JPH10153531A - Method and apparatus for sampling liquid sample - Google Patents

Abstract

PROBLEM TO BE SOLVED: To make it possible to safely and efficiently sample a liquid sample by taking the sampling liquid in an isolated state into a sampling chamber, which has a partition wall to the outside partially made of rubber while being made separable from a bypass through an open/close valves and then, an injection needle is stuck into the partition wall to sample the liquid into an injector. SOLUTION: A bypass 4 is branched off on the upstream side from a valve 2b to be converged on the downstream side from the valve 2b and arranged in parallel with a pipeline 1. Valves 5a and 5b are arranged in the path of a bypass 4, closed to allow the interruption of a sampling chamber 6 and the branched point and the converged point are linked by a link part 7 through a valve 5c immediately before the valves 5a and 5b. A sampling port 6a is protrusively arranged at the center of the sampling chamber 6 and a partition wall 8 made of rubber is provided at an open end thereof. A hole 9a is bored in a lid 9 piercing it at the center of a contact surface with the partition wall 8 and the injection needle 12a of the injector 12 is inserted thereinto. The injection needle 12a is stuck into the partition wall 8 made of rubber to sample a specimen from the sampling chamber 6 and an injection mark of the partition wall 8 is closed elastically. This method enables safely and efficiently sampling of the specimen.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for collecting a liquid sample, and more particularly to a method for safely and efficiently collecting a liquid hazardous substance or a toxic substance, or a liquid sample containing a dangerous substance or a toxic substance. The present invention relates to a method and an apparatus for collecting.

[0002]

2. Description of the Related Art In the process of manufacturing chemical substances, various liquids such as raw materials, products, intermediates, and by-products are stored in tanks or flow through pipelines. Are periodically collected, and quality control is performed by inspecting this sample using an analytical instrument such as gas chromatography analysis or infrared absorption spectrum analysis.

Conventionally, when collecting a sample from a liquid-containing device system such as the above-mentioned tank or pipeline, a sample collection port is provided in the device system, and a sample is collected from this collection port into a glass bottle or a plastic container. Had been subjected to analysis.
However, in the sample collection method described above, since the sample is exposed to the outside air, if the liquid is a dangerous substance or a harmful substance, or if the liquid contains such a substance, it is harmful to the human body and the environment is polluted. In addition, there is a problem that the handling is complicated and the working efficiency is reduced. For example, when the sample is chlorosilanes or organochlorosilanes, chlorosilanes and organochlorosilanes are corrosive hazardous substances exhibiting strong acidity,
Hydrogen chloride gas emitted from this reacts with moisture in the atmosphere to become hydrochloric acid, emitting a strong pungent odor. Since this hydrogen chloride gas and hydrochloric acid have a bad effect on the human body, it is necessary for workers to wear protective equipment, and it is necessary to enhance ventilation equipment such as a draft device. Corrosion easily occurs in external equipment of the built-in device system. In addition, the instruments used for collecting such a dangerous substance liquid need to be thoroughly washed each time.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to make it possible to safely and efficiently collect a sample from a liquid hazardous substance or a toxic substance, or an apparatus system containing a liquid containing these substances. An object of the present invention is to provide a method and an apparatus for collecting a liquid sample.

[0005]

According to the liquid sampling method of the present invention which achieves the above object, a bypass is divided into an apparatus system containing a liquid to be collected, and the bypass can be isolated via an on-off valve. And, using a collection device provided with a collection chamber made of rubber with a part of the partition wall to the outside, after separating the liquid to be collected into the collection chamber in an isolated state, the liquid to be collected to the partition wall It is characterized in that a syringe needle is pierced and pulled out into a syringe.

[0006] As described above, the liquid to be collected is separated from the bypass into the collection chamber in an isolated state, and an injection needle is inserted into a rubber partition wall constituting a part of the collection chamber to extract a sample from the collection chamber. The septum after removing the injection needle automatically closes the injection mark by the elastic force of rubber, so that the sample can be collected without exposing the sample to the outside air. Therefore, a liquid containing a dangerous substance or a toxic substance can be safely sampled, and after collection, the sample collected in the syringe can be directly used for analysis, so that the working efficiency can be improved.

In the liquid sample collecting apparatus according to the present invention, which achieves the above object, a bypass is provided in an apparatus system containing the liquid to be collected, and the bypass can be isolated via an on-off valve. A collection chamber in which a part of the partition wall is made of rubber is provided, and the liquid to be sampled is drawn by piercing the partition wall with a syringe needle attached to a syringe.

[0008] According to the sample collecting apparatus configured as described above, it is possible to carry out the above collecting method.

[0009]

FIG. 1 shows an example of an apparatus for collecting a liquid sample according to the present invention. In the figure, in a pipeline 1, valves 2a to 2d are inserted at an interval from each other, and a pump 3 is inserted between valves 2b and 2c, and these valves 2a to 2d and pump 3
Thereby, the flow of the liquid in the pipeline 1 is controlled.

On the other hand, the bypass 4 is provided in parallel with the pipeline 1 with a branch point on the upstream side of the valve 2b and a return point on the downstream side of the valve 2b. This bypass 4
Is provided with valves 5a and 5b in its path, and connects the sampling chamber 6 which can be cut off from the pipeline 1 by closing these valves 5a and 5b, and the branch point and return point of the bypass 4 to the valves 5a and 5b. And a connecting portion 7 connected via a valve 5c immediately before. Further, one end of the sampling chamber 6 is provided with a valve 5d for degassing, and the other end is provided with a valve 5e for draining.

As shown in FIGS. 2 to 4, a sampling port 6a communicating with the sampling chamber 6 protrudes from the center of the sampling chamber 6, and a rubber partition wall 8 is formed at the open end of the sampling port 6a. Is arranged. The partition 8 is detachably attached to the outer end of the sampling port 6a so as to be replaceable, and a lid 9 screwed to this outer end is provided.
To hold the open end of the sampling port 6a in a liquid-tight manner. The lid 9 has a hole 9a passing through the center of the contact surface with the partition wall 8, and the syringe 12 is inserted through the hole 9a.
Of the injection needle 12a is inserted. The injection needle 12a penetrates the partition wall 8 made of rubber and reaches the inside of the collection chamber 6.

A pair of handles 9b are provided on the outer peripheral surface of the lid 9 at right angles to the direction of the rotation axis of the lid 9, and the lid 9 can be rotated by the pair of handles 9b to firmly tighten the lid 9. I have. A lid 11 is screwed to an outer end of the lid 9 with an O-ring 10 made of an elastic body interposed therebetween. Next, a method for collecting a sample from the liquid flowing through the pipeline 1 using the above-described collection device will be described.

When the process including the pipeline 1 is in a normal operation state, the valve 5c of the bypass 4 is opened and the valves 5a, 5b, 5d and 5e are closed, and the liquid flowing through the pipeline 1 is bypassed. 4 through the connecting portion 7. And when you take a sample,
The valve 5c of the bypass 4 is closed and the valve 5c is closed.
The liquid is introduced into the collection chamber 6 of the bypass 4 by opening a and 5b.

After the predetermined time has elapsed and the liquid in the collection chamber 6 has been almost completely replaced, the valve 5c of the bypass 4 is opened again and the valves 5a and 5b are closed. As a result, the sampling chamber 6 of the bypass 4 is cut off from the pipeline 1, and the latest state of liquid is stored therein. The time required for replacing the liquid in the collection chamber 6 can be determined based on the flow rate of the liquid in the collection chamber 6, the length of the collection chamber 6, and the like, or from the temperature change in the collection chamber 6. It is also possible to know.

Next, as shown in FIG. 4, the lid 11 is removed, the injection needle 12a of the syringe 12 is pierced into the rubber partition 8 through the hole 9a of the lid 9, and the tip of the injection needle 12a is inserted into the collection chamber 6. Intrusion. After the liquid in the collection chamber 6 is drawn into the syringe 12, the injection needle 12 a is connected to the partition wall 8.
Sampling is completed by extracting from the. The injection mark on the partition wall 8 is spontaneously closed almost simultaneously with the removal of the injection needle 12a by the elastic force of the rubber. After the sample is collected, a rubber stopper is attached to the tip of the injection needle 12a, the sample is transported so as not to be exposed to the atmosphere, and the sample is directly injected from the syringe 12 into an analytical instrument such as gas chromatography.

According to the sampling method using the above-described sample collecting device, the injection needle 12a is pierced into the rubber partition wall 8 to extract a sample from the collection chamber 6, and the injection mark of the partition wall 8 is formed by the elastic force of the rubber. Since it can be closed, a sample can be collected from the liquid flowing through the pipeline 1 without exposing it to the outside air. Therefore, even if the liquid flowing through the pipeline 1 is a dangerous substance such as chlorosilanes or organochlorosilanes or a liquid containing these, a sample can be safely collected from the pipeline 1. After the sample is collected, the syringe 1
Since the sample collected in 2 can be used for analysis as it is, there is no need to wash the collection container or collect the excessively collected sample as in the conventional case, and the work efficiency can be improved. Further, when the liquid in the pipeline 1 is a corrosive liquid, the generation of corrosive gas can be prevented, so that the external equipment including the pipeline 1 is hardly corroded.

Although the partition wall 8 made of rubber can be used repeatedly, it is physically deteriorated by repeatedly piercing the injection needle 12a, or the pipeline 1 is not used.
Since it is chemically degraded by reacting with the liquid, it needs to be replaced periodically according to the frequency of use. When replacing the bulkhead 8 in the above-mentioned sampling device, the valve 5 of the bypass 4
With the a and 5b closed and the collection chamber 6 shut off from the pipeline 1, the valve 5d for degassing and the valve 5e for draining are opened, and the liquid in the collection chamber 6 is discharged. Thereafter, the partition 9 can be replaced by removing the lid 9.

In the present invention, the kind of rubber constituting the partition 8 is appropriately selected from those having high corrosion resistance according to the properties of the liquid flowing through the pipeline 1. In particular, hydrochloric acid, sulfuric acid,
For nitric acid, chlorosilanes, organochlorosilanes and the like and corrosive liquids containing them, fluorine rubber such as propylene hexafluoride / vinylidene fluoride copolymer,
It is preferable to use an acid-resistant rubber such as polyepichlorohydrin rubber, chlorosulfonated polyethylene, butyl rubber, and ethylene / propylene rubber. Among these, a propylene hexafluoride / vinylidene fluoride copolymer is preferable. By using the above-mentioned acid-resistant rubber against a corrosive liquid to extend the life of the partition wall 8, the workability is further improved.

FIG. 5 shows another embodiment of the sample collecting apparatus of the present invention. 5, the open end of the sampling port 6a is closed by a wall 13, and a hole 13a is provided at the center of the wall 13, that is, at a position facing the hole 9a of the lid 9. The hole 9a of the lid 9 and the hole 13a of the wall portion 13 are each formed such that the inside diameter is smaller than the outside diameter and expand from the inside to the outside. The partition 8 has a projection 8a formed at a position corresponding to the hole 13a of the wall 13 so that the projection 8a is aligned with the hole 13a so as to be sandwiched between the wall 13 and the lid 9. Is held.

In the above-described embodiment, the partition wall 8 is held so as to be sandwiched between the wall portion 13 and the lid 9, and the injection needle 12 is held.
Since the deformation of the partition 8 at the time of insertion of a is regulated,
The bending fatigue of the partition 8 can be reduced, and the liquid tightness can be improved. In addition, the partition 8 having the convex portion 8a has the hole 13
Since the position corresponding to a is selectively thickened, its liquid tightness can be effectively improved. Further, since the hole 9a of the lid 9 and the hole 13a of the wall portion 13 are formed so as to expand from the inside to the outside, even if the inside diameter on the high-pressure side is reduced, the large-diameter outside is not removed. Injection needle 12
a can easily pierce the partition wall 8, and the tip can be easily guided into the collection chamber 6.

In the above-described embodiment, a case where a liquid sample is collected from a pipeline has been exemplified. However, the present invention can be similarly applied to a liquid stored in a tank. The collection method of the present invention as described above allows a sample to be safely and efficiently collected from a device system containing a liquid containing a liquid dangerous substance, a harmful substance, and the like, and in particular, monochlorosilane, dichlorosilane, and trichlorosilane. Suitable as a method for collecting a sample from a system incorporating organochlorosilanes such as chlorosilanes such as chlorosilane and tetrachlorosilane, methyltrichlorosilane, dimethyldichlorosilane, trimethylmonochlorosilane, vinyltrichlorosilane, phenyltrichlorosilane and methylphenylchlorosilane. Used for

[0022]

As described above, according to the method and the apparatus for collecting a liquid sample of the present invention, the liquid to be collected is separated from the system containing the liquid into the collection chamber via the bypass via the bypass. By inserting a syringe needle into a rubber septum that constitutes a part of the sample and extracting the sample into the syringe, the septum after the needle is withdrawn automatically closes the injection mark by the elastic force of the rubber. A sample can be safely collected from a dangerous substance or a toxic substance, or a liquid containing the same. In addition, after the collection, the sample collected in the syringe can be directly used for analysis, so that the working efficiency can be improved.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing an apparatus for collecting a liquid sample according to an embodiment of the present invention.

FIG. 2 is an enlarged perspective view of a portion A in FIG.

FIG. 3 is a sectional view taken on line AA of FIG. 2;

FIG. 4 is a cross-sectional view showing a state at the time of sampling of FIG. 3;

FIG. 5 is a schematic diagram showing a main part of a liquid sample collecting apparatus according to another embodiment of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Pipeline 4 Bypass 5a-5e Valve 6 Sampling room 8 Partition wall 12 Syringe 12a Injection needle

 ──────────────────────────────────────────────────の Continued on the front page (72) Inventor Ryoji Baba 2-2 Chikusa-kaigan, Ichihara-shi, Chiba Toray Dow Corning Silicone Co., Ltd. Chiba Plant

Claims (6)

[Claims] A bypass is provided in an apparatus system containing a liquid to be collected, and the bypass is provided with an isolation valve through an on-off valve, and a collection chamber is provided in which a part of a partition wall to the outside is made of rubber. A method for collecting a liquid sample, wherein the liquid to be collected is separated into the collection chamber in an isolated state using a collecting device, and the liquid to be collected is inserted into a syringe by piercing the partition wall with a syringe needle. 2. The method according to claim 1, wherein the liquid to be collected is an organochlorosilane. 3. The method according to claim 1, wherein the rubber is a propylene hexafluoride / vinylidene fluoride copolymer. 4. A bypass system is provided in an apparatus system containing a liquid to be collected, and the bypass system is provided with a collection chamber in which a part of a partition wall to the outside is made of rubber while being separable through an on-off valve. A liquid sample collection device configured to pierce the partition wall with a syringe needle attached to a syringe to withdraw the liquid to be collected. 5. The liquid sample collecting apparatus according to claim 4, wherein the liquid to be collected is an organochlorosilane. 6. The liquid sample collection device according to claim 4, wherein the rubber is a propylene hexafluoride / vinylidene fluoride copolymer.