JPH0712698A - Moisture meter filter - Google Patents

Abstract

PURPOSE:To improve the measurement efficiency of a moisture meter. CONSTITUTION:A moisture meter comprises a gas introduction division which generates a carrier gas, a heating division 12 which introduces the carrier gas from the introduction division to heat a measurement target X, a moisture collection division 14 which adsorbs vaporization moisture from a carrier gas B led out of the heating division, an electronic balance unit 16 which detects an increment weight of the moisture collection division 14. The fore stage of the moisture collection division is provided with a filter 18 which adsorbs off vaporization products other than vaporization products other than vaporization moisture in the carrier gas B. The filter 18 has a holder 18a, an insertion division 18b, a container division 18c, an adsorbent 18d, and a cap 18e. The container division 18c is pierced by a penetrating hole 18f which communicates with the insertion division 18b and provided with a mesh 18g. The outer periphery of the holder 18a is provided with a temperature sensor 18j, a heater 18k, and a heat insulator 18l.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a filter for a moisture meter, and more particularly to heating an object to be measured to vaporize the water in the object to be measured, and collecting and measuring the vaporized water. The present invention relates to a filter for a moisture meter that measures the amount of moisture in a measurement object.

[0002]

2. Description of the Related Art The KF method (Karl Fisher method) is known as a means for measuring the amount of water in a solidified or liquid. This KF method is widely used as a highly accurate water quantification method and has become a standard method in each field.
The KF method uses a Karl Fischer reagent (KF reagent) containing iodine, sulfur dioxide, pyridine and methanol as components.
It is a method that utilizes quantitative reaction with water. In this way, the titer of reagent (H ₂ 0 / ml) leave orientation with standard, by measuring the equilibrium dropping amount of KF reagent was added dropwise to the reagent in the measurement object, and orientation titer , It is possible to know the water content in the measured object.

However, such a method for measuring the amount of water has a drawback that it requires a considerable skill in handling and requires special reagents and containers. Therefore, recently, there has been proposed a moisture meter that measures the amount of water in an object to be measured by heating the object to be measured, vaporizing the water in the object to be measured, and collecting and measuring the vaporized water. ing. However, even such a moisture meter has the technical problems described below.

[0004]

That is, in the above-mentioned moisture meter, when the object to be measured is heated, vaporized substances other than the vaporized water are also generated, and if they are collected together with the water, the object to be measured is There was a problem that the water content in the product could not be obtained accurately. The present invention has been made in view of such conventional problems, and the purpose thereof is to:
It is to provide a filter for a moisture meter that can improve the measurement accuracy of the moisture content.

[0005]

In order to achieve the above object, the present invention provides a gas introducing section for generating a carrier gas,
A heating unit that introduces a carrier gas from the gas introduction unit to heat an object to be measured, a moisture collection unit that adsorbs vaporized moisture from the carrier gas that is derived from the heating unit, and an increased weight of the moisture collection unit is detected. A filter for a moisture meter having an electronic balance unit to perform the filter, wherein the filter is provided in the preceding stage of the moisture collection unit and adsorbs and removes vaporized substances other than the vaporized moisture, and the adsorbent. It has a heater for heating.

[0006]

According to the moisture meter having the above structure, the filter is provided in the preceding stage of the moisture collecting unit for adsorbing the vaporized moisture in the carrier gas that carries the vaporized moisture vaporized from the object to be measured by being heated. Since this filter has an adsorbent that adsorbs and removes vaporized substances other than vaporized moisture, and a heater that heats this adsorbent, vaporized substances other than vaporized moisture that have separated from the object to be measured are adsorbed by the adsorbent. Therefore, the increased weight of the water collecting portion is only the water vaporized from the measured object.

In this case, when the heater is energized to heat the adsorbent, the moving speed of H ₂ O in the filter is increased and the measurement time is shortened.

[0008]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT A preferred embodiment of the present invention will be described in detail below with reference to the accompanying drawings. 1 to 6 show an embodiment of a filter for a moisture meter according to the present invention. FIG. 1 is a path and functional block diagram of a fluid system of a moisture meter to which the filter of the present invention is applied. The moisture meter shown in FIG. 1 includes a gas introducing unit 10 that generates a carrier gas A, and a gas introducing unit 10. A heating part 12 for introducing the carrier gas A from the part 10 to heat the object to be measured X, a water collecting part 14 for collecting vaporized water from the carrier gas B derived from the heating part 12, and the water collecting part A known electromagnetic balance type electronic balance unit 16 for detecting the increased weight of the portion 14 is provided.

A filter 18 for adsorbing and removing vaporized substances other than vaporized moisture in the carrier gas B is provided in the preceding stage of the moisture collector 14. The gas introduction unit 10 is an electromagnetic valve that switches between the air pump 10a, the air supplied from the air pump 10a, and the dry nitrogen N ₂ (which may be an inert gas such as He) supplied from the outside. 10b, a desiccator unit 10c that produces a carrier gas A by drying the mixed or single gas C delivered from the electromagnetic valve 10b, and a needle valve 10d that controls the flow rate of the carrier gas A supplied to the heating unit 12.
And a flow sensor 10e that detects the flow rate of the carrier gas A supplied to the heating unit 12.

2 and 3 are detailed views of the heating unit 12, which is a cylindrical heating tube 1 having an opening at one end.
2a, and the heating tube 12a is supported by a plurality of support plates 12b. Further, the heating tube 12a is provided with a heating zone a and a non-heating zone b such that the longitudinal axis direction thereof is divided into two substantially equal parts, and a portion corresponding to the heating zone a has its outer periphery covered. Thus, the planar heater 12c is wound and fixed.

Further, a square door receiving plate 12d is fixedly provided at the open end of the heating pipe 12a, and a door 12e for opening and closing the open end of the heating pipe 12a is hingedly attached to the lower end of the door receiving plate 12d. There is. The heating pipe 12a is provided on the inner surface of the door 12e.
A heat-resistant cushion material 12f that abuts the open end of the sheet and a heat-resistant, non-breathable cover 12g that covers the surface of the cushion material 12f are attached.

At the rear end side of the heating zone a of the heating tube 12a, there is provided an inlet 12h (see FIG. 3) for the carrier gas A which communicates with the flow sensor 10e of the gas inlet 10 and the heating tube 12a. A through hole 12i penetrating the heating tube 12a is formed at substantially the center of the non-heating zone, and a filter 18 is fixedly installed in the through hole 12i. Are guided into the filter 18.

The object to be measured X is housed in the carrier 20 and is first introduced into the non-heating zone b of the heating pipe 12a with the door 12e opened, and after being closed by the door 12e, transferred to the heating zone a. Then, the heater 12c applies heat thereto. The carrier 20 includes a frame 20a formed in a substantially rectangular shape, a pair of front and rear rollers 20b and 20c rotatably supported on a short side of the frame 20a, and a heat-resistant container 20d for placing and storing an object to be measured X. It consists of and.

The frame 20a and the rear roller 20c of the carrier 20 are made of stainless steel which is a non-magnetic material, and the front roller 20b is made of a permanent magnet. The moving mechanism 22 of the carrier 20 uses the non-heating zone b of the heating tube 12a.
Suction arm 22a installed on the outer periphery of the heating tube 12a
A guide rail 22b extending below the guide rail 22b along the longitudinal axis thereof, a flexible rack 22c movably mounted on the lower surface side of the guide rail 22b, and the rack 2
It has a pinion 22d that meshes with 2c and a geared motor (not shown) that rotationally drives the pinion 22d.

A magnet 22e for attracting the front roller 20b is provided on the tip end side of the suction arm 22a.
The guide rails 22b are provided on the lower case 26 of the upper and lower cases 24 and 26 that cover the outer circumference of the heating unit 12, and are fixed to the plurality of fixtures 22
It is supported by f. Further, on the upper surface side of the guide rail 22b, a pair of limit switches (not shown) for detecting the position of the suction arm 22a corresponding to the movement stroke of the carrier 20 is installed. In FIG. 3, a member indicated by reference numeral 28 is a protective cylinder that covers the outer circumference of the heater 12c wound around the outer circumference of the heating tube 12a.

In the moving mechanism 22 configured as described above, the object to be measured X is stored in the carrier 20 and the door 12e
With the open state, first, the non-heating zone b of the heating pipe 12a
When the pinion 22d is driven by the geared motor after being introduced into the above and closed by the door 12e, the rack 22c meshing with the pinion 22d moves to the heating zone a side of the heating pipe 12a.

Along with this movement, the suction arm 22a also moves to the heating zone a side of the heating tube 12a. At this time, since the magnet 22e attracts the front roller 20b of the carrier 20, the suction arm 22a moves. The carrier 20 also moves to the heating zone a side of the heating pipe 12a. Then, when the carrier 20 is completely moved into the heating zone a, this is detected by the limit switch, and the rotational drive of the motor is stopped.

When the heating of the object to be measured X is completed, the operation reverse to the above is performed and the door 12e is opened to take out the residue of the object to be measured X that has been burnt from the heating pipe 12a. You can FIG. 4 shows details of the filter 18 and its mounting structure. Filter 1 shown in the figure
Reference numeral 8 denotes a hollow-cylindrical holder 18a having an open upper end, a hollow-cylindrical insertion portion 18b projecting from the center of the lower end of the holder 18a, and a hollow-cylindrical container portion 18c housed in the holder 18a. The container 18c has an adsorbent 18d filled therein, and a cap 18e screwed to the upper end of the holder 18a.

The insertion portion 18 is provided at the center of the lower end of the container portion 18c.
A through hole 18f communicating with b is bored, and a mesh 18g is placed on the inner bottom surface of the container portion 18c. Also,
A packing 18h is interposed between the outer bottom surface of the container portion 18c and the inner bottom surface of the holder 18a, and a packing 18i is provided between the upper end surface of the container portion 18c and the inner surface side of the cap 18d. It is inserted and the cap 18e
When is screwed onto the holder 18a, the upper and lower ends of the container portion 18c are sealed.

A temperature sensor 18j is arranged on the outer periphery of the holder 18a, and the temperature sensor 18j
A sheet-shaped heater 18k is wound so as to cover the outer periphery of j, and a heat insulating material 18l is provided on the outer periphery of the heater 18k. The filter 18 configured in this manner has the insertion portion 18b formed in the upper portion of the heating tube 12a and the through hole 12 formed therein.
It is attached by inserting it into i and fixing it by welding or the like.

Then, by connecting the connector 30 to the protrusion 18m provided on the cap 18e, the filter 18 and the water collecting unit 14 are connected to each other via the tube 32. In addition, the part shown by the code | symbol 18n in FIG. 4 is a ventilation hole provided in the protrusion part 18m. The installation location of the filter 18 is not limited to the illustrated location, but may be provided on the heating zone a side, for example.

5 and 6 show details of the water collecting section 14. The water collection unit 14 shown in the figure has a cell stand 14a to which one end of the tube 32 is connected, and an adsorbent 14b for adsorbing vaporized water, for example, a cell 14c filled with zeolite. A connector portion 14d for mounting the tube 32 is fixedly attached to the side surface of the cell base 14a, and a hole portion 14e having a closed lower end is provided inside thereof.

Further, a cylindrical projection 14f projecting downward is integrally formed on the lower end surface of the cell base 14a, and the lower end of the cylindrical projection 14f is the load of the electromagnetic balance type electronic balance unit 16. The load of the water collecting unit 14 is transmitted to the electronic balance unit 16 by being brought into contact with the upper end of the transmission shaft 16a. The cell 14c has a substantially hollow cylindrical shape with open upper and lower ends, and has a small-diameter insertion portion 14h that is inserted into the hole 14e of the cell base 14a with packings 14g installed in a plurality of stages interposed therebetween. Is integrally formed at the lower end. A mesh 14i for preventing the adsorbent 14b from falling off is inserted inside the cell 14c, and a cap 14k holding a packing 14j is attached to the upper end side.

The cap 14k is provided at its upper end with a plurality of symmetrically arranged discharge ports 14l oriented in the horizontal direction. The discharge reaction force of the discharged carrier gas acts evenly on the cell 14c at the discharge port 14l.
The discharge reaction force prevents the measured value of the balance unit 16 from changing. Next, an operation for measuring the water content of the object X to be measured with the water content meter having the above configuration will be described.
In the measurement of the water content of the object to be measured X, first, the object to be measured X is moved to the heating zone a of the heating pipe 12 a of the heating unit 12 by the moving mechanism 2.
Positioned via 2. Then, in this state, the carrier gas A is introduced into the inside of the heating tube 12a through the inlet 12h, and the heater 12c of the heating unit 12 is energized and heated.

Moisture vaporized and separated from the object to be measured X by heating and vaporized substances other than water are carried in the carrier gas A and led out as the carrier gas B from the through hole 12i. The carrier gas B thus derived is introduced into the filter 18, and vaporized substances other than vaporized water carried in the carrier gas B are adsorbent 18d filled in the container portion 18c of the filter 18. Adsorbed on
It is removed from the carrier gas B.

At this time, in order to increase the removal efficiency of the adsorbent 18d, the heater 18k is appropriately energized to heat the adsorbent 18d to a predetermined temperature. Then, the carrier gas from which vaporized substances other than vaporized moisture have been removed is then introduced into the moisture collection section 14, and the vaporized moisture is adsorbed and held by the adsorbent 14b filled in the cells 14c. The amount of water of the object to be measured X is obtained by detecting the weight increased by the adsorbent 14b adsorbing and holding the vaporized water by the electronic balance unit 16.

The moisture meter constructed as described above does not require special skill, is simple in operation, and is a carrier gas for carrying vaporized moisture vaporized from the object X to be measured by being heated. Since the filter 18 for adsorbing and removing the vaporized substances other than the vaporized moisture is provided before the moisture collecting unit 14 for adsorbing the vaporized moisture in B, the increased weight of the moisture collecting unit 14 is vaporized from the object X to be measured. Only water
The measurement accuracy of the moisture meter is improved.

In this case, in the filter 18 of the present embodiment, the adsorbent 18d is a vaporized substance other than vaporized water that is generated when the object X to be measured is heated, for example, basic gases such as ammonia and trimethylamine, and various kinds. It is appropriately selected depending on the organic substance or the inorganic substance, and for example, activated carbon having different pore sizes mixed therein or activated carbon impregnated with an acidic substance is preferably used. At this time, by energizing the heater 18k, the adsorbent 18d can be heated to improve the adsorption performance of vaporized substances other than vaporized water, and the carrier gas passing between the adsorbents 18d from the lower side to the upper side. It is possible to increase the speed of B and avoid a decrease in measurement efficiency.

Further, the heater 18k is energized to turn on the adsorbent 18
When heating d, the adsorption performance of the adsorbent 18d can be changed by controlling the temperature of the adsorbent 18j. Further, since the adsorbent 18d adsorbs and removes vaporized substances other than vaporized water, the adsorbent 1 in the cell 14c
The life of the adsorption function of 4b can be extended. Further, when heated by the heater 18k, it is possible to prevent the temperature of the carrier gas B flowing between the adsorbents 18d from lowering and condensing the vaporized water being carried.

7 and 8 show the filter 1 of the present invention.
The result of the experiment conducted in order to confirm the effect of 8 is shown. In this experiment, the adsorbent 18d of the filter 18
As the commercially available activated carbon having a particle size of about 3 to 5 mm,
About 2 g was filled in a container portion 18c having a diameter of 10φ and a length of 55 mm. Nylon 6 is used as the object X to be measured, and a carrier gas is collected in a state where the filter 18 is passed and a state where the filter 18 is not passed, and gas chromatographic analysis is performed for the presence or absence of ε-captralactam in the carrier gas, In addition, the amount of ε-captolactam in the carrier gas was measured while raising the heating temperature.

As is clear from the results shown in FIG.
When activated carbon is not passed (upper side of FIG. 7), a peak of ε-captolactam is observed, but when activated carbon is passed (lower side of FIG. 7), the peak of ε-captolactam disappears and ε-captolactam is reduced. It can be seen that it is adsorbed and removed by activated carbon. Further, as is clear from the results shown in FIG. 8, when the activated carbon is not passed, the amount of ε-captralactam increases as the heating temperature rises, but when the activated carbon is passed, the amount is extremely high. It was found that the amount was significantly reduced, and the operational effect by using the filter 18 of the present invention was confirmed.

[0032]

As described above in detail in the embodiments,
According to the moisture meter of the present invention, it is possible to measure only vaporized moisture separated from the object to be measured by heating, without requiring special skill, and in addition to being easy to operate,
Measurement accuracy is improved.

[Brief description of drawings]

FIG. 1 is a functional configuration block diagram of a moisture meter to which the present invention is applied.

FIG. 2 is a perspective view of a heating unit and a filter of the same moisture meter.

FIG. 3 is a cross-sectional view of a heating unit of the moisture meter.

FIG. 4 is a cross-sectional view of a filter of the same moisture meter.

FIG. 5 is a perspective view of a moisture collecting unit of the moisture meter.

FIG. 6 is a cross-sectional view of a moisture collection unit of the moisture meter.

FIG. 7 is a graph showing the results of tests conducted to confirm the effects of the filter of the present invention.

FIG. 8 is a graph showing the results of tests conducted to confirm the effects of the filter of the present invention.

[Explanation of symbols]

 10 Gas Introducing Section 10c Desiccator Unit 10e Flow Sensor 12 Heating Section 12a Heating Tube 12c Heater 12h Inlet Port 14 Moisture Collecting Section 14a Cell Platform 14b Adsorbent 14c Cell 16 Electronic Balance Unit 18 Filter 18a Holder 18d Adsorbent 18j Temperature Sensor 18k Heater A Carrier gas B Carrier gas C Mixed gas X DUT

Claims (1)

[Claims] 1. A gas introducing section for generating a carrier gas,
A heating unit that introduces a carrier gas from the gas introduction unit to heat an object to be measured, a moisture collection unit that adsorbs vaporized moisture from the carrier gas that is derived from the heating unit, and an increased weight of the moisture collection unit is detected. A filter for a moisture meter having an electronic balance unit to perform, wherein the filter is provided in a preceding stage of the moisture collecting unit,
A filter for a moisture meter, comprising an adsorbent that adsorbs and removes vaporized substances other than the vaporized moisture, and a heater that heats the adsorbent.