JPH063233A - Agricultural chemicals residue automatic preliminary treatment device - Google Patents

Abstract

PURPOSE:To perform automatically preliminary treatment from first to last by grinding-stirring sample so as to solvent-extract, stirring filtrate with rotary solution solvent in a rotary solution tank, filtering emulsion so as to feed to a separating tank, sensor-detecting the sample and water content so as to feed to respective tanks, and cake-filtrating the sample in a sample tank so as to be provided in a sampling container. CONSTITUTION:A sample cup 8 is held by a sample stock table 3, sample in the cup 8 is grinding-stirring by a disperser 15, filtrate, extracted after adding solvent thereto, is fed from the cup 8 to a rotary solution tank 53, and after the filtrate is stirred with rotary solution solvent, the filtrate is filtered in order to remove emulsion, and is fed to a separating tank 82. In the tank 82 water content and the sample in the filtrate is detected by an interface sensor 85, and according to its result, the water content and the sample are fed to a water content tank 94 and a sample tank 90. A funnel 101 is provided on a turn table 99 below the tank 90 so as to cake-filtrate the sample, and the treatment agent sample is sampled in a flask 102.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic pesticide residue pretreatment system.

[0002]

2. Description of the Related Art From the viewpoint of ensuring the safety of diversified imported agricultural products, there has recently been an active discussion that the regulation of agricultural chemical residues on agricultural products should be greatly strengthened.

Further, from this, the Ministry of Health and Welfare has established a policy of newly establishing a residue standard for about 40 kinds of pesticides in addition to the conventional 26 kinds of pesticides.

Therefore, the analytical inspection of pesticide residues will become more and more important in the future, and the opportunities will increase. However, the analytical inspection of pesticide residues requires pretreatment. However, the conventional pretreatment method has a problem that it takes much time and labor. That is, the pretreatment of the residual pesticide test is a step of homogenizing the agricultural product by finely crushing it, adding an extraction solvent to the homogenized sample and shaking for a predetermined time, and then filtering and extracting with hexane, and the extracted filtrate with hexane, Although it comprises a phase transfer step of adding a phase transfer solvent such as an aqueous solution of sodium chloride and shaking, a liquid separation step of separating the sample and water, and a dehydration filtration step of dehydrating and filtering the sample, the above-mentioned steps are conventionally performed. We couldn't do this consistently, which was too laborious and time consuming to do this quickly.

[0005]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above-mentioned problems, and it is made possible to consistently and automatically perform pretreatment for residual pesticide inspection by a single device. Therefore, it is intended to provide an automatic pretreatment device for residual pesticides, which can be efficiently performed in a short time.

[0006]

The gist of the present invention is to provide a sample stock table capable of holding a required number of sample cups, a filter paper inside, and an extraction port at the bottom. A sample cup provided with a disperser that moves onto the sample cup at a predetermined timing and crushes and stirs the sample in the sample cup, and an extraction solvent supply that injects a predetermined extraction solvent into the sample cup at the same time as the operation of the disperser. Apparatus, sample delivery apparatus for delivering the extracted filtrate from the sample cup to a later-described transfer tank, a transfer tank for stirring the filtrate and transfer solvent with a stirrer, and a predetermined transfer solvent for the transfer tank For supplying the filtrate, a filtration device for removing the emulsion in the filtrate sent from the transfer tank, a separation tank for receiving the filtrate that has passed through the filtration device, and a discharge tank for the separation tank. An interface sensor for detecting a sample and water content of the filtrate, an apparatus for sending the sample and the water content to different containers according to the detection result of the interface sensor, a sample tank for containing the sample, and a water content tank for containing the water content. An automatic pesticide residue pretreatment device comprising a turntable disposed below the sample tank, which holds a required number of funnels and sample collection vessels, and which receives a sample from the sample tank and dehydrates and filters it It is in.

[0007]

Next, the operation of the present invention will be described. First,
The extraction process will be described. Position the disperser offset above any one of the sample cups arranged on the sample stock table. Next, the disperser is lowered into a sample cup and rotated, and at the same time, acetone or acetonitrile as an extraction solvent is sucked out from a container containing it by a dispenser and injected into the sample cup. After that, the solution in the sample cup is filtered through a filter paper provided at the bottom of the sample cup and sent to the transfer tank. After that, the required amount of extraction solvent is injected again into the residue in the sample cup and filtered, and this filtrate is also sent to the transfer tank.

In order to send the filtrate from each sample cup to the transfer tank, first, the automatic 1-point 10-way valve and the automatic 4-way valve provided in the middle of the pipe connecting the sample cup and the transfer tank are appropriately switched. Then, the inside of the transfer tank is brought to a negative pressure state with a vacuum pump, and thereby the filtrate is sucked.

Next, the transfer process will be described. When the filtrate enters the phase transfer tank, dichloromethane or n-hexane as a phase transfer solvent is sucked out of the container by a dispenser and injected into the phase transfer tank. Next, 5% NaCl or 10% NaCl is sucked out of the container with a dispenser and injected into the transfer tank. Then, the agitator is operated in this state. After that, the filtrate in the transfer tank is sent to the separation tank, and filtration is performed again by the filtration device provided in the middle of the pipe connecting the transfer tank and the separation tank. This removes the emulsion and smoothes the subsequent separation. In addition, the liquid sent from the liquid separating tank to the moisture tank described later is sent back to the transfer tank again. Then, the liquid is sent to the liquid separation tank through the same steps as above.

Next, the liquid separation step will be described. After the filtrate enters the separating tank, it is allowed to stand for a predetermined time, and the interface sensor is used to detect the sample and water. This is
This is done by an interface sensor provided at the bottom of the liquid separation tank. Then, the sample and the water are separated by an automatic one-point three-way valve, the sample is sent to the sample tank, and the water is sent to the water tank. Then, again, the water in the water tank is sent to the drain storage bottle.

Next, the dehydration filtration step will be described. The sample sent into the sample tank was extensively scattered on a funnel containing sodium sulfate arranged on a turntable, dropped, dehydrated and filtered, and became the final sample in the flask held below the funnel. To fall.

Next, the cleaning will be described. First, the cleaning of the disperser will be described. After the extraction is completed, the disperser is lifted from the sample cup and moved to the position of the washing cup. Then, shower in the washing cup to wash.

In order to clean the pipe between the sample cup and the transfer tank, the disperser is lifted from the sample cup after completion of the extraction, and a predetermined type of cleaning liquid such as acetone, detergent and water is sucked out from the cleaning liquid container, and the pipe is removed. Each valve provided in the middle part of is switched appropriately. Then, contrary to the case of sending the solution to the transfer tank, inject the cleaning solution from the bottom of the sample cup,
It is something to wash. The residue of the sample is stored in the sample cup together with the cleaning solution. And finally, after cleaning with acetone, injection cleaning with air is carried out.

Next, cleaning of the transfer tank and the separation tank will be described. A predetermined type of cleaning liquid is sucked out from the cleaning liquid container, each valve provided in the middle of the pipe is appropriately switched, and the cleaning liquid is injected into the transfer tank or the liquid separating tank to perform shower cleaning.

Next, the cleaning of the sample tank and the water tank will be described. When cleaning the sample tank, first, the drain pan is displaced right below the sample tank. After that, as in the case of the above-mentioned transfer tank, etc., a cleaning liquid of a predetermined type is sucked out from the cleaning liquid container, each valve provided in the middle of the pipe is appropriately switched and injected into the sample tank, and shower cleaning is performed. is there. The washing of the water tank is the same as the washing of the sample tank except that a drain pan is used.

[0016]

Embodiments of the present invention will be described below with reference to the drawings. 1 is a schematic explanatory view of an extraction step portion, FIG. 2 is a schematic explanatory view of a phase transfer / liquid separation step portion, FIG. 3 is a schematic explanatory view of a dehydration filtration step portion, and FIG. 4 is a schematic illustration of a washing step portion. Explanatory drawing, FIG. 5 is an overall front view of the apparatus, FIG. 6 is an overall plan view of the apparatus, FIG. 7 is an exploded perspective view of a sample cup, FIG. 8 is a central vertical section front view of a sample stock table, and FIG. 9 is a central vertical section of a disperser. A side view, FIG. 10 is a plan view of the disperser, FIG. 11 is a central longitudinal front view of a transfer tank, FIG. 12 is a front view of a filtering device, FIG. 13 is a central longitudinal side view of a filtering device, and FIG.
Is a central longitudinal front view of the separating tank, and FIG. 15 is an automatic 1 point 10
1 is a front view of a one-way valve, FIG. 16 is a side view of a longitudinal section of an automatic 1-point 10-way valve, and FIG. 17 is a front view of an automatic 4-way valve.
8 is a central vertical side view of the automatic 4-way valve, FIG. 19 is a front view of the dispenser, FIG. 20 is a central vertical side view of the dispenser, FIG. 21 is a plan view of the dispenser, and FIG. 22 is a turntable. FIG. 23 is a plan view of the turntable, FIG. 23 is a plan view of the drain pan, FIG. 25 is a plan view of the drain pan, and FIG. 26 is a perspective view of the turntable and the drain pan.

In the figure, reference numeral 1 is a housing having casters 2 on its bottom surface. Reference numeral 3 denotes a sample stock table, which has a pinion 5 fixed to a rotation shaft of a motor 4 and a rack 6 meshing with the pinion 5, and is horizontally movable in the front-rear direction along rails 7, 7. Also, the sample stock table 3
Is designed to hold 10 sample cups side by side. In the present embodiment, the case of 10 is shown, but the number is not limited to this, and the number may be more or less than that.

Reference numeral 8 is a sample cup, which is provided with an extraction port 9 at the bottom and is capable of connecting the connecting portion 10 with the transfer pipe with one touch. Further, a filter paper 11, a net 12 supporting the filter paper 11, and a plate 13 are provided at the bottom of the sample cup 8. Incidentally, 14 is an O-ring.

Reference numeral 15 is a disperser. The disperser 15 includes a motor 16 and a screw shaft 17 fixed to its rotation shaft.
A motor 22 fixed to a horizontal moving plate 21 and a pinion 23 fixed to its rotation shaft and a support frame are moved up and down along guides 20 and 20 with a fitting member 19 of the screw shaft 17 fixed to a lift plate 18. With the rack 25 provided on the bottom surface of 24, it can be horizontally moved along the rail 26 in the left-right direction.

Reference numeral 27 is an extraction solvent injection nozzle, which is designed to move together with the disperser 15.
The extraction solvent injection nozzle 27 is connected to an automatic one-point three-way valve 29 with a pipe 28. The automatic one-point three-way valve 29 is connected by pipes 30 and 31 to a container 32 of acetonitrile as an extraction solvent and a container 33 of acetone, respectively. The automatic one-point three-way valve 29 is also connected to a dispenser 35 by a pipe 34.

The dispenser 35 includes a screw shaft 38 connected to a rotary shaft of a motor 37 fixed to a support frame 36, and a lift plate 39.
The fitting member 40 of the screw shaft 38 fixed to the elevating plate 3
9, a piston rod 41 connected to the piston rod 41, a piston 42 fixed to the piston rod 41, and a cylinder 43 into which the piston 42 slides.

Each of the sample cups 8 has a pipe 4
4 is connected to an automatic one-point ten-way valve 45. The automatic 1-point, 10-way valve 45 includes a motor 46 and a valve body 47 whose connection is switched by rotation of the motor 46.

The automatic one-point ten-way valve 45 is connected to an automatic four-way valve 49 by a pipe 48.
The automatic four-way valve 49 includes a motor 50 and a motor 50.
Of the valve main body 51 whose connection of each port is switched by the rotation of. Also, the automatic 4-way valve 49
Is connected to a transfer tank described later with a pipe 52.

Reference numeral 53 is a transfer tank. The transfer tank 5
3 is made of transparent Pyrex glass, like the liquid separating tank, sample tank, and water tank described later. The transfer tank 53 is connected to a vacuum pump 55 via a pipe 54. Furthermore, the transfer tank 53 is connected to an automatic one-point three-way valve 57 with a pipe 56, and the automatic one-point three-way valve 57 has pipes 58 and 59 for a container 60 of n-hexane as a transfer solvent and dichloromethane. Connected to the container 61. Reference numeral 62 is a dispenser connected to the automatic one-point three-way valve 57.

Furthermore, the transfer tank 53 includes a pipe 6
3 is connected to the two-way valve 64, and the two-way valve 6
No. 4 has pipes 65 and 66 and is 5% Na as a transfer solvent.
It is connected to a Cl container 67 and a 10% NaCl container 68. Incidentally, 69 is a dispenser connected to the two-way valve 64. Further, the transfer tank 53 is connected by a pipe 70 to an automatic one-point four-way valve for a cleaning liquid described later, and is also connected to a discharge part of a moisture tank described later by a pipe 71.

Reference numeral 72 is a shower nozzle provided in the transfer tank 53, and 73 is a stirrer. The agitator 73 is a motor 7
By the rotation of 4, the stirring blade 75 rotates at a predetermined speed.

The transfer tank 53 is connected to a filtration device 77 by a pipe 76. The filtering device 77
The tape-shaped filter medium 80 is intermittently delivered from the delivery reel 78 to the take-up reel 79 by a predetermined amount at a predetermined timing. The filtrate discharged from the transfer tank 53 is filtered by passing through the filter medium 80.

The filtering device 77 is connected to a liquid separating tank described later by a pipe 81. Numeral 82 is a liquid separating tank, and a pipe 83 is used to automatically add 1
Connected to a point 4-way valve. Reference numeral 84 is a pipe connecting the liquid separating tank 82 and the atmosphere.

Reference numeral 85 is an interface sensor for detecting a sample and water. The interface sensor 85 is provided below the liquid separation tank 82. In addition, the interface sensor 8
5 is connected to an automatic one-point three-way valve 87 by a pipe 86. The automatic one-point three-way valve 87 is connected to the sample tank and the water tank described later by pipes 88 and 89. The automatic one-point three-way valve 87 separates the sample and the water based on the analysis of the interface sensor 85.

Reference numeral 90 is a sample tank. Further, the sample tank 90 is connected to an automatic one-point four-way valve for the cleaning liquid described later by a pipe 91 and is also connected to an air supply device 93 by a pipe 92.

Reference numeral 94 is a water tank. The water tank 9
Reference numeral 4 is connected to an automatic one-point four-way valve for the cleaning liquid described later through a pipe 95, and is connected to the atmosphere through a pipe 96. Furthermore, the water tank 94 is a pipe 97.
It is also connected to the drain bottle described later.

Reference numeral 98 is a nozzle provided in the lower portion of the sample tank 90 and having the same area as the flow path, and is formed in a mesh shape. 99 is a turntable, which is formed in upper and lower two stages. The turntable 99 is intermittently rotated horizontally by a motor 100 at a predetermined timing.

Reference numeral 101 is a funnel which is arranged and held on the upper stage of the turntable 99 and is filled with powdery sodium sulfate. Reference numeral 102 denotes a flask which is arranged and held in the lower part of the turntable 99, and which has the funnel 1
It is held right under each of 01. In addition, these funnels 10
1 and the number of flasks 102 correspond to the number of the sample cups 8.

Reference numeral 103 is a drain pan, which is a motor 104.
Is rotated at a predetermined timing in the horizontal direction and positioned directly below the nozzle 98. Further, the drain tray 103 is connected to the drain port with a pipe 105.

Reference numeral 106 denotes a cleaning cup for the disperser 15, which is automatically connected to a cleaning liquid described later with a pipe 107.
Connected to a point 4-way valve. Reference numeral 108 is a shower nozzle provided in the cleaning cup 106. A drain port of the cleaning cup 106 is connected to a drain bottle described later through a pipe 109.

Reference numerals 110 to 113 are containers containing a cleaning liquid, 110 is a container containing acetone, 111 is a container containing detergent, 112 is a container containing water, and 113 is a container containing a preparatory liquid. Also, the containers 110, 1
11, 112, 113 are respectively connected to an automatic one-point four-way valve 115 by a pipe 114. Furthermore, the automatic one-point four-way valve 115 is installed in the middle of the electromagnetic pump 1
A pipe 117 provided with 16 is connected to another automatic one-point four-way valve 118. Reference numeral 119 is a syringe mounted between the electromagnetic pump 116 and the automatic one-point four-way valve 118 in the pipe 117, and is used when the cleaning liquid is first drawn up.

The automatic one-point four-way valve 118 is connected to a three-way valve 121 with a pipe 120. The three-way valve 121 is connected to the automatic four-way valve 49 by a pipe 122 and the pipe 1
23 is connected to the air supply device 93.
Reference numeral 124 is a drain bottle. Further, reference numeral 125 is a pan at the bottom of the housing 1, which is attached with a slight inclination. A liquid detector (not shown) is provided on the receiving tray 125 to sound an alarm when a liquid leak occurs during operation, and to stop the entire operation at night.

[0038]

EFFECTS OF THE INVENTION Since the present invention has the above-described structure and operation, it is possible to consistently and automatically perform pretreatment for residual pesticide inspection with a single apparatus. Therefore, the pretreatment can be efficiently performed in a short time,
This is very useful for efficiently conducting pesticide residue inspection, which is expected to increase in the future.

[Brief description of drawings]

FIG. 1 is a schematic explanatory view of an extraction step portion of the present invention.

FIG. 2 is a schematic explanatory diagram of a phase transfer / liquid separation step portion.

FIG. 3 is a schematic explanatory diagram of a dehydration filtration step portion.

FIG. 4 is a schematic explanatory view of a cleaning process portion.

FIG. 5 is an overall front view of the device.

FIG. 6 is an overall plan view of the device.

FIG. 7 is an exploded perspective view of a sample cup.

FIG. 8 is a central longitudinal front view of a sample stock table.

FIG. 9 is a vertical sectional side view of the center of the disperser.

FIG. 10 is a plan view of the disperser.

FIG. 11 is a central vertical front view of a transfer tank.

FIG. 12 is a front view of the filtration device.

FIG. 13 is a central longitudinal side view of the filtering device.

FIG. 14 is a central vertical sectional front view of the liquid separation tank.

FIG. 15 is a front view of an automatic one-point ten-way valve.

FIG. 16 is a central longitudinal side view of an automatic one-point ten-way valve.

FIG. 17 is a plan view of an automatic 4-way valve.

FIG. 18 is a central longitudinal side view of the automatic 4-way valve.

FIG. 19 is a front view of the dispenser.

FIG. 20 is a central longitudinal side view of the dispenser.

FIG. 21 is a plan view of the dispenser.

FIG. 22 is a central vertical front view of the turntable.

FIG. 23 is a plan view of a turntable.

FIG. 24 is a central longitudinal side view of the drain pan.

FIG. 25 is a plan view of the drain pan.

FIG. 26 is a perspective view of a turntable and a drain pan.

[Explanation of symbols]

 1 Case 3 Sample Stock Table 8 Sample Cup 15 Disperser 27 Extraction Solvent Injection Nozzle 32 Acetonitrile Container 33 Acetone Container 35 Dispenser 45 Automatic 1-Point 10-Way Valve 49 Automatic 4-Way Valve 53 Transfer Tank 55 Vacuum Pump 60 n-Hexane Container 61 Dichloromethane container 62 Dispenser 67 5% NaCl container 68 10% NaCl container 69 Dispenser 73 Stirrer 77 Filtration device 82 Separation tank 85 Interface sensor 87 Automatic 1-point 3-way valve 90 Sample tank 93 Air supply device 94 Moisture tank 99 Turntable 101 Funnel 102 Flask 103 Drain pan 106 Washing cup 110 Acetone container 111 Detergent container 112 Water container 115 Automatic 1-point 4-way valve 118 Automatic 1-point 4-way valve 124 Drain bottle 125 Casket pan

Claims (1)

[Claims] 1. A sample stock table capable of holding a required number of sample cups, a sample cup provided with a filter paper inside and provided with an extraction port at the bottom, and moved onto the sample cup at a predetermined timing. Then, a disperser for crushing and stirring the sample in the sample cup, an extraction solvent supply device for injecting a predetermined extraction solvent into the sample cup at the same time as the operation of the disperser, and the extracted filtrate from the sample cup to a transfer tank described later. A sample delivery device for delivering, a transfer tank for stirring the filtrate and the transfer solvent with a stirrer, a device for supplying a predetermined transfer solvent to the transfer tank, and an emulsion in the filtrate delivered from the transfer tank. For removing the water, a separation tank for receiving the filtrate that has passed through the filtration apparatus, an interface sensor for detecting the sample of the filtrate and the water discharged from the separation tank, and the interface separator. Depending on the detection result of the sensor, a device for sending the sample and the moisture to separate containers, a sample tank for storing the sample and a moisture tank for storing the moisture, and a turntable arranged below the sample tank. An automatic pesticide residue pretreatment device comprising a required number of funnels and a sample container, and a dehydration filtration device for receiving the sample in the sample tank and performing dehydration filtration.