JPH06180273A - Method and device for collecting sample - Google Patents

Abstract

PURPOSE:To accurately measure a trace amount of content in a sample without being affected by atmosphere or outside environment by assigning an ampoule in a housing vessel and allowing the sample to flow into the housing vessel through pipings. CONSTITUTION:An ampoule 1 is put in a housing vessel 2, and is sandwitched with an upper lid 3 and a lower lid 4, and then clasping force is adjusted by an adjustment screw 6 so that presser rings 7a and 7b are inserted for attachment, and then fixed with a clip 5. Then pure water, used as a sample, is overflowed from a condensing pore, through a piping 8a, the housing vessel 2 and a piping 8b. Then a tip of the ampoule 1 is bent by way of the lower lid 4, for the pure water to be sucked into the ampoule 1, and then the ampoule 1 is taken out of the housing vessel 2 without delay, for stirring. At that time, for the purpose of suppressing the effect from the gas in the atmosphere, the entire housing vessel 2 is put in the water tab with pure water overflowed, and the lower lid 4 of the vessel 2 is opened for stirring without delay. Then, by using colorimetry, the quantity of dissolved oxygen is measured.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample collection technique for measuring the concentration of dissolved gas in liquid or gas,
It is used in the semiconductor field where it is necessary to measure an extremely small amount of gas, and in the industrial field which is carried out using biological reactions such as fermentation and brewing.

[0002]

2. Description of the Related Art Conventionally, as shown in FIG. 4, a sample is introduced from a condensing port through a rubber tube 10 into a sampling jig called a sampling tube 12 such as a funnel for 500 to 10 minutes.
While the sample is overflowing at a rate of 00 ml / min, a sample collection bottle (hereinafter referred to as “ampoule”) 1 containing a reagent is put in a vacuum state, and the ampoule 1 is pushed from the upper part to the tip of the ampoule 1. Fold it in half and make an ampoule 1
Aspirate the sample inside. Next, after putting a rubber cap on the opening of the ampoule 1 and pressing it with a finger to stir the sample and the reagent inside, after that, as shown in FIG. 5, compared with the standard color for colorimetry, the same color or The method to read the display value of a close color is used.

FIG. 4 is a diagram showing a conventional sample collecting method, FIG. 5 (a) is a diagram showing a colorimetric method when the color of the sample is dark, and FIG. It is a figure which shows the colorimetric method at the time of thin. In addition, in FIG. 4, 11 shows a water tank.

[0004]

In the above-mentioned prior art,
Since the method of sucking the sample by folding the tip of the ampoule 1 while overflowing the sample was adopted, the sample comes into contact with the atmosphere, and the components in the atmosphere (mainly nitrogen,
Oxygen, carbon dioxide, and other substances such as chemical substances and metals such as suspended mist and foreign substances) were adsorbed or mixed in, and the target substances (elements and components) requiring analysis in the sample were contained in the atmosphere. In this case, an error occurs, which is a serious problem especially when a trace amount of component is analyzed.

Further, in order to prevent adsorption or mixing of the target component from the atmosphere due to contact with the atmosphere, the flow rate of the sample is increased to reduce the rate of mixing from the atmosphere due to adsorption or the like. However, because of that, a large amount of sample will be wasted out, and even if a large amount of sample is flowing, when trying to analyze a very small amount of components, the amount of components from the atmosphere due to adsorption will be greater. In some cases, the analysis error will be very large.

An object of the present invention is to provide a means for accurately measuring a trace component in a sample without being affected by the atmosphere or the external environment.

[0007]

The sample collecting method of the present invention according to claim 1 is a sample in which the inside is in a vacuum state, contains a reagent, and is partially opened by applying an external force. In a sample collecting method in which the opening of the collection bottle is set in the sample, the opening is formed by applying an external force, and the sample is sucked into the sample collection bottle, the sample is flowed. It has a sample inlet and outlet to which a pipe is connected, is cylindrical and has a shorter length than the sample collection bin, and at least one end can open a part of the sample collection bin by an external force. A storage container for the sample collection bottle, which is provided with a lid made of removable rubber having a moderate softness, is provided, the sample collection bottle is arranged in the storage container, and the sample is stored through the pipe. Pour into container and overflow After that, by applying an external force through the lid, a part of the sample collection bottle is opened, the sample is sucked into the sample collection bottle, the lid is removed, and the sample collection bottle is removed. Is taken out, and the sample and the reagent are stirred.

Further, in the sample collecting apparatus of the present invention as set forth in claim 2, the inside of the sample collecting bottle is in a vacuum state, contains a reagent, and is partially opened by an external force. A place to be an opening is installed in the sample, the opening is formed by applying an external force, and the sample collecting device used when performing the sample collection for sucking the sample into the sample collection bottle, It has a sample inlet and outlet to which a pipe for flowing a sample is connected, is cylindrical and has a shorter length than the sample collection bin, and at least one end is part of the sample collection bin due to an external force. It is characterized by having a container for the sample collection bottle, which is provided with a lid made of a removable rubber having a softness capable of opening.

Further, in the sample collecting method of the present invention as set forth in claim 3, the inside of the sample collecting bottle is in a vacuum state, contains a reagent, and is partially opened by applying an external force. In a sample collecting method in which a place to be an opening is installed in a sample, the opening is formed by applying an external force, and the sample is sucked into the sample collecting bottle, the sample is flown, and an external force is applied. By arranging the sample bottle in a rubber tube having a softness such that a part of the sample collecting bottle can be opened, and flowing the sample into the rubber tube,
After overflowing, a part of the sample collection bottle is opened by applying an external force through the rubber tube, the sample is sucked into the sample collection bottle, and the sample is collected from the end of the rubber tube. The collecting bottle is taken out, and the sample and the reagent are stirred.

[0010]

By using the present invention, the sample can be sucked into the sample collecting bottle without contacting with the atmosphere, and the sample collecting bottle can be immediately taken out and stirred.

[0011]

EXAMPLES The present invention will be described in detail below based on examples.

FIG. 1 is an external view of a sample collecting apparatus according to an embodiment of the present invention as set forth in claim 2, and FIG. 2 is a structure of a container for holding a sample collecting bottle and a fixing jig in the sample collecting apparatus. FIG. 3 shows a sample collecting process chart of one embodiment of the present invention as set forth in claim 3.

As shown in FIGS. 1 and 2, a sample collection bottle (hereinafter referred to as "ampoule") 1 is placed inside a sample collection bottle storage container (hereinafter referred to as "storage container") 2 and is stored therein. The upper and lower sides are sandwiched by the upper lid 3 and the lower lid 4, and are fixed by a fixing jig including a clip portion 5, an adjusting screw portion 6 and pressing rings 7a and 7b. Further, pipes 8a and 8b are connected to a sample introduction port 21 for introducing the sample and a sample introduction port 31 for extracting the sample, which are provided in the storage container 2. The upper lid 3 and the lower lid 4 are made of rubber and also serve as packing for the storage container 2. Further, the lower lid 4 has a soft structure such that the tip of the ampoule 1 can be grasped from the outside of the lower lid 4 by hand so that the tip of the ampoule 1 can be broken without touching the atmosphere.

Next, a sample collection method for dissolved oxygen in pure water according to an embodiment of the present invention will be described.

First, an ampoule 1 (commercially available, for example, a product name "CHEMets" or the like is used) is put in a storage container 2 as shown in FIGS. 1 and 2, and an upper lid 3 and a lower lid 4 are placed.
Adjust the tightening amount with the adjusting screw 6 and presser ring 7a
And 7b are inserted and fixed with the clip 5. Since the ampoule 1 needs to be stirred immediately after sucking the sample, the clip 5 is used so that it can be easily taken out from the storage, but a screw type may be used.

Next, the sample is passed from the condensate port through the pipe 8a, the storage container 2 and the pipe 8b, and the sample is 500 ml / min to 1000 ml.
Overflow at a rate of / minute. At this time, the pipe 8b
Is sufficiently long so that dissolved oxygen does not flow backward, and a sample outlet of the pipe 8b is preferably a narrow-necked flask 9 so that contact with the atmosphere is suppressed as much as possible. Immediately after the ampoule 1 is placed in the storage container 2 and pure water, which is a sample, starts flowing, the gas adsorbed on the surface of the ampoule 1 is dissolved in pure water to change the analysis value.
It is preferable to collect pure water after flowing pure water for measurement for 0 minutes or more. In this embodiment, glass is used as the container 2 to confirm the position of the ampoule 1, whether bubbles or the like are generated in the pure water, or to confirm the flow of the sample. For this purpose, it is preferable to use metal, nylon or the like, which does not easily transmit or adsorb oxygen.

Next, the tip of the ampoule 1 is folded through the lower lid 4 so that pure water is sucked into the ampoule 1, and immediately the ampoule 1 is pressed.
Is taken out from the storage container 2 and stirred. At this time, in order to suppress the influence of gas in the atmosphere, it is preferable that the storage container 2 and the storage container 2 are placed in a water tank in which pure water has overflowed and the lower lid 4 of the storage container 2 is opened and immediately stirred.

Thereafter, the amount of dissolved oxygen is measured by using the conventional colorimetric method.

Further, the present invention is not limited to the method of directly collecting pure water from the pipe as in the above-mentioned embodiment. By collecting pure water, it is feasible and requires less pure water than the conventional method.

As an embodiment of the present invention as set forth in claim 3, as shown in FIG. 3, the ampoule 1 is inserted into the rubber tube 10, pure water is flowed for about 30 minutes, and overflowed in the water tank 11. After that, the method of applying force through the rubber tube 10 to fold the tip of the ampoule 1 and sucking pure water, remove the rubber tube 10 from the condensate port, take out the ampoule 1 and agitate is also the same as the above embodiment. The same effect can be obtained.

[0021]

As described above in detail, by using the present invention, it is possible to collect the sample in the ampoule without mixing the gas in the atmosphere into the sample. Gas analysis becomes possible.

Since there is no adsorption of gas in the atmosphere, the sample flow rate for measurement can be reduced.

Furthermore, by using the present invention according to claims 1 and 2, the sample can be sucked into the ampoule, and then the part stopped by the clip can be warmed, so that the ampoule can be taken out and immediately stirred.

[Brief description of drawings]

FIG. 1 is an external view of a sample collection device according to an embodiment of the present invention.

FIG. 2 is a configuration diagram of a container for a sample collection bottle and a fixing jig in the sample collection device.

FIG. 3 is a sample collection process chart of another embodiment of the present invention.

FIG. 4 is a diagram showing a conventional sample collection method.

FIG. 5A is a diagram showing a colorimetric method in the case where the color of the sample is dark. (B) is a figure which shows the colorimetric method when the color of a sample is light.

[Explanation of symbols]

 1 Sample Collection Bottle 2 Sample Collection Bottle Storage Container 3 Upper Lid 4 Lower Lid 5 Clip 6 Adjusting Screw 7 Holding Ring 8 Piping 9 Flask 10 Rubber Tube

Claims (3)

[Claims] 1. The inside of the sample is placed in a vacuum state, contains a reagent, and is provided with an external force to set a portion of the sample collection bottle, which is partially opened, to be the opening, in the sample,
Forming the opening by applying an external force, in a sample collecting method for sucking the sample into the sample collecting bottle, having a sample inlet and outlet to which a pipe for flowing the sample is connected, A cylindrical lid having a shorter length than the sample collection bottle, and at least one end made of a removable rubber having a softness such that an external force can open a part of the sample collection bottle, A storage container for the sample collection bottle is provided, the sample collection bottle is arranged in the storage container, the sample is flowed into the storage container through the pipe, and after overflowing, an external force is applied via the lid. Opening a portion of the sample collection bottle by adding
A method for collecting a sample, which comprises sucking the sample into the sample collecting bottle, removing the lid, taking out the sample collecting bottle, and stirring the sample and the reagent. 2. The inside of the sample is placed in a vacuum state, the reagent is contained therein, and a portion which becomes the opening of the sample collection bottle in which a part is opened by applying an external force is installed in the sample. In the sample collection device used when performing the sample collection by forming the opening by adding the sample into the sample collection bottle, the sample inlet to which the pipe for flowing the sample is connected, and A removable rubber having an outlet, having a cylindrical shape, having a length shorter than that of the sample collection bottle, and having at least one end soft enough to open a part of the sample collection bottle by an external force. A sample collecting device, comprising: a container for storing the sample collecting bottle, which is provided with a lid. 3. A sample collection bottle having a vacuum inside, containing a reagent, and partly opened by applying an external force, is provided in the sample so as to provide the external force. A sample collecting method in which the opening is formed by adding the sample and the sample is sucked into the sample collecting bottle. In the sample collecting method, a part of the sample collecting bottle can be opened by flowing the sample or applying an external force. A part of the sample collection bottle is arranged by arranging the sample collection bottle in a rubber tube having a softness, flowing the sample into the rubber tube, causing the sample to overflow, and then applying an external force through the rubber tube. Opening the sample collection bottle, the sample is sucked into the sample collection bottle, the sample collection bottle is taken out from the end of the rubber tube, and the sample and the reagent are stirred. .