JPH01242942A - Method and apparatus for analysis - Google Patents

Abstract

PURPOSE:To enable the automatic and continuous execution of all operations including collecting of a sample soln., reaction thereof with a reagent, absorbing and thickening of the resultant reaction product to granular materials and measuring of absorbancy by adsorbing and thickening of the chromatic resultant reaction product to the granular material in a measuring cell. CONSTITUTION:The granular materials are captured by a filter 42 provided in the outlet of a cell 41 and are packed into the cell 41 body when the liquid suspended with the granular materials is fed in a specified volume by a pump 23 to the measuring cell 41 side. On the other hand, the chrometic chemical species are formed by mixing the sample soln. and the reaction reagent to bring the same into reaction in a capillary communicated via a selector valve 32 to the cell 41. The measuring cell 41 packed with the granular materials for adsorbing and thickening the chromatic chemical species and the capillary are communicated to thicken the chromatic chemical species in the cell 41. The pump 21 is thereafter stopped and the absorbancy at the cell 41 is measured by an absorptiotometer 53. All of the operations including the collecting of the sample soln., the reaction thereof with the reagent, the absorbing and thickening of the resultant reaction product with the granular materials and measuring of the absorbancy are thereby automatically and continuously executed.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method and apparatus for analyzing trace components contained in a liquid sample.

[Prior Art] In various research and industrial fields, it is desired to increase the sensitivity of ultratrace component analysis in samples. If the sensitivity of the analyzer is not sufficient for the concentration of the component to be analyzed in the sample, the sensitivity can be improved by concentrating the component. One of the concentration methods is a method of adsorbing the component to a particulate material such as an ion exchange resin and concentrating it. Either the component is adsorbed and concentrated on the granular material and colored, or the component is colored and the colored component is adsorbed and concentrated on the granular material, and then the granular material layer is separated from the solution layer. A method for quantifying the component by directly measuring the absorbance of the component has been reported (Talan
ta), 32.5, 345.1985).

2 to 5 illustrate the conventional method.

As shown in FIG. 2, a predetermined liquid sample is placed in a reaction container 81, a predetermined reaction reagent and particulate material 82 are added thereto, and the mixture is reacted while being stirred by a stirrer 83 and a magnetic stirring device 84. It is adsorbed and concentrated by After a certain period of time, the reaction vessel 81 is left still to allow the particulate matter to settle and separate. Next, as shown in FIG. 3, the particulate matter and a small amount of the reaction solution are collected with a dropper 96 and filled into the sample space 95 of the cell body 91 for spectrophotometric analysis. Note that FIGS. 4 and 5 show the above cell body 91 for spectrophotometric analysis and the particulate matter 82 filled therein. In the figure, 92
93 is a spacer, and 94 is a pore. The absorbance of the particulate material is measured by loading the cell into a spectrophotometer.

By carrying out the procedure described above, it is possible to quantify the component to be analyzed that has been adsorbed and concentrated on the particulate material.

[Problems to be Solved by the Invention] However, in the conventional batch method analysis shown in Figures 2 to 5, the cell unit must be attached and detached from the spectrophotometer for each sample and the sample replaced, making the operation complicated. It is difficult to speed up the analysis, and filling the cell with particulate matter requires some skill.

The purpose of the present invention is to solve the drawbacks of the conventional technology and to provide an analysis system that can automatically and continuously perform all of the steps of sample solution collection, reaction with reagents, adsorption and concentration on particulate matter, and absorbance measurement. The goal is to provide equipment.

[Means for Solving the Problem] The present invention mixes a sample solution flowing continuously in a pipe at a predetermined flow rate and a reaction reagent from another pipe in a thin tube.
By reacting to form a colored reaction product of the analytical component, and then adsorbing and concentrating this colored reaction product on a particulate material in a measurement cell communicating with the capillary, and then measuring the absorbance of the particulate material. An analysis method characterized by qualitatively or quantitatively determining the analytical components, and a reaction comprising sample solution piping and reaction reagent piping provided with pumps, and thin tubes for mixing and reacting substances from each of the pipings. a particulate material filling system comprising a measuring cell with a filter on the outlet side and a pump for supplying a suspension of particulate material to the cell; and connecting the reaction line and the particulate material filling system to the measuring cell. This analysis device is characterized by comprising: a switching valve that communicates and disconnects; an absorption photometer; and a control system that controls the operation of each of the pumps and switching valves and processes measured values.

[Operation] When a certain volume of a liquid in which particulate matter is suspended is sent to the cell side by a pump, the particulate matter is captured by a filter provided at the outlet of the measurement cell and filled into the cell body.

On the other hand, the sample solution and the reaction reagent are mixed and reacted in a thin tube connected to the measurement cell via a switching valve to generate colored chemical species. The capillary tube is then communicated with the measurement cell filled with particulate matter that adsorbs and concentrates the colored chemical species, and the colored chemical species are concentrated within the measurement cell. enrichment bonds,
Measure the absorbance of particulate matter.

[Example] Hereinafter, an example of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a schematic diagram of an embodiment of the present invention.

In the figure, 1 is a sample solution tank, 2 is a reaction reagent tank, 3 is a suspension tank for particulate matter, 4 is a PU regulator tank, and 5 is a cleaning liquid tank.

When the device starts operating, the switching valves 31 to 34 are in the solid line state.

Collecting a sample solution from the sample solution tank 1 with a pump 21,
The reaction line from pump 21 to valve 32 is cleaned. Meanwhile, for a predetermined period of time, the particulate matter suspension is pumped from the particulate matter suspension tank 3 to the valve 34.32.31 by the pump 23.
The liquid is sent to the measurement cell 41 through the .

Particulate matter is filtered through a filter 42 provided on the outlet side of the measurement cell 41.
, and fills the optical path section 43 of the measurement cell 41. After that, switch the switching valve 34 to the broken line state,
The pH adjuster is sent from the pH adjuster tank 4 by the pump 24, and the suspension of particulate matter remaining in the piping from the valve 34 to the inlet of the measurement cell is sent to the measurement cell, and the pH of the particulate matter is analyzed. Adjust the pH so that the target component is adsorbed.

After a predetermined period of time, a reaction reagent that selectively reacts with the analytical component and develops color is fed from the reaction reagent tank 2 by the pump 22, and mixed with the sample solution fed by the pump 21 in the reaction coil 52 as a thin tube. , a heating reaction is carried out in the reaction oven 51.
Performs color development. The switching valve 32 is switched to the broken line state, and the colored solution is introduced into the measurement cell 41. The colored analytical component is adsorbed and concentrated by the particulate material filled in the optical path portion 43 of the measurement cell 41.

After a predetermined time, the pump 22 is stopped, and the colored liquid remaining in the reaction line is sent into the measurement cell 41 by the sample solution sent by the pump 21. Thereafter, the pump 21 is stopped, and the absorbance of the particulate matter in the measurement cell 1 at a certain wavelength is measured by the spectrophotometer 53. By measuring a sample solution containing a known concentration of an analytical component under the same conditions in advance, quantification is performed based on a prepared calibration curve, and the concentration is output.

When the absorbance measurement is completed, the switching valves 31 and 33 are switched to the broken line state. The cleaning liquid is sent from the cleaning liquid tank 5 by the pump 25, and the switching valve 33 and the filter 4
2 from the outlet side of the measuring cell 41, and the particulate matter filled in the measuring cell 41 is discharged into the drain tank 11 through the switching valve 31 on the inlet side of the measuring cell 41. When the discharge is completed, the pump 25 is stopped and each switching valve returns to the solid line state.

Note that the operation of the pump and switching of the valves are controlled by a control system (not shown).

[Effects of the Invention] As detailed above, according to the analysis method and analyzer of the present invention, the analytical components in a liquid sample can be analyzed automatically and semi-continuously, so that they can be used in various research and industrial fields. It is possible to improve the efficiency, speed, and reliability of quality control of liquids such as purified water and chemical solutions and monitoring of wastewater.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram of an embodiment of the present invention, and FIGS. 2 to 5 are diagrams of a conventional analysis method. 1...Sample solution tank 2...Reaction reagent tank
.

Claims (2)

[Claims] (1) A sample solution that flows continuously in a pipe at a predetermined flow rate and a reaction reagent from another pipe are mixed and reacted in a thin tube to form a colored reaction product of an analytical component, and then this colored reaction product is mixed and reacted with a reaction reagent from another pipe. An analysis method characterized in that the reaction product is adsorbed and concentrated on particulate matter in a measurement cell communicating with the capillary, and then the analytical component is qualitatively or quantitatively determined by measuring the absorbance of the particulate matter. (2) A reaction line equipped with sample solution piping and reaction reagent piping equipped with pumps, thin tubes for mixing and reacting substances from each piping, and a measurement cell equipped with a filter on the outlet side; a particulate matter filling system comprising a pump for supplying a suspension of particulate matter to the cell; a switching valve that connects and disconnects the reaction line and the particulate matter filling system to the measuring cell; an absorptiometer; and each of the above. An analytical device comprising a control system that controls the operations of a pump and a switching valve and processes measured values.