JPH06123737A - Measurement method in moisture analyzer - Google Patents

Abstract

(57) [Summary] [Purpose] To accurately detect and measure the water content of the sample to be measured, which is sealed and stored in the sample container under dry purge. [Structure] A sample 2 to be measured is stored in a sample container 1 that has been dry-purged in advance, and an opening 1 of the sample container 1
a is covered with a thin film sheet-like lid piece 3 that is incapable of infiltration of water, and is hermetically sealed and used as described above. On the other hand, the hollow measuring tube 62 communicated with the measuring section
The hollow communication needle 61 that holds the inside of the hollow and supplies the dry gas a is directly pierced, or the hollow communication needle 61 that is connected to the measurement unit and supplies the dry gas a is directly pierced. And perform the measurement operation.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a measuring method in a moisture measuring device, and more specifically, it heats a sample to be measured contained in a sample container to vaporize the moisture, and the amount of moisture contained in the sample. Measuring method for accurately detecting and measuring the water content of the sample to be measured that is hermetically stored in the sample container under dry purge in a moisture measuring device for carrying out the Karl Fischer moisture determination method Related to the improvement of.

[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 lid of the lid member, and for 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.

[0004]

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 process, and the lid is once opened. Then, after moving to the measurement position of the device and sealing again, the sample container in which the sample to be measured was hermetically stored under the dry purge was once opened. After that, even if it is a very small amount, water will invade from the ambient atmosphere until the airtight sealing is performed again, and the water content of the sample to be measured cannot be measured accurately and exactly. There was a problem that could be a fatal defect for this moisture measuring device.

The present invention has been made to solve the above-mentioned conventional problems, and its object is to contain the water content of the sample to be measured which is hermetically stored in the sample container under dry purge. The present invention is to provide a measuring method in a moisture measuring device of this kind, which is capable of accurately detecting and measuring.

[0006]

In order to achieve the above object, a measuring method in a moisture measuring apparatus according to the present invention stores a sample to be measured in a sample container which has been dry-purged in advance, and has an opening portion. The lid is covered with a thin film sheet lid and hermetically sealed, and a hollow communicating needle is directly pierced through the thin film sheet lid piece so that a measurement operation can be performed.

That is, according to the first aspect of the present invention, the sample to be measured is stored in a sample container which has been previously dry-purged, and the opening of the sample container is covered with a thin film sheet-like lid piece in which moisture cannot penetrate. A hollow measuring tube that is in communication with the measuring section for the thin film sheet-like lid piece of the sample container that tightly accommodates the sample to be measured under the dry purge in this way, and then uses the same. Is a measuring method in a moisture measuring apparatus, wherein a hollow communicating needle for holding dry air inside the hollow is directly inserted to perform a measuring operation.

A second aspect of the present invention stores a sample to be measured in a sample container that has been previously dry-purged, and covers the opening of the sample container with a thin film sheet-like lid piece in which moisture cannot enter. A hollow communication needle that is used as a lid to hermetically seal the thin film sheet-shaped lid piece of the sample container in which the sample to be measured is hermetically stored under the dry purge in this manner, and which is in communication with the measurement unit and also supplies dry gas. Is a measuring method in a moisture measuring device, characterized in that the measuring operation is carried out by directly piercing.

[0009]

Therefore, in the first method of the present invention, the hollow measuring tube communicating with the measuring section and the hollow communicating needle for holding the hollow measuring tube inside the hollow and supplying the dry gas are provided. Therefore, before the measurement is started, the dry gas is continuously supplied through the hollow communication needle, so that the needle tip of the hollow communication needle and the hollow measuring tube held inside are completely dried. Can be maintained in a purged state.

Then, the hollow communicating needle maintained in such a complete dry purge state is directly pierced under the dry purge into the thin film sheet-like lid piece of the sample container in which the sample to be measured is hermetically stored. The inside of the sample container can be communicated with the measurement unit through the hollow measuring tube held by the hollow communication needle, and in this communication state, the water vaporized from the sample to be measured in the sample container is supplied to the dry unit. Since the gas is led out from the hollow measuring tube to the measuring section to perform the measurement operation, when measuring the moisture content of the sample to be measured, the moisture content from the ambient atmosphere and the hollow Intrusion of water through the hollow communication needle including the measuring tube can be completely prevented, and accurate and strict measurement can be performed.

Further, according to the second invention method of the present invention, since the hollow communicating needle for supplying the dry gas in communication with the measuring portion is provided, the hollow communicating needle is also provided before the measurement is started. By continuously supplying the dry gas through the inside of the hollow communicating needle, the needle tip portion of the hollow communicating needle can be maintained in a completely dry-purged state, and almost the same operation as in the case of the first invention method can be obtained.

[0012]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The embodiments of the measuring method in the moisture measuring apparatus according to the present invention will be described in detail below with reference to FIGS.

FIG. 1 is a longitudinal sectional view sequentially and schematically showing an example of a means for hermetically storing a sample to be measured in a sample container in a moisture measuring apparatus used in the method of the present invention, and FIG.
Same as the above, a longitudinal sectional view schematically showing in sequence the modes at the time of measuring the amount of water to which one embodiment of the first invention method of the present invention (hereinafter referred to as the first embodiment method for convenience of description) is applied, FIG. FIG. 3 is a vertical cross-sectional view sequentially and schematically showing a mode at the time of measuring a water content to which an embodiment of the second invention method of the present invention (also referred to as a second embodiment method) is applied.

In each of the methods of the first and second embodiments, a heat-resistant container body 1 having an opening 1a is used as a sample container, and the inside of the heat-resistant container body 1 is dry-purged. Then, the sample 2 to be measured is stored in the inside, and a thin film sheet-like lid piece in which moisture cannot penetrate into the opening 1a, here, an aluminum foil film sheet piece (hereinafter referred to as an aluminum sheet piece). ) 3 is adhered to apply a hermetically sealed surface. In this case,
The heat-resistant container body 1 as a sample container is sealed and stored with the aluminum sheet piece 3 of the sample 2 to be measured, for example, as follows.

That is, as shown in FIG. 1 (a), a heat-resistant container 1 having an upper opening is used, and as shown in FIG. 1 (b), an opening 1a of the container 1 is used. Is in contact with the lower surface of an appropriate moisture shielding plate 100 and is shielded from the external atmosphere, the heating purge unit 10 and the dry gas purge unit 2
0, the sample loading section 30, and the aluminum seal section 40 are made to step by step so that each step can be processed, and after each of these processing steps, as a result, dry The sample container 50 in which the sample 2 to be measured is sealed and stored is obtained under purging.

To describe this in more detail, first, in the heating purge section 10, hot air is introduced from the hot air introducing pipe 11 to purge the water in the container body 1, and the waste containing the water after the processing is removed. Hot air is discharged from the waste hot air discharge pipe 12, and in the dry gas purge unit 20, for example, N ₂ gas is used as a dry gas, and the hot air blows moisture into the container body 1 once, By introducing the N ₂ gas through the dry gas introducing pipe 21, the water content in the container body 1 can be purged more reliably again, and even in this case, some residual water content after the treatment is removed. The N ₂ gas is discharged from the waste dry gas discharge pipe 22.

Therefore, with respect to the container body 1 that has undergone each of these processing steps, the water content that hinders the subsequent measurement of the water content of the sample 2 to be measured is completely purged and removed, and the inside of the container body 1 is completely removed. There will be no water at all.

Subsequently, in the sample charging section 30,
While the water purging state in the container body 1 is maintained, the sample 2 to be measured is introduced into the container body 1 through the introduction chute 32 from the sample introduction device 31, for example, if necessary,
As in the case of all stages, the container body 1 is introduced under the introduction of the dry gas a such as N ₂ gas from the dry gas introduction pipe 33 and the discharge of the waste N ₂ gas from the waste dry gas discharge pipe 34.
The sample 2 to be measured is placed in the container and stored therein. Further, in the aluminum seal portion 40, an opening seal is provided for the opening 1a of the container body 1 in which the sample 2 to be measured is stored in the water-purged state. The device 41 performs a hermetic seal by bonding the aluminum sheet piece 3 in which moisture cannot enter.

Therefore, after passing through these processing steps, the sample 2 to be measured is stored in the container body 1 in a water-purged state, and the aluminum sheet piece 3 is hermetically sealed in the opening 1a. As a result, the sample container 50 in which the sample 2 to be measured is hermetically stored under the dry purge is obtained.

In the method of the first embodiment, however, the sample container 50 obtained as described above is used, and the sample container 50 is heated by the heating coil 51 as shown in FIG. 2 (a).
In this case, the hollow measuring pipe 62 communicated with a measuring unit (not shown), and the hollow measuring pipe 62 is held inside the hollow to hold dry gas a such as N2 gas. A hollow communication needle 61 for supplying
With respect to the aluminum sheet piece 3 that hermetically seals the opening 1a, first, the lower end needle tip portion of the hollow communicating needle 61 including the hollow measuring tube 62, in this case, as described below, The lower end needle tip portion 61a, which is obliquely cut to be suitable for smoothing, is exposed from above, and in this state, that is, before starting the measurement, the dry gas a is continuously passed through the hollow communicating needle 61. By the supply, the needle tip portion of the hollow communication needle 61 and the hollow measuring tube 62 held inside are maintained in a completely dry purge state.

Subsequently, as shown in FIG. 2B, the lower end of the hollow communicating needle 61 including the hollow measuring tube 62 which is continuously supplied with the dry gas a and maintained in the dry purge state. By directly inserting the needle tip portion 61a into the aluminum sheet piece 3, the lower end needle tip portion 61a
Is directly communicated with the inside of the sample container 50, and thereby, without opening the inside of the sample container 50 again, that is, inside the sample container 50, and by extension,
The sample to be measured 2 is not exposed to the external atmosphere to allow moisture to enter, and the hollow measuring tube 6 does not bring moisture by the hollow communication needle 61 including the hollow measuring tube 62.
The inside of the sample container 50 and the measuring part can be communicated with each other through the inside of the sample container 50. Then, the heating coil 51 is used to move the sample 2 to be measured in the sample container 50 in exactly the same manner as in the conventional method. The amount of water contained in the sample is measured by heating the gas as it is to vaporize the water and taking the vaporized water b into the measuring section by the dry gas a supplied from the hollow communication needle 61. .

Therefore, in the case of the method of this embodiment, the sample container 50 in which the sample 2 to be measured is sealed and stored under the dry purge.
By directly piercing the lower end needle tip portion 61a of the hollow communication needle 61 including the hollow measurement tube 62 with respect to the aluminum sheet piece 3 of No. 3, the inside of the sample container 50 can be communicated with the measurement unit. When measuring the water content in the sample to be measured 2, it is possible to completely prevent the intrusion of water from the ambient atmosphere into the sample container 50 and the infiltration of water through the hollow communication needle 61 including the hollow measuring tube 62. It enables accurate moisture measurement.

Next, in the second embodiment method, as shown in FIG.
As shown in (a) and (b), the hollow measuring tube 62 in the method of the first embodiment is eliminated and only the hollow communicating needle 61 is used. According to the above, it is possible to supply the dry gas a and to derive the vaporized moisture b by the dry gas a through a switching valve or the like. In the method of the second embodiment as well, The same operation and effect as in the case of the method of the first embodiment can be obtained.

[0024]

As described above in detail with reference to each embodiment, according to the method of the present invention, the sample to be measured is stored in the sample container which has been dry-purged in advance, and the opening of the sample container is filled with moisture. It is used by covering with a non-penetrable thin film sheet lid and sealingly sealed.In this way, the thin film sheet lid of the sample container in which the sample to be measured is hermetically stored under dry purge is communicated with the measuring section. Hollow measuring tube and a hollow communication needle that holds the hollow measuring tube inside the hollow and directly supplies the dry gas, or directly connects the measuring section and the hollow communication needle that supplies the dry gas. Since the needle is directly pierced to perform the measurement operation, before the measurement is started, in the former means, by continuously supplying the dry gas through the hollow communication needle, the needle of the hollow communication needle is Tip, Each of the hollow measuring pipes held inside can be maintained in a completely dry purged state, and in the latter means, by continuously supplying dry gas through the hollow communicating needle, the needle tip portion of the hollow communicating needle is Can be maintained in a completely dry-purged state, and at the time of measuring the water content in the sample to be measured, it completely blocked the invasion of water from the ambient atmosphere into the sample container and the infiltration of water through the hollow communication needle. It is possible to measure in the state, and as a result, it is possible to measure the water content of the sample to be measured extremely accurately and exactly, and, unlike the conventional case, to open the sample container Since this means is unnecessary, it has an excellent feature that the device structure can be simplified and can be easily implemented.

[Brief description of drawings]

1 (a) and 1 (b) are vertical cross-sectional views each schematically showing an example of means for hermetically storing a sample to be measured in a sample container in a moisture measuring apparatus used in the method of the present invention.

2 (a) and 2 (b) are vertical cross-sectional views each schematically showing in sequence the modes at the time of measuring the amount of water to which one embodiment of the method of the first invention of the present invention is applied.

3 (a) and 3 (b) are longitudinal cross-sectional views each schematically showing in sequence the modes at the time of measuring the amount of water to which the embodiment of the second invention method of the present invention is applied.

[Explanation of symbols]

1 Heat-Resistant Container Body as Sample Container 1a Opening of Heat-Resistant Container Body 2 Sample to be Measured 3 Aluminum Sheet Piece (Thin Film Sheet-Like Lid Piece Incapable of Entering Moisture) 10 Heating Purging Section 11 Hot Air Inlet Tube 12 Waste Hot Air Discharge Tube 20 Dry Gas Purging Section 21 Dry Gas Introducing Tube 22 Waste Dry Gas Exhausting Tube 30 Sample Introducing Section 31 Sample Introducing Device 32 Introducing Chute 33 Dry Gas Introducing Tube 34 Waste Dry Gas Exhausting Pipe 40 Aluminum Sealing Section 41 Opening Sealing System 50 Dry Purging Under A container for sealing and storing the sample to be measured with 51 Heating coil 61 Hollow communication needle 61a Needle tip of hollow communication needle 62 Hollow measuring tube a Dry gas b Evaporated moisture of the sample to be measured

Claims (5)

[Claims] 1. A sample container to be measured is stored in a sample container that has been dry-purged in advance, and the opening of the sample container is covered with a thin film sheet-like lid piece into which water cannot penetrate, and is hermetically sealed. In this way, the thin measurement sheet-like lid of the sample container in which the sample to be measured is hermetically stored under the dry purge is connected to the measuring section, and the hollow measuring tube is held inside the hollow to dry it. A measuring method in a moisture measuring device, characterized in that a hollow communicating needle for supplying gas is directly pierced to perform a measuring operation. 2. The sample to be measured is stored in a sample container which has been previously dry-purged, and the opening of the sample container is covered with a thin film sheet-like lid piece into which water cannot penetrate to be hermetically sealed. In this way, the measurement operation is performed by directly inserting a hollow communication needle that feeds dry gas into the thin film sheet lid of the sample container in which the sample to be measured is sealed and stored under dry purge. A method for measuring in a moisture measuring device, which comprises: 3. The measuring method in a moisture measuring apparatus according to claim 1, wherein the thin film sheet-like lid piece is an aluminum sheet piece. 4. The thin film sheet lid piece is an aluminum sheet piece, and the aluminum sheet piece is adhered to the opening of the sample container to hermetically seal it. Method of Moisture Measurement Equipment of. 5. The measuring method for a moisture measuring apparatus according to claim 1, wherein the lower end of the hollow communicating needle is cut obliquely so as to facilitate the piercing operation. .