水中硫化物的极谱法测定.pdfVIP

Summary Thiourea is determined by Differ-ential Pulse Polarography. A Hanging Mercury Drop Electrode (HMDE) is used in combination with a differential pulse measure-ment. Due to the protonation of the thiourea compound, an acidic supporting electrolyte must be used. The thiourea is then in ionic form. The determination is performed by potential scanning in the cathodic direction. The new compound is stripped back into the solution in a neutral form. The resulting stripping current is proportional to the concentration of the ions in solution. During scanning, a mercury-thiou-rea compound may also be formed. The supporting electrolyte used is 1M H 2SO 4 . The method for the determination of thiourea has been tested on standard water samples with a content in the range: Thiourea: 1.5 mg/l - 18 mg/l Reagents (1) Supporting electrolyte: 1M H 2 SO 4 . (2) 1000 mg/l thiourea stock solu- tion. Dissolve 0.1 g of thiourea in 100 ml deionised water. (3) 100 mg/l thiourea standard solution. Add 10 ml 1000 mg/l of thiourea stock solution and dilute to 100 ml with water. (4) 10 mg/l thiourea standard so- lution Add 1 ml of 1000 mg/l thiourea stock solution and dilute to 100 ml with water. Always use reagent grade chemi- cals for reagent preparation. Apparatus - MDE150 Polarographic Stand - POL150 Polarographic Analyser Electrodes - TR020 Reference Electrode - TM010 Platinum Electrode - MDE/CAP 70 µm Capillary Primary settings ° Stand MDE150: - Nitrogen pressure0.5 bar ° Operating conditions: - Method DIRECT ° Cell parameters: - Electrode HMDE - Drop Nbr3 - Stirrer300 rpm - Purge time300 s - Hg drop growth time0.7 s ° Signal parameters: - T echnique DPP - E initial+300 mV E final-200 mV - Step duration0.2 s - Step amplitude 1 mV - Pulse duration40 ms - Pulse amplitude-25 mV Thiourea in Water ° Current range:- Minimum 1 nA - Maximum 1 mA ° Element identification: - Thiourea:+50 mV Depending on the concentra