Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 1, 5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH), and further determination by flame ato...Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 1, 5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH), and further determination by flame atomic absorption spectrometry (FAAS) using Triton X-114 as surfactant. The main factors affecting the CPE, such as concentration of Triton X-114 and DPTH, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimum conditions i.e., pH 5.4, [DPTH] = 6x10-3%, [Triton X-114] = 0.25% (v/v), an enhancement factor of 10.5 fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.95 μg L?1. The precision for 8 replicate deter- minations at 20 and 100 μgL?1 Cd were 2.4 % and 2 % relative standard deviation (R.S.D.). The calibration graph using the preconcentration method was linear with a correlation coefficient of 0,998 at levels close to the detection limit up to at least 200 μgL?1. The method was successfully applied to the determination of cadmium in water, environmental and food samples and in a BCR-176 standard reference material.展开更多
This work proposes the use of experimental design for optimization of microwave-assisted digestion of bio- morphic ZrO2-ceramic. Cedar wood is used as template and it was infiltrated with ZrO2 via sol-gel process. XPS...This work proposes the use of experimental design for optimization of microwave-assisted digestion of bio- morphic ZrO2-ceramic. Cedar wood is used as template and it was infiltrated with ZrO2 via sol-gel process. XPS, SEM and XRD have been used to verify the effectiveness of the synthesis. The effects of different combination of acids in the digestion of this sample have been optimized taking as response the concentra- tion of several metallic ions measured by ICP-MS.展开更多
文摘Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 1, 5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH), and further determination by flame atomic absorption spectrometry (FAAS) using Triton X-114 as surfactant. The main factors affecting the CPE, such as concentration of Triton X-114 and DPTH, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimum conditions i.e., pH 5.4, [DPTH] = 6x10-3%, [Triton X-114] = 0.25% (v/v), an enhancement factor of 10.5 fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.95 μg L?1. The precision for 8 replicate deter- minations at 20 and 100 μgL?1 Cd were 2.4 % and 2 % relative standard deviation (R.S.D.). The calibration graph using the preconcentration method was linear with a correlation coefficient of 0,998 at levels close to the detection limit up to at least 200 μgL?1. The method was successfully applied to the determination of cadmium in water, environmental and food samples and in a BCR-176 standard reference material.
文摘This work proposes the use of experimental design for optimization of microwave-assisted digestion of bio- morphic ZrO2-ceramic. Cedar wood is used as template and it was infiltrated with ZrO2 via sol-gel process. XPS, SEM and XRD have been used to verify the effectiveness of the synthesis. The effects of different combination of acids in the digestion of this sample have been optimized taking as response the concentra- tion of several metallic ions measured by ICP-MS.
