle 5 can be moved in the one-dimensional direction L above the one-dimensional arrangement of the columns 1a, 1b, the sample container 2, the solvent containers 3a, 3b and the needle washing / drying units 4a, 4b. And is configured to be able to move up and down. The moving direction is indicated by a one-dot chain line as in the one-dimensional direction L, and the ascending / descending direction is indicated by a two-dot chain line. Hereinafter, similarly, the one-dimensional direction is indicated by a one-dot chain line, and the vertical direction is indicated by a two-dot chain line.

  In this embodiment, the dispensing needle 5 is composed of a dispensing needle 5a having an opening at the lower end and a shower needle 5b having an opening around the lower portion, and can be independently moved in the one-dimensional direction L. And is configured to be movable up and down in the vertical direction. Note that the dispensing needle 5a and the shower needle 5b can be configured to be movable together with respect to the movement in the one-dimensional direction L.

  Next, the concentrating heating device 7 to which the concentrating container 6 is attached below the one-dimensional arrangement of the columns 1a and 1b, the sample container 2, the solvent containers 3a and 3b, and the needle washing and drying units 4a and 4b. The waste liquid container support device 9 for mounting the waste liquid container 8 is configured to be movable in the one-dimensional direction L.

  In this embodiment, there are two concentrating heating devices 7 (7a, 7b), and therefore, two concentrating containers 6a, 6b are mounted on them. On the other hand, one waste liquid container support device 9 is configured, and therefore one waste liquid container 8 is mounted. These concentrating warming devices 7a and 7b and the waste liquid container support device 9 can be configured to be movable independently of each other, or can be configured to be movable together. Reference symbol R indicates a trajectory along which the heating and concentrating devices 7a and 7b and the waste liquid container supporting device 9 move.

  Although not shown here, the concentrating warming devices 7a and 7b, or their moving mechanisms are provided with vibration generating means for vibrating the attached concentrating containers 6a and 6b. In this embodiment, the vibration generating means applies the vibration in the one-dimensional direction L to the concentrating containers 6a and 6b by the moving mechanism of the concentrating warming devices 7a and 7b, and a horizontal direction orthogonal to the one-dimensional direction L. The vibration in the direction is applied by a vibration mechanism provided separately from the moving mechanism.

  Next, the connection head 10 capable of contacting the upper openings of the concentration containers 6a and 6b above the concentration heating devices 7a and 7b is configured to be movable in the one-dimensional direction L and capable of moving up and down. ing.

  Corresponding flange portions 11a, 11b, and 11c are formed in the upper openings of the concentration containers 6a and 6b and the lower portion of the connection head 10, and the flange portions 11a and 11b on the concentration containers 6a and 6b side have O-rings or the like. The sealing material 12 is attached.

  The upstream side of the connection head 10 is branched and is connected to a decompression system 13 and a purge gas supply system 14, respectively, and are provided with switching valves 15a and 15b.

  A condenser 16 having a cooling mechanism and a condensate container 17 are provided upstream of the decompression system 13. A decompression unit 18 connected to a vacuum pump or the like is provided in the upper part of the condensate container 17, and a discard unit 20 connected to a disposal valve 19 is provided in the lower part. And the liquid level sensor 21 is installed in the intermediate part of the condensate container 17, and this liquid level sensor 21 is an electrostatic capacitance type, an optical type, etc. suitably.

  On the other hand, the purge gas supply system 14 is connected to a purge gas supply source such as a nitrogen gas cylinder (not shown) via the switching valve 15b.

  The decompression system 13, the purge gas supply system 14, and the connection head 10 can be provided in a plurality of systems as described above.

  Reference numeral 22 denotes a control system constituted by a computer system or the like. The control system 22 includes a needle operation unit 24 controlled by the control device 23, a valve operation unit 25 for operating the switching valves 15a and 15b, and the above-mentioned concentration system. It comprises an operation unit 26 for controlling the operation of the heating devices 7a and 7b, the operation of the moving mechanism of the waste liquid container support device 9 and the operation of the vibration generating means, and the like via these operation units. Then, each element is controlled in the automatic operation described later.

  In such a configuration, the dispensing needle 5 is moved in the one-dimensional direction L above the column 1, the sample container 2, the solvent container 3, and the needle washing / drying unit 4, and moved up and down at a predetermined position. , Washing and drying operation of the dispensing needle 5, automatic operation of feeding the sample in the sample container 2 and the solvent in the solvent container 3 to the column 1, and the concentration container below the column 1 The concentrating warming device 7 equipped with 6 or the waste liquid container supporting device 9 equipped with the waste liquid container 8 is moved in the one-dimensional direction L, and a predetermined concentration container, for example, a concentration container 6a, is provided immediately below the predetermined column 1. Can be automatically fed from the column 1 to the concentration container 6a, and the waste liquid container 8 is positioned immediately below the predetermined column 1 to discard the conditioning solvent fed into the column 1. By recovering the container 8, it is possible to automatically conditioning operations of the column 1.

  After the liquid passing through the column 1 is sent to the concentration container 6a in this way, the connection head 10 is moved in the one-dimensional direction L to reach just above the predetermined concentration container 6a, and then is lowered to The flange part 11c is brought into contact with the flange part 11a at the upper part of the concentration container 6a to be in an airtight connection state. The positioning of the connection head 10 and the concentration container 6a can be performed by using not only the connection head 10 but also the movement on the concentration container 6a side.

  In this state, the switching valve 15a of the decompression system 13 is opened, the switching valve 15b of the purge gas supply system 14 is closed, each element of the decompression system 13 is operated, and the concentrating warming device 7a and the vibration The concentration means is operated by operating the generating means.

  The solvent in the concentration container 6a evaporates and is recovered in the decompression system 13 by the heating by the concentrating warming device 7a, the decompression by the decompression system 13, and the vibration applied by the vibration generating means. The liquid in the container 6a is gradually concentrated.

  The solvent vapor recovered in the decompression system 13 is cooled and condensed in the condenser 16, and the condensate gradually accumulates in the condensate container 17.

  Since the amount of liquid accumulated in the condensate container 17 matches the amount of solvent evaporated from the condensate container 6a, the amount of residual liquid in the condensate container 6a is obtained from the liquid level of the liquid accumulated in the condensate container 17a. Can do. Since no sample or salt adheres to the inner wall of the condensate container 17, the liquid level can be accurately detected by the appropriate liquid level sensor 21.

  Therefore, the liquid level of the condensate container 17 detected by the liquid level sensor 21 can be used to detect that the amount of the remaining liquid in the concentration container 6a has reached a predetermined level, and to stop the concentration operation automatically and accurately. it can.

  Here, if the amount of liquid sent from the column 1 to the concentration container 6 is set as a constant amount at all times, the same liquid in the condensate container 17 indicates that the residual liquid amount in the concentration container 6 has reached a predetermined amount. Since it can be detected by the surface, the control becomes easy.

  And in this embodiment, the operation is automatically stopped when the amount of residual liquid in the concentration container 6 reaches a predetermined amount by the concentration by operating the decompression system 13 described above. Furthermore, it can be dried by gas purge concentration.

  That is, when the gas purge type concentration operation is performed after the decompression type concentration operation, if the procedure is set in the control device 23 described above, the amount of the remaining liquid in the concentration container 6a reaches a predetermined amount as described above. Concentration is automatically stopped at the time, the switching valve 15a of the decompression system 13 is closed and the connection head 10 is raised, and appropriately between the flange portion 11c of the connection head 10 and the flange 11a of the concentration container 6a. A space is formed.

  In this state, the switching valve 15b of the purge gas supply system 14 is opened, and a purge gas such as nitrogen gas from the purge gas supply source is ejected from the connection head 10 into the concentration vessel 6a, and the liquid solvent in the concentration vessel 6a is discharged. Evaporation is promoted and concentration can proceed.

  Next, an embodiment in which a part of the procedure of the test solution adjustment method in the residual agricultural chemical inspection is automated by the automatic concentration apparatus of the present invention will be specifically described.

That is, the test solution adjustment method is defined as follows in the above-mentioned “simultaneous test method for agricultural chemicals (agricultural products) by GC / MS”. In addition, the underline and the code | symbol are attached | subjected to the target part in the following sentence for convenience.
"4. Test solution preparation method 1) Extraction
(1) For cereals, beans and seeds Add 20 mL of water to 10.0 g of the sample and leave it for 15 minutes.
Add 50 mL of acetonitrile, homogenize, and suction filter. Add 20 mL of acetonitrile to the residue on the filter paper, homogenize, and suction filter. Combine the resulting filtrates and add acetonitrile to make exactly 100.
Set to mL.
Take 20 mL of the extract, add 10 g of sodium chloride and 20 mL of 0.5 mol / L phosphate buffer (pH 7.0), and shake for 10 minutes. After standing, discard the separated aqueous layer. ... A
Octadecylsilylated silica gel mini column (1,000
Inject 10 mL of acetonitrile into mg) and discard the effluent. Inject the above acetonitrile layer into this column, then inject 2 mL of acetonitrile, collect the whole eluate, add anhydrous sodium sulfate to dehydrate, filter off anhydrous sodium sulfate, and then filter the filtrate at 40 ° C or lower. Concentrate with and remove the solvent. Add 2 mL of a mixture of acetonitrile and toluene (3: 1) to the residue and dissolve.
(2) For fruits, vegetables, herbs, tea and hops For fruits, vegetables and herbs, weigh 20.0 g of the sample. For tea and hops, add 20 mL of water to 5.00 g of sample and leave for 15 minutes.
Add 50 mL of acetonitrile, homogenize, and suction filter. Add 20 mL of acetonitrile to the residue on the filter paper, homogenize, and suction filter. Combine the resulting filtrates and add acetonitrile to make exactly 100.
Set to mL.
Take 20 mL of the extract, add 10 g of sodium chloride and 20 mL of 0.5 mol / L phosphate buffer (pH 7.0) and shake. After standing, discard the separated aqueous layer. Anhydrous sodium sulfate is added to the acetonitrile layer for dehydration, and the anhydrous sodium sulfate is filtered off. The filtrate is concentrated at 40 ° C. or lower to remove the solvent. Add 2 mL of a mixture of acetonitrile and toluene (3: 1) to the residue and dissolve.
2) Purification Inject 10 mL of a mixture of acetonitrile and toluene (3: 1) into a graphite carbon / aminopropylsilylated silica gel laminated mini-column (500 mg / 500 mg), and discard the effluent. After injecting the solution obtained in 1) into this column, 20 mL of a mixture of acetonitrile and toluene (3: 1) is injected, and the entire eluate is concentrated to 1 mL or less at 40 ° C. or less. Add 10 mL of acetone to this, concentrate to 1 mL or less at 40 ° C. or lower, add 5 mL of acetone again to concentrate, and remove the solvent. Dissolve the residue in a mixture of acetone and n-hexane (1: 1) to make exactly 1 mL. "

  This embodiment is intended to automate the work from the underlined part in “(1) In the case of cereals, beans and seeds” of the extraction process to the underlined part of “2) Purification”. 1 to 10 and the process flow charts of FIGS. 11 to 14 will be described.

  First, FIG. 11 shows a sample dehydration procedure. First, in step S1, preparation work is performed by an operator. That is, as a preparatory work, the acetonitrile layer solution after the work of A in the above regulations is put in the sample container 2 as a sample, acetonitrile is put in the solvent container 3a, and acetonitrile and toluene are put in the solvent container 3b at a ratio of 3: 1. Put the mixed solvent in place. Further, a dehydration column 1a containing anhydrous sodium sulfate and a deoiling column 1b in which graphite carbon and aminopropyl silica gel are laminated are set at predetermined positions.

  Next, when automatic execution is started in step S2, in step S3, the waste liquid container support device 9 is operated to move the test tube as the waste liquid container 8 directly below the dehydration column 1a.

  Next, in step S4, the dispensing needle 5a is moved to the needle cleaning / drying unit 4, cleaned in the cleaning unit 4a, and then dried in the drying unit 4b.

  Next, in step S5, the dispensing needle 5a is moved directly above the solvent container 3a and lowered to dispense the solvent A.

  Next, in step S6, the dispensing needle 5a is moved immediately above the dehydration column 1a, lowered, mounted on the upper opening of the dehydration column 1a, and the solvent A is fed. The solvent A passes through the dehydration column 1a, is dropped from the lower opening, and is collected in the test tube 8. By this step, the dehydration column 1a is conditioned. In addition, the transition of the process so far is typically shown by a two-dot chain line and a broken line in FIG.

  Next, in step S7, the concentration heating device 7a is moved to move the concentration container 6a directly below the dehydration column 1a.

  Next, in step S8, the dispensing needle 5a is moved to the needle cleaning / drying unit 4, cleaned in the cleaning unit 4a, and then dried in the drying unit 4b.

  Next, in step S9, the dispensing needle 5a is moved directly above the sample container 2 and lowered to dispense the sample.

  Next, in step S10, the dispensing needle 5a is moved directly above the dehydrating column 1a, lowered and mounted on the upper opening of the dehydrating column 1a to feed the sample. The sample passes through the dehydration column 1a and is dropped from the lower opening and collected in the concentration container 6a. By this step, the sample is dehydrated. In addition, the transition of the process so far is typically shown by a two-dot chain line and a broken line in FIG.

  Next, in step S11, the shower needle 5b is moved to the needle washing / drying unit 4 for washing and drying, and then in step S12, the shower needle 5b is moved directly above the solvent container 3a as shown in FIG. A is dispensed. Next, in step S <b> 13, as shown in FIG. 5, the shower needle 5 b is moved immediately above the sample container 2, and is lowered to send the solvent A into the sample container 2. Since the liquid supply of the solvent A from the shower needle 5b is performed by ejecting it laterally from an opening formed around the lower portion, the solvent A can be collected by washing the sample adhering to the inner wall of the sample container 2.

  The above steps S8 to S18 are repeated a predetermined number of times set in advance, whereby a predetermined amount of sample can be sent into the concentration container 6a through the dehydration column 1a.

  FIG. 12 shows a sample concentration procedure. As shown in the connector A, this concentration procedure is a procedure performed following the procedure of FIG.

  First, in step S14, only the connection head 10 or the connection head 10 and the concentrating warming device 7a are moved, and the flange portion 11c of the connection head 10 is brought into contact with the flange portion 11a on the upper side of the concentration container 6a for airtightness. Connected to.

  Next, in step S15, the switching valve 15a of the depressurization system 13 is opened, the switching valve 15b of the purge gas supply system 14 is closed, each element of the depressurization system 13 is operated, and the concentration heating device 7a and Concentration work is performed by appropriately operating the vibration generating means.

  In step S <b> 16, the liquid level in the condensate container 17 is detected by the liquid level sensor 21 to obtain the remaining liquid amount in the concentration container 6 a. In this step, when it is detected from the liquid level of the condensate container 17 detected by the liquid level sensor 21 that the residual liquid amount in the concentration container 6a has reached a predetermined amount, the concentration operation is automatically stopped. Then, the process proceeds to the next step S17. The operations in steps S14 to S16 are schematically shown in FIG.

  That is, in step S17, the concentration automatically stops when the amount of the remaining liquid in the concentration container 6a reaches a predetermined amount, the switching valve 15a of the decompression system 13 is closed, and the connection head 10 is raised. Thus, an appropriate space is formed between the flange portion 11c of the connection head 10 and the flange 11a of the concentration container 6a.

  Next, in step S18, as shown in FIG. 7, the switching valve 15b of the purge gas supply system 14 is opened, and the purge gas from the purge gas supply source, for example, nitrogen gas is ejected from the connection head 10 into the concentration vessel 6a. Then, the evaporation of the liquid solvent in the concentration container 6a is promoted and the concentration can proceed.

  In step S18, the heating operation by the concentrating heating device 7a, the vibration applying operation by the vibration generating means, and the time and timing for supplying the purge gas can be set as appropriate.

  Next, FIG. 13 shows a sample purification procedure. This purification procedure is performed following the procedure of FIG. In the following description, for example, the operations in the needle cleaning / drying unit 4 and the obvious operations such as the movement and lowering operations of the dispensing needle 5a are omitted.

  First, in step S19, the shower needle 5b is moved to the needle cleaning / drying section 4 for cleaning and drying, and then in step S20, as schematically shown by the one-dot chain line and two-dot chain line in FIG. To dispense the solvent B in the solvent container 3b.

  Next, in step S21, as shown by the solid line in FIG. 8, the shower needle 5b is moved to the concentration container 6a, and the solvent B is fed into the concentration container 6a. Thus, since the solvent B from the shower needle 5b is ejected in the horizontal direction and is sent into the concentration container 6a, the solvent B is efficiently collected by washing the sample adhering to the inner wall of the concentration container 6a. can do.

  Next, in step S22, the test tube as the waste liquid container 8 is moved directly below the deoiling column 1b, and in step S23, the dispensing needle 5a is moved to the needle cleaning / drying unit 4 to perform cleaning / drying.

  Next, in step S24, the dispensing needle 5a is moved directly above the solvent container 3b and lowered to dispense the solvent B.

  Next, in step S25, the dispensing needle 5a is moved immediately above the deoiling column 1b, is lowered, is attached to the upper opening of the deoiling column 1b, and the solvent B is fed. The solvent B passes through the deoiling column 1b, drops from the lower opening, and is collected in the test tube 8. By this step, the deoiling column 1b is conditioned.

  Next, in step S26, the concentration container 6b is moved directly below the deoiling column 1b. Next, in step S27, the dispensing needle 5a is moved to the needle washing / drying unit 4 and washed / dried.

  Next, in step S28, as shown in FIG. 9, the dispensing needle 5a is moved immediately above the concentration container 6a and lowered to dispense the sample in the concentration container 6a.

  Next, in step S29, the dispensing needle 5a is moved immediately above the deoiling column 1b, lowered and attached to the upper opening of the deoiling column 1b to feed the sample. As shown in FIG. 10, the sample passes through the deoiling column 1b, drops from the lower opening, and is collected in the concentration container 6b. By this step, it is possible to remove pigment components, contaminants, and the like, which are interfering substances when the sample is deoiled, for example, analyzed using GC-MS.

  Next, in step S30, the shower needle 5b is moved to the needle cleaning / drying unit 4 to perform cleaning / drying, and then in step S31, the shower needle 5b is moved immediately above the solvent container 3b and lowered to dispense solvent B. Next, in step S32, the shower needle 5b is moved directly above the concentration container 6a, and is lowered to send the solvent B into the concentration container 6b as shown in FIG. As described above, since the solution B of the solvent B from the shower needle 5b is ejected in the lateral direction, the solvent B can be collected by washing the sample adhering to the inner wall of the concentration container 6a.

  The above steps S27 to S32 are repeatedly performed a predetermined number of times, so that a predetermined amount of the sample in the concentration container 6b can be sent into the concentration container 6b through the deoiling column 1b.

  FIG. 14 shows the concentration procedure of the sample sent from the concentration container 6a to the concentration container 6b through the deoiling column 1b. This concentration procedure follows the procedure of FIG. It is a procedure performed. This procedure, that is, steps S33 to S7, is the same as steps S14 to S18 in which the concentration is performed on the sample in the concentration container 6a except that the concentration is performed on the sample in the concentration container 6b. Since there is, overlapping description is omitted.

  As described above, the automatic concentration apparatus of the present invention has a lot of fine work as in the case of executing the test solution preparation method in the pesticide residue inspection, and a solvent that affects the human body, such as acetonitrile and toluene. Even when it is necessary to use the solvent, the concentration work and a series of related work can be performed safely, and the introduction of the so-called positive list system expands the scope of food pesticide residue inspection. In connection with this, since inspections for a large number of agricultural chemicals can be performed efficiently and in a short period of time, the industrial applicability is extremely high.

  In particular, in the present invention, a condenser and a condensate container are provided in the decompression system, and a liquid level sensor is provided in the condensate container, whereby the residual liquid in the concentration container is determined by the liquid level of the condensate container detected by the liquid level sensor. The amount can be determined, and since no sample or salt adheres to the inner wall of the condensate container, the liquid level can be accurately detected by an appropriate liquid level sensor. .

  Furthermore, in the present invention, the concentration operation can be performed by switching from the depressurization method concentration in the state where the depressurization system is operated to the gas purge method concentration in the state where the purge gas supply system is operated. A trace amount of substance to be detected is obtained by performing concentration in a reduced pressure system in the activated state and then switching to the gas purge method in a state in which the purge gas supply system is activated when the residual liquid amount reaches a predetermined amount. It has a special feature that the time required for concentration can be shortened without evaporating.

It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention. It is explanatory drawing which shows notionally the structure and operation | movement of a process of the automatic concentration apparatus which concerns on this invention. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is explanatory drawing which shows notionally the structure of the automatic concentration apparatus which concerns on this invention, and operation | movement of a process in another situation. It is a process flowchart which shows the Example of operation | movement of the automatic concentration apparatus which concerns on this invention. It is a process flowchart of another situation showing an example of operation of an automatic concentration device concerning the present invention. It is a process flowchart of the other situation which shows the Example of operation | movement of the automatic concentration apparatus which concerns on this invention. It is a process flowchart of the other situation which shows the Example of operation | movement of the automatic concentration apparatus which concerns on this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Column 1a Dehydration column 1b Deoiling column 2 Sample container 3 (3a, 3b) Solvent container 4 Needle washing drying part 4a Washing part 4b Drying part 5 Dispensing needle 5a Dispensing needle 5b Shower needle 6 (6a, 6b ) Concentration container 7 (7a, 7b) Concentration heating device 8 Waste liquid container (test tube)
9 Waste liquid container support device 10 Connection heads 11a, 11b, 11c Flange part 12 Sealing material 13 Depressurization system 14 Purge gas supply system 15a, 15b Switching valve 16 Condenser 17 Condensate container 18 Decompression part 19 Disposal valve 20 Disposal part 21 Liquid Surface sensor 22 Control system 23 Control device 24 Needle operation unit 25 Valve operation unit 26 Other operation unit

Claims (9)

A column, a sample container, and a solvent container are arranged in a one-dimensional direction, and above the arrangement, the dispensing needle is configured to be movable in the one-dimensional direction and vertically movable, and the column The concentrating warming device for mounting the concentrating container and the waste liquid container supporting device for mounting the waste liquid container are configured to be movable in the above one-dimensional direction, and further above the concentrating warming device. The automatic concentrating device according to claim 1, wherein the connection head of the decompression system capable of coming into contact with the upper opening of the concentration container is configured to be movable in the one-dimensional direction and movable up and down. The automatic concentration apparatus according to claim 1, wherein a condenser and a condensate container are provided in the decompression system, and a liquid level sensor is provided in the condensate container. 2. The automatic concentrator according to claim 1, wherein the concentrating warmer is provided with vibration generating means. 4. The automatic concentrator according to claim 3, wherein the vibration generating unit is configured as a moving unit of the concentrating warmer. 2. The automatic concentrator according to claim 1, wherein a purge gas supply system that is branched and switched from the decompression system is connected to the connection head. The automatic concentration apparatus according to claim 1, wherein a needle cleaning / drying unit is provided in an arrangement including the column. The automatic concentrator according to claim 1, wherein a plurality of columns are arranged and include a dehydration column and a deoiling column. 2. The automatic concentrator according to claim 1, wherein the dispensing needle is composed of a plurality of needles, a part of which has a shower hole. The automatic concentrator according to claim 1, wherein a plurality of concentrating warmers are arranged.

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