JPS593336A - Reaction measuring device - Google Patents

Abstract

PURPOSE:To carry out reaction at the b.p. of a carrier liquid or high temp., by connecting a flow resisting tube with a reaction tube, maintaining the reaction tube in a pressurized state, introducing a sample into the carrier liquid to react it, and detecting a reaction state with a detector. CONSTITUTION:A carrier liquid 2 is contained in a carrier liquid tank 1 together with a reaction reagent. An oven 6 is first set to a temp. higher than the b.p. of the carrier liquid 2, and a thermostat 8 is set to a temp. lower than that. A pump 5 is actuated to feed the liquid 2 in a reaction tube 7, and the sample is introduced into the liquid 2 from a sample introduction part 3. The sample is reacted with the reaction reagent in the tube 7 and develops color. An extent of the color developed is detected with a detector 10, concn. of an objective component is obtained by calculation and recorded in a recorder 11. Although the inside of the reaction tube 7 is set to the b.p. of the carrier liquid or higher, but it is not evaporated because it is maintained in a pressurized state.

Description

Detailed Description of the Invention The present invention is a flow injection analysis method in which a sample is introduced into a carrier liquid, a reaction is carried out while the carrier liquid moves and reaches a detection part, and the reaction state is detected in the detection part.
This invention relates to a reaction measuring device using the FIA method.

In the flow injection analysis method, a sample is introduced into a carrier liquid flowing in a reaction conduit, and the sample is reacted while the carrier liquid moves and reaches a detection section, and the state of this reaction is detected at the detection section. , for example, "Unexamined Japanese Patent Publication No. 53-1-06
No. 090 Publication" and the like. Although this FIA method has the advantage of easily and quickly analyzing small amounts of samples, it requires that the temperature of the reaction tube be kept relatively low, and the temperature of the reaction tube must be kept above the boiling point of the carrier liquid. Then, the carrier liquid vaporizes and becomes inoperable, resulting in a problem that the range of application is limited.

The present invention has been made in view of the above circumstances, and is achieved by interposing a flow path resistor between the reaction conduit and the detection section and keeping the temperature of the flow path resistor below the boiling point of the carrier liquid. It is an object of the present invention to provide an FIA device capable of raising the temperature of a reaction conduit to above the boiling point of a carrier liquid.

Hereinafter, one embodiment of the present invention will be described with reference to the drawings.

In the figure, 1 is a carrier liquid tank containing a carrier liquid 2. The carrier liquid 2 can be an organic solvent such as methanol, ethanol, THF, acetone, benzene, toluene, or chloroform, water, or a combination of these with an acid or a base. A mixed liquid or the like can be used, and a reaction reagent that reacts with the sample introduced from the sample introduction section 3, which will be described later, is mixed therein. One end of the suction i4 and f4 is immersed in the carrier liquid 2, and the other end is connected to the suction section of the feed pump 5. The pump 5 is capable of pumping the carrier liquid 2 at a desired flow rate, and for example, a constant flow pump for high performance liquid chromatography can be used. Said pump 5
The inflow section of the sample introduction section 3 is connected to the discharge side of the sample introduction section 3 . This introduction section 3 is a sample introduction section of a known high performance liquid chromatograph, such as one using a multi-way stopcock or one that injects through a sezotam such as silicon im.
t can be used. At the outflow part of the introduction part 3, there is a reaction conduit 7 housed in an oven 6 equipped with a Glodalam device that automatically changes the temperature to an arbitrary temperature or according to the passage of time.
One end of is connected. The reaction conduit 7 is a capillary tube made of stainless steel, glass, quartz, etc., and its dimensions are appropriately determined depending on the purpose of use, but generally the inner diameter is 0.1 to About 15m,
The length is preferably about 30α to 50 m.

The other end of the reaction conduit 7 is connected to a flow path resistance inflow section housed in a constant temperature bath 8 that can be set at a desired temperature. This flow path resistor 9 is a capillary tube.

Although it can be formed by a noclebe, an orifice, etc., it is particularly preferably formed by a capillary tube with a smaller diameter than the reaction conduit 7.
In this case, the capillary has an inner diameter of about 0.02 to 0.1-
A length of about 10crIt to Ion is preferably used. The outflow section of the reaction conduit 7 is connected to a detection section 10, and the detection section 10 measures the concentration of various components in the reaction mixture sent from the outflow section of the flow path resistor 9. It is recorded on the recorder 11. The detection unit 10 is an ultraviolet monitor or differential refractometer used in a high-performance liquid chromatograph.

Fluorescence spectrometers, etc. are used selectively depending on the component to be measured.
A high-performance liquid chromatograph may be used as a detection unit, and the reaction mixture from the flow path resistor 9 may be introduced into the high-performance liquid chromatograph, thereby separating and quantifying each component in the reaction mixture.

Next, to explain the quantitative analysis of the target component in a sample using the above-mentioned apparatus 1, first, the oven 6 is set to an appropriate temperature higher than the boiling point of the carrier liquid 2, and the constant temperature oven 8 is set. Set the temperature to be lower than the boiling point of the carrier liquid (for example, near room temperature). Next, the pump is operated to supply the carrier liquid to the reaction conduit 7, and this carrier liquid contains in advance a predetermined concentration of a reaction reagent that reacts with the target component in the sample to develop a color.

When a predetermined amount of sample is introduced into the carrier liquid from the sample introduction section 3 in this state, the sample flows into the reaction conduit 7 together with the carrier liquid, where it is heated above the boiling point of the solvent, and the target component in the sample is combined with the sample. The reaction reagent in the carrier liquid starts to react and color development begins, but since the inside of the reaction conduit 7 is pressurized by the flow path resistor 9, the carrier liquid can be vaporized and is kept in a liquid state. ing. The reaction mixture, which develops color by passing through the reaction conduit 7 at a temperature higher than the boiling point of the carrier liquid, then passes through the flow path resistor 9 at the temperature of the constant temperature bath 8 (the boiling point of the carrier liquid After that, it flows into the detection section, and the degree of color development is detected. From this, the concentration of the target component in the sample is calculated and recorded on the recorder 11.

According to this device, a flow path resistor 9 is provided on the downstream side of the reaction conduit 7.
Since the inside of the reaction conduit 7 is pressurized by connecting the two, even if the temperature inside the reaction conduit 7 (oven temperature) is raised above the boiling point of the solvent, the solvent remains in a liquid state that can be vaporized. The reaction can be easily carried out at a temperature higher than the boiling point of the solvent without using it, and the reaction can be carried out and detected over a wide temperature range. Then, the reaction mixture that has passed through the reaction conduit 7 is cooled in the flow path resistor 9 to the temperature in the constant temperature bath 6 (approximately room temperature in this embodiment), so that it is heated above the boiling point in the reaction conduit 7. When the solvent is removed from the flow path resistor 9
After leaving the room, it will not evaporate even if the pressure is returned to normal.

FIG. 2 shows another embodiment of the present invention, in which two feed pumps 5a and 5b are used to feed carrier liquids 2m and 2b, which are combined upstream of the reaction conduit 7. In this case, the carrier liquids 2a and 2b do not contain any reaction reagent. Then, the reaction reagent is introduced from the reaction reagent introduction section 3b in synchronization with the time when the sample is introduced into the carrier liquid from the sample introduction section 3&, so that the sample and the reaction reagent meet upstream of the reaction conduit 7. How is it?
The other configurations are the same as those of the above embodiment, so the same parts are given the same reference numerals and the explanation thereof will be omitted.

This embodiment has the advantage that the amount of reaction reagent consumed is small because the reaction reagent is introduced only when the sample is introduced.

In the above embodiments, a coloring reagent is used as a reaction reagent, but the present invention is not limited to this, and the detection section is not limited to an absorptiometer or the like that measures the degree of coloration, but a detector based on various detection principles may be used. Furthermore, this device is not only used as an analyzer, but can also be used to analyze the reaction by changing the temperature of the reaction conduit and the flow rate of the carrier liquid, changing the reaction conditions, and examining the detection signal at this time. When used as a measurement device for reaction conditions to easily determine the effects of temperature and time on the reaction, or when filling a reaction pipe with a catalyst, etc., the performance of the catalyst can be easily determined.

Thus, the present invention provides a reaction conduit, a means for continuously feeding a carrier liquid into the reaction conduit from one end of the reaction conduit, and a sample introduction section for introducing a sample into the carrier liquid at one end of the reaction conduit. , a flow path resistor connected to the other end of the reaction conduit to keep the inside of the reaction conduit in a pressurized state, a detection section connected to an outflow portion of the flow path resistor, and a flow path resistor connected to the reaction conduit and the flow path resistor, respectively. By introducing the sample into the carrier liquid in the reaction conduit from the sample introduction part, the sample is reacted in the reaction conduit and sent to the detection part, and the detection part detects the reaction state. Since this method detects , the reaction can be carried out even in a temperature range above the boiling point of the carrier liquid, which has the advantage that the range of application of the FIA method is greatly expanded.

[Brief explanation of the drawing]

1 and 2 are block diagrams showing one embodiment of the present invention, respectively, and 0 2 , 2 m , 2 b-=carrier liquid, 3 *
3 m''・Sample introduction part, 5...Feeding pump, 6...
・Oven, 7...Reaction conduit, 8...Thermostat, 9.
...Flow path resistor, 10...Detection unit, 11...Recorder.

Claims (1)

[Scope of Claims] 1. A reaction conduit, means for continuously feeding a carrier liquid into the reaction conduit from one end of the reaction conduit, and a sample introduction section for introducing a sample into the carrier liquid at one end of the reaction conduit. , a flow path resistor connected to the other end of the reaction conduit to keep the inside of the reaction conduit in a pressurized state, a detection section connected to an outflow portion of the flow path resistor, and a flow path resistor connected to the reaction conduit and the flow path resistor, respectively. By introducing the sample into the carrier liquid in the reaction conduit from the sample introduction section, the sample is sent to the detection section while being reacted in the reaction conduit, and the reaction state is detected at the detection section. A reaction measuring device configured to detect. 2. An apparatus according to claim 1 for instantaneously introducing a relatively small amount of sample into a carrier liquid. 3. The apparatus according to claim 1 or 2, wherein the temperature of the reaction conduit is set above the boiling point of the carrier liquid, and the temperature of the flow path resistor is set below the boiling point of the carrier liquid. 4. It has a plurality of carrier flow channels that meet upstream of the reaction conduit, and a sample introduction part is provided in the -〇 flow path and a reaction reagent injection part is interposed in the remaining flow path, and the sample and the reaction reagent are inserted into the reaction conduit. 4. A device according to any one of claims 1 to 3, characterized in that the mixing is carried out in a carrier liquid upstream of the device. 5. The device according to any one of claims 1 to 4, wherein the flow path resistor is formed of a capillary tube having a smaller diameter than the reaction conduit.