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Novel derivatization reagent, method for testing sulfur-containing component and application

A technology for derivatizing reagents and testing methods, applied in the field of instrumental analysis, can solve the problems of lack of separation pretreatment and inaccurate test results, etc., and achieve the effect of accurate control of reagent addition and derivation time, and accurate results

Active Publication Date: 2021-01-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods mainly produce components with specific visible light or specific absorption in the fluorescent region through the reaction of the target component with the derivative reagent, and then perform quantitative analysis of the substance, lack of pre-separation treatment, if there are interfering substances in the system, the test result will be inaccurate
At the same time, the method mainly focuses on the quantitative analysis of a sulfur-containing compound, and there is no literature or patent that can simultaneously analyze sulfur ions and mercaptans

Method used

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  • Novel derivatization reagent, method for testing sulfur-containing component and application
  • Novel derivatization reagent, method for testing sulfur-containing component and application
  • Novel derivatization reagent, method for testing sulfur-containing component and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Synthetic derivatization reagents.

[0068] 4,4-Diphenylethylene dicarboxylic acid (11.3g, 50mmol), hydroquinone (13.2g, 120mmol) and methanesulfonic acid (0.48g, 10mmol%) were sequentially added to the reaction tube. Add 50 mL of acetone to the reaction bottle and stir to dissolve at room temperature, move the reaction bottle to an oil bath at 60°C and heat to reflux for 2 hours, return the reaction system to room temperature, wash with water, remove the solvent by rotary evaporation, wash with n-hexane, and recrystallize to 93 % (21.01 g) yield gave Intermediate K.

[0069] Get intermediate product K (4.52g, 10mmol) and 50ml acetone and install it in a three-necked flask in a 100ml separating funnel, get tert-butyl hydroperoxide (1.35g, 15mmol) and install it in a three-necked flask in a 100ml separating funnel with 50ml acetone, add Put 50ml of acetone in a three-necked flask, reflux at 90°C, open two separatory funnels, add the material dropwise in 30 minutes, refl...

Embodiment 2

[0072] Synthetic derivatization reagents.

[0073] 4,4-Diphenylethylene dicarboxylic acid (11.3g, 50mmol), hydroquinone (12.1g, 110mmol) and trifluoromethanesulfonic acid (0.37g, 5mmol%) were sequentially added to the reaction tube. Add 50mL of 1,4-dioxane to the reaction bottle, stir and dissolve at room temperature, move the reaction bottle to an oil bath at 60°C and heat to reflux for 2 hours, return the reaction system to room temperature, wash with water, remove the solvent by rotary evaporation, and wash with n-hexane , recrystallized to obtain the intermediate product K in a yield of 86% (19.43 g).

[0074] Get intermediate product K (4.52g, 10mmol) and 50ml1,4-dioxane in a 100ml separatory funnel and install it into a three-necked flask, get tert-butyl hydroperoxide (0.99g, 11mmol) and 50ml1,4-dioxane Install the ring in a 100ml separating funnel to the three-necked flask, add 50ml 1,4-dioxane to the three-necked flask, reflux at 90°C, open the two separating funnels,...

Embodiment 3

[0076] Synthetic derivatization reagents.

[0077] 4,4-diphenylethylene dicarboxylic acid (11.3g, 50mmol), hydroquinone (27.5g, 250mmol) and p-toluenesulfonic acid (4.3g, 50mmol%) were sequentially added into the reaction tube. Add 50mL dimethyl sulfoxide to the reaction bottle, stir and dissolve at room temperature, move the reaction bottle to an oil bath at 60°C and heat to reflux for 2 hours, return the reaction system to room temperature, wash with water, remove the solvent by rotary evaporation, wash with n-hexane, and re- Crystallization afforded intermediate K in 94% (21.24 g) yield.

[0078] Get intermediate product K (4.52g, 10mmol) and 50ml dimethyl sulfoxide in a 100ml separatory funnel and install it into a three-necked flask, get tert-butyl hydroperoxide (1.80g, 20mmol) and 50ml dimethyl sulfoxide in 100ml Install the liquid funnel to the three-necked flask, add 50ml dimethyl sulfoxide to the three-necked flask, reflux at 90°C, open the two separatory funnels, dr...

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Abstract

The invention provides a novel derivatization reagent, a method for testing a sulfur-containing component and application. The derivatization reagent has a special structure, and can be used for directionally analyzing and testing sulfide in wastewater and mercaptan components in an organic phase by using an online derivatization chromatographic analysis method. The novel derivatization reagent can react with sulfur-containing compounds in wastewater and can further react with mercaptan in organic components, and can be used for testign sulfur-containing components in wastewater and organic phases at the same time, so that sulfur ions and mercaptan substances are monitored on line at the same time. By adpoting the liquid chromatography on-line derivatization analysis method, the sample reproducibility is good, the detection limit is high, interference factors are few, and the test result is accurate.

Description

technical field [0001] The invention belongs to the field of instrumental analysis, and in particular relates to a novel derivative reagent and a method and application for testing sulfur-containing components. Background technique [0002] Waste water and sewage produced in chemical production, because they contain some intermediate components in chemical production, are extremely harmful to the environment. Sulfur compounds contained in chemical wastewater will reduce the activity and growth rate of anaerobic bacteria that treat wastewater, slow down the degradation rate of organic matter, seriously affect the treatment effect of anaerobic organisms in chemical plants, and cause permanent poisoning of catalysts used in the plant. [0003] Sulfur-containing compounds in wastewater include soluble hydrogen sulfide, sodium sulfide, etc., which generally exist in suspended solids, including soluble sulfides, acid-soluble metal sulfides, combined organic and inorganic sulfides,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 国欣孔祥明徐艳飞徐丹朱子忠陈良进张宏科
Owner WANHUA CHEM GRP CO LTD
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