JPH0321469Y2 - - Google Patents

Description

[Detailed description of the invention] (a) Industrial application field This invention is a solvent solution that allows multiple solvent solutions mixed by shaking to stand still, separates each solution, and then sequentially separates and extracts the solvent from the solvent solution with a heavier specific gravity. This relates to an automatic extraction device.

(b) Prior Art For example, when analyzing pesticides dissolved in water, the water is sucked into a syringe, injected into a sample vaporization chamber, vaporized, and introduced into a column together with a carrier gas, where various components of the pesticide are analyzed. Sample components are separated and eluted and quantitatively detected using a detector.
Usually, the amount of pesticide dissolved in water is so small that sensitive detection cannot be performed.

Therefore, the water containing the pesticide dissolved in it and a smaller amount of hexane are mixed in a separating container and left to stand. Since the specific gravity of water is heavier than hexane, water and hexane are separated from each other in the lower part of the container and the hexane in the upper part of the container, forming a boundary liquid with each other. next,
Open the discharge valve provided at the bottom of the container, extract only water, close the discharge valve, and separate and extract hexane into a new sample container. Since the amount of hexane is small and the pesticide dissolved in a large amount of water is dissolved in hexane, the pesticide is concentrated.
Therefore, by aspirating this with a syringe and analyzing it with a gas chromatograph, the detector can perform highly sensitive detection.

In the conventional technology for separating and extracting the two liquids separated in the liquid separation container, the discharge valve provided in the transparent discharge pipe of the liquid separation container is opened, and the liquid located at the lower part of the liquid separation container is removed. A method is used in which the discharge valve is visually checked, the discharge valve is closed, a new sample container is placed directly under the discharge tube, the discharge valve is opened again, and the remaining liquid is discharged. is not desirable from the viewpoint of labor saving.

Therefore, along the discharge pipe of the transparent liquid separation container, 2
A photoelectric detector was disposed to detect the interface between the liquids based on the difference in refractive index, and the discharge valve was automatically closed after a predetermined time elapsed from the detection time when the interface between the two liquids was detected.

However, when the viscosities of the liquids to be separated and extracted are different, the flow rate of the liquid from the photoelectric detector to the discharge valve is different, so that the discharge valve is closed before the two-liquid interface reaches the discharge valve. Otherwise, the two-liquid interface was closed after passing through the discharge valve, making it impossible to perform accurate solvent extraction.

(C) Purpose The present invention solves the drawbacks of the prior art described above, and aims to measure the passing velocity of the liquid boundary surface passing through the discharge pipe of a liquid separation container using first and second detectors. It is an object of the present invention to provide an automatic solvent extraction device that can perform accurate solvent extraction by detecting the liquid boundary surface and closing the discharge valve at the time when the liquid boundary surface reaches the discharge valve arranged at a predetermined distance.

(d) Configuration Figure 1 is a functional block diagram for clearly showing the configuration of the present invention.

In the same figure, a plurality of types of liquids having different specific gravities and not being mixed are injected into a liquid separation container and flowed down by opening a discharge valve, and a first detector is placed at a predetermined distance in the discharge pipe of the separation liquid container. The boundary liquid level is detected by the first detector and the second detector.
The speed of the boundary liquid level passing through the second detector is determined by the speed determining means, and the valve closing time determining means determines the time required for the boundary liquid level to reach the discharge pipe located a predetermined distance from the second detector. The valve is closed when the boundary liquid level reaches the discharge valve.

(e) Examples Examples of the automatic solvent extractor of the present invention will be described below.

FIG. 2 is an overall configuration diagram of the apparatus of this embodiment.

In the figure, 1 is a liquid separation container holding device;
It consists of an L-shaped pedestal 1c, an arm 1a supported so as to be movable up and down along the pedestal 1c, and a rotatable arm 1b supported so as to be rotatable for inverting a liquid separation container 5, which will be described later. 2 is a transparent liquid separation container made of, for example, plastic material,
Similarly, a transparent introduction section 2a and a discharge pipe 2b are integrally constructed, into which water and hexane are injected. Note that the introduction part 2a is connected to the rotating arm 1.
b, and is fixedly held by a fixing member (not shown) so as not to be displaced upward or downward. Reference numeral 6 denotes a reciprocating motion generating device, which has a built-in drive source such as a motor and a reciprocating drive mechanism consisting of a rack, etc., and receives a control signal and operates the illustrated liquid separating container 2 fixedly held on the rotating arm 1b. It is held upside down at an angle of 180 degrees, and together with the arm 1a, the rotating arm 1b is given vertical reciprocating motion. Reference numeral 7 denotes a rotation device, which incorporates a drive source such as a motor and a rotation mechanism such as gears, and receives a control signal to rotate the rotation arm 1b by 180 degrees, thereby moving the separation container 2 to the state shown in the figure. from
It can be rotated 180° and turned upside down. Reference numeral 3 denotes a solution injection/gas vent valve opening/closing device, which opens and closes the valve upon input of a control signal.

8 and 9 are photosensors, 10 and 1
1 is a light emitting diode, the photosensor 8 and the light emitting diode 10 constitute a first detector,
It detects the descent of the two-liquid interface between water and hexane based on the difference in refractive index, and is composed of a photosensor 9 and a light emitting diode 11 located at a predetermined distance _L1 from the first detector. A second detector is arranged to similarly detect the drop of the two-liquid interface based on the difference in refractive index. Reference numeral 4 denotes a discharge valve constituted by a solenoid valve, and is provided at a predetermined distance _L2 from the second detector.

12 is a control device, which includes a reciprocating motion generating device 6;
A control signal is input to the rotation device 7 to control its drive, and a control signal is input to the solution injection/gas vent valve opening/closing device 3 to open and close the valve to perform solution injection or gas venting. Furthermore, to explain the closing control of the discharge valve 4 by the control device 12, first, the water located in the lower layer in the liquid separation container 2 is discharged while the discharge valve 4 is opened, and the water located in the lower layer in the liquid separation container 2 is first and a second detector, and the transit time Δt ₁ is measured. Since the arrangement distance L ₁ between the first detector and the second detector is known, the speed S of the two-liquid interface is determined from S=L ₁ /Δt ₁ . Since the arrangement distance L ₂ between the second detector and the discharge valve 4 is known, the time Δt ₂ for the two-liquid interface to reach the discharge valve 4 from the second detector is Δt ₂ =
It is calculated from L ₂ ×S, and after Δt ₂ hours have passed, the discharge valve 4 is closed to discharge only water. Thereafter, the discharge valve 4 is opened again and hexane is extracted.

The circuit device that performs the above-mentioned control operation will be explained based on FIG. ,
Generates an output pulse. When the second detector detects the arrival of the two-liquid interface, a pulse signal is generated;
This is input to the reset terminal of flip-flop 13 to stop generating output pulses. This output pulse is applied to the AND gate 15 to which the clock signal of the high-precision clock oscillator 14 is input.
2 that passed through the first detector and the second detector
A first distance setting device 16 that converts the passage time of the liquid boundary surface into a digital signal and generates a digital signal indicating the distance L ₁ is inputted to a divider 17 connected to the first distance setting device 16 .
The velocity S of the liquid interface is determined from S=L ₁ /Δt ₁ .

The circuit device from the flip-flop 13 to the divider 17 described above constitutes a means for determining the speed of the two-liquid interface.

Now, the speed signal output from the divider 17 is
The time Δt ₂ for the two-liquid interface to reach the discharge valve 4 is input to the multiplier 18 connected to the second distance setting device 19 that generates a digital signal indicating the distance L _{2 .}
is obtained by Δt ₂ =L ₂ ×S, and after converting this into a binary signal, it is input to a down counter 21 connected to a high-precision clock oscillator 20, and subtraction is performed using the clock signal of the clock oscillator 20.
A control signal for closing the discharge valve 4 is generated when the value reaches zero.

From the multiplier 18 described above to the down counter 2
1 constitutes a closing time determining means for the discharge valve 4. Note that 5 is a sample container.

To explain the operation of the embodiment device having such a configuration, a control signal is inputted from the control device 12 to the sample injection/gas vent valve opening/closing device 3, the valve is opened, and after water and hexane are injected into the separation container 2, the valve is closed. to close. A control signal is applied from the control device 12 to the rotation device 7, the rotation arm 1b is rotated 180 degrees, and the separation container 2 is rotated by 180 degrees.
Next, a control signal is applied from the control device 10 to the reciprocating motion generating device 6 to cause the arm 1a to perform reciprocating motion, mixing and stirring the water and hexane in the liquid separation container 2, and after a predetermined time. make it stop.
Applying a control signal to the rotation device 7 again, the liquid separation container 2 is rotated to return to the initial state shown in the figure.
The mixture is left to stand for a predetermined period of time, and water and hexane are separated in the liquid separation container 2.

Applying a control signal from the control device 12 to the discharge valve 4,
Open the discharge valve 4 and start extracting water into the sample container 5. As a result, the two-liquid interface descends, and when it passes the first detector and the second detector, the detection signal is input to the control device 12 via the lead wire, and the two-liquid interface is lowered as described above. The speed S of is detected by the speed determining means, and then the discharge valve closing time Δt ₂ is determined by the discharge valve closing time determining means, and Δt ₂
After a period of time, a control signal is input from the control device 12 to the discharge valve 4, and the discharge valve 4 is closed. This results in
Only water is collected into the sample container 5. Next, after a predetermined period of time has elapsed, a control signal for opening the discharge valve 4 is input to the discharge valve 4, the discharge valve 4 is opened, and hexane is fractionated into a new sample container 5.

Next, a flowchart for controlling the apparatus of this embodiment will be explained based on FIG. In addition,
The steps in the flowchart are shown in the figure.

First, the control device 12 is started, and in step, a control signal is applied to the sample injection/gassing valve opening/closing device 3, the valve is opened, and the sample is injected into the separation container 2, and then the valve is closed. In step, a control signal is applied to the rotating device 7 to invert the liquid separating container 2. In step, a control signal is input to the reciprocating motion generating device 6 to apply reciprocating motion to the liquid separating container 2. In step, the operation of reciprocating motion generating device 6 is stopped, and in step, a control signal for returning liquid separation container 2 to the initial position is input to rotating device 7. In step, a control signal is input to the discharge valve 4, the discharge valve 4 is opened, and the water in the liquid separating container 2 is discharged. In steps and, passage of the two-liquid interface is detected by the first detector and the second detector, and in step, the speed S of the two-liquid interface is determined by the speed determining means. In step, the discharge valve closing time determining means determines the closing time of the discharge pipe valve 4, and in step, a control signal for closing the discharge valve 4 is applied to extract only water. In step, a control signal is generated to reopen the discharge valve 4, the discharge valve 4 is opened, and hexane fractionation is started.

In the description of the device of this embodiment, only two liquids are injected into the liquid separation container 2, but
The invention is not limited to this, and even if three or more types of liquids are mixed, as long as they have different specific gravity and do not mix with each other, solvent extraction can be performed accurately.

(f) Effects As explained above, according to the present invention, the first and second detectors are arranged at a predetermined distance apart from each other in the discharge pipe portion of the separation container, and the first and second detectors are arranged at a predetermined distance from the second detector. Since the configuration includes a discharge valve, a means for determining the speed of the boundary liquid level, and a means for determining the time for the boundary liquid level to reach the discharge valve, the liquid must be separated and extracted from the liquid separating container. Accurate solvent extraction can be performed even if the liquids have different viscosities.

[Brief explanation of the drawing]

Figure 1 is a functional block diagram of the present invention, Figure 2 is an overall configuration diagram of an embodiment of the automatic solvent extraction device of the present invention,
FIG. 3 is a block diagram of a circuit device for determining the velocity of the boundary liquid level and the closing time of the discharge valve in the control device shown in FIG. 2, and FIG. 4 explains the operation of the device shown in FIG. 2. It is a flowchart. 1 is a liquid separation container holding device, 1a is an arm, 1b is a rotating arm, 1c is a pedestal, 2 is a liquid separation container, 2a and 2b are the introduction part and discharge pipe of the liquid separation container 2, 3 is a sample injection/gas vent Valve opening/closing device, 4 is a discharge valve, 5 is a sample container, 6 is a reciprocating motion generator, 7 is a rotating device, 8
and 9 are photosensors, 10 and 11 are light emitting diodes, is a first detector consisting of the photosensor 8 and the light emitting diode, is a second detector consisting of the photosensor 9 and the light emitting diode 11, 12 is a control device,
13 is a flip-flop, 14 and 20 are clock oscillators, 15 is an AND gate, 16 is a first distance setter, 17 is a divider, 18 is a multiplier, 19 is a second distance setter, and 21 is a down counter. .

Claims (1)

[Claims for Utility Model Registration] A separation container into which a plurality of liquids having different specific gravities and which do not mix are injected; a first detector and a second detector for detecting a boundary liquid level; a discharge valve provided at a predetermined distance from the second detector along the discharge pipe; and the first detector. An automatic solvent extraction device comprising: speed determining means for determining the speed of the boundary liquid level from the output of the second detector; and discharge valve closing time determining means for determining the time at which the boundary liquid level reaches the discharge valve.