Electrocatalytic reduction of ortho nitrobenzaldehyde using modified aluminum electrode and its determination

A simple, cost effective and rapid electrochemical method has been developed for the determination of micro level ortho nitrobenzaldehyde（ONB） based on outstanding properties of modified aluminum electrode tin nanorods/anodic aluminum oxide/aluminum（SnNR/AAO/Al） for the first time. The SnNR/AAO/Al electrode was fabricated by a second step anodization, followed by electrodeposition and its electrochemical behavior was investigated in detail. The cyclic voltammetry results indicated that the SnNR/AAO/Al electrode exhibited efficient electrocatalytic activity toward reduction of ONB in the acidic solution. It provides an appreciable improvement of reduction peak for ONB at-0.721 V.Furthermore, various kinetic parameters such as transfer electron number, transfer proton number and standard heterogeneous rate constant were calculated from the scan rates.The electrocatalytic behavior was further exploited as a sensitive detection scheme for the ONB determination by differential pulse voltammetry. Under the optimized conditions, the concentration range and detection limit are 0.1-100 μmol/L and 0.05 μmol/L, respectively,for ONB. The analytical performance of this modified sensor has been evaluated for detection of real sample such as river water and recovery of ONB was achieved all-out up to102.3% under standard addition method.     

Recovery of metal values from zinc solder dross

Zinc solder dross containing 14.8% Sn, 16.3% Pb, 0.41% Al and 64.5% Zn was leached with 3% H₂SO₄ at 45°C for 1 h. Zinc and aluminum went into solution, whereas lead and tin remained with the residue. Aluminum was selectively precipitated as calcium aluminum carbonate by treating the sulphate leachate with limestone at pH 4.8. Zinc sulphate solution was either evaporated to obtain zinc sulphate crystals or precipitated as basic zinc carbonate at pH 6.8. The undissolved lead and tin were leached with 5 M hot hydrochloric acid. The major part of lead chloride ( 73%) was separated by cooling the leached products down to room temperature. From the soluble fraction, tin was recovered as hydrated tin oxide by alkylation with caustic soda at pH 2.4, while the remaining lead was separated at pH 8.5 as lead hydroxide. A process flowsheet had been suggested which involved two-stage hydrometallurgical treatment. Parameters affecting the recovery efficiency of the suggested method such as temperature, time, pH and acid: solid stoichiometric ratio were investigated. Results obtained revealed that the optimum leaching conditions were achieved by using 20 ml of 3% H₂SO₄ acid/g dross for 1 h at 45°C. Recovery efficiency of the metal salts was 99.1, 99.4, 99.6 and 99.5% for Zn, Al, Pb and Sn respectively. Recovery efficiency was related to the solubility of the concerned salts under the given experimental conditions.     

原子荧光光谱法同时测定环境水体中痕量锡和锌

采用原子荧光光谱法同时测定环境水样中痕量锡和锌,优化了试验条件。锡在1.00μg/L～10.0μg/L、锌在20.0μg/L～200μg/L范围内线性良好,方法检出限锡为0.13μg/L,锌为1.76μg/L,锡和锌标准溶液测定的相对标准偏差分别为2.9%和4.0%,环境水样加标回收率锡为96.4%～106%,锌为92.0%～111%。     

原子荧光光谱法测定水中低含量锡

采用原子荧光光谱法测定水中锡,结果表明,方法检测限为0．14μg／L,在0、0μg／L～100μg／L范围内线性良好。不同浓度标准溶液测定的相对误差≤2．0％,实际样品测定的加标回收率在90．0％～109％之间,相对标准差≤6．1％,准确度和精密度均较好。