JP3031834B2 - Liquid bubble removal device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for removing bubbles in liquid for removing bubbles mixed in a sample liquid.

[0002]

2. Description of the Related Art A sample solution is irradiated with light of a specific wavelength, the absorbance is measured from the transmitted light, and Lambert's light is measured from the measured value.
An absorptiometric method for detecting the concentration of a component using a conversion formula such as the Lambert-Beer's law is well known. When measuring the concentration of a sample liquid in which the component concentration changes momentarily by such a measurement method, the measurement is performed by irradiating the flow cell with light of a specific wavelength while supplying the sample liquid to the flow cell with a pump. It is.

However, simply supplying the sample liquid to the flow cell by the pump, when bubbles are mixed in the sample liquid, also introduces the bubbles into the flow cell. In such a case, excessive transmission or scattering of light is caused by the bubbles, so that an error may occur in a measured value or measurement may not be possible.

Accordingly, the present applicant has already disclosed in Japanese Unexamined Patent Publication No.
Japanese Patent Application Laid-Open No. 249745 proposes a liquid measurement device capable of performing accurate measurement by removing bubbles mixed in a sample liquid. In this apparatus, as shown in FIG. 4, the sample liquid 21 containing bubbles flowing into the degassing closed tank 25 is separated into a gas phase and a liquid phase by gravity.
When the valve 8 is closed and the other solenoid valve 30 is opened, the sample liquid at the bottom from which bubbles have been removed is taken into the flow cell 24 and measurement is started.

During this time, air bubbles in the sample liquid accumulate in the gas phase in the degassing closed tank 25 and the gas phase gradually increases. There is. At this time, the other solenoid valve 30 is normally closed. After the completion of the deaeration, one of the solenoid valves 28
Is closed, and the other solenoid valve 30 is opened to start measurement. The measurement may be performed with both the solenoid valves 28 and 30 closed. Reference numeral 31 denotes an electromagnetic valve control device that controls the electromagnetic valves 28 and 30.

[0006]

However, the above-mentioned conventional device requires two solenoid valves 28 and 30, which not only increases the cost of the device but also requires opening and closing operations of the solenoid valves 28 and 30. Therefore, there is a problem that the running cost is increased, and there is a concern that a trouble may occur due to the opening / closing operation of the solenoid valves 28 and 30. Furthermore, the solenoid valve control device 31 also requires a complicated operation such as adjusting the length of the opening time of the solenoid valve 28 according to the amount of bubbles.

The present invention has been made in view of such circumstances,
An object of the present invention is to provide a device for removing bubbles in a liquid having a simple configuration capable of efficiently removing bubbles in a sample liquid.

[0008]

According to the present invention, means for solving the above-mentioned problems are constituted as follows .

That is, a small-diameter outlet for allowing gas to be discharged is provided at the upper part of the closed vessel into which the sample liquid is introduced from the outside, and the lower part of the closed vessel is provided with a sample liquid connected to the measuring cell. A discharge port is provided, and one electromagnetic valve for stopping the flow of the sample liquid immediately before and during the measurement is provided between the discharge port and the measurement cell.

[0010]

When a liquid containing air bubbles is introduced into an airtight container, the air bubbles rise and separate into a gas phase and a liquid phase in the airtight container. Therefore, it is possible to guide the liquid containing no air bubbles from the liquid outlet provided at the lower part of the closed container to the measurement system line. On the other hand, gas can be discharged to the outside from an outlet provided at the upper part of the closed container.

At the outlet for allowing the gas to be discharged,
By providing pinholes or capillaries,
Gas can be discharged with priority over liquid.

In addition, since the measuring cell is connected to the outlet and one solenoid valve is provided between the outlet and the measuring cell, the sample liquid is previously led out of the closed vessel to the measuring system line. By closing the solenoid valve, the flow of the sample liquid to the measurement system line is stopped, and the sample liquid can be retained in the measurement system line. During this time, bubbles remaining in the sample liquid move to the downstream side of the measurement system line due to buoyancy. Therefore, after the elapse of the predetermined time, the sample liquid from which bubbles have been removed can be used for measurement.

[0013]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the apparatus for removing bubbles in liquid according to the present invention will be described below in detail with reference to the drawings. FIG. 1 is a schematic cross-sectional view of an apparatus 1 for removing bubbles in liquid. Reference numeral 2 denotes an airtight container formed in a cylindrical shape, reference numeral 3 denotes an upper lid, reference numeral 4 denotes a body, and reference numeral 5 denotes an O-ring. Is formed.

The inside of the upper lid 3 is formed in an upward funnel shape, and a pinhole-shaped (0.2 mmφ) gas discharge port (outlet) 6 is opened at the center of the uppermost part thereof. An exhaust pipe 8 is attached to the connected plug 7a.
Is connected.

On the other hand, an opening 9 formed in the upper side wall of the main body 4
A sampling pipe 10 for introducing the sample liquid 13 is connected to the connection plug 9a screwed into the connector plug 9a, and a connection plug 11a screwed into an opening (discharge port) 11 opened at the bottom of the main body 4 has Sample liquid 1 from which bubbles have been removed
One end of a connection pipe 12 for leading the sample 3 to the measurement system is connected, the other end of the connection pipe 12 is connected to the lower part of the flow cell 14, and the upper part of the flow cell 14 is connected to the exhaust pipe 8 through the connection pipe 15. With discharge pipe 17
The three-way joint 16 is connected to

With such a configuration, the sample liquid 13 containing bubbles introduced from the sampling pipe 10 into the closed container 2 has bubbles rising in the closed container 2 and the gas phase G
And a liquid phase (13), and only the gas is discharged from the gas discharge port 6 which is opened to face the gas phase G,
Bubbles in the sample liquid 13 are removed. For this reason, the sample liquid at the bottom of the container free of air bubbles is transferred to the flow cell 1
4, the flow cell 14 can be irradiated with light of a specific wavelength from a separately arranged light source (not shown), and the absorbance can be measured with high accuracy by a detector. . The sample liquid 13 that has passed through the flow cell 14 is discharged from the discharge pipe 17 to the outside of the system together with the gas discharged from the discharge pipe 8.

The above-described pinhole-shaped gas discharge port 6 allows gas to pass therethrough more easily than liquid, and can always remove gas, and generates a large amount of bubbles in the sample liquid 13 like hydrogen peroxide water. Even if it is contained, air bubbles can be efficiently removed, and the sample liquid 13 without air bubbles can be introduced into the flow cell 14 via the connection pipe 12 by the pressure of the sample liquid 13 flowing in. . Note that even if a small amount of the sample liquid 13 flows into the exhaust pipe 8, the sample liquid 13 is discharged out of the system from the discharge pipe 17, and thus does not affect the measured value.

Such a device 1 for removing bubbles in liquid is not particularly provided with a movable member, and can be provided at extremely low cost. Further, it is characterized in that there are few troubles and the running cost is low. It is. Further, since the bubbles can be removed at any time, the bubbles can be efficiently removed whether the amount of the bubbles is small or large. Although not shown, the pinhole-shaped gas outlet 6 may have a normal diameter, and a capillary may be used instead of the exhaust pipe 8.

When the sample liquid 13 is circulated, a loop as shown in FIG. 2 may be formed. For example, when hydrogen peroxide solution is introduced into the flow cell 14 in order to measure the concentration of the hydrogen peroxide solution, the discharge pipe 17 is introduced into the container 19 storing the hydrogen peroxide solution, and the hydrogen peroxide solution is discharged from the container 19. Pump 18
What is necessary is just to communicate with the sampling pipe 10 through 0.

In this case, the flow rate of the sample liquid 13 flowing through the flow cell 14 is determined by the discharge force of the pump 20, but even if the sample liquid 13 may be mixed into the exhaust pipe 8. And the sample liquid 13 that has flowed through the flow cell 14, is once collected in the dye container 19, introduced again into the closed container 2, separated into a gas phase and a liquid phase, and
Can be introduced inside.

Further, in the present invention, as shown in FIG.
Between the outlet 11 and the measuring cell 24, just before the measurement and
And one electromagnetic stop to stop the flow of the sample liquid 13 during measurement
A valve is provided.

That is, in FIG. 3, reference numeral 32 denotes one solenoid valve provided between the outlet 11 of the closed container 2 and the measuring cell 24. The sample liquid 13 passing through the closed container 2
By the pump 20, the solenoid valve 32 from the connection pipe 12a,
It is transferred to the measurement cell 24 via the connection pipe 12b.

By the way, when the solenoid valve 32 is not provided, the sample liquid 13 from which most of the air bubbles have been removed is discharged from the outlet 11 of the closed vessel 2, but some air bubbles are discharged from the connection pipe 12 and the measuring cell 24. May remain in the sample liquid 13 in the inside.

Therefore, in this embodiment, an electromagnetic valve 32 is provided between the closed vessel 2 and the measuring cell 24. Then, the electromagnetic valve 32 is closed from the start of the measurement, for example, about one second before the measurement is completed. In this way, the connection pipe 12 and the measurement cell 24
Bubbles remaining in the sample liquid 13 in the
It moves to the connection pipe 15 upstream of the measurement cell 24.

Thereafter, measurement is performed. When the measurement is not performed, the solenoid valve 3 is used to replace the sample liquid 13.
Set 2 to open.

As described above, in the present embodiment, the electromagnetic valve 32 is closed before the measurement is started. Therefore, immediately before the measurement, the air bubbles remaining in the sample liquid have disappeared. Since it is in the closed state, there is no supply of the sample liquid thereafter, and no air bubbles enter the measurement cell 24 during the measurement.

[0027]

As described above, according to the apparatus for removing bubbles in liquid of the present invention, the sample liquid containing bubbles introduced into the closed vessel is separated into a gaseous phase and a liquid phase and provided on the upper part thereof. Gas can be discharged from an outlet such as a pinhole or a capillary, and only a sample liquid without bubbles can be discharged from a sample liquid discharge port provided below the gas hole.

A single electromagnetic valve is provided between the sealed container and the measuring cell, and the electromagnetic valve is closed from immediately before the measurement is started in the measuring cell until the measurement is completed. Therefore, there is an effect that bubbles in the sample liquid to be measured can be reliably removed.

[Brief description of the drawings]

FIG. 1 is a configuration explanatory view showing a preferred embodiment of an apparatus for removing bubbles in liquid according to the present invention.

FIG. 2 is an explanatory diagram of a configuration in the embodiment.

FIG. 3 is a configuration explanatory view showing an embodiment of the apparatus for removing bubbles in liquid according to the present invention.

FIG. 4 is a configuration explanatory view showing a conventional example.

[Explanation of symbols]

2 ... closed container, 6 ... outlet, 11 ... outlet, 32 ... solenoid valve.

────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Toshiya Ito 2 Higashi-cho, Kichijoin-gu, Minami-ku, Kyoto, Kyoto Inside Horiba, Ltd. (56) References JP-A-48-100181 (JP, A) Sho Akai 63-20061 (JP, U) (58) Fields investigated (Int. Cl. ⁷ , DB name) G01N 1/10 G01N 35/00

Claims (3)

(57) [Claims] 1. A small-diameter outlet for allowing gas to be discharged is provided at an upper portion of a closed container into which a sample liquid is introduced from the outside, and a sample liquid connected to a measurement cell is provided at a lower portion of the closed container. An apparatus for removing air bubbles in a liquid, comprising: a discharge port; and a single electromagnetic valve between the discharge port and the measurement cell to stop the flow of the sample liquid immediately before and during the measurement. 2. The apparatus for removing bubbles in liquid according to claim 1 , wherein an outlet having a small diameter for allowing the gas to be discharged is a pinhole. 3. A capillary according to claim 1, wherein said small-diameter outlet for allowing discharge of said gas is a capillary.
A device for removing bubbles in liquid according to item 1.