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[b] 1IntroductionThere is agrowing interest in the impact of agriculture related activitieso ns oil and water quality.P ractices like fertilization, irrigation and application of pesticides are considered potential sources of introduction and deposition of certainh eavy metals and other elements in the environment [1][2][3][4].Phosphate fertilizers are manufactured from rock phosphates and according to their origin they may contain various major and trace elements,n aturally occurring radionuclides and their decay products. Usually,there is apositive correlation between the uraniuma nd the phosphate contenti nr aw material from sedimentary rocks [5,6]. Despite the unquestionablerequirement of phosphate fertilizers,t he application of fertilizers derived from naturally enriched uraniump hosphate rocks configures an anthropogenic source of this analyte [7][8][9][10].S ince an expressiveuranium concentration has been reported in sedimentary phosphate rocks (30-120mgUkg À1)a nd continuous application of manufacturedp roducts has been performed worldwide in many cultures,t he radionuclide levels are expected to rise over the following years [7,11]. Thus,t he determination of uraniuma nd trace elements such as cadmium and lead in phosphate fertilizersi si mportant, considering that processes like biomagnification and bioaccumulation may occur.Since trace uranium monitoring is significant because of its chemical and radiologic toxicity [ 5,9,[12][13][14][15],e fforts have been devoted for developing sensitive analytical methods applied to uraniumq uantification [16][17][18][19][20][21][22]. Because of their portable character, rapidity,s implicity and sensitivity, voltammetric techniques are especially suitable for this purpose.I np articular,a dsorptive stripping voltammetry (AdSV) has been widely used for trace metal analyses [23][24][25] Thee lectrochemical stripping analysis of tracem etals such as cadmium and lead is widely reported [23,25].A lthough AdSV has been found usefulf or the monitoring of e.g. cadmium concentrations [38],t he anodic stripping voltammetry (ASV) has been commonlye mployed by using the bismuth film electrode (BiFE) [39][40][41][42][43]s ince cadmium and lead signals are ideally placed in the electrode operational potential window [39].With respect to stripping analyses,t here are many published procedures with respect to sequential voltammetric determinations.T he employment of mercury as working electrode is predominant due to the high performance. By using the hangingm ercury drop electrode (HMDE), C. Locatelli has reported the sequential determination of platinum group metals and lead [44,45] and the determiAbstract:Asequential voltammetric procedure for the determination of uranium, cadmium and lead wasi nvestigated at an ex situ bismuth film electrode (BiFE). First, the adsorptive stripping voltammetry was applied to assay the U(VI)-cupferron complexi nt he differential pulse mode (detection limit of 1.0 mgL À1 ,2 00 sa ccumulation time). Through the manipulation of the same aliquo...
[b] 1IntroductionThere is agrowing interest in the impact of agriculture related activitieso ns oil and water quality.P ractices like fertilization, irrigation and application of pesticides are considered potential sources of introduction and deposition of certainh eavy metals and other elements in the environment [1][2][3][4].Phosphate fertilizers are manufactured from rock phosphates and according to their origin they may contain various major and trace elements,n aturally occurring radionuclides and their decay products. Usually,there is apositive correlation between the uraniuma nd the phosphate contenti nr aw material from sedimentary rocks [5,6]. Despite the unquestionablerequirement of phosphate fertilizers,t he application of fertilizers derived from naturally enriched uraniump hosphate rocks configures an anthropogenic source of this analyte [7][8][9][10].S ince an expressiveuranium concentration has been reported in sedimentary phosphate rocks (30-120mgUkg À1)a nd continuous application of manufacturedp roducts has been performed worldwide in many cultures,t he radionuclide levels are expected to rise over the following years [7,11]. Thus,t he determination of uraniuma nd trace elements such as cadmium and lead in phosphate fertilizersi si mportant, considering that processes like biomagnification and bioaccumulation may occur.Since trace uranium monitoring is significant because of its chemical and radiologic toxicity [ 5,9,[12][13][14][15],e fforts have been devoted for developing sensitive analytical methods applied to uraniumq uantification [16][17][18][19][20][21][22]. Because of their portable character, rapidity,s implicity and sensitivity, voltammetric techniques are especially suitable for this purpose.I np articular,a dsorptive stripping voltammetry (AdSV) has been widely used for trace metal analyses [23][24][25] Thee lectrochemical stripping analysis of tracem etals such as cadmium and lead is widely reported [23,25].A lthough AdSV has been found usefulf or the monitoring of e.g. cadmium concentrations [38],t he anodic stripping voltammetry (ASV) has been commonlye mployed by using the bismuth film electrode (BiFE) [39][40][41][42][43]s ince cadmium and lead signals are ideally placed in the electrode operational potential window [39].With respect to stripping analyses,t here are many published procedures with respect to sequential voltammetric determinations.T he employment of mercury as working electrode is predominant due to the high performance. By using the hangingm ercury drop electrode (HMDE), C. Locatelli has reported the sequential determination of platinum group metals and lead [44,45] and the determiAbstract:Asequential voltammetric procedure for the determination of uranium, cadmium and lead wasi nvestigated at an ex situ bismuth film electrode (BiFE). First, the adsorptive stripping voltammetry was applied to assay the U(VI)-cupferron complexi nt he differential pulse mode (detection limit of 1.0 mgL À1 ,2 00 sa ccumulation time). Through the manipulation of the same aliquo...
Herein, we report a facile method for the synthesis of silver nanochains (Ag nanochains) using pyridine as growth directing agent and citrate ions as capping agents in alkaline medium. The characterization of the synthesized high aspect ratio Ag nanochains was accomplished with the help of Transmission Electron Microscopy (TEM) and High Resolution Transmission Electron Microscopy (HRTEM) which demonstrates the thickness below 100 nm. Crystalline nature of the synthesized Ag nanochains was investigated using X‐ray diffractrometry. A sensitive electrochemical nitrite sensor was assembled using synthesized Ag nanochains as electrode modifier. An improved cyclic voltammetric response for the oxidation of nitrite ions was witnessed at the modified GCE surface in comparison to bare GCE in Britton Robinson (BR) buffer (pH 4). The influence of pH on the oxidation peak current of nitrite ions was also examined using cyclic voltammetry. The electrocatalytic oxidation currents attained through amperometric measurements at Ag nanochains modified GCE were linearly dependent on the concentration of nitrite ions in the two ranges of 0.5–7.5 µM, 5–480 µM. Linear calibration plots of Ip vs. concentration of nitrite were also constructed at the proposed sensor using square wave voltammetry and differential pulse voltammetry. The proposed sensing strategy was successfully employed for the determination of nitrite in water samples with excellent recoveries.
Electrochemical reduction of vanadium(V) complex with cupferron (N‐nitroso‐N‐phenylhydroxylamine), VVO(cupf)2OH, has been studied by polarography in wide potential range to verify the catalytic mechanism of electroreduction of coordinated cupferron ligand. Reduction of the complex was studied in the concentration range from 2 ⋅ 10−5 M to 10−3 M. Depending on the process conditions kinetics of catalytic reduction of coordinated cupferron is either controlled by adsorption step or governed by mixed control of diffusion and chemical reaction. Kinetic parameters of the reduction process are reported. Reduction of VVO(cupf)2OH complex is accompanied by adsorption and autoinhibition phenomena. V(II) ion in the surface bound complex of vanadium with cupferron catalyzes reduction of coordinated cupferronate ligands. In 1 mM solutions, the catalytic reduction of coordinated cupferron ligand shifts to more cathodic potentials due to formation of a monolayer of adsorbed vanadium(III)‐cupferron complexes. Reduction kinetics in the presence of tetraalkylammonium salt is consistent with multilayer cooperative adsorption of anionic vanadium(II)‐cupferron complex and tetraalkylammonium cations.
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