JPH0341343A - Sample container mounting method and apparatus of moisture measuring apparatus - Google Patents

Abstract

PURPOSE:To enhance the treatment efficiency of a measuring apparatus and to prevent the lowering of measuring accuracy due to the mixing with the moisture of the outside by placing a lid body on the opening part of a sample container in such a state that a heat-resistant nonvolatile viscous material is applied between the lid body and the opening edge of the sample container. CONSTITUTION:In heating a sample to evaporate the moisture thereof and supplying the heated sample to a moisture measuring apparatus, a lid body 16 is placed on the opening part of a sample container 8 in such a state that a heat-resistant nonvolatile viscous material is applied between the lid body 16 and the opening edge of the sample container 8. The sample container 8 is supplied to the lower part of the gasifying part 3 connected to both of a sample supply passage and a carrier gas introducing passage and, immediately after the lid body 16 is detached from the sample container 8, the sample container 8 is raised to press the opening edge thereof to the opening part of the lower end of the gasifying part 3 in an airtight state. By this method, the airtightness of the sample container 8 from the placement of the lid body 16 to the detachement thereof is enhanced and the lid body 16 is detached rapidly to make it possible to mount the gasifying part 3 and, therefore, the amount of moisture penetrating in the sample container 8 from the outside can be suppressed to the min. degree and the lowering of measuring accuracy can be prevented.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to an apparatus for vaporizing and supplying a sample to an apparatus for measuring moisture in a measurement sample. The present invention relates to a device for attaching.

[Prior Art] As a reliable method for measuring moisture in a sample, the most commonly used method is the Karl-Fischer moisture determination method. Automation has made remarkable progress in the field of moisture measurement.

Until now, in automatic moisture measuring devices, the sample was stored in a container and the opening was closed with a lid before being supplied to the device, and after the lid was removed from the sample container, the moisture was vaporized into the container. A device to which a sample container is attached has been proposed.

[Problems to be Solved by the Invention] However, the biggest problems with the sample container mounting means described above are the infiltration of moisture from the outside air due to the low airtightness of the sample container with the lid closed, and The problem is that moisture from the outside air gets mixed in from the time the product is installed to the vaporizer.

For example, in order to improve the airtightness of a container, it is possible to securely attach a lid equipped with a gasket or the like to the opening of the container using a threaded joint. However, with automatic measuring devices that must be attached to the vaporizer, it is difficult to remove the lid, and it takes time to process each sample.Also, even if such a lid is adopted, it is difficult to remove the lid. Since it takes a long time, other problems such as external moisture entering the sample container during that time may occur.

The present invention has been made in view of the above-mentioned conventional problems and aims to solve them.

[Means for solving the problem] In other words, the gist of the first means adopted in order to achieve the above object is to heat the sample, evaporate its moisture, and supply it to the moisture measuring device. A heat-resistant, non-volatile viscous material is applied between the cap 16 and the opening edge of the sample container 8, and the lid 16 is placed on the opening of the sample container 8.
Immediately after supplying the sample container 8 under the vaporization section 3 to which the sample supply path and the carrier gas introduction path are connected and removing the lid 16 from the sample container 8, the sample container 8 is raised.
This is a method for mounting a sample container in a moisture measuring device, in which the edge of the opening is hermetically pressed against the edge of an opening 3a opened at the lower end of the vaporizer 3.

Furthermore, the gist of the second method is to heat the sample, evaporate the water, and reduce the water content to 7J! In a device for attaching a sample container 8 of a device for supplying to a lJ constant device to a vaporizing section 3, a sample supply path and a carrier gas introduction path are connected, and an opening 3a is provided.
The vaporizing section 3 is opened downward, and a heat-resistant, non-volatile viscous material is applied between the lid 16 and the opening edge of the sample container 8, and a magnetic material 28 is provided on the top surface of the lid. A means for supplying the sample container 8 with the sample container 16 placed on the opening thereof under the vaporization section, a magnet 25 and a magnetic shielding plate 2 that is pushed in and retracted under the magnet 25.
6, which is inserted between the lid 16 of the sample container 8 and the vaporization section 3 in accordance with the transportation of the sample container 8 by the container supply means;
A sample of a moisture measuring device comprising a magnetic chuck 21 to be retracted, and a means for pushing up the sample container 8 and applying its opening to the opening 3a of the vaporizer 3 as the magnetic chuck 21 is retracted. This is a container mounting device.

[Function 5] According to the first means, since the lid 16 of the sample container 8 is simply placed on the opening of the sample container 8, it is extremely easy to remove it from the sample container 8. , it is convenient for application to an automated device that sequentially handles many sample containers 8. Moreover, since a heat-resistant, non-volatile viscous material is applied between the lid 16 and the opening edge of the sample container 8, the sample container 8 is highly airtight from the time the lid 16 is placed on until it is removed. Moreover, since the lid 16 can be quickly removed and the vaporizer 3 can be attached, the amount of moisture that enters the sample container 8 from the outside between the time the lid 16 is removed and the sample container 8 is attached to the vaporizer 3 can be reduced. can be minimized.

Furthermore, according to the second means, after moving the magnetic chuck 21 onto the lid 16 with the magnetic shielding plate 26 inserted under the magnet 25 as shown in FIG. As shown in FIG. 5, by retracting the magnetic shielding plate 26 from under the magnet 25, the magnetic body 28 of the lid 16 is attracted, and as shown in FIG. Can be removed. This means is advantageous in quickly and reliably removing the lid 16 that is stuck to the sample container 8 due to viscosity from the sample container 8.

[Examples] Examples of the present invention will be described below with reference to the accompanying drawings.

FIG. 1 is an example of a sample vaporization supply device for moisture measurement to which the sample container mounting device of the present invention is applied.

Reference numeral 1 is a moisture measuring device, and the part surrounded by the - dotted chain line is a moisture vaporization supply device. Reference numeral 8 denotes a sample container, in which a pre-weighed sample 4 is placed and a lid 16 is placed on the upper opening. Apply a viscous material for sealing, such as fluorine grease or silicone grease.

Note that it is desirable that the bottom surface of the lid 16 and the opening edge of the sample container 8 be polished sufficiently smooth so that the lid 16 can completely seal the sample container 8 .

The lower end of the vaporization section 3 is in an open state 7 before the sample container 8 is pushed in, and a cylindrical conduit section 23 into which the sample container 8 is inserted is formed extending below the lower end. Connected to the upper end of the vaporization section 3 are a sample supply path shown as line D in the figure and a carrier gas introduction path also shown as line C. Separately, the arrow shown as the A line is the initial supply system of the carrier gas that directly sends the carrier gas to the main body of the moisture measuring device. Furthermore, the arrow shown as the B line is a carrier gas measurement and supply system that sends carrier gas to the vaporization section 3.

9 is a heater for heating the sample, 11 is a zeolite column, 12
is a silica gel column, 13 is a flow meter, ■1 to v4
are solenoid valves, and 5 to v7 are adjustment valves.

17 is a turntable on which the sample container 8 is placed and rotates;
Together with an auxiliary table 18 that holds the sample container 8 so that it does not vibrate or move, it is pivotally mounted as an extension of a shaft 24 parallel to the rotation axis of the electric motor Ml. Electric motor M■
The turntables 17 and 17 are connected via a speed change mechanism to constitute sample container supply means.

The electric motor M2 is equipped with a sample container lifting rod 19 connected via a speed change mechanism, and an arm 20 for removing the lid 16 of the sample container 8 is attached to the rotating shaft of the electric motor M3.
is provided.

The tip of this arm 20 serves as a magnetic chuck 21 for holding the lid 16. 27 is a container in which the used lid 16 removed from the sample container 8 is stored.

The structure of the magnetic chuck 21 is shown in FIGS. 2 to 6 and 8, which consists of a magnet 25 provided at the tip of the arm 20, and a magnetic shield that is pushed under the magnet 25 and retracted. A plate 26 is provided.

Further, a stopper 29 is provided on the left side of the lower surface of the distal end of the arm 20 in FIGS. 2 to 6. For example, as shown in FIG. 8, the second magnetic shielding plate 26 uses a magnetically shielding plate whose rotation center is common to the rotational axis 30 of the arm 20, and is arranged independently of the arm 20. By rotating it, it is pushed in or withdrawn from below the magnet 25.

9- When the magnetic shielding plate 26 is pushed under the magnet 25, the magnet 25
loses its downward magnetic influence, and the attraction force of the magnetic material below is released.

Next, to explain the operation of the above device, firstly, Fig. 1 and Fig. 2
As shown in the figure, when there is no sample container 8 directly below the vaporization section 3 (including the case where the sample container 8 is already attached to the vaporization section 3), the magnetic chuck 21 at the tip of the arm 20 is attached to the container 2.
It is above 7. From this state, when the sample container 8 carrying the attached body 16 is carried by the turntable 17 directly below the vaporization section 3, the magnetic shielding plate 26 is inserted under the magnet 25, as shown in FIG. In this state, the magnetic chuck 21 is pushed between the lid 16 of the sample container 8 and the conduit section 23 below the vaporization section 3.

In this state, because of the magnetic shielding plate 26, the magnetism of the magnet 25 does not reach the magnetic body 28 of the lid 16, and the lid 16 remains as it is. As already mentioned, a viscous substance such as fluorine grease or silicone grease is applied between the lid 16 and the opening edge of the sample container 8.

0- Next, as shown in FIG. 4 from this state, when the magnetic shielding plate 26 is retracted from below the magnet 25, the magnetic force of the magnet 25 reaches the magnetic body 28 of the lid body 6, and the lid body 16 is It is attracted and held by a magnetic chuck.

Here, due to the adhesive force of the viscous material applied between the lid 16 and the edge of the opening of the sample container 8, the sample container 8 is also normally lifted while remaining attached to the lid 16. Subsequently, as shown in FIG. 6, the arm 20 rotates while the magnetic shielding plate 26 is retracted from below the magnet 25, and the magnetic chuck 21 is retracted from between the sample container 8 and the conduit portion 23. At this time, only the lid 16 that has hit the stopper 29 is transported along with the magnetic chuck 21, and since the sample container 8 is held on the turntable 17, it is separated from the lid 16 and remains in place. Then, as shown in FIG. 6, when the magnetic chuck 21 moves above the container 27, the magnetic shielding plate 26
is pushed under. As a result, the attraction force of the lid 16 due to the magnetic force of the magnetic chuck 21 is released, and the lid 16 is dropped into the container 27.

11 Immediately after the magnetic chuck 21 is retracted from above the sample container 8, as shown in FIG. Attach it to the opening 3 of the vaporization section 3 at the back of 23. In the vaporization section 3, for example, the opening edge of the sample container 8 is pressed against an O-ring 22 fitted around the opening 3, thereby airtightly connecting the sample container 8 to the vaporization section 3. In this state, the heat from the heater 9 vaporizes the moisture contained in the sample 4 in the sample container 8, and sends this together with the carrier gas to the moisture measuring device. Thereafter, the lifting rod 19 is lowered and the sample container 8 is returned to the turntable 17. Furthermore, when the turntable 17 rotates and another sample container 8 with the lid 16 placed thereon comes directly under the conduit section 23, the operations described above are repeated.

[Effects of the Invention] As explained above, according to the present invention, airtightness can be ensured when the sample container 8 is closed with the lid 16, and the process from removing the lid 16 to attaching it to the vaporization section 3 can be quickly performed. This has the effect of increasing the processing efficiency of an automated moisture measuring device and preventing deterioration in measurement accuracy due to contamination with external moisture.

[Brief explanation of drawings]

FIG. 1 is a configuration diagram showing an example of a sample supply device of a moisture measuring device to which the sample container mounting device according to the present invention is applied, and FIGS. 2 to 6 show the vicinity of the sample container in the sample container mounting device according to the present invention. Fig. 7 is a side view showing the movement of the magnetic chuck according to the order of operation; Fig. 7 is a longitudinal side view of the sample container attached to the vaporizer; Fig. 8 is an example of an arm with a magnetic chuck configured at the tip. FIG. 3... Vaporization section 4... Sample 8... Sample container 1
6... Lid of sample container 17... Turntable
19... Lifting rod 20... Arm 21...
・Magnetic chuck 25...Magnet 26...Magnetic shielding plate
28...Magnetic material of lid

Claims (2)

[Claims] (1) When heating the sample to evaporate its moisture and supplying it to the moisture measuring device, a heat-resistant, non-volatile viscous material is applied between the lid 16 and the opening edge of the sample container 8. The lid 16 is placed on the opening of the sample container 8, and the sample container 8 is supplied under the vaporization section 3 to which the sample supply path and the carrier gas introduction path are connected, and the lid 16 is placed on the sample container 8.
Immediately after the sample container 8 is removed from the container, the sample container 8 is raised and its opening edge is pressed airtightly against the edge of the opening 3a opened at the lower end of the vaporizer 3. . (2) In a device that heats a sample, evaporates its moisture, and supplies the sample to the moisture measuring device, the sample container 8 is attached to the vaporizer 3, in which the sample supply path and the carrier gas introduction path are connected, and an opening is provided. Vaporizing section 3 with section 3a opening downward
and a sample container 8 in which the lid 16, which has a heat-resistant, non-volatile viscous material applied between the lid 16 and the opening edge of the sample container 8 and a magnetic material 28 provided on its upper surface, is placed on the opening. A magnet 25 and a magnetic shielding plate 26 that is inserted and retracted under the magnet 25 are provided. and a magnetic chuck 21 inserted and retracted between the vaporizer 3 and the vaporizer 3;
At the same time that the magnetic chuck 21 is retracted, the sample container 8 is pushed up and its opening is opened into the opening 3 of the vaporization section 3.
1. A sample container mounting device for a moisture measuring device, characterized in that the sample container mounting device comprises: