JP2004093194A - Column treatment apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To automate the connection of a supply route to an exhaust route by preventing a clogging and installing a specimen water feeding pump capable of accurately feeding specimen water. <P>SOLUTION: To arrest and extract trace harmful substances in the specimen water a containing SS, this column treatment apparatus comprises at least a feed route 21 feeding the specimen water a, pure water b as washing fluid, and methanol d as extract, a feeding route 22 feeding nitrogen gas c as heating gas, a discharge route 61 connected to discharge pumps p3, p4, and p5, and columns 5 detachably disposed thereon. A specimen water feeding means 4 constantly feeding the specimen water by using the depressurization and pressurization of gas by a syringe pump is disposed in the specimen water feed route 21. <P>COPYRIGHT: (C)2004,JPO

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an improvement of a pretreatment device that captures and extracts harmful components as a pretreatment for measuring trace harmful components contained in sewage, industrial wastewater, environmental water, and the like, and is particularly used for on-site monitoring. It relates to a pretreatment device that can be used.
[0002]
[Prior art]
Conventionally, various types of wastewater such as inflow sewage, first sinking runoff water, secondary treated water, effluent, factory drainage, road drainage, and various environmental waters such as river water, lake water, groundwater, seawater, etc. Often contains harmful substances. These harmful substances include environmental hormones, dioxins, PCBs, PAHs (polycyclic aromatic hydrocarbons), pesticides and the like.
[0003]
In order to measure these harmful substances, it is necessary to capture, extract and concentrate specific harmful substances from sample water containing a large amount of solids and impurities such as SS. Method is used. The applicant of the present application has proposed a solid phase extraction method suitable for such a purpose and a column packed with a solid phase filler used for the purpose as a patent application of 2001-315478.
[0004]
The outline thereof will be described with reference to FIG. 5. In the solid-phase extraction column 1, the upper layer is filled with the SS capturing material 11, and the lower layer is filled with the solid-phase filler 12. From above, a sample water pump 13, a pure water pump 14, A supply path connected to a methanol pump 15, a hot air purge 16 and the like is connected, and a switching valve 1a, a dehydration pump 17, a main pump 18, and a recovery pump 19a (hereinafter, connected to a concentration / solvent adjustment 19b and a detector 19c) are connected below. Is connected).
[0005]
The method of capturing and extracting the harmful substances is generally as follows. First, sample water is introduced into the solid phase extraction column 1, and the SS adsorbed and dissolved components of the substance to be measured are captured by the upper SS capturing material 11 and the lower solid phase filler 12, respectively. Next, the column 1 is washed with pure water or methanol, and the dehydration pump 17 is operated while supplying hot air from the hot air purge 16 to dry the inside of the column 1. Next, an extract of an organic solvent such as acetone, methanol, or dichloromethane is introduced into the column 1 to extract the trapped components.
[0006]
However, when automating such a column processing apparatus, the following problems occurred. First, there is a problem that the sample water pump 13 for feeding the sample water containing a considerable amount of SS is easily clogged and cannot be used stably, and the amount of the supplied liquid cannot be accurately controlled. Second, a supply path such as a sample water pump 13, a pure water pump 14, a methanol pump 15, a hot air purge 16, a discharge path such as a switching valve 1a, a dehydration pump 17, a main pump 18, a recovery pump 19, and a column. Each time, it was necessary to manually establish a connection with 1.
[0007]
[Problems to be solved by the invention]
The present invention has been made in order to solve the above-described problems, and has a sample water feed pump capable of preventing sample clogging and accurately feeding sample water, and connecting the supply path and the discharge path. To provide a column processing apparatus capable of automating the process.
[0008]
[Means for Solving the Problems]
In order to capture and extract trace harmful substances in sample water containing SS, the above problems are at least a feed route that feeds sample water, a washing solution, a warming gas and an extract, and a discharge route such as a discharge pump. A column processing apparatus having a column detachably disposed in a feeding socket connected to the feeding path and a discharging socket connected to a discharging path, a space in which the column can be moved. In the space, there is provided a transport means capable of loading and unloading the column, and the sample water supply path is supplied with a fixed amount of sample water by depressurizing and pressurizing gas. This problem can be solved by the column processing apparatus according to the present invention, in which a sample water supply unit is provided.
[0009]
And, the present invention can be embodied in a form in which the sample water supply means sucks a fixed amount of sample water into the trap by depressurization of the syringe pump, and discharges a fixed amount of the sample water from the trap by pressurization. The conveying means is preferably embodied in the form of a turntable, a traveling conveyor, or a gantry capable of moving forward and backward.
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
Next, an embodiment of the column processing apparatus of the present invention will be described with reference to FIGS.
In order to capture and extract trace harmful substances in the sample water a containing SS, the column processing apparatus of this embodiment supplies at least the sample water a, pure water b as a washing liquid, and a methanol d extraction liquid. A column having a feed path 21 for feeding nitrogen gas c as a heating gas, a discharge path 61 connected to discharge pumps p3, p4, p5, and the like, and a column 5 detachably provided to these. Processing device. The feed path 21 also serves as a feed path for the sample water a, the pure water b, and the extract methanol d, but each may be individually installed. Although the pump p2 and the path 23 for supplying the conditioning methanol e are provided here, the supply path 21 for supplying the extract methanol d may also be used.
[0011]
Next, the features of the present invention will be described separately for items relating to a sample water supply unit and items relating to a column transport unit.
(Sample water supply means)
First, the feature of the present invention resides in that a sample water feeding means 4 for quantitatively feeding sample water by depressurizing and pressurizing gas with a syringe pump or the like is provided in the sample water feeding path 21. Specifically, as shown in FIG. 2, the sample water supply means 4 sucks a fixed amount of sample water a into the trap 41 by depressurizing the syringe pump p1 via the air reservoir 41c (the upstream valve 41a). Is opened, and the downstream side valve 41b is closed), and the syringe pump p1 and the trap 41 are combined so as to discharge a fixed amount from the trap 41 by pressurization (close the valve 41a and open the valve 41b).
[0012]
According to such a sample water feeding means 4, since the sample water can be sucked and discharged through the air reservoir 41c, the pump is not clogged and the sample water is not contaminated by the pump. In addition, since the syringe pump is used, the sample water can be accurately fed. Further, by programming the suction and discharge operations of the syringe pump p1 and the opening and closing operations of the valves 41a and 41b, there is an advantage that the operation of the pump can be easily automated.
[0013]
(Column transport means)
Next, the column transport means will be described with reference to FIGS.
In this embodiment, the feeding socket 2 connected to the feeding paths 21, 22, 23, etc., and the discharge socket 6, which can be moved up and down, connected to the discharging path 61 are connected via a space in which the column 5 can be moved. It is characterized in that the transport means 3 which can be loaded and unloaded by mounting the column 5 is provided in the space. As the transfer means 3, an appropriate transfer device such as a turntable, a traveling conveyor, or a gantry capable of moving forward and backward can be used.
[0014]
Then, the column 5 at the position shown in FIG. 3 is conveyed, loaded immediately below the feed socket 2, and, for example, positioned using an optical sensor, the lower discharge socket 6 is raised, and the discharge path 61 is provided. A socket port 62 communicating with the column 5 is pressed against the lower discharge nozzle 51 of the column 5 and fitted with sealing with an O-ring or the like so that the discharge path 61 can be connected without leaking liquid. Then, the sample water a and the heated nitrogen gas c are supplied to the column 5 carried immediately below from the supply ports 21a, 22a, and 23a of the supply paths 21, 22, and 23 provided in the supply socket 2. Can be sent. The feed socket 2 is connected to a release path 24 for opening the inside of the column 5 to the atmosphere. A liquid level sensor can be fixed to the open path 24 so as not to completely block the path.
[0015]
The feed socket 2 is preferably arranged so as to cover the upper surface of the column 5, but need not be close to the upper surface of the column.
Thus, as described in detail below, predetermined operations such as capturing and extracting harmful components can be performed on the column 5. When these processes are completed, the discharge socket 6 is lowered, the socket port 62 is detached from the lower discharge nozzle 51 of the column 5, and the connection with the discharge path 61 can be cut off. By operating, the used column 5 can be unloaded and a new column 5 can be loaded.
[0016]
Here, a column operation procedure will be described with reference to FIGS.
(1) Column setting: The column 5 (filled with a solid phase filler) is set on the transport means 3 such as a turntable.
(2) Loading of the column: The column 5 is moved between the supply and discharge sockets 2 and 6, and the discharge socket 6 is raised and connected to the column 5.
(3) Conditioning of the column: methanol e and pure water b are fed to the column 5 and discharged as a drainage f through a discharge path 61 by pump suction.
[0017]
(4) Capture of target substance: A predetermined amount of sample water is poured into the column 5 by the sample water supply means 4, the target substance is captured in the column 5, and the remainder is simultaneously pumped out as drainage f and taken out. .
(5) Washing of the column: Pure water b is supplied to the column 5 to wash the inside, and as a drainage f, it is taken out by pump suction.
(6) Dehydration and drying of the column: The heated nitrogen gas c is supplied to the column 5, and at the same time, the inside is dehydrated and dried by pump suction as the drain h in the discharge path 61.
[0018]
(7) Extraction of the target substance: A predetermined amount of the extract liquid methanol d is fed to the column 5 and retained in the column for a predetermined time to extract the target substance. Then, it is taken out as a recovery liquid g and sent to an analyzer (not shown).
(8) Unloading of the column: The discharge socket 6 is removed, the used column is unloaded, and a new column is loaded. Hereinafter, these operations are repeated.
[0019]
Here, in order to prevent the sample water and its components from adsorbing and remaining in the equipment such as pipes and contaminating the next sample water, after removing the used column, a column for cleaning the equipment (nothing is filled) (Empty column) is carried in, and the apparatus is preferably washed with pure water b, methanol d or the like every time. After the device cleaning, the column for device cleaning is carried out, a new column is carried in, and the subsequent operations are performed.
[0020]
According to the combination of the column conveying means 3, the supply socket 2, and the discharge socket 6 described above, a series of harmful substance capturing and extracting operations of the above (1) column setting to (8) column unloading and repetition thereof. The advantage is that the operation can be programmed and automated.
[0021]
Further, according to the present invention, the following preferable technical advantages can be obtained.
(1) Since the inside of the column 5 is released under the atmospheric pressure, both the feed path and the discharge path have to be tightly connected to the column in the case of the conventional closed system. It is only necessary to tightly connect one discharge path, so that the configuration of the apparatus becomes extremely easy and the cost can be significantly reduced.
(2) Since the operation of the supply path and the discharge path can be operated at a low pressure (under the atmospheric pressure), this also causes a cost reduction.
[0022]
(3) Countermeasures against clogging in the column are facilitated. In the conventional closed system, an expensive pressure sensor was required, and there was a risk of liquid leakage due to an increase in the internal pressure. The rise in the liquid level may be detected by a liquid level sensor, which simplifies the configuration of the device and is particularly advantageous in terms of cost.
[0023]
(4) The amount of liquid retained in the column can be freely varied. In the column operation, it is necessary to eliminate the liquid on the way and then store the required amount. Specifically, a dehydration / drying operation and an extraction operation are performed. This has the advantage that the target substance can be efficiently extracted and recovered without mixing water.
[0024]
【The invention's effect】
Since the column processing apparatus of the present invention is configured as described above, the sample water supply pump can accurately supply the sample water without clogging, and automation becomes easy. In addition, since the connection between the column, the supply path, and the discharge path is simple, automation of the entire column processing apparatus is also facilitated.
[0025]
Further, since the column is released under the atmospheric pressure, there is an excellent effect that the entire apparatus can be simplified as compared with the conventional closed system, and the cost becomes advantageous. Therefore, the present invention has a very large practical value as a column processing apparatus which can solve the conventional problems and can be used for on-site monitoring.
[Brief description of the drawings]
FIG. 1 is a main block diagram showing an embodiment of the present invention.
FIG. 2 is a main block diagram showing a sample water supply pump.
FIG. 3 is a schematic cross-sectional view of a main part for describing loading and unloading of a column.
FIG. 4 is a schematic cross-sectional view of a main part for describing a mounting state of a column.
FIG. 5 is a configuration block diagram of a column processing apparatus.
[Explanation of symbols]
2 feed socket, 21 feed route, 22 feed route, 23 feed route, 24 release route, 3 transport means, 4 sample water feed means, 41 trap, 41a, 41b valve, 41c air reservoir, 5 columns, 51 lower discharge nozzle, 6 discharge socket, 61 discharge path, 62 socket opening, a sample water, b pure water, c nitrogen gas, d extract methanol, e conditioning methanol, p1 syringe pump, p2 pump, p3, p4, p5 Discharge pump.

Claims (3)

In order to capture and extract trace harmful substances in the sample water containing SS, at least a feed path for feeding the sample water, washing liquid, warming gas and extract, and a discharge path such as a discharge pump, are detachably provided to them. A column processing apparatus having a column provided, wherein a feed socket connected to the feed path and a discharge socket connected to a discharge path are arranged vertically via a space in which the column can be moved. The space is provided with transport means capable of loading and unloading the column, and the sample water supply path is provided with a sample water supply for quantitatively supplying sample water by decompression and pressurization of gas. A column processing apparatus, wherein means is provided. 2. The column processing apparatus according to claim 1, wherein the sample water supply means sucks a fixed amount of the sample water into the trap by reducing the pressure of the syringe pump and discharges the sample water from the trap by increasing the pressure. 3. The column processing apparatus according to claim 1, wherein the column transport unit is a turntable, a traveling conveyor, or a pedestal capable of moving forward and backward.

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