JP4545976B2 - Sample moisture vaporizer - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
In the present invention, in order to measure the moisture content contained in a sample, the sample is heated in a closed space, the moisture contained in the sample is vaporized, this moisture is sent to a moisture meter with a carrier gas, and the moisture content is measured. The present invention relates to a sample moisture vaporizer.
[0002]
[Prior art]
An indirect vaporization method using a moisture vaporizer is used as an effective measurement method for moisture measurement of a solid sample using the Karl Fischer moisture determination method. This can measure the moisture content of a sample such as a plastic pellet that does not dissolve in the electrolytic solution for moisture measurement or the titration solvent.
[0003]
FIG. 4 shows an outline of a conventional sample moisture vaporizer. This sample moisture vaporizer has a cylindrical vaporization chamber 1 made of a glass tube or the like, and a heating furnace 8 is provided outside the left end in FIG. A sample dish introduction port is provided at the right end of the vaporization chamber 1 in FIG. 4, and this sample introduction port is hermetically closed with a lid 7. A carrier gas introduction port 3 for introducing a carrier gas such as dry air or nitrogen gas into the vaporization chamber 4 is provided at the lower end of the vaporization chamber 1 in FIG. At the left end of the vaporizing chamber 1 in FIG. 4, a gas discharge port 4 is provided to discharge moisture evaporated from the vaporizing chamber 1 together with the carrier gas. A sample insertion port 2 is provided obliquely at the upper part of the substantially middle part of the vaporizing chamber 1 and a stopper 10 for fitting the sample closing port 10 is fitted.
[0004]
When the moisture content in a sample is measured using such a sample moisture vaporizer, first, the lid 7 of the sample dish inlet is opened, and the sample dish 5 and the sample dish 5 are made of a magnetic material or the like. The sample extruded body 6 is introduced into the vaporizing chamber 1 and the lid 7 of the sample introduction port is closed.
In this state, the sample tray 5 is located directly below the sample insertion port 2.
[0005]
Below the vaporization chamber 1 is disposed a moving mechanism 9 that holds the sample extrudate 6 by magnetic force or the like and moves the sample extrudate 6 left and right in the vaporization chamber 1 in FIG. The moving mechanism 9 moves the sample extrudate 6 in the vaporizing chamber 1 from the position shown in FIG. 4 to the left in the figure, and moves the sample pan 5 to the position of the heating furnace 8. Here, while introducing the dried carrier gas from the gas inlet 3, the sample dish 5 is heated in the heating furnace 8, and the water adhering to the sample dish 5 and the wall of the vaporizing chamber 1 is vaporized. The vaporized water is transported by the carrier gas introduced from the gas inlet 3 and is transported from the gas outlet 4 to a moisture meter (not shown). Next, the sample dish 4 is returned to the original position shown in FIG. 4, and the sample dish 4 is cooled to room temperature.
[0006]
Next, when the moisture measurement value of the carrier gas sent from the vaporization chamber 1 to the moisture meter is stabilized, the sample stopper 2 of the sample inlet 2 is removed, the sample inlet 2 is opened, and the sample weighed in advance is taken as the sample pan 5. Then, the stopper 2 of the sample inlet 2 is fitted and the sample inlet 2 is closed. Thereafter, the sample pan 5 is moved again to the position of the heating furnace 8. Here, while introducing the dried carrier gas from the gas inlet 3, the sample in the sample dish 5 is heated in the heating furnace 8, and the moisture of the sample is vaporized. The vaporized water is transported by the carrier gas introduced from the gas inlet 3 and is transported from the gas outlet 4 to the moisture meter, where the moisture is measured.
[0007]
Thereafter, the sample tray 5 is returned to the original position shown in FIG. 4, the lid 7 of the sample tray introduction port is opened, and the sample tray 5 and the sample pusher 6 are taken out from the vaporization chamber 1. After connecting another sample pan 5 to the sample extrudate 6 and introducing them into the vaporizing chamber 1, the lid 7 is closed. In the same manner, the water content of the next sample is measured with the new sample pan 5.
[0008]
[Problems to be solved by the invention]
In the conventional sample moisture vaporizer, a sample is loaded from the sample loading port 2 into the sample tray 5 immediately below it as described above. At this time, the sample may spill out of the sample tray 5. When a sample spills from the sample pan 5, the moisture content of the sample is measured with a corresponding amount, and an error occurs in the measured value of the moisture content. In addition, it takes time to take out the sample spilled from the sample dish 5 from the vaporization chamber 1.
[0009]
Moreover, the sample introduction port 2 provided in the vaporization chamber 1 of the conventional sample moisture vaporizer is fixed at a certain angle, and the angle cannot be changed. For this reason, depending on the size and particle size of the sample to be loaded, it may be difficult to load the sample from the sample inlet 2, which is one factor that causes the sample to easily spill from the sample dish 5.
[0010]
Furthermore, since the conventional sample moisture vaporizer requires a space for moving the sample pan 5 between the sample inlet 2 and the heating furnace 8, the vaporization chamber 1 has an inner diameter of about 30 mm and a length of There are about 300 to 400 mm, and the internal volume is about 200 to 800 cm ³ . As described above, preliminary drying for sufficiently drying the inside of the vaporizing chamber 1 together with the sample dish 5 is performed before vaporizing the moisture of the sample. However, the larger the internal volume of the vaporizing chamber 1 is, the more time is required for this preliminary drying.
[0011]
In particular, when the sample tray 5 is replaced, moisture adhering to the sample tray 5 and the sample extruded body 6 is mixed in the vaporizing chamber 1 in the atmosphere. At this time, moisture in the atmosphere is also mixed into the vaporizing chamber 1 together with the atmosphere. In some cases, moisture from a human fingertip may adhere to the sample extrudate 6. These moisture are gradually released from the vaporizing chamber 1 by the preliminary drying as described above, but a drying time corresponding to the internal volume of the vaporizing chamber 1 is required until all the mixed water is discharged. .
[0012]
In addition, after the preliminary drying, the sample dish 5 is cooled before the sample is added. However, in the conventional sample moisture vaporizer, the sample dish 5 is inside the vaporization chamber 1, so Only the sample dish 5 can be cooled, and the use dish 5 cannot be directly cooled. For this reason, in the vaporizing chamber 1 having a large volume, it is necessary to cool the sample dish 5 after the preheating for a long time.
[0013]
In view of the problems in the conventional sample moisture vaporizer, the present invention can put a sample into a sample container without spilling it, and reduce the volume of the container for heating the sample to perform preliminary heating and subsequent cooling. It is an object of the present invention to provide a sample moisture vaporization apparatus that can be carried out in a short time and therefore can easily and easily vaporize the moisture in the sample.
[0014]
[Means for Solving the Problems]
In the present invention, in order to achieve the above object, the sample container 21 is attached to the sample container holder 11 having the sample insertion port 12, and the opening on the upper surface of the sample container 21 faces the sample insertion port 12. 12 is arranged just below. Then, the sample container 21 is not moved, but the heating furnace 26 is moved up and down, and is moved between the position below the sample container 21 and the position surrounding the sample container 21.
[0015]
That is, the sample water vaporizer according to the present invention includes a sample container holder 11 having a sample inlet 12, a stopper 13 that hermetically closes the sample inlet 12, and a sample container holder 11 at a position directly below the sample inlet 12. A sample container 21 having an upper surface opened toward the sample inlet 12, a carrier gas inlet 14 provided in the sample container holder 11 for introducing a dried carrier gas into the sample container 21, and a sample container The holder 11 includes a carrier gas discharge port 16 that discharges a carrier gas from the sample container 21, and a heating furnace 26 that is disposed so as to surround the sample container 21 and heats the sample container 21. The heating furnace 26 is moved up and down by an elevating mechanism, and is disposed so as to surround the sample container 21 held vertically by the sample container holder 11 when it is raised to the highest position.
[0016]
In such a sample moisture vaporizer, the sample container 21 and the sample inlet 12 into which the sample is introduced are fixed up and down via the sample container holder 11, so that the sample introduced from the sample inlet 12 Is directly stored in the sample container 21. For this reason, the sample does not spill from the sample container 21.
[0017]
In this case, if the sample container holder 11 can be tilted, the sample inlet 12 and the sample container 21 with the heating furnace 26 lowered when the sample is put into the sample container 21 from the sample inlet 12 with a cartridge case or the like. Since the sample can be thrown at an arbitrary angle, the sample can be put into the sample container 21 easily.
[0018]
After loading the sample into the sample container 21, the sample inlet 12 is closed with the stopper 13, the sample container 21 is made vertical, the heating furnace 26 is raised to the position of the sample container 21, and the sample container 21 is heated. Vaporize sample moisture. The vaporized water is transported by the dry carrier gas sent from the carrier gas inlet 14 into the sample container 21, and is transported together with the carrier gas from the carrier gas outlet 16 to the moisture meter.
[0019]
Since the volume of the space to be vaporized when the moisture of the sample is vaporized is substantially the same as the volume of the sample container 21, the sample container 21 is preheated, dried, and further cooled prior to the introduction of the sample. Time can be shortened, and the time for vaporization and measurement of moisture in the sample can be reduced as a whole.
[0020]
Further, the flange 22 projecting the sample container 21 to the outside of the upper surface opening is inserted between the sample container holder 11 and the container mounting spring 19 provided on the lower surface thereof, and is detachably attached to the sample container holder 11. As a result, the sample container 21 can be easily replaced, and a plurality of sample containers 21 can be sequentially attached to the sample container holder 11 to efficiently evaporate the moisture of the sample.
[0021]
DETAILED DESCRIPTION OF THE INVENTION
Next, embodiments of the present invention will be described specifically and in detail with reference to the drawings.
1 and 3 are longitudinal sectional front views of a sample moisture vaporizer according to an embodiment of the present invention, and FIG. 2 is a side view of the sample moisture vaporizer.
[0022]
As shown in these figures, the frame 25 is provided with a sample container holder 11 made of a heat-resistant material such as glass, ceramics or fluorine resin. The lower surface of the sample container holder 11 is subjected to planar finishing by polishing or the like.
The sample container holder 11 is attached to the frame 25 via a rotation shaft of a rotation mechanism 23 attached to the back of the frame 25 and can be inclined at an arbitrary angle with respect to the frame 25.
[0023]
A cylindrical upright sample inlet 12 is provided at the center of the sample container holder 11, and a taper is formed on the inner peripheral surface of the sample inlet 12 so that the inner diameter becomes smaller as it goes downward. . A through-hole 33 is provided in the lower wall surface of the sample inlet 12, and the through-hole 33 is provided in the wall of the sample inlet 12 on the side opposite to the carrier gas inlet 14 described later.
The sample inlet 12 is fitted with a stopper 13 having a taper corresponding to the taper on the lower end side in an airtight manner so that the sample inlet 12 can be airtightly closed. In the main surface of the lower end portion of the cock, only one groove 34 is formed vertically.
[0024]
Further, a pair of guides 18 and 18 are provided on both sides of the lower surface of the sample container holder 11. Further, a pair of container mounting springs 19 and 19 are provided below the guides 18 and 18 at a distance from the lower surface of the sample container holder 11. 2 are fixed to the frame 25 and the sample container holder 11, and the left end in FIG. 2 is a free end. The free ends of the container mounting springs 19, 19 are curved downward and away from the lower surface of the sample container holder 11.
[0025]
As the sample container 21 for storing a sample for vaporizing moisture, a heat-resistant and highly airtight material such as Pyrex glass is used. The sample container 21 is in the shape of a bottomed container having an open upper end and a flange 22 protruding outward from the open upper end. The upper surface of the flange 22 is planarized by polishing.
[0026]
The sample container 21 is attached so that the flange 22 is suspended from the sample container holder 11 by fitting the flange 22 between the guides 18 and 18, the sample container holder 11 and the container attachment springs 19 and 19. That is, the sample container 21 has a flange 22 sandwiched between the sample container holder 11 and the pair of container mounting springs 19 and 19 and the flange 22 is sandwiched between the pair of guides 18 and 18 from both sides. It is attached to the sample container holder 11 in a position-controlled state. When the flange 22 of the sample container 21 is inserted to the deepest position where it is stopped by the guides 18 and 18, the upper surface opening of the sample container 21 is positioned directly below the sample insertion port 12. In this state, the smooth upper surface of the flange 22 of the sample container 21 is pressed against the smooth lower surface of the sample container holder 11 by the elasticity of the container mounting springs 19, 19 and the airtightness of the sample container 21 is ensured. The distance between the container mounting springs 19 and 19 and the sample container holder 11 is adjusted by an adjusting screw 20.
[0027]
A carrier gas introduction port 14 for supplying a carrier gas such as dry air or nitrogen gas is provided on one side surface of the sample container holder 11, and this carrier gas introduction port 14 is connected via a flexible pipe 15. Connected to a carrier gas supply source (not shown). The carrier gas inlet 14 communicates from the lower surface of the sample container holder 11 to the upper surface opening of the sample container 21 attached to the holder 11.
[0028]
On the other side surface of the sample container holder 11, a carrier gas discharge port 16 that discharges moisture evaporated in the sample container 21 together with the carrier gas is provided. The carrier gas discharge port 16 is connected to a moisture meter (not shown) through a flexible pipe 17. The carrier gas outlet 16 communicates with the lower part of the sample inlet 12 on the center side of the sample container holder 11.
A cooling fan 24 is provided on the back side of the frame 25 toward the sample container 21 attached to the sample container holder 11.
[0029]
Further, a heating furnace 26 is provided below the sample container 21 attached to the sample container holder 11. The heating furnace 26 has an upper surface opened and a heater on the peripheral wall or the peripheral wall and the bottom wall. The heating furnace 26 is fixed to a movable frame 27 attached to the frame 25 so as to be movable up and down. A rack 28 is attached to the movable frame 27, and a pinion 30 that is rotated by a motor 31 attached to the frame 25 is engaged with the rack 28. Thereby, the heating furnace 26 can be moved up and down by the rotation of the motor 31.
[0030]
1 and 2 show a state where the heating furnace 26 is at the lowest position, and FIG. 3 shows a state where the heating furnace 26 is at the highest position. As shown in FIG. 3, when the heating furnace 26 is at the highest position, the heating furnace 26 surrounds the periphery and bottom of the sample container 21 attached to the sample container holder 11. The frame 25 is provided with, for example, a sensor 32 in which a pair of light emitting elements and light receiving elements are opposed to each other. The sensor 32 is movable when the heating furnace 26 is at the highest position as shown in FIG. The position of the heating furnace 26 is detected by the presence of.
[0031]
Next, a procedure for vaporizing the moisture of the sample using the sample moisture vaporizing apparatus having such a configuration will be described.
First, as shown in FIGS. 1 to 3, an empty sample container 21 is attached to the sample container holder 11. A sample boat made of aluminum foil may be attached to the bottom of the sample container 21. This is to prevent the sample from sticking to the inner wall of the sample container 21 due to heating.
[0032]
In this state, the heating furnace 26 is raised from the position shown in FIGS. 1 and 2 to the position shown in FIG. 3, the empty sample container 21 is heated by the heating furnace 26, and moisture adhering to the inner wall of the sample container 21 Moisture contained in the air in the sample container 21 is vaporized. At this time, as shown in FIG. 3, the groove of the stopper 13 is shifted from the through hole 33 of the sample introduction port 12. A carrier gas such as dried air or nitrogen gas is introduced into the sample container 21 from the carrier gas inlet 14, and the water vaporized together with the carrier gas is sent from the carrier gas outlet 16 to the moisture meter.
[0033]
When the moisture in the sample vessel 21 evaporates and the moisture measurement value of the moisture meter is stabilized at a low level close to almost zero, the heating of the sample vessel 21 is stopped, and the heating furnace 26 is moved from the position shown in FIG. Lower to the position shown in 2. Further, the fan 24 is operated to cool the sample container 21.
After the sample container 21 is sufficiently cooled, the stopper 13 is removed from the sample introduction port 12 of the sample container holder 11, and a cartridge case or a dedicated sample collecting tool is used to enter the sample container 21 from the opened sample introduction port 12. Load the sample. At this time, the sample container holder 11 may be inclined by the rotation mechanism 23 at an angle at which the sample can be easily introduced into the sample container 21 from the sample introduction port 12.
[0034]
After inserting the sample, the stopper 13 is fitted into the sample inlet 12, and the sample container holder 11 is returned to the horizontal position, that is, the sample container 21 is returned to the vertical position as shown in FIGS. At this time, the stopper 13 is fitted into the sample inlet 12 so that the groove 34 of the stopper 13 coincides with the through hole 33 of the inlet 12. In this state, when the dried carrier gas is fed into the sample container 21 from the carrier gas introduction port 14, the air mixed into the sample container 21 when the sample is charged enters from the groove 34 of the stopper 13 and the through hole 33 of the sample insertion port 12. Discharged.
Thus, after the air mixed in the sample container 21 is discharged for a certain period of time, the stopper 13 is rotated to shift the groove 34 from the through hole 33 of the sample inlet 12, and the sample inlet 12 is hermetically closed by the stopper 13. .
[0035]
Thereafter, the heating furnace 26 is raised from the position shown in FIGS. 1 and 2 to the position shown in FIG. 3, the sample container 21 is heated, and the moisture measurement is started. Moisture vaporized from the sample in the sample container 21 is sent to the carrier gas discharge port 16 by the dried carrier gas sent from the carrier gas inlet port 14 and conveyed to the moisture meter, where the moisture content is transferred. Is measured.
[0036]
When the amount of water detected by the moisture meter becomes almost zero, the measurement of the amount of water is finished. Thereafter, the heating furnace 26 is lowered from the position shown in FIG. 3 to the position shown in FIGS. In this state, the sample container 21 is removed from the sample container holder 11, another new sample container 21 is attached to the sample container holder 11, and the water content of the next sample is measured in the same manner.
[0037]
In the above-described embodiment, the air mixed in the sample container 21 is discharged by the groove 34 of the stopper 13 and the through-hole 33 of the sample inlet 12, but the pipe 17 connected to the carrier gas outlet 16 is used. A three-way valve may be provided in the middle, and the air mixed in the sample container 21 at the time of sample introduction may be discharged prior to vaporizing the moisture of the sample by switching the three-way valve.
[0038]
【The invention's effect】
As described above, in the sample moisture vaporization apparatus according to the present invention, the sample container 21 and the sample inlet 12 into which the sample is charged are fixed up and down with the sample container holder 11, so that the sample is charged. The sample can be introduced without spilling from the mouth 12 into the sample container 21. In addition, since the sample can be introduced by tilting the sample introduction port 2 and the sample container at an arbitrary angle, it is easy to introduce the sample, and also in this respect, sample spillage can be prevented.
[0039]
Furthermore, since it is not necessary to move the sample in the sample container 21 and the heating furnace 26 is moved to preheat the sample or heat the sample, the sample container 21 having a small volume can be used. For this reason, preheating of the sample container before vaporizing the moisture of the sample and subsequent cooling can be performed in a short time.
[Brief description of the drawings]
FIG. 1 is a partially cutaway longitudinal front view showing a state when a heating furnace is at a lowest position in a sample moisture vaporizer according to an embodiment of the present invention.
FIG. 2 is a side view showing a state when the heating furnace is at the lowest position in the sample moisture vaporizer according to the embodiment.
FIG. 3 is a longitudinal sectional front view of a main part showing a state when the heating furnace is at the highest position in the sample moisture vaporization apparatus according to the embodiment.
FIG. 4 is a schematic longitudinal sectional side view showing a conventional example of a sample moisture vaporizer.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 11 Sample container holder 12 Sample inlet 13 Cock 14 Carrier gas inlet 16 Carrier gas outlet 21 Sample container 26 Heating furnace 28 Rack 30 Pinion

Claims (4)

In an apparatus for vaporizing moisture from a sample for measuring water content, a sample container holder (11) having a sample inlet (12), a stopper (13) for hermetically closing the sample inlet (12), and a sample inlet A sample container (21) attached to the sample container holder (11) at a position directly below the mouth (12) and having an upper surface opened toward the sample insertion port (12); and a sample container holder (11), A carrier gas inlet (14) for introducing a dried carrier gas into the sample container (21), and a carrier gas outlet (19) provided in the sample container holder (11) for discharging the carrier gas from the sample container (21). 16) and a heating furnace (26) arranged so as to surround the sample container (21) and heating the sample container (21). The heating furnace (26) is arranged so as to surround the sample container (21) held vertically by the sample container holder (11) when the heating furnace (26) is moved up and down by an elevating mechanism and raised to the highest position. 2. The sample moisture vaporizer according to 1. The sample water vaporizer according to claim 1 or 2, wherein the sample container holder (11) is tiltable. The sample container (21) is detachable by inserting a flange (22) projecting outside the upper surface opening between the sample container holder (11) and a container mounting spring (19) provided on the lower surface thereof. The sample water vaporizer according to any one of claims 1 to 3, wherein the sample moisture vaporizer is attached to a sample container holder (11).

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