JPH08261889A - Device for sampling sample-liquid - Google Patents

Abstract

PURPOSE: To make possible the image sampling of high concentration slurry solution by providing a means for contacting and absorbing sample liquid to a sampling part and a liquid supply means for leading the sample liquid exuded by contacting it with pressure and pressing it, and setting a plurality of exchangeable filter member in a filter part. CONSTITUTION: A sampling part 20 has a rotation body 21 provided with a permeating member 24 for permeating and absorbing sample liquid 40 and its rotation means. A liquid sending pipe 22 is provided sidewards of the rotation body 21, the member 24 is pressed with pressure, the sample liquid 40 is exuded and it is sent to a filter part 30. The filter part 30 has a plurality of filter members 31, which is detachably mounted on a rotatable support base 32. Because the sample liquid is permeated and sampled, for instance, even if the sample liquid 40 in the form of slurry of high concentration such as sediment exists, a load of the filter member 31 is small, and a filtering capacity is not lowered for a long time.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample liquid sampling device for analysis. More specifically, the present invention relates to a sampling device that can continuously sample and filter a sample liquid in the form of a slurry containing a residue to prepare a sample liquid for analysis.

[0002]

2. Description of the Related Art In zinc hydrometallurgy, an electrolytic solution is produced by cleaning the leachate through several steps of purification. This liquid purification step is performed for the purpose of removing the impurity metal that deteriorates the electrolysis efficiency in the subsequent electrolysis step, and the concentration analysis of the impurity metal is also performed in this step. Conventionally, as a method of analysis, a part of the electrolytically purified liquid is manually pumped out individually, and a residue (precipitate, etc.) is filtered, followed by concentration analysis. Therefore, it takes time to collect the required number of sample liquids for analysis, and continuous analysis is difficult.
Furthermore, this purified solution has a high precipitate concentration and is slurried, and when filtering with a filter paper, the filter paper is clogged with residues in a short time, and the filter paper must be replaced frequently, so the analysis work It is extremely complicated.

The present invention solves the above-mentioned problems of the prior art and continuously collects and filters a high-concentration slurry solution that causes clogging of filter paper with residue in a short period of time for analysis. It is an object of the present invention to provide a sampling device that uses a suitable sample solution.

[0004]

According to the present invention, a sample liquid can be collected separately from a residue by using a means for collecting a high-concentration slurry solution in a collecting portion.
Further, by arranging the filter media in the filtration portion so that they can be exchanged sequentially, it is possible to continuously sample even a high-concentration slurry solution. That is, according to the present invention, there is provided a sample liquid sampling apparatus having the following configuration.

(1) A sampling device having a sample liquid sampling part and a filtering part for filtering the sample liquid sampled, wherein the sample liquid is brought into contact with the sample liquid to impregnate the sample liquid. Means for absorbing the liquid and means for feeding the sample liquid pressed against the absorbing means and leached by the pressure to the filtering portion are provided, and the filtering portion is supplied from the liquid feeding means. A plurality of exchangeable filter members for sequentially receiving the sample liquid are arranged, and the sampling device. (2) The absorbing means is formed by a rotating body having a member on which the sample solution permeates and the rotating means, and the rotating body is rotated with the permeating member being in contact with the liquid surface of the sample solution. The device according to (1). (3) The liquid feeding means is made of a pipe material, an upper opening end of the liquid feeding pipe is pressed upward against the permeating member, and a plurality of filtering members are sequentially fed below the lower opening of the liquid feeding pipe.
The device according to (2). (4) The device according to any one of (1) to (3) above, wherein the filtering member is formed of a filter paper and a cloth material that covers the filter paper.

[0006]

[Detailed Description] A sample liquid sampling apparatus according to the present invention comprises a sampling unit for sampling the sample liquid and a filtering unit for filtering the sample liquid sampled. The sampling part is provided with a means for sampling a part of the sample liquid and supplying it to the filtering part. That is, (a) means for contacting and absorbing the sample solution and absorbing the sample solution, and (b) pressure contact with the absorbing means in the sampling section,
A liquid feeding means is provided for guiding the sample liquid leached from the absorbing means by this pressing to the filtering section. In addition, (c) in the filtration section
A plurality of exchangeable filter members that sequentially receive the sample liquid supplied from the liquid supply unit are provided.

The means for impregnating and absorbing the sample liquid can be formed by a rotating body having a member (permeation member) through which the sample liquid permeates, and the rotating means. The rotating body is arranged so as to rotate while the permeating member on the surface is in contact with the liquid surface of the sample liquid. As the material of the permeation member, a material that sufficiently penetrates the sample solution and is inactive to the sample solution is used, and for example, a sponge material made of glass fiber or other inorganic fiber can be used.

Suitable commercially available products are sponge-like filtering materials or air filters used in aquariums for ornamental fish, and inorganic fiber quake-proof materials used when shipping small precision equipment. Although a commercially available synthetic resin sponge has an advantage of being excellent in water absorption, it is not suitable for the above-mentioned permeation member because it cannot cope with a high temperature and is easily deteriorated by a chemical change.

As a concrete shape of the absorbing means, a rotating body having a permeation member attached to the outer peripheral surface of a disk or a cylinder is used. When collecting a large amount of sample liquid, it is preferable to use a cylindrical body so that a wide outer peripheral area can be obtained.
Further, a structure may be adopted in which support plates are provided on both sides of the disk-shaped permeation member so that the sample liquid penetrates into the inside of the rotating body. Further, a belt-shaped member having a permeation member on the surface can also be used. Appropriate means such as a motor can be used as the rotating means of the rotating body.

The liquid feeding means provided in the sampling portion is for feeding the sample liquid that has penetrated into the permeating member on the surface of the rotating body to the filtering portion, presses against the permeating member, and permeates by this pressing. A flow path is formed to receive the sample solution and guide it to the filtering section. As a specific configuration example, a pipe material (liquid feed pipe) is used, and the upper opening end of the liquid feed pipe is pressed upward against the permeation member, and the sample liquid leached from the permeation member flows into the upper opening. The lower end of the liquid supply pipe is provided so as to open to the filtration section. As the material of the liquid feeding pipe, a glass pipe or the like is suitable so as not to be attacked by the sample liquid, and the pipe end should be opened obliquely toward the permeation member so that the leached sample liquid can easily flow into the pipe. . According to the structure using such a liquid supply pipe, the liquid supply means and the means for pressing the permeation member can be used in common, and the device structure is simplified. The pressing means of the permeating member and the liquid feeding means may be formed separately.

Further, the rotating body may be provided with means for scraping off and removing the residue attached to the permeation member. The removing means is provided, for example, under the contact portion between the permeation member and the liquid supply pipe while being in pressure contact with the permeation member. By this means, it is possible to prevent scraps adhering to the surface of the permeating member from being scraped off every time the rotating body makes one revolution, and to prevent the residue from accumulating on the surface.

A plurality of filter members are exchangeably provided in the sample liquid filtering section. As the filtering member, a glass funnel fitted with filter paper is generally used, but the surface of the filter paper may be covered with cloth as a means for surely preventing clogging of the filter material. As the cloth, towels and other absorbent materials are suitable. By wrapping the filter paper with cloth,
Since most of the residue in the supplied sample liquid is captured by the cloth, clogging of the filter paper due to the residue is effectively prevented. The cloth is not limited to the front side of the filter paper, but the entire filter paper may be wrapped with the cloth and may be interposed between the filter paper and the funnel. In this case,
Since the sample liquid is guided over the upper end of the filter paper and between the filter paper and the funnel due to the capillary phenomenon of the cloth, the filtration efficiency is improved.

Since the above-mentioned filter member performs continuous filtration, a plurality of filter members are replaceably provided. As a specific configuration example, it is preferable that a plurality of filter members be detachably installed on a rotatable support so that the individual filter members are alternately fed to the drainage port of the liquid feed pipe in sequence. It is possible to automatically rotate a series of operations from the collection of the sample solution to the filtration by interlocking the rotation of the support provided with the rotating body and the filtering material provided in the sample solution collecting section through the control means.

[0014]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An example of the apparatus of the present invention shown in the drawings will be specifically described below. FIG. 1 is a schematic perspective view showing an example of a sampling device according to the present invention. In the illustrated device configuration, the sampling device 10 includes a sampling unit 20 for sampling the sample liquid 40 and a filtering unit 3 for filtering the sample liquid 41 collected.
0 is provided. As shown in FIG. 2, the sampling unit 20 has a rotating body 21 provided with a permeation member 24 for impregnating and absorbing the sample liquid 40, a liquid feeding pipe 22, and a rotating means 25 for rotating the rotating body 21. As shown in FIG. 3, the rotating body 21 is provided with support plates 23 having a diameter smaller than that on both sides of a thick disk-shaped infiltrating member 24, and the infiltrating member 24 has a shape protruding to the outer periphery of the rotating body 21, It has a structure in which this is integrated by screwing or the like.

A liquid tank 41 containing a sample solution 40 is provided below the rotating body 21, and the rotating body 21 is positioned perpendicular to the sample solution 40 and penetrates a part of its outer periphery. The member 24 is installed at a height at which it is slightly immersed in the sample liquid 40.
Further, a plate-shaped removing tool 28 for scraping off the residue is attached to the upper surface of the side of the liquid tank 41, and the tip of the removing tool 28 is provided in pressure contact with the permeation member 24. The rotating body 21
Is rotatably supported by rotating means 25.

A liquid delivery pipe 22 made of glass is disposed on the side of the rotating body 21. The liquid feed pipe 22 is a permeation member 24.
The rotating body 2 has both a function of pressing the sample liquid to ooze out the sample liquid and a function of sending the leached sample liquid to the filtering unit 30.
1. The penetrating member 2 is provided so as to face upwards and has its upper end.
4, the upper end 26 of the liquid feeding pipe 22 is formed obliquely along the outer periphery of the rotating body 21 so that the exuded sample liquid can easily flow into the pipe. It is open toward.

Further, the inlet 26 of the liquid supply pipe 22 is provided so as to face the rotating direction of the rotating body 21. in this case,
Since the portion of the permeation member 24 containing the sample liquid is located above the inlet 26, the sample liquid permeated by the pressure of the permeation member 24 easily flows into the inlet 26. When the liquid supply pipe 22 is provided at a position which is open upward toward the rotation direction side on the opposite side to this, the permeating member 24 containing the sample liquid is pressed at the lower side of the inlet, so that the sample leached out. It is not preferable because the liquid does not flow into the pipe but flows downward. Outlet 2 of liquid supply pipe 22
7 is open to the filtration unit 30.

FIG. 4 shows an outline of the filtering section 30. Filter part 3
Reference numeral 0 has a plurality of filtering members 31, and the filtering member 31 is detachably installed on a rotatable support base 32. In the illustrated example, the support base 32 is formed by a disk-shaped rotary base 38 supported by a vertical rotary shaft 39 and its rotating means 33, and the plurality of filtering members 31 are arranged on the rotary base 35 along the circumference. Are installed at equal intervals. These filter members 31 are connected to the outlet 27 of the liquid supply pipe 22 by the rotation of the support 32.
It is continuously fed to the lower side of the. In addition, the filtering member 3
A liquid feed path 50 for guiding the filtered sample liquid to an analyzer (not shown) is provided below the position where 1 is sequentially fed, and the upper end inlet of the liquid feed path 50 is formed in a funnel shape. ing.

As shown in FIG. 5, the filter member 31 comprises a glass funnel 36 and a filter paper 34 attached to it, but preferably, the filter paper 34 is covered with a cloth 35. The cloth 35 is preferably a cloth having good permeability such as towel cloth, and in the illustrated example, the cloth 35 is covered with the cloth 35 from the front side of the filter paper 34 beyond the upper end to the back side between the funnels 36.

[0020]

When the rotor 21 comes into contact with the liquid surface of the sample liquid 40 containing the residue, the sample liquid 40 penetrates into the permeation member 24 of the rotor 21. When the rotator 21 rotates and the portion where the sample liquid 40 is soaked reaches the portion where the liquid sending pipe 22 is provided, the sample liquid 40 is soaked by pressing the liquid sending pipe 22. The leached sample liquid flows into the pipe from the inlet 26 of the liquid feed pipe 22, and is guided to the filtration unit 30 through the liquid feed pipe 22. At this time, when the sample liquid 40 is in the form of a slurry containing a large amount of residue, the residue remains on the surface but most of the residue remains in the liquid tank 4.
1, the sample liquid 40 mainly soaks into the permeation member 24, so that the sample liquid 40 separated from the residual substance flows into the liquid feed pipe 22 and the concentration of the residual substance of the sample liquid 40 sent to the filtering unit 30. Is significantly reduced.

In the filtering section 30, the sample liquid is supplied to the liquid feed pipe 22.
From the outlet 27 to the filtering member 31 and is filtered. While the sample solution passes through the filter paper 34 at this filtering portion,
The residue contained in the sample solution is captured by the cloth 35 wrapping the filter paper 34, further separated from the residue by the capillary phenomenon and transmitted through the cloth 35 and guided to the back side of the filter paper 34 through the gap with the funnel 36. It flows down to the liquid feeding path 50.

When the filtering capacity of the filtering member 31 is lowered, the rotation of the support 32 causes a new filtering member 31 to be sent to the lower side of the outlet 27 of the liquid supply pipe 22, and this is repeated sequentially. The used filtering member 31 is removed from the supporting base 32 and a new filtering member 31 is mounted while the supporting base makes one rotation. The supply amount of the sample liquid supplied to the filtration unit 30 can be adjusted by the rotation speed of the rotating body 21,
It can be controlled according to the filtering ability of the filtering member 31. Further, the replacement time of the filter member 31 is adjusted by the rotation speed of the support 32. If necessary, the rotations of the rotating body 21 and the support base 32 are interlocked with each other via a control means, and are intermittently operated by a timer or the like at regular intervals.

[0023]

[Example of use] Using the device shown in Fig. 1, as a sample liquid containing residue, the second purified liquid (liquid temperature 60 to 70
℃, residue (dry weight) concentration 30g / l, specific gravity 1.37 ~ 1.41g / cm
³ ) was collected at a flow rate of 15-20 ml / min and filtered.
As the permeation member, a disc-shaped PVC sponge with a diameter of 110 mm was sandwiched between discs with a diameter of 90 mm and integrated, and rotated at a rotation speed of 30 to 40 rpm. A glass tube was used. Also, as the filtering member,
The filter paper with the front and back surfaces covered with a towel cloth was used by mounting it on a funnel.

As a result, the residue concentration (dry weight) of the sample liquid collected by the liquid feeding tube was 3 to 5 g / l, and the concentration of the residue was significantly lower than that of the stock solution. A sample solution of 7200 ml per member could be filtered in 8 hours. The concentration of residue in the sample liquid after filtration was below the detection concentration. Also, the cloth covering the filter paper could be washed and reused after use. When the stock solution was directly supplied to the filtration member without using this sampling device, the filtration rate suddenly decreased when the sample solution exceeded 200 ml, and it took 4 hours to filter 400 ml of the sample solution. spent.

[0025]

[Test example] As a filtering member, (1) a sample in which only filter paper is mounted on the funnel, (2) a sample in which the surface of the filter paper is covered with cloth, (3)
A sample in which the cloth was directly used instead of the filter paper, and (4) a sample in which the front surface and the back surface of the filter paper were covered with the cloth, respectively, and the aqueous solution having the composition and properties shown in the following table was used,
The filtration efficiency was tested for each filter member when supplied to the filter member at ml / min. As a result, in any of the above (1) and (2) samples, the filter paper became clogged, resulting in poor filtration in about 30 minutes.
The sample of (3) above could be continuously filtered for 5 hours.
The filtration time per operation required about 200 seconds on average. on the other hand,
The sample of the above (4) was capable of continuous filtration for 10 hours, and the average filtration time per time was about 20 seconds, and the filtration time was significantly shortened.

[0026]

[Table 1]

[0027]

The sampling device of the present invention uses means for impregnating and absorbing the sample liquid and collecting it.
Even if the concentration of the residue is extremely high and the sample liquid is in the form of a slurry, the burden on the filtration portion is small and the filtration performance does not decrease for a long time. Further, since the filter member is provided so as to be replaceable, continuous filtration processing can be performed. Further, by using a filter material in which the filter paper is covered with a cloth, the durability of the filter material is improved to about 20 times that of the filter paper, and the filtration time is significantly shortened.
Such a sampling device of the present invention is suitable for continuous sampling of a slurry solution having a high concentration of residue such as a zinc smelting and purification process, and is simple in configuration because the device has a simple structure.

[Brief description of drawings]

FIG. 1 is a schematic perspective view showing a specific example of the device of the present invention.

FIG. 2 is a partial schematic view of a sampling unit.

FIG. 3 is an exploded perspective view of a penetrating member.

FIG. 4 is a partial schematic view of a filtering unit.

FIG. 5 is a schematic sectional view of a filtering member.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 10 ... Sampling device, 20 ... Collection part, 21 ... Rotating body, 22 ... Liquid supply pipe, 30 ... Filtration part, 31 ... Filtration member, 4
0 ... Sample solution.

Claims (4)

[Claims] 1. A sampling device comprising a sample liquid sampling section and a filtering section for filtering the sample liquid sample,
Means for contacting the sample liquid in the collecting section to soak the sample solution for absorption, and liquid feeding means for pressing the absorbing solution into the sample unit and guiding the sample solution permeated by the pressure to the filtering section. And a plurality of exchangeable filter members for sequentially receiving the sample liquid supplied from the liquid supply means are provided in the filtering unit. 2. An absorbing means is formed by a rotating body having a member for permeating the sample solution on its surface and its rotating means, and the rotating body is rotated while the permeating member is in contact with the liquid surface of the sample solution. The device according to claim 1, wherein 3. The liquid feeding means is made of a pipe material, an upper opening end of the liquid feeding pipe is pressed against the permeating member upward, and a plurality of filtering members are sequentially fed to the lower side of the lower opening of the liquid feeding pipe. The device according to claim 2, which is provided. 4. The apparatus according to claim 1, wherein the filter member is formed of a filter paper and a cloth material that covers the filter paper.