A New Method for Determination of Thiourea Content Based on Benzyne Fluorescent Reagent
A fluorescent reagent and benzyne technology, applied in the field of thiourea detection, can solve the problems of health hazards, low detection limit, and inability to popularize operators, and achieve the effects of low detection limit, good accuracy and high sensitivity
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[0036] The preparation method of benzyne organic matter p-acid, brominated p-acid and the detection of thiourea content comprise the following steps:
[0037] (1) Mix 2.76 g of 1,4-dimethoxybenzene, 20 mL of acetic acid, 2 mL of distilled water, 1 mL of concentrated sulfuric acid, 9.22 g of sodium periodate and 10.22 g of iodine, heat to 70 °C, condense and reflux for 36 h, then filter, wash the dissolved solid with dichloromethane, wash with saturated sodium sulfite solution until the color of dichloromethane does not change, then wash the organic phase with sodium chloride, dry, filter, rotary evaporate, and recrystallize to obtain product 2;
[0038] (2) Mix 1.17 g of product 2 obtained in (1) with 5 mL of triethylamine, 15 mL of tetrahydrofuran, 0.02 g of Pd(pph 3 ) 2 Cl 2 , 0.023g cuprous iodide and mix well, add 0.9 mL trimethylsilyl acetylene with a constant pressure funnel, condense and reflux at 70 ℃ for 3 h, overnight, wash with saturated ammonium chloride solution...
Embodiment 1
[0046] Embodiment 1 (natural water, such as river water)
[0047] (1) Mix 2.76 g of 1,4-dimethoxybenzene, 20 mL of acetic acid, 2 mL of distilled water, 1 mL of concentrated sulfuric acid, 9.22 g of sodium periodate and 10.22 g of iodine, heat to 70 °C, condense and reflux for 36 h, then filter, wash the dissolved solid with dichloromethane, wash with saturated sodium sulfite solution until the color of dichloromethane does not change, then wash the organic phase with sodium chloride, dry, filter, rotary evaporate, and recrystallize to obtain product 2;
[0048] (2) Mix 1.17 g of product 2 obtained in (1) with 5 mL of triethylamine, 15 mL of tetrahydrofuran, 0.02 g of Pd(pph 3 ) 2 Cl 2 , 0.023g cuprous iodide and mix well, add 0.9 mL trimethylsilyl acetylene with a constant pressure funnel, condense and reflux at 70 ℃ for 3 h, overnight, wash with saturated ammonium chloride solution, separate liquid to remove water, and then use saturated chlorine Wash with sodium chloride...
Embodiment 2
[0056] Embodiment 2 (sewage, such as factory wastewater)
[0057] (1) Mix 2.76 g of 1,4-dimethoxybenzene, 20 mL of acetic acid, 2 mL of distilled water, 1 mL of concentrated sulfuric acid, 9.22 g of sodium periodate and 10.22 g of iodine, heat to 70 °C, condense and reflux 36 h, then filtered, washed the dissolved solid with dichloromethane, washed with saturated sodium sulfite solution until the color of dichloromethane remained unchanged, then washed the organic phase with sodium chloride, dried, filtered, rotary evaporated, and recrystallized to obtain product 2;
[0058] (2) Mix 1.17 g of product 2 obtained in (1) with 5 mL of triethylamine, 15 mL of tetrahydrofuran, 0.02 g of Pd(pph 3 ) 2 Cl 2 , 0.023g cuprous iodide and mix well, add 0.9 mL trimethylsilyl acetylene with a constant pressure funnel, condense and reflux at 70 ℃ for 3 h, overnight, wash with saturated ammonium chloride solution, separate liquid to remove water, and then use saturated chlorine Wash with so...
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