Determination of trace amount of antimony (Ⅲ) by adsorption voltammetry on carbon paste electrode

A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: preconcentration,reduction and stripping. Optimal conditions were found to be an electrode containing 25% paraffin oil and 75% high purity graphite powder as working electrode;a 0.10 mol/L HCl solution containing 40 μmol/L BPR as accumulation medium;a 0.20 mol/L HCl solution as reduction and stripping electrolyte;accumulation time,150 s;reduction potential and time,-0.50 V,60 s;scan range from -0.50 to 0.20 V. Interferences by other ions were studied as well. The detection limit was found to be 0.5 nmol/L for 150 s preconcentration. The linear range was from 1.0 nmol/L to 0.50 μmol/L. Application of the proposed method to the determination of antimony in water and human hair samples gave good results.

Trace Determination of Scandium Using Adsorption Voltammetry of Mix-Polynuclear Complex of Scandium-Calcium-Alizarin Red S at Carbon Paste Electrode

A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste electrode (CPE). The 2nd-order derivative linear scan voltammograms of the adsorbed complex were recorded by model JP-303 polarographic analyzer from 0.0 to -1.0 V (vs. SCE). The experimental conditions of the working procedure were optimized. The results show that the complex can be adsorbed on the surface of the CPE, yielding one peak at -0.61 V, corresponding to the reduction of the alizarin red S in the mix-polynuclear complex at the electrode. The detection limit of Sc^(3+) is 1.0×10^(-10) mol·L^(-1) for 3 min of accumulation time. The procedure was successfully applied to the determination of trace amount of scandium in the sample ores.

Determination of trace amounts of morphine in human plasma by anodic adsorptive stripping differential pulse voltammetry

New adsorptive anodic differential pulse stripping voltammetry method for the direct determination of morphine at trace levels in human plasma of addicts is proposed.The procedure involves an adsorptive accumulation of morphine on a HMDE,followed by oxidation of adsorbed morphine by voltammetry scan using differential pulse modulation.The optimum conditions for the analysis of morphine are pH 10.5,Eacc of -100 mV（vs.Ag/AgCl）,and tacc of 120 s.The peak current is proportional to the concentration of morphine,and a Linear calibration graph is obtained at 0.01-3.10μg mL^-1.A relative standard deviation of 1.06%（n=5）was obtained,and the limit of detection was 3 ng mL^-1.The capabiLity of the method for the analysis of real samples was evaluated by the determination of morphine in spiked human plasma and addicts human plasma with satisfactory results.

ADSORPTIVE STRIPPING VOLTAMMETRY OF A FENTANYL DERIVATIVE DNPME AT Hg ELECTRODE

A quasi-reversible reduction peak of a fentanyl derivative DNPME is found by cyclic voltammetry at Hg electrode. E_(pc)=-1.58 V (vs. Ag/AgCl). The cathodic peak shows adsorptive characteristics. The adsorbed species is DNPME neutral molecule. The method for measuring trace amount of DNPME by adsorptive stripping voltammetry is established.

Adsorptive Stripping Voltammetry of Ultra Trace Lanthanum（Ⅲ） Using an Alizarin S as Complexing Agent and Carbon Paste as Working Electrode

Ultra trace determination of lantanum（Ⅲ） has been studied by adsorptive stripping voltammetry methods using an alizarin S as complexing agent and carbon paste electrode as working electrode. The electrode was made from mixed of carbon powder and paraffin in micropipette tip with diameter of 4 ram. This method consists of two steps. The first step is the formation and adsorptive accumulation of metal ion with chelator at the electrode surface. The second step is stripping the complex from the electrode surface into the solution. The stripping step generates current which is recorded as voltammogram. The optimum conditions of instrumental parameter obtained were accumulation potential of 600 mV, accumulation time of 120 seconds, and pH of solution of 5.5. In this research, the limit detection obtained was 2.3348 × 10^-12 M （3.24× 10^-11μg/L） with sensitivity of 16.52 （nA/10u M） and the precision of standard solution of La3＋ with concentration of 2 × 10^-12 M, 4× 10^-12 M, 6 × 10^-12 M, 8 × 10^-12 M, and 10 × 10^-12M were 3.50%, 9.88%, 7.19%, 7.48% and 1.85% respectively. The linierity of this method is very good with correlation coefficient is 0.9780. Recovery percentage from La3＋ with concentration of 6× 10^-12 M and 10 × 10^-12 M are 108.84% and 91.51%, respectively.

STUDY ON THE DETERMINATION OF METRONIDAZOLE IN HUMAN SERUM BY ADSORPTIVE STRIPPING VOLTAMMETRY

In Britton-Robinson buffer,metronidazole is preconcentreted on HHDE at 0.0 V(Vs.Ag- AgCI),An adsorptive stripping peak is observed at-0.62 V.Tho response is linear from 1x10^(-8)to 1×10^(-6)mol/L with 1.5 min accumulation.The method has been successfully applied to the deternation of metronidazole in human serum and formulations.

Selective determination of trace cobalt in zinc electrolytes by second-derivative catalytic polarography

We report herein a highly selective method for directly determining the trace Co^2+in highly concentrated zinc electrolyte.This novel method is based on a second derivative wave of catalytic adsorptive polarography generated by complexing Co^2+with dimethylglyoxime and nitrite onto a dropping mercury electrode.By employing a medium with NH3-NH4Cl buffer,DMG and NaNO2 during determining the trace Co^2+,any interferences of highly concentrated Zn^2+and other coexisting metal ions in the electrolyte are completely eliminated due to the selective masking effect of EDTA.When the concentration of Co^2+is within 1.0×10^–10–3.2×10^–7 mol/L range,it shows a good linear relationship with the current peak.Detection limit is 1.0×10^–11 mol/L,and RSD≤2.7%for six successive assays.We have compared the efficiency of the current method to that obtained by cobalt nitroso-R-salt spectrophotometry,and the absolute values of relative deviations are≤4.2%.The method developed and described herein has been successfully employed in determining the trace Co2+in actual zinc electrolyte.

Adsorptive stripping voltammetric methods for determination of aripiprazole

Anodic behavior of aripiprazole(ARP) was studied using electrochemical methods.Charge transfer,diffusion and surface coverage coefcients of adsorbed molecules and the number of electrons transferred in electrode mechanisms were calculated for quasi-reversible and adsorp-tion-controlled electrochemical oxidation of ARP at 1.15 V versus Ag/AgCl at pH 4.0 in Britton-Robinson buffer(BR) on glassy carbon electrode.Voltammetric methods for direct determination of ARP in pharmaceutical dosage forms and biological samples were developed.Linearity range is found as from 11.4 μM(5.11 mg/L) to 157 μM(70.41 mg/L) without stripping mode and it is found as from 0.221 μM(0.10 mg/L) to 13.6 μM(6.10 mg/L) with stripping mode.Limit of detection(LOD) was found to be 0.11 μM(0.05 mg/L) in stripping voltammetry.Methods were successfully applied to assay the drug in tablets,human serum and human urine with good recoveries between 95.0% and 104.6% with relative standard deviation less than 10%.

Catalytic Adsorptive Stripping Voltammetry at a Carbon Paste Electrode for the Determination of Amiodarone

Voltammetry using solid electrodes usually suffers from the contamination due to the deposition of the redox products of analytes on the electrode surface. The contamination has resulted in poor reproducibility and overelaborate operation procedures. The use of the chemical catalysis of oxidant on the reduction product of analyte not only can eliminate the contamination of analyte to solid electrodes but also can improve the faradaic response of analyte. This work introduced both the catalysis of oxidant K2S2O8 and the enhancement of surfactant Triton X-100 on the faraday response of amiodarone into an adsorptive stripping voltammetry at a carbon paste electrode for the determination of amiodarone. The method exhibits high sensitivity, good reproducibility and simple operation procedure. In 0.2 mol·L^-1 HOAc-NaOAc buffer （pH=5.3） containing 2.2×10^-2 mol·L^-1 K2S2O8 and 0.002% Triton X-100, the 2.5th-order derivative stripping peak current of the catalytic wave at 0.3 V （vs. Ag/AgCl） is rectilinear to amiodarone concentration in the range of 2.0×10^-10-2.3×10^-8 mol·L^-1 with a detection limit of 1.5×10^-10 mol·L^-1 after accumulation at 0 V for 30 s.