JPH0743269A - Arrangement of three-way switching valve in moisture measuring apparatus - Google Patents

Abstract

PURPOSE:To realize smooth and accurate measuring operation by coupling a plurality of three-way switching valves through short channels and fixing onto a common board thereby simplifying the constitution of channel. CONSTITUTION:A series of three three-way switching valves 25, 27, 28 are arranged at a regularly shortened interval on a fixing board 17 which is then arranged on the upper face of a housing 16 in the frame 15 of measuring apparatus thus blocking the entirety. This structure minimizes the lengths of a gas introduction channel 31 between the valves 15, 27, 28, a gas short circuit channel 41, a gasified moisture lead-out channel 51, and a bypass channel 61 thus simplifying the constitution of channel. For example, respective COM sides and NO sides are aligned and the channels 31, 41, 51 coupled thereby produce a series of flow and a channel 61 is also arranged in parallel therewith. Furthermore, the channels to the gas introduction needle 24 and the gasified moisture lead-out needle 26 on the NC side in the valves 25, 27 can be shortened significantly.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention implements a Karl Fischer moisture determination method in which a sample to be measured contained in a sample container is heated to vaporize moisture and the amount of moisture contained in the sample is measured. The present invention relates to the improvement of the arrangement structure of the three-way switching valve in the water content measuring device.

[0002]

2. Description of the Related Art Generally, in a moisture measuring apparatus using the Karl Fischer moisture determination method, a sample to be measured is stored in a dry-purged sample container, and the inside of the sample container is connected to a measuring section. Then, this is heated from the outside to vaporize the moisture, and the vaporized moisture is introduced into the measurement section by the carrier gas to measure the amount of the moisture.

That is, in the case of this type of conventional moisture measuring apparatus, for example, as disclosed in Japanese Patent Laid-Open No. 1-216226, the sample to be measured is stored in a sample container which has been previously dry-purged. At the same time, the opening is hermetically sealed by the cover of the lid member, and with respect to the sample container in which the sample to be measured is hermetically stored under the dry purge in this way, the lid member is removed and opened immediately before the heating vaporization process. And, the opened sample container is moved to the measurement position of the device, and again sealed by the interposition of the O-ring, and thereafter,
The operation is processed and measured as described above.

However, in the above-mentioned conventional moisture measuring apparatus, in the measurement using the sample container in which the sample to be measured is stored, first, the lid member is removed immediately before the heating and vaporizing treatment, and the lid is once opened. Since it is moved to the measurement position and sealed again, the inside of the sample container in which the sample to be measured is hermetically stored under the dry purge should be opened once and then sealed again. In the meantime, even if it is a small amount, moisture invades from the ambient atmosphere, and the moisture content of the sample to be measured cannot be measured accurately and exactly. It has a fatal defect.

Therefore, the present inventors have previously proposed the following means for sealing and sealing the sample container.

[0006] That is, in the proposed new means, a thin film sheet-like lid piece that is incapable of infiltration of moisture from the outside is used to store the sample to be measured in the sample container under dry purge and to open the sample container. The thin film sheet-like lid piece is adhesively sealed to the part to be closed and sealed. According to the sample container configured as described above, when the moisture content of the sample to be measured is measured, the thin film sheet-like By directly piercing the lid piece with a communication needle or the like from the outside, the vaporized water of the sample to be measured can be easily taken out to the measurement section through the communication needle without opening the sample container again. it can.

[0007]

In the case of the means for sealing and sealing the opening of the sample container proposed by the present inventors with a thin film sheet-like lid piece, the problem to be solved remains. Each operation for measuring the water content of the sample to be measured in the water content measuring apparatus using the sample container, that is, the prior operation such as dry purge of the main part of the measurement system and confirmation of the stability of the carrier gas, and the purpose. It means that the required moisture measurement operation to be performed is not always easy to perform, and on the other hand, the flow path arrangement of each part of the measurement system that composes the device according to this is complicated and is not preferable. .

The present invention has been made in order to solve the problems in such a moisture measuring apparatus, and its object is to use a sample container which is hermetically sealed with a thin film sheet-like lid piece. In a device for measuring the water content of a sample to be measured in a sample container by the Karl Fischer moisture determination method, the flow passage arrangement in each part of the measurement system that constitutes the device, especially the three-way switching valves essential for the measurement operation It is an object of the present invention to provide an arrangement structure of a three-way switching valve in a moisture measuring device of this type, in which the arrangement of the flow paths is simplified as much as possible, thereby facilitating smoothness and accuracy of each measuring operation.

[0009]

In order to achieve the above object, the arrangement structure of the three-way switching valve in the moisture measuring apparatus according to the present invention is such that the opening of the sample container body for accommodating the sample to be measured is a thin film sheet. Using a sample container that is closed and hermetically sealed with a lid piece, for the thin film sheet-like lid piece of the sample container that has been transferred to the heating measurement operation section including the heating control means, use a dry gas supply source that also serves as a carrier gas. The gas introduction needle communicated with the first three-way switching valve and the vaporized water derivation needle communicated with the moisture measurement detection unit through the second three-way switching valve are pierced, and the first and second In the moisture measuring device in which at least the dry purge operation, the background operation, and the moisture measuring operation can be individually performed by the selective switching control of the respective 2-way 3-way switching valves, the 3-way switching, which is the main operating part of the measuring system, is performed. The arrangement of the example valve is obtained by the following configuration.

That is, the gas introduction passage from the dry gas supply source is connected to the first three-way switching valve, and the first three-way switching valve is connected to the second three-way switching valve via a gas short-circuit passage. Of 3
A three-way switching valve close to and connected to the second three-way switching valve, and a third three-way switching valve installed on the upstream side of the vaporized water derivation flow path to the second three-way switching valve. The third three-way switching valve is connected to the upstream side of the first three-way switching valve via a bypass flow path, and the downstream side of the vaporized moisture derivation flow path is connected to a moisture measurement detection unit. In this way, the first, second and third three-way switching valves are connected in series on a common mounting substrate with a flow path connection at the shortest possible interval. By the selective switching control of each of the first, second and third three-way switching valves, the desired device operation can be performed.

[0011]

Therefore, in the arrangement structure of each three-way switching valve of the measuring system according to the present invention, each operation in the device is performed as follows by the selective switching control of each of the first, second and third three-way switching valves. Will be performed.

That is, during the dry purge operation, the dry gas whose flow rate has been adjusted is supplied to the heating measurement operation unit from the gas introduction needle and the vaporized water extraction needle. Further, during the background operation, the carrier gas whose flow rate has been adjusted is supplied from the gas short circuit flow path to the moisture measurement detection unit. Further, during the moisture measuring operation, the carrier gas whose flow rate has been adjusted is supplied from the gas introduction needle into the sample container, and the vaporized moisture in the sample container is supplied from the vaporized moisture derivation needle to the moisture measurement detection unit by the carrier gas.

[0013]

[Examples] 3 in the moisture measuring apparatus according to the present invention
1 to 7 for an embodiment of the arrangement structure of the one-way switching valve.
Will be described in detail with reference to.

FIGS. 1 (a) and 1 (b) show a sample container in which a sample to be measured is sealed in a moisture measuring apparatus according to the present invention, and a gas for a thin film sheet-like lid piece for sealing the sample container. FIGS. 2 to 4 are cross-sectional explanatory views each showing a piercing state of an introducing needle and a vaporized water deriving needle, and FIGS.
FIG. 7 is a schematic diagram of the flow channel system showing an example of the configuration of the measurement flow channel system applied to the present invention and a flow mode of the dry purge gas or the carrier gas for each measurement operation, and FIGS. FIG. 2A is a plan view and a side view of a main part schematically showing a schematic configuration of an arrangement structure of each three-way switching valve according to an embodiment of the present invention.

1 (a) and 1 (b), a heat-resistant sample container body 11 having an opening 11a is used as the sample container 10 according to this embodiment, and the inside of the heat-resistant container body 11 is dried. In the purged state, the sample to be measured 12 is
In addition, the opening 11a accommodates a thin film sheet-like lid piece in which moisture cannot enter from the outside, here, an aluminum foil film sheet piece (hereinafter referred to as an aluminum sheet piece) 1
A structure in which the entire surface is hermetically sealed by bonding 3 is used.

Thus, the sample container 1 thus constructed
0 is used by directly piercing the aluminum sheet piece 13 that hermetically seals the opening 11a with a gas introduction needle 24 and a vaporized water derivation needle 25 described below.
With the carrier gas supplied from the gas introduction needle 24, the vaporized moisture of the sample to be measured 12 vaporized inside the container is taken out from the vaporized moisture derivation needle 25, and the amount of contained moisture is measured.

2 to 4, the measurement flow path system 20 according to the present example is configured as shown in FIG.

That is, the heating / measurement operating section 21 is provided with a measurement substrate 22a on the upper side and an opening on the lower side, and the partition wall 22.
It has a heating measurement chamber 22 that is divided from the surroundings by b and has a volume that allows the sample 12 to be measured to be stored and sealed. The outside of the heating measurement chamber 22 serves as heating control means. A gas introduction needle 24, in which a heating unit 23 is arranged, and which is projected toward the inside of the heating measurement chamber 22 and is connected to a first three-way switching valve 25, with respect to the surface of the measurement substrate 22a, It is projected slightly shallower than the second 3
A vaporized water derivation needle 26 connected to the one-way switching valve 27 is provided for each.

In this case, nitrogen gas is used as the dry gas which also serves as the carrier gas, and the gas introduction flow path 31 from the dry gas supply source 30 selectively switches the supply gas pipeline. A flow path switching valve 32, a parallel conduit of a flow rate control valve 33 for a dry purge gas and a flow rate control valve 34 for a carrier gas, which are selectively flow path switchable by the flow path switching valve 32, and the parallel pipe. A mass flow sensor 35 as a flow rate detecting means and a gas drying section 37a, 37b via an open / close valve 36 for opening to the atmosphere are sequentially provided on the wake side of the passage, and the mass flow sensor 35 is connected to the gas flow sensor. It is connected to a first three-way switching valve 25 connected to the introduction needle 24.

On the other hand, the first three-way switching valve 25 and the second three-way switching valve 27 are connected to each other by a gas short-circuit passage 41.

Further, for the moisture measuring and detecting section 50,
In this case, in the vaporized moisture derivation flow path 51 from the second three-way switching valve 27 connected to the vaporized moisture derivation needle 26, the vaporized moisture derivation flow path 51 is communicated via the third three-way switching valve 28, and the third The three-way switching valve 28 and the upstream side of the first three-way switching valve 25 are connected by another bypass flow passage 61.

Here, in the case of this example, the first, second,
As the third three-way switching valves 25, 27, and 28, so-called electromagnetic switching valves capable of electromagnetic switching are used, and their connection forms are shown in FIGS. 2 to 4, and FIGS. 5 and 6. As shown.

That is, regarding the first three-way switching valve 25,
The inlet (COM) side is connected to the gas introduction flow path 31 side, the normally open outlet (NO) side is connected to the short circuit flow path 41 side, and the normally closed outlet (NC) side is connected to the gas introduction needle 24 side. Further, regarding the second three-way switching valve 27, the vaporized moisture derivation flow path 5 is placed on the COM side.
1, the NO side is connected to the short circuit channel 41 side, and the NC side is connected to the vaporized water derivation needle 26 side. Third 3-way switching valve 2
8, the COM side and the NO side are vaporized moisture derivation flow paths 5
In 1, the NC side is connected to the bypass flow path 61 side, respectively.

In the above-mentioned flow path configuration, the gas introducing flow path 31 is equipped with a parallel conduit of the flow rate adjusting valve 33 for dry purge gas and the flow rate adjusting valve 34 for carrier gas, which is the former dry purge. This is because a relatively large amount of dry purge gas is used during operation, whereas a relatively small amount of carrier gas is used during background operation and moisture measurement operation in the latter case.

Next, the operation of the measurement flow path system according to this embodiment will be described by taking up the flow of the dry purge gas or the carrier gas for each operation.

At the time of the dry purge operation of the apparatus (corresponding to the state of FIG. 2, the flow of the dry purge gas is indicated by the arrow a.) This dry purge operation is performed for removing the adhered water in the water measuring system of the apparatus. In the case of the present embodiment, as shown in FIG. 2, the first three-way switching valve 25 is closed on the side of the short circuit passage 41, opened on the side of the gas introduction needle 24, and the second And close the three-way switching valve 27 on the short-circuit passage 41 side.
It opens on the side of the vaporized water lead-out needle 26, and the third 3-way switching valve 28
Is closed on the downstream side of the vaporized moisture derivation flow path 51 and opened on the bypass flow path 61 side, so that the dry purge gas of the dry gas supply source 30 is
After the gas introduction flow path 31 is dry-purged, it is supplied from the gas introduction needle 24 into the heating measurement chamber 22 of the heating measurement operation unit 21, and on the other hand, is bypassed by the gas introduction flow path 31 and the bypass flow path 61. Inner and third 3-way switching valve 2
After performing a dry purge on the upstream side of the vaporized moisture derivation flow path 51 through the respective parts 8, the vaporized moisture derivation needle 26 is similarly supplied into the heating measurement chamber 22 of the heating measurement operation unit 21 to perform the heating measurement. The inside of the chamber 22 is dry-purged.

At this time, the sample container 10 in which the sample 12 to be measured is sealed in the heat-resistant container 11 is in the ascending process toward the heating and measuring chamber 22 and the dry purge is completed. It enters into the heating measurement chamber 22.

During the background operation of the apparatus (corresponding to the state of FIG. 3, the flow of the carrier gas is indicated by the arrow b.) This background operation is performed to confirm the stability of the carrier gas in the apparatus. In the case of the present embodiment, as shown in FIG. 3, the first three-way switching valve 25 is opened on the side of the short circuit passage 41, and the gas introduction needle 24
Side, the second three-way switching valve 27 is opened on the short-circuit flow path 41 side, the vaporized water derivation needle 26 side is closed, and the third three-way switching valve 28 is opened on the vaporized water derivation flow path 51 to bypass. By closing on the side of the flow path 61, the carrier gas of the dry gas supply source 30 is closed by the gas introduction flow path 3 as shown by the arrow b.
1, the short-circuited flow channel 41 and the vaporized moisture derivation flow channel 51 are respectively supplied to the moisture measurement detection unit 50, and the stability is confirmed in the moisture measurement detection unit 50.

At this time, the sample container 10 in which the sample 12 to be measured is contained and sealed in the heat-resistant container body 11 is completely inserted into the heating and measuring chamber 22, and the aluminum sheet piece 13 thereof is inserted.
First, the gas introduction needle 24 is pierced, and subsequently the vaporized water derivation needle 26 is pierced, and at the same time, the heating unit 23 heats the inside of the heating measurement chamber 22 and thus vaporizes the water content of the sample 12 to be measured. Is heated.

At the time of the moisture measuring operation of the apparatus (corresponding to the state of FIG. 4, the flow of the carrier gas is shown by an arrow c.) In this moisture measuring operation, the moisture content of the sample to be measured of the apparatus is vaporized and detected. In the case of the present embodiment, as shown in FIG. 4, the first three-way switching valve 2
5 is closed on the short-circuit flow path 41 side and opened on the gas introduction needle 24 side,
The second three-way switching valve 27 is closed on the short-circuited flow passage 41 side, opened on the vaporized moisture derivation needle 26 side, the third three-way switching valve 28 is opened on the vaporized moisture derivation flow passage 51, and the bypass flow passage 61 side. By closing with, the carrier gas of the dry gas supply source 30 is supplied from the gas introduction needle 24 into the sample container 10 through the gas introduction passage 31, as shown by the arrow a.
The moisture content of the sample 12 to be measured vaporized in the sample container 10 is taken out by the vaporized moisture derivation needle 26 and is supplied to the moisture measurement detection unit 50 through the vaporized moisture derivation flow path 51 to measure the moisture content. The water content is measured by the detection unit 50.

In accordance with the end of the measurement of the water content, the sample container 10 whose measurement has been completed shifts to the descending process from the inside of the heating measurement chamber 22, and the above operation is repeated. It is.

As is apparent from the above explanations, therefore, in the case of this type of measurement flow channel system, generally, each flow channel configuration and these flow channels are selectively switched. Since each switching valve to be connected is mainly used and its measuring operation is performed by the selective operation of each switching valve, the flow shortened as much as possible between the switching valves here. The important point is how to perform the measurement process efficiently and rationally according to the arrangement configuration by the road connection.

Therefore, in the present embodiment, with respect to the measurement flow path system of FIGS. 2 to 4, the first 3-way switching valve 25 and the second 3-way switching valve 25 directly related to the heating measurement operation unit 21 are provided.
The one-way switching valve 27 and the third three-way switching valve 28 are respectively
Each flow path 31, 41, 51, 61 according to each setting described above.
In view of being connected by the above, as shown in FIG. 5 and FIG.
And each of the third three-way switching valves 25, 27, and 28 are arranged in series in order at intervals as short as possible, and the mounting substrate 17 is arranged on the upper surface of the housing 16 in the device frame 15. It is fastened and fixed, and the whole is what is called a block.

Therefore, in the case of the present embodiment having such a configuration, the minimum length which requires the length of each flow path 31, 41, 51, 61 between each three-way switching valve 25, 27 and 28. Can be shortened, resulting in a streamlined configuration of the flow path. That is, for example, the first, second, and third three-way switching valves 25, 27, and 28 arranged in series on the mounting board 17 are clear from the indications shown in FIGS. 5 and 6. As described above, the respective COM side and NO side are arranged in a line, and the respective flow paths connected through them, that is, the gas introduction flow path 31, the gas short circuit flow path 41 and the vaporized moisture derivation flow path 51 are arranged in a series of flow. The bypass flow path 61 is also arranged in parallel to the bypass flow path 61, and further, to the NC side gas introduction needle 24 and the vaporized water derivation needle 26 in each of the first and second three-way switching valves 25 and 27. The flow path connection of can also be connected with an extremely short flow path.

In FIG. 5, the connection from the NC side of the first three-way switching valve 25 to the gas introduction needle 24 is made through the gas short-circuit passage 41 as shown by the solid line. This is because a commercially available product is used as the first three-way switching valve 25, and it can be directly connected as shown by a chain line if necessary.

Incidentally, the above-mentioned first, second and third three-way switching valves 25, 27 and 2 are used in the normal form.
In the case where each of the three eight-way switching valves 25, 27 and 2 is generally arranged without considering the flow path connection relationship, as shown in FIG.
8 are relatively widely separated from each other, and the flow paths 31, 41, 51, 61 connecting the two are also relatively long. In such a mode, in FIG. As is clear from FIG. 7, each flow path 31, 41, 5
A large amount of waste is generated in each of the Nos. 1 and 61, the configuration itself becomes complicated, smooth, quick and effective operation becomes unclear, and maintenance is not easy.

As described above, in the structure of this embodiment,
Sample container 1 with aluminum sheet piece 13 hermetically sealed
When measuring the water content of the sample 12 to be measured in 0, the first directly related to the heating measurement operation of the sample container 10,
Since the second and third three-way switching valves 25, 27, 28 are arranged close to each other and arranged in a series of flow paths, the measurement flow path system 20 of the apparatus itself is relatively simple and simplified. In addition to being configured, each measurement operation by the measurement flow path system 20 can be easily and efficiently performed, and smoothness and accuracy of each measurement operation can be achieved.

[0038]

As described above in detail with reference to the embodiments,
According to the arrangement structure of each three-way switching valve in the moisture measuring apparatus of the present invention having the above-mentioned configuration, the opening of the sample container body is stored in the sample container body which has been previously dry-purged in a state where the sample to be measured is stored. When measuring the moisture content of the sample to be measured in this sample container by the Karl Fischer moisture determination method using a sample container sealed and sealed by a thin film sheet lid that is incapable of moisture infiltration, Since the main three-way switching valves, which are directly related to the heating measurement operation unit of the container, here, the first to third three-way switching valves, are arranged in a series so as to be close to each other, the measurement flow path is arranged. According to the effective simplification of the system itself and the simplification of its maintenance, the smoothness and accuracy of each measurement operation associated with the respective switching operations of the first to third three-way switching valves are facilitated. To plan Those having an excellent feature that kill.

[Brief description of drawings]

1 (a) and 1 (b) are a sample container in which a sample to be measured in a moisture measuring apparatus according to an example of the present invention is stored and sealed, and gas is introduced into a sealing thin film sheet-like lid piece of the sample container. It is each cross-sectional explanatory view which shows the piercing state of a needle and a vaporized water extraction needle, respectively.

FIG. 2 is a flow chart system configuration diagram showing a schematic construction and a flow of dry gas at the time of a dry purge operation in a measurement flow passage system in an example applied to the present invention.

FIG. 3 is a flow path system configuration diagram showing a flow of a carrier gas during a background operation in the measurement flow path system configuration according to the same example.

FIG. 4 is a flow path system configuration diagram showing a flow of a carrier gas during a moisture measurement operation in the measurement flow path system configuration according to the same example.

FIG. 5 is a plan explanatory view schematically showing a schematic configuration of an arrangement structure of each three-way switching valve according to an embodiment of the present invention.

FIG. 6 is an explanatory side view of the main part schematically showing the schematic configuration of the arrangement structure of each three-way switching valve according to the same embodiment.

FIG. 7 is an explanatory plan view schematically showing a schematic configuration of an arrangement structure of general three-way switching valves in the same normal form.

[Explanation of symbols]

10 Sample Container 11 Heat-Resistant Container 11a Opening of Heat-Resistant Container 12 Sample to be Measured 13 Aluminum Sheet Piece (Thin-Film Sheet-Shaped Lid Piece That Cannot Intrude Moisture) 15 Device Frame 16 Housing 17 Mounting Board 20 Measurement Channel System 21 Heating measurement operation unit 22 Heating measurement chamber 22a Measurement substrate 22b Partition wall 23 Heating unit (heating control means) 24 Gas introduction needle 25 First three-way switching valve 26 Vaporized moisture derivation needle 27 Second three-way switching valve 28 Third 3-way switching valve 30 Dry gas supply source 31 Gas introduction flow path 32 Flow path switching valve 33 Flow rate control valve for dry purge gas 34 Flow rate control valve for carrier gas 35 Mass flow sensor (flow rate detection means) 36 Open / close valve for atmosphere release 37a, 37b Gas drying section 41 Short-circuited channel 50 Moisture measurement detection section 51 Vaporized moisture derivation channel 61 Bypass channel Flow of dry purge operation time of the dry gas stream b background operation when the carrier gas flow c moisture measurement operation when the carrier gas

Claims (1)

[Claims] 1. A sample transferred to a heating and measurement operation unit including a heating control unit, using a sample container in which an opening of a sample container body accommodating a sample to be measured is closed and hermetically sealed with a thin film sheet lid piece. The thin film sheet-like lid of the container is connected to a dry gas supply source that also serves as a carrier gas through a first three-way switching valve, and a moisture measuring and detecting unit is provided with a second gas introducing needle.
The vaporized moisture outlet needle, which is communicated via the three-way switching valve, is pierced and the selective switching control of the first and second three-way switching valves allows at least a dry purge operation, a background operation, and a moisture measurement. In a moisture measuring device capable of performing respective operations, a gas introduction flow path from the dry gas supply source is connected to the first three-way switching valve, and the first three-way switching valve includes:
The second three-way switching valve is closely connected via a gas short-circuit flow path, and the second three-way switching valve has a third flow path incorporated in a front side of the vaporized moisture derivation flow path. The three-way switching valve is closely connected, and the third three-way switching valve is connected to the upstream side of the first three-way switching valve via a bypass flow path, and the vaporized moisture derivation flow is further provided. By connecting the wake side of the channel to the moisture measuring / detecting section, these first, second and third three-way switching valves can be connected to each other with a flow path connection at the shortest possible interval. When the dry purge operation is performed, the dry gas whose flow rate is adjusted is vaporized with the gas introduction needle by the selective switching control of the first, second and third three-way switching valves. It is supplied to the heating measurement operation unit from the water extraction needle, and the background operation is performed. At the time of operation, a carrier gas whose flow rate is adjusted is supplied from the short-circuit flow path to the moisture measuring and detecting unit, and at the time of a moisture measuring operation, a carrier gas whose flow rate is adjusted is supplied from the gas introduction needle into the sample container, and An arrangement structure of a three-way switching valve in a moisture measuring device, wherein vaporized moisture in the sample container is supplied from the vaporized moisture derivation needle to the moisture measurement detection unit by a carrier gas.