JPH04279863A - Flow injection analyzer - Google Patents

Abstract

PURPOSE:To analyze components in aqueous solution speedily and accurately by means of the least reagent consumption by combining plural number of multi-way valves together. CONSTITUTION:Transport liquid is sent to a detector 15 through a transport liquid sending pipe 2, a liquid sending pump 1, a flow passage selector valve 9 and a reaction pipe 14. Sample solution is injected from a solution injecting pipe 5 of a flow passage selector valve 8 so as to be filled in a pipe 11. Coloring matter containing solution to be reacted upon analyzing components in the sample solution is injected from a solution injecting pipe 4 of a flow passage selector valve 7 so as to be filled in a pipe 10. Reaction adjusting solution is injected from a solution injecting pipe 6 of the flow passage selector valve 9 so as to be filled in a pipe 12. After these solutions are all filled in the pipes 10, 11 and 12, by switching the flow passage selector valves 7, 8 and 9 in 7, 8 and 9 order, the sample solution, the coloring matter containing solution and the reaction adjusting solution are introduced into the flow passage for the transport liquid at one time, and are mixed in the reaction pipe 14 of a reaction tank 13, and are reacted upon each other, and reaction products can be detected by means of the detector 15.

Description

[Detailed description of the invention]

0001

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an analyzer for analyzing components such as manganese, chromium, and ammonium ions in an aqueous solution using a flow injection method.

0002

[Prior Art] Analysis of components such as manganese, chromium, and ammonium ions in aqueous solutions such as well water and industrial wastewater is
This is an essential step in water quality testing when using water. Conventionally, for example, analysis of Mn in an aqueous solution, especially trace quantitative analysis, has been carried out by using an aqueous solution containing Mn and a reagent that reacts with the Mn contained therein to develop a color derived from Mn, such as formaldoxime, or a reagent that oxidizes Mn. A method in which a reagent that generates color by producing permanganic acid, such as sodium bismuthate, ammonium persulfate, potassium periodate, etc., is mixed and reacted, and the resulting coloration is measured using a spectrophotometer. An aqueous solution containing Mn. and reagents that react with the Mn contained therein to erase the coloring of the dye, such as hydrogen peroxide, potassium periodate, and dyes that undergo fading, such as malachite green, methylene green, 3-(2-
In addition to contact analysis, which involves mixing and reacting with hydroxyphenylazo)pyridine-2,6-diol (HPAPD) and measuring the fading rate using a spectrophotometer, analysis methods include atomic absorption spectrometry, inductively coupled plasma luminescence, etc. A method is proposed.

0003

[Problem to be solved by the invention] However, in recent years, in fields where technology has become complex and prompt judgment and response are required, it is necessary to grasp various conditions as quickly as possible through continuous measurement and take measures for the next step. It is necessary to do so. The same applies to the analysis and understanding of the components in wastewater mentioned above. There is a need for improved analytical methods that require less solution.

0004

[Means for Solving the Problems] As a result of various studies on quantitative analysis methods for each component in an aqueous solution, the present inventors have found that the amount of reagent used can be reduced by appropriately combining a plurality of multi-way valves. The present invention was completed based on the discovery that components in an aqueous solution can be analyzed quickly and accurately with little amount of oxidation.

That is, in the present invention, a transport liquid feeding section, a sample injection channel switching section, a reaction tank section, and a detection section are connected in order through a transport liquid feeding pipe, and the sample injection channel switching section Consisting of n (n≧2) channel switching valves, a first channel switching valve is connected to the transport liquid feeding pipe, and n-1 channel switching valves are connected to the first channel switching valve. The present invention provides a flow injection analyzer in which the liquid crystals are connected in series through a pipe line, and the n-th end flow path switching valve is provided with a solution holding pipe line.

[0006]

[Operation] The present invention will be explained in detail below.

The analyzer of the present invention reacts an analytical component in a sample solution with a dye solution such as a coloring reagent that reacts with the component, and detects color development or color reduction of the reaction product to quantify and measure the analytical component. In order to do this, a plurality of flow path switching valves are connected to a flow path switching valve in the middle of the flow path through which the transport liquid flows, and the valves are connected by a flow path having a solution holding pipe. After holding the solution, the dye solution that reacts with the analytical component, the reaction adjustment solution, etc. in the pipes that connect the flow path switching valves, each solution flows into the transport liquid flow path by switching the flow path switching valves, and the reaction begins. The reaction takes place in a tank, and the reaction products can be detected with a detector.

The apparatus of the present invention will be explained in detail below with reference to the drawings.

FIG. 1 is a schematic diagram showing one embodiment of the apparatus of the present invention. A liquid sending pump 1 as a transport liquid sending section, a transport liquid sending pipe 2, and a sample injection flow path switching section 3 include pipes 11 and 1.
three flow path switching valves 7, 8, 9 connected by 2;
The end channel switching valve 7 includes a solution holding pipe 10, solution injection pipes 4, 5, 6 to each flow switching valve, and a reaction tank section 1.
3, a reaction line 14 and a detector 15.

[0010] Each configuration can be appropriately selected from those used in ordinary liquid chromatograph apparatuses.

Next, the operation of the apparatus of the present invention will be explained.

[0012] The liquid to be transported is passed through the liquid transport pipe 2 to the liquid transport pump 1.
Flow path switching valve 9, reaction pipe 14 and detector 1
The liquid is sent to 5. The sample solution is injected from the solution injection conduit 5 of the flow path switching valve 8 and filled into the conduit 11 . A dye solution that reacts with the analytical component in the sample solution is injected from the solution injection conduit 4 of the flow path switching valve 7 and filled into the conduit 10 . The reaction adjustment solution is injected from the solution injection conduit 6 of the flow path switching valve 9 and filled into the conduit 12 . After all the solutions are filled in the pipes 10, 11, and 12, the sample solution and the dye solution filled in the pipes are changed by switching the flow path switching valves 7, 8, and 9 in the order of 7 → 8 → 9. , the reaction adjustment solution is introduced into the transport liquid channel all at once. Then, each solution is mixed and reacted in the reaction pipe line 14 of the reaction tank section 13,
The reaction product is detected by detector 15.

[0013] The injection lines for the sample solution, dye solution, and reaction adjustment solution can be appropriately selected from those described above depending on the components to be analyzed, the type of reaction, and the like.

[0014] These operating procedures can also be controlled according to a program.

The analysis apparatus shown in FIG. 1 enables the following analysis, for example. When using the reaction between ammonium ions and Nessler's reagent, water is used as the transport liquid, Nessler's reagent is used as the dye solution, and 0.0% is used as the reaction adjustment solution.
Ammonium ions can be determined using 5M NaOH, and Zn-[4-(2-pyridylazo)
When indirectly quantifying calcium ions by measuring the color of the resorcinol (PAR) complex, water is used as the transport liquid and Zn-ETGA tetraacetic acid complex + PA is used as the dye solution.
R, borate buffer solution (pH 7.
5) respectively, Cr(III) is Ce(IV)
is oxidized to Cr(VI) by
- In the measurement of chromium using the reaction with diphenylcarbazide (DPC), which shows coloration, 0.0.
8MHNO3, 0.05W/V% DPC as dye solution
, 0.025W/V%Ce(SO
4) Using 2-0.07M H2SO4, total chromium, chromium (III) and chromium (VI) depending on whether or not the reaction adjustment solution is introduced into the flow path of the transport liquid.
It is possible to separate and quantify the

FIG. 2 is a schematic diagram showing an embodiment of the apparatus of the present invention in which two flow path switching valves 7 and 8 are used. This analyzer can measure chemical oxygen demand (COD) using water as a transport liquid and K2Cr2O7-H2SO4 as a dye solution.

[0017]

[Examples] The present invention will be explained below with reference to Examples, but the present invention is not limited thereto.

EXAMPLE A method for quantitatively analyzing Mn in waste liquid using the analyzer shown in FIG. 1 will be explained. All liquid transport pipes 2 have an inner diameter of 0.5 m.
Using a Teflon tube of 20 m, the length of the reaction pipe 14 is 20 m.
0 cm, and pipes 10, 11, and 12 were each equipped with a solution volume adjusted to be 30 μl. The flow rate of liquid pump 1 is 1.50 ml/min, reaction tank 1
The temperature in step 3 was 50° C., and an ultraviolet-visible detector was used as the detector 15, and its wavelength was set to 472 nm.

[0019] The transport liquid is a 40 vol% ethanol aqueous solution,
The dye solution was a mixture of an ethanol solution of HPAPD and a buffer solution (NH4Cl + NH4OH + NaCl) adjusted to pH 9.3, [HPAPD] = 0.35 mM, [NH3] = 0.9.
3M, [NaCl]=0.32M, and a 0.08M hydrogen peroxide solution was used as the reaction reagent solution.

[0020] When the temperature, flow rate, and detector signal are all stabilized, the dye solution is introduced from conduit 4, the sample solution is introduced from conduit 5,
The reaction reagent solution is transferred from pipe 6 to pipes 10, 11, and 1, respectively.
2, and by switching the flow path switching valves 7, 8, and 9 in the order of 7→8→9, the solutions in the pipes 4, 5, and 6 were introduced into the transport liquid flow path at once. After switching the flow path switching valve 9, the mixed liquid reaches the detector 15 in about 60 seconds. Read the absorption profile peak height at 472 nm at that point, and from the difference from the blank test value, create a M
The amount of Mn was determined using an n calibration curve.

The quantitative concentration range of Mn under these measurement conditions was 0.1 to 3 μg/ml, and the relative standard deviation rate of the measurement was 3%. Additionally, approximately 50 samples could be measured per hour.

[0022]

[Effects of the invention] The present invention provides simple operation, short time, high precision,
This is an analytical device that can perform quantitative analysis of each component in an aqueous solution quickly and with a small amount of reagents.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing an analysis device using three flow path switching valves as an embodiment of the device of the present invention.

FIG. 2 is a diagram showing an analyzer using two flow path switching valves as an embodiment of the present invention.

[Explanation of symbols]

Claims (1)

[Claims] [Claim 1] A transport liquid feeding section, a sample injection channel switching section,
The reaction tank section and the detection section are sequentially connected by a transport liquid feeding pipe, and the sample injection flow path switching section is composed of n pieces (n≧2) of flow switching valves, and the transport liquid feeding pipe A first channel switching valve is connected to the first channel switching valve, n-1 channel switching valves are connected in series to the first channel switching valve, and a solution holding pipe is connected to the n-th end channel switching valve. A flow injection analysis device characterized by being provided with a channel.