JP2001264221A - Sampling device of dioxin - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sampling device capable of collecting dioxins existing in water without generating plugging of a collection part, shortening a collection time, and separating an analytical extract at a water sampling place. SOLUTION: This sampling device is characterized by mounting detachably a vessel for storing a sample therein, a stirrer for stirring the inside of the vessel, and a collection means on the outlet of the vessel. The device is also characterized by mounting detacbably a solid phase for extraction on the downstream side of the collection means.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to dioxins existing in water ("dioxins" defined in Article 2 of the Law No. 105 of 1999, "Special Measures against Dioxins", A polychlorinated dibenzofuran, polychlorinated dibenzo-para-dioxin, and coplanar-polychlorinated biphenyl).

[0002]

2. Description of the Related Art Conventionally, the measurement of the concentration of dioxins contained in river water, lake water, seawater, wastewater, etc. has been carried out by a sampling step of sampling a predetermined amount of a sample at a sampling point and a sampling step. Filter the sample, extract the filtration residue,
The filtrate is subjected to solid-phase extraction or liquid-liquid extraction, that is, a separation step of separating an extract for analysis, a cleanup step by Soxhlet extraction of the extract obtained in the separation step, and a cleanup step. It is performed by an analysis step of performing mass spectrometry on the extract by gas chromatography.

Meanwhile, the solid-phase extraction generally performed in the separation step is generally performed by a solid-phase extraction device as shown in FIG. This solid-phase extraction device comprises a disk-shaped solid phase 32 (silica gel having octadecyl groups chemically bonded thereto, hereinafter referred to as "ODS32") between a funnel 30 and a base 31, a support screen 33, a gasket. This device is provided with a clamp 34 and the like. This device is
The sample flows into the funnel 30 and is sucked from the downstream side of the base 31 by a suction device (not shown), whereby the ODS 32, the support screen 33, and the gasket 3
4, flow into the base 31, and at this time, SS particles and colloid particles are collected by the ODS 32.

That is, in the filtration in the separation step,
By filtering the collected sample, a suspension fraction (eg, SS particles) larger than the retained particle size of the filter paper (about 0.5 μm) is collected. Thereafter, the solid phase extraction device is used to adsorb the ODS32 to collect the colloid particles and the like of the dissolved fraction. However, the colloid particles are liable to be clogged because some particles are larger than the ODS 32, so that the collection time is prolonged due to a decrease in the processing flow rate and the ODS 32 needs to be replaced.

[0005] Further, even when a method of passing a sample through a polyurethane foam (hereinafter referred to as "PUF") instead of the ODS 32 is used, clogging is liable to occur as in the case of using the ODS 32. Therefore, it is necessary to prolong the collection time due to a decrease in the processing flow rate and to replace the PUF.

[0006] Further, the sample collected in the sampling step is
Generally, it is transported to an analysis room which performs a process after the above-mentioned separation step by putting it into a water sampler of a predetermined capacity. Therefore, mass transportation of the sample is required (in the case of environmental water (river water, seawater, etc.), the minimum sampling amount is 20 liters), so the transportation cost is high, and dioxins during transportation are high. There is a problem that it is adsorbed to a glass bottle or the like, and a washing operation for the glass bottle or the like is added thereto, and the glass bottle may be damaged during transportation.

[0007]

SUMMARY OF THE INVENTION In view of the above-mentioned problems, the present invention makes it possible to collect dioxins present in water without causing clogging of a collecting section, and to shorten the collecting time. It is another object of the present invention to provide a sampling device capable of separating an extract for analysis at a water sampling place. That is, an object of the present invention is to provide a sampling apparatus capable of simultaneously sampling a sample at a sampling place and separating an extract for analysis.

[0008]

Means for Solving the Problems The present invention has been made to solve the above problems, and the invention according to claim 1 has a container for accommodating a sample and a stirring device for stirring the inside of the container. A collecting means is detachably attached to the body and the container outlet.

Further, the invention according to claim 2 is characterized in that a solid phase for extraction is detachably mounted downstream of the collecting means.

[0010]

Next, an embodiment of the present invention will be described. INDUSTRIAL APPLICABILITY The present invention can be suitably implemented for sampling for measuring the concentration of dioxins in water. The present invention has a configuration in which a container for accommodating samples such as environmental water and drainage, a stirrer for stirring the inside of the container, and a collecting means are detachably attached to an outlet of the container.

[0011] The agitator mixes the flocculant and the coagulant charged for flocculating the SS particles, colloid particles and the like in the sample to promote floc formation. That is, by stirring, the flocculant is uniformly mixed with the sample, the reaction rate between the flocculant and the SS particles or colloid particles is increased, and floc formation is promoted.

Further, PUF, cylindrical filter paper, filter paper, filter cloth, etc. can be used as a means for collecting floculated SS particles, colloid particles, and the like. It is suitable.

Further, it is preferable that the filtrate after passing through the collecting means is further passed through a solid phase for extraction (such as ODS or PUF (polyurethane foam)). According to this configuration, it is possible to more reliably adsorb the colloid particles and the like containing dioxins in the dissolved fraction. In this case, since the floculated SS particles and colloid particles are collected by the collecting means, clogging of the solid phase for extraction can be reduced. This allows
The collection rate of SS particles and colloid particles containing dioxins can be further increased.

[0014]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, specific embodiments of the present invention will be described in detail with reference to the drawings. FIG. 1 is an explanatory view schematically showing a first embodiment of the present invention.

In FIG. 1, the sampling apparatus according to the present invention has, as a basic configuration, a container 1 for accommodating a sample, a stirrer 2 for stirring the inside of the container 1, and a detachably attached outlet of the container 1. The apparatus includes a collection means 3 mounted thereon and a suction device 4.

The container 1 contains a predetermined amount of a sample, such as river water, which is water to be measured at a sampling point.
It is configured to be portable so that it can be carried to the collection site. Since this type of concentration measurement is to measure the concentration of a predetermined amount of sample, the container 1 is provided with a water level detecting means (not shown) such as an appropriate measurement scale or a ball tap. . Here, it is desirable that the container 1 can accommodate at least a 20 liter sample. This is generally
This is because the amount of environmental water collected is approximately 20 liters. The material of the container 1 is not particularly limited, and a stainless steel container or a container coated with Teflon (registered trademark) is preferably used. This is to prevent the substance to be measured from adsorbing on the inner wall of the container 1. Further, the container 1 has, inside thereof,
Since the flocculant is used to flocculate SS particles and the like present in the sample due to the action of the flocculant, it is designed so that the sample and the flocculant are easily mixed.

Next, the agitator 2 is an apparatus for agitating the inside of the vessel 1 containing a predetermined amount of a sample such as river water, which is water to be measured, at a water sampling place. And the stirring body 2
Is equipped with a stirring blade 5 driven by a motor (not shown) to improve the stirring efficiency. Here, a predetermined amount of the sample is accommodated in the container 1, and after adding the flocculant into the container 1, the flocculant is uniformly present in the sample by stirring at a high speed. Thereafter, by stirring at a low speed, flocculation of SS particles, colloid particles and the like contained in the sample is promoted by the action of the flocculant. Further, it is preferable that the agitator 2 is detachably attached to the container 1, so that it is easy to carry, and it is easy to perform operations such as pre-washing and post-washing.

Next, the trapping means 3 will be described. The trapping means 3 is a device for trapping floculated SS particles, colloid particles and the like. The specific configuration of the collecting means 3 will be described first with reference to the embodiment shown in FIG. In this embodiment, a PUF (polyurethane foam) 6 and a three-layer cylindrical filter paper 7 (100 μm, 6 μm,
0.6 μm).

The collecting means 3 is detachably mounted on the mounting flange 8 of the container 1, and comprises a collecting container 9, a PUF 6, and a support 10 for loading the cylindrical filter paper 7. And both are detachable. First, the support body 10 has
An accommodating section 11 for loading the PUF 6 is defined. The accommodation portion 11 is formed by a cylindrical rising portion 12 that protrudes from the upper surface of the support 10 at an appropriate height. Then, in the support 10, a portion defined by the rising portion 12, that is, the accommodation portion 1.
A number of holes 13, 13,... Through which the sample having passed through the PUF 6 flows down are formed at the bottom of 1. On the other hand, a mounting support section 14 for mounting the cylindrical filter paper 7 in a fitted state is provided on the lower surface side of the support 10. The mounting support portion 14 has a cylindrical shape having substantially the same diameter as that of the rising portion 12 and is configured to hang down from the lower surface of the support body 10 as appropriate.

Here, the mounting of the collecting means 3 on the container 1 will be described. First, on the lower surface side of the support 10, the cylindrical filter paper 7 is mounted in a state fitted to the mounting support portion 14. In this state, it is stored in the collection container 9. In this case, it is preferable that the cylindrical filter paper 7 is tightly fitted to the mounting support portion 14. Next, the PUF 6 is loaded into the storage section 11. The outer edge of the mounting flange 8, the outer edge of the support 10, and the flange 15 of the collection container 9 are integrated at a plurality of locations in the circumferential direction via bolts and nuts (not shown). To be connected.

As described above, according to the collecting means 3 attached to the outlet of the container 1, the inside of the container 1
The sample containing floculated SS particles and the like was prepared using the PUF6
Thus, a large floc is collected, that is, roughing is performed, and flows down into the cylindrical filter paper 7 through the holes 13. The sample that has flowed into the cylindrical filter paper 7 reliably collects small flocs that have passed through the PUF 6 by the cylindrical filter paper 7 having a three-layer structure. At this time, since the sample is roughened by the PUF 6, the sample can be filtered in a relatively short time without causing clogging.

Therefore, according to the collecting means 3 shown in FIG. 2, it is possible to surely collect the SS particles and the colloid particles in the sample, and of course, it becomes detachable from the container 1. Therefore, the exchange of the PUF 6 and the cylindrical filter paper 7 can be performed simply and easily.

Next, another embodiment of the collecting means 3 will be described with reference to FIG. 3, the same reference numerals as those in FIG. 2 denote the same members as those in FIG. 2, and a detailed description thereof will be omitted.

The collecting means 3 shown in FIG. 3 basically comprises the PUF 6 and a single-layer or multi-layer filter paper 16. In this embodiment, the PUF 6 has a relatively large thickness. In this case, the PUF 6 is loaded in the collection container 9 in a state where the PUF 6 is placed on the first support 17 disposed near the lower portion of the collection container 9. The first support 17 is preferably relatively rigid and porous, and for example, a gasket is used. Further, it is preferable that the PUF 6 in this embodiment has a concave shape as shown by an imaginary line in FIG. Of course, also in this embodiment, the mounting flange 8 and the flange portion 15
It is detachable by the same method as the embodiment of FIG.

The filter paper 16 used in the collecting means 3 in FIG.
m, one layer, 100 μm, 6 μm,
In some cases, there are three layers of 0.6 μm, which are appropriately selected according to the implementation. In the illustrated embodiment, 100 μm, 6 μm,
One having a thickness of 0.6 μm has three layers.

The filter paper 16 is provided in the collection container 9.
Is mounted in a filter paper container 18 which is detachably attached to the lower part of the filter paper container. That is, the filter paper container 18 is configured to be detachable and integrally connected to the lower flange 19 of the collection container 9 (specific description is omitted), and the filter paper 16 is formed of the filter paper In the container 18, it is loaded while being placed on a second support 20 disposed near the lower portion of the filter paper container 18. This second support 20 is also
As with the first support 17, the gasket or the like is used.

Here, the mounting of the collecting means 3 to the container 1 in the embodiment of FIG. 3 will be described. First, the filter paper 16 is loaded into the filter paper container 18 and the filter paper container 18 is attached to the lower flange. Connect with 19. Next, the collection container 9 loaded with the PUF 6 is integrally connected to the mounting flange 8 via the flange portion 15.

Therefore, according to the collecting means 3 shown in FIG. 3, as in the case of the collecting means 3 shown in FIG. That is, roughing is performed, and it flows down into the filter paper container 18. The sample that has flowed into the filter paper container 18 reliably collects small flocs that have passed through the PUF 6 by the filter paper 16 having a three-layer structure. At this time, since the sample is roughened by the PUF 6, the sample can be filtered in a relatively short time without causing clogging.

Next, still another embodiment of the collecting means 3 will be described with reference to FIG. 4, the same reference numerals as those in FIGS. 2 and 3 denote the same members as those in FIGS. 2 and 3, and a detailed description thereof will be omitted.

The collecting means 3 shown in FIG. 4 basically includes the filter cloth 21 (100 μm to 10 μm) and the PUF.
6 and 3 layers of the filter paper 16 (100 μm, 6 μm, 0.6
μm). In this embodiment, the filter cloth 21 is provided upstream of the PUF 6 of the collecting means 3 shown in FIG. The filter cloth 21 is not particularly limited, and cellulose fibers and Teflon fibers are used, and fibers whose surfaces are processed with ODS (fixed silica gel having octadecyl groups chemically bonded) are preferably used. Used. In this case, the filter cloth 21
Is loaded in a state of being sandwiched between the mounting flange 8 and the flange portion 15.

Here, the PUF6 shown in FIG.
The filter paper 16 is the same as that in the embodiment of FIG.

The mounting of the collecting means 3 to the container 1 in the embodiment of FIG. 4 will be described. First, the filter paper 16 is loaded into the filter paper container 18 and the filter paper container 18 is connected to the lower flange 19. connect. Next, after loading the PUF 6 into the collection container 9, the filter cloth 2
1 is placed in the collection container 9, and then both ends of the filter cloth 21 are sandwiched between the flange portion 15 and the mounting flange 8, and are integrally rolled with the mounting flange 8 via the flange portion 15. Tie.

Therefore, according to the collecting means 3 shown in FIG. 4, as in the case of the collecting means 3 shown in FIGS. Large flocs are collected by the PUF 6, that is, roughened, and flow down into the filter paper container 18. The sample that has flowed into the filter paper container 18 reliably collects small flocs that have passed through the filter cloth 21 and the PUF 6 by the filter paper 16 having a three-layer structure. At this time, the sample was the filter cloth 21 and the PUF
6, the sample can be filtered in a relatively short time without clogging.

Next, the suction device 4 for controlling the collecting flow rate in the collecting step will be described. The suction device 4 includes:
When the suction force is strong, the collection flow speed is high, and when the suction force is low, the collection flow speed is low. That is, if the trapping flow rate is too fast, the flocculated SS particles and colloid particles are forcibly pulled out from the trapping means 3, so that the flow-down amount increases and the trapping amount decreases. Conversely, if the collection flow rate is too slow, the collection time will be long. Therefore, the collection flow rate is a speed at which the collection amount does not decrease.
And it is necessary to keep the speed taking into account the collection time. Here, the collection flow rate by the suction device 4 is 0.5 to 20.
It is preferably 1 liter / minute, more preferably 2 to 10 liter / minute. The suction device 4 is not particularly limited, and a suction device 4 that matches the collection flow rate is used.

Further, a second embodiment of the present invention will be described with reference to FIG. In FIG. 5, the same reference numerals as those in FIG.
It is the same as the member of FIG. 1, and a detailed description thereof will be omitted.

In the second embodiment, the collecting means 3
The extraction solid phase 22 is detachably mounted between the downstream side of the suction device 4 and the upstream side of the suction device 4. This extraction solid phase 22 is applied with a conventionally known one.
Detailed description is omitted.

According to the second embodiment, the extraction solid phase 22 adsorbs the dioxin-containing colloid particles and the like of the dissolved fraction which has passed through the collecting means 3 in the first embodiment. . In this case, since the flocculated suspension fraction is collected by the collecting means 3, clogging of the solid phase for extraction 22 can be prevented. Furthermore, by providing the extraction solid phase 22 detachably on the downstream side of the collecting means 3, the collected dissolved fraction can be easily taken out.

[0038]

As described above, according to the present invention, dioxins present in water can be collected without clogging of the collecting section, and the collecting time can be shortened. Separation of the extract for analysis at the sampling point becomes possible. This is effective for simplifying the transportation work from the water sampling place to the analysis room and reducing the transportation cost, and can contribute to the overall efficiency in measuring the concentration of dioxins contained.

[Brief description of the drawings]

FIG. 1 is a schematic sectional explanatory view showing a first embodiment of the present invention.

FIG. 2 is a schematic sectional explanatory view showing a specific example of a collecting means in the present invention.

FIG. 3 is a schematic sectional explanatory view showing another specific example of the collecting means in the present invention.

FIG. 4 is a schematic sectional explanatory view showing still another specific example of the collecting means in the present invention.

FIG. 5 is a schematic sectional explanatory view showing a second embodiment of the present invention.

FIG. 6 is an explanatory diagram of a conventional solid-phase extraction device (extraction unit).

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Container 2 Stirred body 3 Collection means 22 Solid phase for extraction

Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat II (Reference) B01D 29/01 B01D 29/04 510A 510D 520E 530Z (72) Inventor Hiroshi Nakamura 7 Horie-cho, Matsuyama-shi, Ehime Miura Kogyo Co., Ltd. In-house (72) Inventor Nobuyasu Seike 7 Horie-cho, Matsuyama-shi, Ehime Miura Industrial Co., Ltd. F-term (reference) 4D017 AA01 BA04 CA05 CA13 CA14 CB05 DA01 DB02 EA05

Claims (2)

[Claims] 1. A container 1 for accommodating a sample, a stirrer 2 for stirring the inside of the container 1, and a collecting means 3 at an outlet of the container 1.
A dioxin sampling device characterized by having a detachably mounted. 2. An extraction solid phase 2 downstream of the collecting means 3.
2. The dioxin collection device according to claim 1, wherein 2 is detachably mounted.