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System and method for online detection of microscale water and trace water in organic phase

A detection system and organic phase technology, applied in the direction of material electrochemical variables, etc., can solve problems such as errors, external reagents interfere with the sealing of the system, and achieve the effects of low detection limit, high sensitivity, and wide application range

Inactive Publication Date: 2015-11-25
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ex-situ detection is easy to cause various errors, such as the adsorption of moisture during sample processing, the interference of external reagents, and the tightness of the system, etc.

Method used

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  • System and method for online detection of microscale water and trace water in organic phase
  • System and method for online detection of microscale water and trace water in organic phase
  • System and method for online detection of microscale water and trace water in organic phase

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Embodiment 1

[0044] Embodiment 1 of the present invention provides a trace water and trace water online detection system in the organic phase, which is used to detect the water content in the organic phase solution. in figure 1 It shows a schematic structural diagram of the trace water in the organic phase and the trace water online detection system provided by Embodiment 1 of the present invention, see figure 1 , the trace water and trace water online detection system in the organic phase, comprising a first experimental device 11 and a water content measuring device 12;

[0045] The first experimental device 11 is used to provide an experimental system for differential pulse cathodic stripping voltammetry; the experimental system is a two-electrode system, wherein the working electrode is a gold ultramicro electrode; the reference electrode is Ag / AgTPB.

[0046] When the gold ultramicroelectrode is applied with a positive voltage, the residual water in the organic phase solution oxidize...

Embodiment 2

[0056] Embodiment 2 of the present invention provides an online determination method of trace water and trace water in the organic phase, the method comprising:

[0057] Step 101: Using the pre-prepared gold ultramicroelectrode as the working electrode, the water content in the pre-prepared organic phase solution is measured by differential pulse cathodic stripping voltammetry.

[0058] Wherein, the preparation process of described gold ultramicroelectrode comprises:

[0059] S1. Preparation of glass capillary: Soak the glass capillary in piranha acid solution and then dry it ultrasonically in secondary water and acetone, and cut it into a glass capillary of preset length; preferably, place the glass capillary in piranha Soak in acid solution for 0.5h, then ultrasonically in secondary water and acetone for 5min, dry, and then cut into two sections with a length of 6cm.

[0060] S2. Insert a gold wire with a preset diameter into one end of the glass capillary, and leave a sect...

Embodiment 3

[0073] In this embodiment, taking the measurement of the water content in the DMF organic phase solution as an example, the method for on-line determination of trace water and trace water in the organic phase provided by the present invention is explained.

[0074] The pre-prepared gold ultramicroelectrode was used as the working electrode, and the water content in the pre-prepared DMF organic phase solution was determined by differential pulse cathodic stripping voltammetry (CDPSV). cathodic stripping voltammetry Figure 5A As shown, when a positive voltage is applied, the residual water in the DMF solution will oxidize the gold surface of the gold microelectrode to form a gold oxide film; then apply a negative voltage, and the gold oxide will be reduced to gold. see Figure 5A , the magnitude of the peak current in the dissolution process is positively correlated with the water content in the organic phase, and the dissolution peak shifts to the left as the water content in...

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Abstract

The invention provides a system and method for online detection of microscale water and trace water in an organic phase; the system includes a first experimental device and a water content measurement device; the first experimental device is used for providing an experimental system for a differentiated pulse cathodic stripping voltammetry; the experimental system is a two-electrode system, wherein a work electrode is a gold ultramicro-electrode; when the gold ultramicro-electrode is applied with a positive voltage, residual water in an organic phase solution oxidizes the surface of the gold ultramicro-electrode into a gold oxide thin film; when the gold ultramicro-electrode is applied with a negative voltage, the gold oxide thin film is reduced into gold, and the peak current value of the dissolution process shows a positive-correlation relationship with the water content in the organic phase; the water content measurement device is used for measuring the water content value in the organic phase solution according to the corresponding relationship of the peak current value of the dissolution process of reducing the gold oxide thin film into gold with the water content in the organic phase. The system and the method can simply and conveniently detect the water content in the organic phase.

Description

technical field [0001] The invention relates to the field of water detection in organic phases, in particular to a system and method for on-line detection of trace water and trace water in organic phases. Background technique [0002] Water is the main impurity present in the organic phase. The presence of water in the organic phase will affect the physical and chemical properties of the organic phase, such as reducing viscosity, increasing conductivity, narrowing the electrochemical window, etc. The concentration of water in the organic phase is not only related to the properties of the solvent, but also depends on the change of the experimental environment. [0003] Currently, most determinations of water content in organic phases are performed by Karl Fischer titration. However, using this method to detect water content under esterification reaction conditions, the results are unreliable, because the water generated during the reaction will bring systematic errors. [...

Claims

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Application Information

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IPC IPC(8): G01N27/48
Inventor 邵元华阴笑弘
Owner PEKING UNIV
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