Derivatization device and derivatization method for on-line production of derivatization reagent

Abstract

The invention discloses a derivatization device and a derivatization method for on-line production of a derivatization reagent, the device comprises a chemical column suppressor, a reaction reagent, a six-way valve, a derivatization reactor, a pump system and a flow path system, and the chemical column suppressor, the reaction reagent, the six-way valve and the derivatization reactor are connected through the flow path system; the six-way valve is provided with a regeneration flow path, a cleaning flow path and a generation flow path, and the three suppression columns of the chemical column suppressor are respectively connected with the regeneration flow path, the cleaning flow path and the generation flow path in turn; the three suppression columns of the chemical column suppressor respectively and sequentially displace hydrogen ions in the regeneration flow path, clean in the cleaning flow path and react in the generation flow path to generate hydriodic acid. By adopting the chemical column suppressor with the three suppression columns, derivative reagents can be continuously generated, and the generation efficiency of the derivative reagents is improved.

Description

Technical Field

[0001] The invention relates to an analytical instrument technology, in particular to a derivatization device and a derivatization method for producing a derivatization reagent online. Background Art

[0002] Potassium bromate was once widely used as a flour strengthening agent in the flour processing industry. It is a special additive powder added to bread. It has been confirmed to be a carcinogen. The National Health Commission has cancelled the use of potassium bromate as a flour treatment agent in wheat flour. However, there are still unscrupulous merchants who illegally add it to flour or flour products. The post-column derivatization ion chromatography method for the determination of bromate has a lower detection limit and is more suitable for the detection of bromate in flour products. Therefore, it is necessary to develop an online derivatization instrument to determine bromate in flour. Summary of the invention

[0003] In order to solve the above-mentioned deficiencies in the prior art, the object of the present invention is to provide a derivatization device and a derivatization method for online production of derivatization reagents, wherein the derivatization device and the derivatization method have higher derivatization reagent generation efficiency.

[0004] The technical solution adopted by the present invention to solve the technical problem is: a derivatization device for online production of derivatization reagents, comprising a chemical column suppressor, a reaction reagent, a six-way valve, a derivatization reactor, a pump system and a flow system, wherein the chemical column suppressor, the reaction reagent, the six-way valve and the derivatization reactor are connected by the flow system;

[0005] The six-way valve is provided with a regeneration flow path, a cleaning flow path and a generation flow path, and the three suppression columns of the chemical column suppressor are respectively connected to the regeneration flow path, the cleaning flow path and the generation flow path in turn, so that the three suppression columns of the chemical column suppressor replace hydrogen ions in the regeneration flow path, clean in the cleaning flow path and react to generate hydroiodic acid in the generation flow path in turn.

[0006] Optionally, the pump system includes an air pump, a peristaltic pump and a chromatographic pump.

[0007] Optionally, a three-way joint is connected between the derivatization reactor and the regeneration flow path of the six-way valve, the first input end of the three-way joint is connected to the regeneration flow path, the second input end of the three-way joint is connected to the ion chromatography analysis column, and the output end of the three-way joint is connected to the derivatization reactor.

[0008] Based on the above-mentioned derivatization device for producing derivatization reagents online, the present invention also provides a derivatization method, comprising the following steps:

[0009] Rotate the chemical column suppressor so that the first suppression column of the chemical column suppressor is connected to the regeneration flow path, the second suppression column is connected to the cleaning flow path, and the third suppression column is connected to the generation flow path; the regeneration reagent enters the first suppression column through the regeneration flow path and replaces hydrogen ions in the first suppression column, the cleaning reagent enters the second suppression column through the cleaning flow path and cleans the second suppression column, the reaction reagent enters the third suppression column through the generation flow path, and reacts in the third suppression column to generate hydroiodic acid;

[0010] Rotate the chemical column suppressor so that the first suppression column of the chemical column suppressor is connected to the cleaning flow path, the second suppression column is connected to the generation flow path, and the third suppression column is connected to the regeneration flow path; the regeneration reagent enters the third suppression column through the regeneration flow path and replaces hydrogen ions in the third suppression column, the cleaning reagent enters the first suppression column through the cleaning flow path and cleans the first suppression column, the reaction reagent enters the second suppression column through the generation flow path and reacts in the second suppression column to generate hydroiodic acid;

[0011] Rotate the chemical column inhibitor so that the first inhibition column of the chemical column inhibitor is connected to the generation flow path, the second inhibition column is connected to the generation flow path, and the third inhibition column is connected to the regeneration flow path; the regeneration reagent enters the third inhibition column through the regeneration flow path and replaces hydrogen ions in the third inhibition column, the cleaning reagent enters the first inhibition column through the cleaning flow path and cleans the first inhibition column, the reaction reagent enters the second inhibition column through the generation flow path, and reacts in the second inhibition column to generate hydroiodic acid.

[0012] Through the above technical solution, the present invention adopts a chemical column suppressor with three suppression columns to continuously and uninterruptedly generate derivative reagents, thereby improving the generation efficiency of the derivatization reagents. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a schematic diagram of the derivative system of this application. DETAILED DESCRIPTION

[0014] The present application is further described in detail below in conjunction with the accompanying drawings and embodiments. It is to be understood that the specific embodiments described herein are only used to explain the relevant invention, rather than to limit the invention. It is also necessary to explain that, for ease of description, only the parts related to the invention are shown in the accompanying drawings.

[0015] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0016] like Figure 1As shown, the present invention discloses a derivatization device for online production of derivatization reagents, which includes a chemical column suppressor, a reaction reagent, a six-way valve 100, a derivatization reactor 200, a pump system and a flow system, wherein the chemical column suppressor, the reaction reagent, the six-way valve 100 and the derivatization reactor 200 are connected by the flow system. Taking the derivatization of bromate as an example, the reagents include a cleaning reagent H2O, a regeneration reagent H2SO2 and a reaction reagent KI.

[0017] In the present invention, the six passages of the six-way valve 100 are paired in pairs to form a regeneration flow path 110, a cleaning flow path 120 and a generation flow path 130. The regeneration flow path 110, the cleaning flow path 120 and the generation flow path 130 are not connected to each other, so the three flow paths complete the corresponding work independently of each other. The chemical column suppressor has three suppression columns, namely the first suppression column, the second suppression column and the third suppression column, and the three chemical column suppressors are distributed in sequence around the circumference. When generating a derivatization reagent, the three chemical column suppressors need to be rotated so that the three chemical column suppressors are connected to the regeneration flow path 110, the cleaning flow path 120 and the generation flow path 130 in sequence, respectively, and then the preparation of the derivatization reagent is completed in sequence.

[0018] The three inhibition columns of the chemical column inhibitor of the present invention are respectively connected to the regeneration flow path 110, the cleaning flow path 120 and the generation flow path 130 in turn. In this way, the three inhibition columns of the chemical column inhibitor can replace hydrogen ions in the regeneration flow path 110, clean in the cleaning flow path 120, and react in the generation flow path 130 to generate hydroiodic acid.

[0019] In the present invention, the pump system includes an air pump 300, a peristaltic pump 400 and a chromatographic pump 500. The air pump 300 is connected to the container of each reagent, and the input end of the air pump 300 is arranged above the liquid level of the reagent in the container. When pumping the reagent, air pressure is applied to the container, and the stable input of the air pressure can ensure the stability of the pressure when the reagent enters the flow path, so that the reaction between the reagents is more fully stable. The peristaltic pump 400 is used to provide power in the cleaning flow path, and it is directly installed in the cleaning flow path to pump cleaning fluid, and the chromatographic pump 500 is used to provide power in the generation flow path and the regeneration flow path.

[0020] In the present invention, a three-way joint 140 is connected between the derivatization reactor 200 and the regeneration flow path 110 of the six-way valve 100, the first input end of the three-way joint 140 is connected to the regeneration flow path 110, the second input end of the three-way joint 140 is connected to the ion chromatography analysis column, and the output end of the three-way joint 140 is connected to the derivatization reactor 200.

[0021] The present invention also provides a derivatization method, which comprises the following steps:

[0022] S1 . Rotate the chemical column suppressor so that the first suppression column of the chemical column suppressor is connected to the regeneration flow path 110 , the second suppression column is connected to the cleaning flow path 120 , and the third suppression column is connected to the generation flow path 130 .

[0023] In this state, the regeneration reagent enters the first inhibition column through the regeneration flow path 110 and replaces the hydrogen ions in the first inhibition column, the cleaning reagent enters the second inhibition column through the cleaning flow path 120 and cleans the second inhibition column, and the reaction reagent enters the third inhibition column through the generation flow path 130 and reacts in the third inhibition column to generate hydroiodic acid.

[0024] S2 , rotating the chemical column suppressor, so that the first suppression column of the chemical column suppressor is connected to the cleaning flow path 120 , the second suppression column is connected to the generation flow path 130 , and the third suppression column is connected to the regeneration flow path 110 .

[0025] In this state, the regeneration reagent enters the third inhibition column through the regeneration flow path 110 and replaces hydrogen ions in the third inhibition column, the cleaning reagent enters the first inhibition column through the cleaning flow path 120 and cleans the first inhibition column, and the reaction reagent enters the second inhibition column through the generation flow path 130 and reacts in the second inhibition column to generate hydroiodic acid.

[0026] S3 , rotating the chemical column suppressor so that the first suppression column of the chemical column suppressor is connected to the generation flow path 130 , the second suppression column is connected to the regeneration flow path 110 , and the third suppression column is connected to the cleaning flow path 120 .

[0027] In this state, the regeneration reagent enters the second inhibition column through the regeneration flow path 110 and replaces the hydrogen ions in the second inhibition column, the cleaning reagent enters the third inhibition column through the cleaning flow path 120 and cleans the third inhibition column, and the reaction reagent enters the first inhibition column through the generation flow path 130 and reacts in the first inhibition column to generate hydroiodic acid.

[0028] The present invention adopts a chemical column suppressor with three suppression columns to continuously and uninterruptedly generate a derivatization reagent, thereby improving the generation efficiency of the derivatization reagent.

[0029] In the embodiment of the present invention, when the regeneration flow path 110 replaces hydrogen ions, the reaction formula is as follows:

[0030] H2SO4+2K + → K2SO4+2H + .

[0031] After replacing hydrogen ions, the regeneration flow path 110 washes away K2SO4 through the water in the cleaning flow path 120, and then enters the generation flow path 130 to react with potassium iodide to generate hydroiodic acid. The reaction formula for generating hydroiodic acid in the generation flow path 130 is:

[0032] KI+H + → HI+K + .

[0033] After the hydroiodic acid is generated, the hydroiodic acid is pumped to the three-way connector 140 through the chromatography pump, and merged with the bromate separated from the ion chromatograph in the three-way connector 140, and enters the derivatization reactor 200 to react at 80° C. The reaction formula is:

[0034] BrO3 - +3I - +3H + →3HIO+Br - ;

[0035] 3HIO+3I - +3H + → 3I2+3H2O;

[0036] 3I2+3I - →3I3 - .

[0037] The finally generated iodine triion enters the ultraviolet detector for detection.

[0038] The above description is only a preferred embodiment of the present application and an explanation of the technical principles used. Those skilled in the art should understand that the scope of the invention involved in the present application is not limited to the technical solution formed by a specific combination of the above technical features, but should also cover other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the inventive concept. For example, the above features are replaced with (but not limited to) technical features with similar functions disclosed in the present application.

[0039] Except for the technical features described in the specification, the remaining technical features are known technologies to those skilled in the art. In order to highlight the innovative features of the present invention, the remaining technical features will not be described here in detail.

Claims

1. A derivatization device for online production of a derivatization reagent, characterized in that: It includes a chemical column suppressor, a reaction reagent, a six-way valve, a derivatization reactor, a pump system and a flow system, wherein the chemical column suppressor, the reaction reagent, the six-way valve and the derivatization reactor are connected through the flow system; The six-way valve is provided with a regeneration flow path, a cleaning flow path and a generation flow path, and the three suppression columns of the chemical column suppressor are respectively connected to the regeneration flow path, the cleaning flow path and the generation flow path in turn, so that the three suppression columns of the chemical column suppressor replace hydrogen ions in the regeneration flow path, clean in the cleaning flow path and react to generate hydroiodic acid in the generation flow path in turn.

2. The derivatization device for producing derivatization reagents online according to claim 1, characterized in that: The pump system includes an air pump, a peristaltic pump and a chromatography pump.

3. The derivatization device for online production of derivatization reagents according to claim 2, characterized in that: A three-way joint is connected between the derivatization reactor and the regeneration flow path of the six-way valve, a first input end of the three-way joint is connected to the regeneration flow path, a second input end of the three-way joint is connected to the ion chromatography analysis column, and an output end of the three-way joint is connected to the derivatization reactor.

4. A derivation method, characterized in that: The following steps are included: Rotate the chemical column suppressor so that the first suppressor column of the chemical column suppressor is connected to the regeneration flow path, the second suppressor column is connected to the cleaning flow path, and the third suppressor column is connected to the generation flow path; The regeneration reagent enters the first inhibition column through the regeneration flow path and replaces hydrogen ions in the first inhibition column, the cleaning reagent enters the second inhibition column through the cleaning flow path and cleans the second inhibition column, and the reaction reagent enters the third inhibition column through the generation flow path and reacts in the third inhibition column to generate hydroiodic acid; Rotate the chemical column suppressor so that the first suppression column of the chemical column suppressor is connected to the cleaning flow path, the second suppression column is connected to the generation flow path, and the third suppression column is connected to the regeneration flow path; the regeneration reagent enters the third suppression column through the regeneration flow path and replaces hydrogen ions in the third suppression column, the cleaning reagent enters the first suppression column through the cleaning flow path and cleans the first suppression column, the reaction reagent enters the second suppression column through the generation flow path and reacts in the second suppression column to generate hydroiodic acid; Rotate the chemical column inhibitor so that the first inhibition column of the chemical column inhibitor is connected to the generation flow path, the second inhibition column is connected to the generation flow path, and the third inhibition column is connected to the regeneration flow path; the regeneration reagent enters the third inhibition column through the regeneration flow path and replaces hydrogen ions in the third inhibition column, the cleaning reagent enters the first inhibition column through the cleaning flow path and cleans the first inhibition column, the reaction reagent enters the second inhibition column through the generation flow path, and reacts in the second inhibition column to generate hydroiodic acid.

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