JPH0375558A - Metal component analyzer - Google Patents

Abstract

PURPOSE:To make it possible to prevent the discharge of organic material to the outside of a system by providing purifying parts for purifying waste liquid discharged from an adjusting part and columns and waste liquid after analysis. CONSTITUTION:The insides of the columns of purifying parts 50a and 50b are filled with ion exchanged resin. The parts are inserted in water draining paths 34 and 39, respectively, so that the parts can be freely attached and removed. Sample water and reaction liquid (generally acidic) are flowed into the water draining path 34 from an overflow container 4 and a three-way switching valve 5. Eluate (generally acidic) which has passed through columns 8 and 9 from a four-way switching valve 10 flows through a line 35. Cation exchanged resin is used for the purifying part 50a. Sample water into which a coloring agent (generally basic) flows into the water draining path 50b. Therefore, an anion exchanged resin is used for the purifying part 50b. Therefore, the ions in the outflowing liquid from the container and the waste liquid after analysis are exchanged in the purifying parts 50a and 50b, respectively. The neutral liquid flows through water draining paths 34a and 39a and thereafter discharged to the outside. The waste liquid can be utilized as cooling water and purifying water.

Description

Detailed Description of the Invention "Field of Industrial Application" This invention relates to a metal component analyzer that uses an ion exchange separation method to efficiently analyze minute amounts of metal components in ultrapure water. It is related to.

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

Reference numeral l in FIG. 3 is an automatic flow path switching valve, and 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 is provided with a liquid feeding pump 2, a reactor 3, an overflow container 4, a three-way automatic switching valve 5, a pressure pump 6, and a pressure switch 6A in this order from the automatic flow path switching valve l side. Furthermore, a first four-way switching valve 7 is connected to the terminal end side of this sample water supply path 30. The first four-way switching valve 7 is connected to an inflow path 8a to the first a-condensation column 8, an inflow path 9a to the second concentration column 9, and an eluent supply path 31, respectively. The elution liquid supply path 31 is provided with a pressure pump 17 and an elution iR storage section 18 .

Further, a second four-way switching valve 10 is connected to the outflow path 8b from the first concentration column 8 and the outflow path 9b from the second concentration column 9, respectively. A line 33 connected to an analysis means 32 consisting of a separation column 11 and an absorption photometer 12, and a line 35 connected to a drainage channel 34 are connected to the second four-way switching valve lO. 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 to
IF is connected. These sample water flow paths I
One of A to IF is changed by switching the automatic flow path switching valve l.
It is selectively connected to the sample water supply channel 30.

The sample water that has flowed into the sample water supply path 3G from the sample water flow paths IA to IF is sent to the adjustment section 40 consisting of the reactor 3 and the overflow container 4 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 supply path 37 is connected to the reaction liquid storage section 15 and a reaction liquid supply path 37 for ionizing metal components in the sample water. liquid is added to the sample water. The sample water to which the reaction solution has been added is mixed in the reactor 3 at a predetermined temperature. The sample water that has passed through the reactor 3 is temporarily stored in an overflow container 4, and the sample water that exceeds a certain storage amount is discharged to a drainage channel 34 through a line indicated by symbols.

The sample water that has passed through the overflow container 4 is transferred to the three-way switching valve 5.
reach. By switching the three-way automatic switching valve 5, a part of the sample water flowing through the sample water supply path 3o is guided to the drainage path 34 through a line indicated by the symbol L3. That is, when the automatic flow path switching valve 1 is switched and another sample water is supplied, the flow path of the three-way switching valve 5 is first switched to the line L side, and the automatic flow switching valve 1 and the three-way switching valve 5 are switched to the line L side. The sample water remaining between the valve 5 and the valve 5 is completely washed away.

Thereafter, the flow path of the three-way switching valve 5 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 pressurizing pump 6, the pressure kasuinochiro A becomes O
N, and a detection signal for stopping the operation of the pressurizing pump 6 is output to the control unit C.

The sample water pressurized by the pressure pump 6 is transferred to the first four-way switching valve 7.
is supplied to the first concentrating column 8 or the first concentrating column 8.

These first four-way switching valve 7 and second four-way switching valve 10 allow the sample water supplied from the sample water supply path 3o to pass through the concentration column 8 or 9, and then pass through the line 35 to the drainage path 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. These four-way switching valves 7 and 10 are switched by measuring the flow rate of the sample liquid passing through the line 35 with the flowmeter 19, and when the measured value reaches a set value, a signal is sent from the control unit C. This is done by sending a message.

When the sample liquid passes through the concentration column 8 or 9, metal ions in the sample liquid are adsorbed within the column 8 or 9.

The metal ions adsorbed in the column 8 or 9 are eluted from the column 8 or 9 by the eluent supplied from the eluent supply path 31 and transported to the analysis means 32.

The metal ions carried to the analysis means 32 are separated by the separation column ti
After being purified, it is colored with a coloring liquid from a coloring liquid supply path 38 that includes a coloring liquid storage section 20 and a supply pump 21, and its concentration is measured with an absorptiometer 12. After the measurement is completed, the measured liquid passes through a drainage channel 39 connected to the spectrophotometer 12, joins with the drainage fluid passing through the drainage channel 34, and is discharged out of the system.

``Problems to be Solved by the Invention'' By the way, in the metal component analyzer mentioned above, the sample water is mixed with a reaction solution consisting of acids such as oxalic acid, acetic acid, hydrochloric acid, various bases, etc., pyridinedicarboxylic acid-lithium hydroxide, etc. An eluent such as Eluent and a coloring agent such as pyridyl azo resorcinol (PAR) are added as appropriate. Therefore, if these reaction solutions, eluents, and color formers are directly discharged from the system together with the sample water after measurement, there is a risk of having an adverse effect on the environment. In other words, when organic acids such as oxalic acid and acetic acid, or organic substances such as PAR are discharged, the organic acids may corrode and deteriorate some metals, or the organic substances may change into high-molecular organic substances that stick to piping and various equipment. This creates a fear that this will happen.

``Means for Solving the Problems'' Therefore, in the metal component analyzer of the present invention, a purification section is provided to purify the effluent discharged from the adjustment section, the effluent discharged from the column, and the effluent after analysis. The above problem was solved.

"Operation" In the metal component analyzer of the present invention, by purifying the waste liquid in the purification section, harmful substances in the waste liquid are removed and the purified liquid is discharged out of the system.

"Example" Hereinafter, the metal component analyzer of the present invention will be described in detail with reference to FIGS. 1 and 2. In these figures, the same components as those shown in FIG. 3 are denoted by the same reference numerals, and their explanations will be omitted.

FIG. 1 shows a first embodiment of the metal component analyzer of the present invention. This analyzer differs from the analyzer shown in FIG. 3 in that drainage channels 34 and 39 are provided with purification sections.

In FIG. 1, purifying sections 50a and 50b are provided in the drain channel 34 and the drain channel 39, respectively.

The purification section 50a and the purification section 50b both have columns filled with ion exchange resin, and are configured to be removably inserted into the drain channel 34 or the drain channel 39, respectively. A cation exchange resin is used as the ion exchange resin in the purification section 50a, while an ion exchange resin is used in the purification section 50b. That is, the drainage channel 34 includes an overflow container 4 and a three-way switching valve 5.
The sample water and the reaction solution flow in from the second four-way switching valve 10, and the eluent that has passed through the columns 8 and 9 flows in through the line 35, but these reaction solutions and eluent are generally acidic solutions. is used, therefore, a cation exchange resin is used for the purification section 50a provided in the drainage channel 34. Similarly, sample water to which a coloring agent has been added flows into the drainage channel 39, but since a basic coloring agent is usually used as the coloring agent, a purification section 50 provided in the drainage channel 39
An anion exchange resin is used for b.

An analyzer having such a configuration is operated in the same manner as the apparatus shown in FIG. And in this case, drain 3
By providing the purification sections 50a and 50b in 4.39, the effluent from the overflow container 4 and the waste liquid after analysis are ion-exchanged in the purification sections 50a and 50b, respectively, and become a neutral liquid, which is then drained into the drainage channel 34a. , 39a, then merge and are discharged from the system. And the purification section 50a,
The ion exchange resin in 50b is exchanged after being used for an appropriate period of time, and the used ion exchange resin is disposed of by incineration or the like.

This analyzer does not directly discharge acidic liquid or basic acid outside the system, so there is no problem of contaminating the environment.Furthermore, since the effluent is neutral, it can be used as a cooling water. It can be used for secondary purposes such as washing water.

In addition, in the above embodiment, two systems of drainage channels 34°39
Although purification sections with different properties were installed in each of the drainage channels 34 and 34,
．． A purification section having a mixed bed type ion exchange resin layer capable of ion-exchanging both acids and bases may be provided after the merging position 39.

FIG. 2 shows a second embodiment of the metal component analyzer of the present invention. Here, the analyzer shown in Figure 2 is as follows:
In particular, organic compounds such as organic acids are used as reagents. This analyzer differs from the analyzer shown in FIG. 3 in that a second reaction section is provided between the reactor 3 and the overflow container 4, and that a second reaction section is provided between the reactor 3 and the overflow container 4, and the The point is that a purification section is provided in the drainage channel 41.

In the analyzer shown in FIG. 2, a second reaction section 22 is provided between the reactor 3 and the overflow container 4. The second reaction section 22 includes a decomposition liquid supply section 24 that sends the decomposition liquid to the sample water supply path 30 via the decomposition liquid supply path 23, and a second reactor 25 arranged downstream of the decomposition liquid supply path 23. It consists of The decomposition liquid supplied from the decomposition liquid supply section 24 is for decomposing intermediate products of metal components that have flowed out of the reactor 3. That is, when oxalic acid is used as the reaction liquid supplied to the reactor 3, the oxalic acid reacts with the metal component in the sample water in the reactor 3 to produce an intermediate, and this intermediate product is then fed into the reactor. It flows out from 3. Then, this intermediate product flows into the second reactor 25, reacts with the decomposition liquid supplied from the decomposition liquid supply section 24, and is decomposed, thereby ionizing the metal component.

By providing such a second reaction section 22, this analyzer has an adjustment section 4 for reaction-conditioning sample water from the reactor 3, second reactor 25, and overflow container 4.
0.

Further, in this analyzer, a purification section 51 is provided in the drain channel 41 after the drain channel 34 and the drain channel 39 join together. This purification section 51 includes a pump 52 that pumps the drained liquid flowing through the drainage channel 41, and a reactor 53 that decomposes the drained liquid.
and a reaction liquid supply section 54 for supplying a reaction liquid (organic substance decomposition liquid) to this reactor 53, which decomposes organic substances in the waste liquid added as the reaction liquid or eluent. It is for. The reaction liquid supply section 54 supplies a reaction liquid containing, for example, sulfuric acid or potassium peroxodisulfate to the reactor 53 from a reaction liquid supply path 55.

Then, in the reactor 53, the waste liquid and the reaction liquid are combined and reacted under conditions of, for example, 200° C. and 20 atm, thereby decomposing the organic matter.

An analyzer having such a configuration is operated in the same manner as the apparatus shown in FIG. And in this case, drain 4
By providing the purification section 50 in I, as described above, the organic matter contained in the effluent from the overflow container 4, the waste liquid after analysis, etc. is decomposed in the purification section 51, and becomes a liquid containing no organic matter. Exhausted from the system.

Since this analyzer does not directly discharge organic matter to the outside of the system, it is possible to prevent the generation of bad odors caused by organic matter, and furthermore it is possible to prevent environmental pollution due to the discharge of organic matter.

In the embodiments shown in FIGS. 1 and 2, purification sections were provided for the purpose of neutralization and for the decomposition of organic matter, but in the analyzer of the present invention, purification sections may be provided as necessary. Both of these may be provided in the drainage channel.

"Effects of the Invention" As explained above, the metal component analyzer of the present invention is equipped with a purification section that purifies the effluent discharged from the adjustment section, the effluent discharged from the column, and the effluent after analysis. Therefore, by removing harmful substances from the waste liquid in the purification section, it is possible to prevent harmful substances from being discharged outside the thread. It is possible to prevent adverse effects on equipment and even the work environment. Furthermore, since the waste liquid does not contain harmful parts, it becomes possible to use the waste liquid for secondary purposes.

[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. 40... Adjustment section, 50a, 50b, 51... Purification section.

Claims (1)

[Claims] A sample water supply path that pressurizes and supplies sample water containing metal components with a pressure pump, an adjustment section that is provided in this sample water supply path and adjusts the sample water by reaction, and a metal ion in the sample water. In a metal component analyzer equipped with an adsorbing column and an analysis means for analyzing metal ions eluted from this column, a waste liquid discharged from the adjustment section, a waste liquid discharged from the column, and a waste liquid after analysis are used. A metal component analyzer characterized by having a purification section for purifying liquid.