JPH02280050A - Metallic component analyzing device - Google Patents

Abstract

PURPOSE:To prevent damage of parts, a piping and a joint part, and a liquid spill caused by clogging of a column by providing a valve for discharging sample water of the inside of a passage at the time when pressure in the passage exceeds prescribed pressure, between the column and a pressure pump. CONSTITUTION:When concentrating columns 8, 9 and a separating column 11 are clogged and internal pressure of passages such as a passage 30a, inflow passages 8a, 9a, a line 33 or the like rise abnormally, a signal for opening check valves 23 - 26 is generated from a control part C based on detecting signals from pressure switches 6A, 17A provided on a sample water supply passage 30 and a solution supply passage 31 and a pressure switch attached to the line 33, and sample water in the passage is discharged to a drainage 34. Accordingly, a high pressure state of the passage is obviated quickly, and damage of parts, a piping and a joint part of switching valves 7, 10, the pressure switches 6A, 17A, the columns 8, 9 and 11 or the like and an accident of a liquid spill therefrom are prevented.

Description

Detailed Description of the Invention "Field of Industrial Application" This invention is a metal component analysis device that uses ion exchange separation to efficiently detect minute amounts of metal components in ultrapure water. This is a related story.

``Prior Art'' FIG. 3 shows a metal component analyzer previously proposed by the present inventors in Japanese Patent Application No. 180529/1983.

The symbol l in the figure is an automatic flow path switching valve. A sample water supply path 30 is connected to the outlet of this automatic flow path switching valve l.

The sample water supply path 30 includes a liquid feeding pump 2 and a reactor 3.
, Overflow container 1: A directional switching valve 5, a pressure pump 6, and a pressure switch 6A are attached. This sample water supply path 30 is finally connected to the first four-way switching valve 7.
It is connected to the. This first four-way switching valve 7 includes a
An inflow path 8a to the condensation column 8, an inflow path 9a to the second concentration column 9, and an eluent supply path 31 are connected. The eluent supply path 31 is provided with a pressure pump 17 and an eluent reservoir 18 . Outflow path 8b from the first concentration column 8
The outflow path 9b from the second a contraction column 9 is connected to a second four-way switching valve 10.

A line 33 connected to an analysis means 32 consisting of a separation column II and an absorption photometer 12 and a line 35 connected to a drainage channel 34 are further connected to the second four-way switching valve IO. A flow meter 19 is attached to the line 35.

Next, the operation of this metal component analyzer will be explained.

The automatic flow path switching valve l has six sample water flow paths IA.
-IF is connected. One of these sample water flow paths IA-IF is selectively connected to the sample water supply path 30.

The sample water flowing into the sample water supply path 30 is sent to the reactor 3 by the liquid feeding pump 2. A reaction liquid supply path 37 including a reaction liquid storage section 15 and a supply pump 16 is connected to the upstream side of the reactor 3, and a reaction liquid for ionizing metals in the sample water is added to the sample water. . The sample water to which this reaction solution has been added is mixed in the reactor 3 at a predetermined temperature.

The sample water that has passed through this reactor 3 is transferred to an overflow container 4.
Sample water that exceeds a certain storage amount is discharged to the drainage channel 34 through a line indicated by . The sample water that has passed through the overflow container 4 is transferred to the three-way switching valve 5 . The three-way automatic switching valve 5 connects the sample water supply path 30
A part of the sample water flowing through the drain is guided to the drainage channel 34 through a line indicated by the symbol L3. That is, when the automatic flow path switching valve I is switched and another sample water is supplied, the flow path is first switched to the 3 side on the line, and the flow path is switched between the automatic flow path switching valve 1 and the three-way switching valve 5. Completely wash away any remaining sample water. After this, the flow path is switched to allow the sample water to flow along the sample water supply path 30.

The sample water that has passed through the three-way switching valve 5 is pressurized by a pressure pump 6. Note that when the sample water is pressurized to a predetermined pressure or higher by this pressure pump 6, the pressure filter A is turned on and the control unit C is instructed to stop the operation of the pressure pump 6. It is designed to output a detection signal.

The sample water pressurized by the pressure pump 6 is transferred to the first four-way switching valve 7.
is supplied to the 1a condensation column 8 or the second concentration column 9.

The first four-way switching valve 7 and the second four-way switching valve 10 allow the sample water supplied from the sample water supply channel 30 to pass through the concentrating column 1.8 or 9, and then pass through the line 35 to the drainage channel 34.
The flow path for the metal ion concentration step leading to the metal ion concentration process and the eluent supply path 31
A flow path for the metal ion elution step in which the eluent supplied from the ionizer passes through the concentration column 9 or 8 and then leads to the analysis means 32 is formed alternately with respect to the concentration column 8.9.

This four-way switching valve7. The switching of lO is performed by a signal sent from the control unit C when the withdrawal value of the sample liquid passing through the line 35 measured by the flowmeter 19 reaches a set value.

When the sample liquid passes through the concentration column 8 or 9, metal ions in the sample liquid are adsorbed by the column 8 or 9. The metal ions adsorbed on the column 8 or 9 are eluted by the eluent supplied from the 1 supply path 31 to the column 8.9.
The sample is eluted from the sample and transported to the analysis means 32.

The metal ions carried to the analysis means 32 are transferred to the separation column 11
After being purified, it is colored by a coloring liquid from the coloring liquid supply path 38, and its concentration is measured by an absorptiometer 12.

"Problem to be solved by the invention" The above conventional metal component analyzer 1! , when the concentration column 8 or 9 becomes clogged and the pressure in the flow path between the pressure pump 6 and the concentration column 8.9 increases abnormally,
The pressure gas isotiro A detects this and stops the pressurizing pump 6, thereby preventing a failure of the device.

However, in the conventional metal analyzer, even if the pressurizing pump 6 is stopped, parts such as the concentration column 89 and the switching valve 7, piping, and joints are likely to be damaged or leak. Ta.

[Means for Solving the Problems] In the metal component analyzer of the present invention, the sample water in the flow path is discharged between the column and the pressure pump when the pressure in the flow path exceeds a predetermined pressure. The above-mentioned problem was solved by providing a valve.

Although a solenoid valve can be used as the surface valve, a mechanical valve whose opening pressure is set by a spring can also be used. When a solenoid valve is used as this valve, its opening operation is performed based on a signal from a pressure sensor that detects the pressure in the flow path.

In the metal component analyzer of the present invention, when the concentration column becomes clogged and the pressure in the flow path increases abnormally, the valve opens and the sample water between the column and the pressure pump flows into the discharge path. The LE force in the flow path quickly decreases.

"Example" Hereinafter, the metal component analyzer of the present invention will be described in detail with reference to the drawings. Note that the same components as those in the conventional example described above are given the same reference numerals to simplify the explanation.

(Example I) FIG. 1 shows a first example of the metal component analyzer of the present invention.

In this device, the pressure pump 6 and the first
The flow path 30a between the four-way switching valve 7 and the drainage path 34 are connected by line I7□, and this line L
1 (a check valve 23 is provided in
I! A check valve 26 is provided here. The inflow passage 9a of the second a contraction column 9 and the drainage passage 34 are connected by a line L, and a check valve 24 is provided here. Further, a line 33 and a drainage channel 34 between the separation column 11 of the analysis means 32 and the second four-way switching valve IO are connected by a line L14, and a check valve 25 is connected to this line L14.
is connected.

The check valves 23, 24, 25.26 are constituted by electromagnetic valves, and three of the check valves 23, 24, 26 are connected to the pressure switch 6A provided in the sample water supply path 30 or the eluent supply path 31. It is controlled based on the detection signal from the pressure switch +7A installed in the pressure switch +7A. That is, when these switches 6A and I7A detect the internal pressure of the flow path at 51, a detection signal is issued to the control section C, and the control section C issues a signal to open the check valves 23, 24, and 26.

A check valve 25 connected to a line 33 on the upstream side of the separation column 11 is opened by a signal from the control +13c when an abnormality in the internal pressure of the line 33 is detected by a pressure sensor (not shown) attached to this line 33. It has become so.

The artificial sides of these check valves 23, 24, 25, and 26 are made of a material that does not release metal ions.

In the metal component analyzer of this embodiment, the a-condensation columns 8, 9
or the separation column 11 is clogged, causing the flow path 30a and the inlet path 8a to become clogged.
, 9a, When the internal pressure of the flow path such as line 33 rises abnormally, the check valves 23, 24, 25, 26 are opened and the sample water in the flow path is discharged to the drain path 34, so that the flow path is The high pressure condition is quickly resolved. Therefore, in the metal component analyzer of this embodiment, the switching valves 7, . 10. Accidents such as damage to parts such as pressure switches 6A, 17A, columns 89, 11, piping, and joints, and leakage of liquid from them can be prevented.

(Example 2) FIG. 2 shows a second example of the metal component analyzer of the present invention. In the device of this second embodiment, one six-way switching valve 22 performs the function of the four-way switching valves 7 and 10 of the device of the first embodiment. Further, the check valves 23, 24, 25, and 26 of the metal component analyzer use valve opening pressures that can be set using springs.

The six-way switching valve 22 can be switched between a first state shown by a solid line in the figure and a second state shown by a broken line. The inflow path 8a to the first concentration column 8 is connected to the first connection port of this six-way switching valve 22, and from there, the inflow path 8a to the first concentration column 8 is sequentially connected clockwise from the sample water supply path 30 and the second concentration column 9. outflow path 9b, line 33 of the analysis means 32, outflow path 8b from the first a condensation column 8, line 35 connected to the drainage path 34, inflow path 9a to the second a condensation column 9, and eluent supply path 31. are connected.

In this metal component analyzer, the six-way switching valve 22 is switched between a first state and a second state by a signal from the control section C.

First, when the six-way switching valve 22 is in the first state shown by the solid line in the figure, sample water is first supplied to the fill condensation column 8 from the sample water supply path 30.

In the first concentration column 8, metal ions contained in the sample water are adsorbed. The sample water that has passed through the first a contraction column 8 flows through a line 35 and its flow rate is measured by a flowmeter 19, and then is discharged into a drainage channel 34. On the other hand, the second concentration column 9
An eluent is supplied from an eluent supply path 31 to the eluent. Second
The eluent that has passed through the a-condensation column 9 flows into the analysis means 32 .

Next, when the flow path of the six-way switching valve 22 is switched to the second state shown by the broken line in the figure, the eluent is supplied to the 16th condensation column 8, and in the first state, the eluent is adsorbed in the first concentration column 8. The metal ions are eluted, and the liquid containing the metal ions flows into the analysis means 22, where the metal ion concentration is measured. On the other hand, sample water flows into the second a condensation column 9, where metal ions in the sample water are adsorbed and concentrated.

This metal component analyzer conventionally uses two four-way switching valves 7.
10, the first and second a reduction columns 8,
Six-way switching valve 2 with one switching operation for the flow path connected to 9.
Since the number of switching valves can be reduced, the frequency of switching valve malfunction accidents can be reduced. Therefore, this metal component analyzer is less prone to failure. Also, since the space required for one switching valve can be reduced,
It is possible to downsize the device and reduce manufacturing costs.

``Effects of the Invention'' As explained above, the metal component analyzer of the present invention is capable of discharging the sample water in the flow path between the column and the pressure pump when the pressure in the flow path exceeds a predetermined pressure. Since it is equipped with a discharge valve, if the concentration column becomes clogged and the pressure in the flow path increases abnormally, the valve will open and the sample water between the column and the pressure pump will flow out to the discharge path. , the high pressure state in the flow path is quickly eliminated.

Therefore, in the metal component analyzer of the present invention, even if the column is clogged, it is possible to prevent parts such as the switching valve, pressure switch, column, piping, and joints from being damaged or leaking from them.

[Brief explanation of drawings]

FIGS. 1 and 2 respectively show the first part of the metal component analyzer of the present invention. A schematic diagram showing the configuration of the second embodiment, and FIG. 3 is a schematic diagram showing the configuration of a conventional metal component analyzer. 6. Pressure pump, 23, 24. 26. Check valve, 3o. Sample water supply path, 32. Analysis means.

Claims (1)

[Scope of Claims] A sample water supply path that pressurizes and supplies sample water containing metal ions with a pressure pump, a column that adsorbs metal ions in the sample water, and a column that adsorbs metal ions eluted from the column. In the metal component analyzer, a valve is provided between the column and the pressurizing pump to discharge the sample water in the flow path when the pressure in the flow path exceeds a predetermined pressure. A metal component analyzer characterized in that: