Gas diffusion-flow injection determination of total inorganic carbon in water using tungsten oxide electrode

A novel gas diffusion-flow injection method has been developed for the rapid and sensitive determination of total inorganic carbon (TIC) in water. The method is based on the diffusion of CO₂ across gas permeable membrane from a donor stream containing 0.1 M HCl to an acceptor stream of sodium acetate (10⁻⁵ mol l⁻¹ and pH 10). The CO₂ trapped in the acceptor stream passes through an electrochemical flow cell contains a tungsten oxide wire and a silver/silver chloride electrode, where it was sensitively detected. The parameters affecting the sensitivity of the electrode such as buffer concentration, pH, flow rate and injected volume were studied in detail. The electrode response was linear in the concentration range from 5 to 100 μg ml⁻¹ CO₃²⁻ with a correlation coefficient (R²) of 0.998. Precision (R.S.D.) was 1.42% for 20 μg ml⁻¹ standard solution of CO₃²⁻ (n=10). The detection limit was 0.20 μg ml⁻¹ CO₃²⁻. The method was evaluated by the injection of real natural water samples and an average recovery of 100.1% was obtained. The sampling rate was 30 samples h⁻¹. The method is simple, feasible with satisfactory accuracy and precision and thus could be used for monitoring TIC in water.     

On-line determination of mercury(II) by membrane separation flow injection analysis

A rapid and inexpensive gas-diffusion (GD) flow injection method for the on-line determination of Hg(II) in aqueous samples is described. The analytical procedure involves the injection of a Hg(II) sample into a 1.5 M H₂SO₄ carrier stream which is merged with a reagent stream containing 0.6% SnCl₂ and 1.5 M H₂SO₄. Under these conditions Hg(II) is reduced to metallic mercury which partially evaporates through a Teflon membrane into an acceptor stream containing 1.75×10⁻⁴ M KMnO₄ in 0.3 M H₂SO₄. The decrease in the absorbance of the acceptor stream at 528 nm corresponding to the absorption maximum of the permanganate anion can be related to the original concentration of Hg(II) in the sample. The method is characterized by a detection limit of 4 μg l⁻¹ and a sampling frequency of 8 h⁻¹. The flow system was successfully applied to the analysis of river samples spiked with Hg(II).     

Gas-diffusion flow injection determination of Hg(II) with chemiluminescence detection

A gas-diffusion flow injection method for the chemiluminescence detection of Hg(II) based on the luminol-H₂O₂ reaction was developed. The analytical procedure involved the injection of Hg(II) samples and standards into a 1.50 M H₂SO₄ carrier stream, which was subsequently merged with a reagent stream of 0.60% (w/v) SnCl₂ in 1.50 M H₂SO₄ to reduce Hg(II) to metallic Hg. The gas-diffusion cell was thermostated at 85 °C to enhance the vaporisation of metallic Hg. Mercury vapour, transported across the Teflon membrane of the gas-diffusion cell into the acceptor stream containing 1.00 × 10⁻⁴ M KMnO₄ in 0.30 M H₂SO₄, was oxidised back to Hg(II). The acceptor stream was merged with a reagent stream containing 2.50 M H₂O₂ in deionised water and then the combined stream was merged with another reagent stream containing 7.50 × 10⁻³ M luminol in 3.00 M NaOH at a confluence point opposite to the photomultiplier tube of the detection system. The chemiluminescence intensity of the luminol-H₂O₂ reaction was enhanced by the presence of Hg(II) in the acceptor stream. The corresponding increase was related to the original concentration of Hg(II) in the samples and standards. Under optimal conditions, the chemiluminescence gas-diffusion flow injection method was characterised by a linear calibration range between 1 μg L⁻¹ and 100 μg L⁻¹, a detection limit of 0.8 μg L⁻¹ and a sampling rate of 12 samples per hour. It was successfully applied to the determination of mercury in seawater and river samples.     

Flow injection analysis of ethyl xanthate by gas diffusion and UV detection as CS2 for process monitoring of sulfide ore flotation

A sensitive and robust analytical method for spectrophotometric determination of ethyl xanthate, CH₃CH₂OCS₂⁻ at trace concentrations in pulp solutions from froth flotation process is proposed. The analytical method is based on the decomposition of ethyl xanthate, EtX⁻, with 2.0 mol L⁻¹ HCl generating ethanol and carbon disulfide, CS₂. A gas diffusion cell assures that only the volatile compounds diffuse through a PTFE membrane towards an acceptor stream of deionized water, thus avoiding the interferences of non-volatile compounds and suspended particles. The CS₂ is selectively detected by UV absorbance at 206 nm (? = 65,000 L mol⁻¹ cm⁻¹). The measured absorbance is directly proportional to EtX⁻ concentration present in the sample solutions. The Beer's law is obeyed in a 1 × 10⁻⁶ to 2 × 10⁻⁴ mol L⁻¹ concentration range of ethyl xanthate in the pulp with an excellent correlation coefficient (r = 0.999) and a detection limit of 3.1 × 10⁻⁷ mol L⁻¹, corresponding to 38 μg L⁻¹. At flow rates of 200 μL min⁻¹ of the donor stream and 100 μL min⁻¹ of the acceptor channel a sampling rate of 15 injections per hour could be achieved with RSD < 2.3% (n = 10, 300 μL injections of 1 × 10⁻⁵ mol L⁻¹ EtX⁻). Two practical applications demonstrate the versatility of the FIA method: (i) evaluation the free EtX⁻ concentration during a laboratory study of the EtX⁻ adsorption capacity on pulverized sulfide ore (pyrite) and (ii) monitoring of EtX⁻ at different stages (from starting load to washing effluents) of a flotation pilot plant processing a Cu-Zn sulfide ore.     

Bia-amperometric quantification of salbutamol in pharmaceutical products

This paper presents a simple, rapid and reproducible method of analysis of salbutamol in pharmaceutical products, utilizing batch injection analysis (BIA) associated with amperometric detection. A study of salbutamol oxidation demonstrated a strong dependence between electrode fouling and pH. All determinations were done utilizing a glassy carbon electrode in presence of 3.0 mol l⁻¹ NaOH. A large linear dynamic range from 8×10⁻⁷ to 2×10⁻⁴ mol l⁻¹ was obtained by using an injected volume of 100 μl with a detection limit of 2.5×10⁻⁷ mol l⁻¹. R.S.D. of 0.92% for 50 successive injections of 4×10⁻⁶ mol l⁻¹ of salbutamol and a sample throughput of 60 samples per hour were achieved. The method was applied for salbutamol quantification in syrups.     

Determination of benorilate in pharmaceutical formulations and its metabolite in urine at carbon paste electrode modified by silver nanoparticles

Benorilate was determined by the differential pulse voltammetry (DPV) using a carbon paste electrode modified by silver nanoparticles in 1.25 × 10⁻³ mol l⁻¹ KH₂PO₄ and Na₂HPO₄ buffer solution (pH = 6.88, 25 °C) .The anodic peak potential was +0.970 V (versus SCE). A good linear relationship was realized between the anodic peak currents and benorilate concentrations in the range of 1.0 × 10⁻⁷ to 2.5 × 10⁻⁴ mol l⁻¹ with the detection limit of 1.0 × 10⁻⁸ mol l⁻¹. The recovery was 95.2-103.6% with the relative standard deviation of 3.6% (n = 9). The pharmaceutical preparations, benorilate tablets samples and its metabolite (salicylic acid) in urine were determined with the desirable results.     

Sensitized extraction spectrophotometric determination of Hg(II) with dithizone after its flotation as ion-associate using iodide and ferroin

This paper describes a simple and highly selective method for the separation, preconcentration and spectrophotometric determination of extremely low concentration of mercury. The method is based on the flotation of an ion-associate of HgI₄²⁻ and ferroin between aqueous and n-heptane interface at pH 5. The ion-associate was then separated and treated with ammonia and dithizone solutions to extract only the mercury chelate with CH₂Cl₂. The measurement is feasible when the volume of the water sample containing Hg(II) was varied over 50-800 ml. Beer's law was obeyed over the concentration range of 8 × 10⁻⁹ to 1.6 × 10⁻⁷ mol l⁻¹ with an apparent molar absorptivity of 6.53 × 10⁶ l mol⁻¹ cm⁻¹ for a 500 ml aliquot of the water sample. The detection limit (n = 7) was 5.0 × 10⁻¹⁰ mol l⁻¹ and the R.S.D. (n = 5) for 8.0 × 10⁻⁷ mol l⁻¹ of Hg(II) was 3.7%. A notable advantage of the method is that the determination of Hg(II) is free from the interference of almost all cations and anions found in the environmental and waste water samples. The determination of Hg(II) in tap, synthetic sea water and human hair samples was carried out by the present method and cold vapor atomic absorption spectrometry (CV-AAS). The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples.     

Voltammetry determination of trace manganese with pretreatment glassy carbon electrode by linear sweep voltammetry

This paper described the determination of trace manganese using linear sweep voltammetry at a pretreatment glassy carbon electrode. The glassy carbon electrode pretreated by electrochemical method in the 0.1 mol l⁻¹ NaOH solution greatly improved the electrode responsibility in the determination of manganese(II). The barrier to the detection of low manganese concentration was overcome by means of autocatalytic effect of manganese oxide deposited on the electrode in advance. Under the optimum experiments condition (0.04 mol l⁻¹ NH₃-NH₄Cl buffer solution, pH 9.0), the linear range was 4×10⁻⁸ to 1×l0⁻⁶ mol l⁻¹ Mn(II) for linear sweep voltammetry and 1×10⁻⁹ to 4×10⁻⁸ mol l⁻¹ Mn(II) for convolution voltammetry. The relative standard deviation for 2×10⁻⁸ mol l⁻¹ Mn(II) is 3.4%. The proposed method is simple, rapid, sensitive and selective. It had been applied to the determination of trace manganese in samples with satisfactory results.     

Amperometric sensor for nitrite using a glassy carbon electrode modified with alternating layers of iron(III) tetra-(N-methyl-4-pyridyl)-porphyrin and cobalt(II) tetrasulfonated phthalocyanine

The development of a highly sensitive amperometric sensor for nitrite using a glassy carbon electrode modified with alternated layers of iron(III) tetra-(N-methyl-4-pyridyl)-porphyrin (FeT4MPyP) and cobalt(II) tetrasulfonated phthalocyanine (CoTSPc) is described. The modified electrode showed an excellent catalytic activity and stability for the nitrite oxidation decreasing the peak potentials about 200 mV toward less positive values and presenting much higher peak currents than those obtained on the bare GC electrode. A linear response range of 0.2-8.6 μmol l⁻¹, with a sensitivity of 0.37 μA l μmol⁻¹ and detection limit of 0.04 μmol l⁻¹ were obtained with this sensor. The repeatability of the proposed sensor, evaluated in term of relative standard deviation, was verified to be 1.4% for 10 measurements of 0.2 μmol l⁻¹ nitrite solution. Interference caused by common ions has been investigated in simulated mixtures containing high concentration level of interfering ions and the sensor was found to be tolerant against these ions. The developed sensor was applied for the nitrite determination in water samples and the results were in agreement with those obtained by a comparative method described in the literature. The average recovery for these samples was 100.1 (±0.7)%.     

High performance liquid chromatography determination of chlorophenols in water samples after preconcentration by continuous flow liquid membrane extraction on-line coupled with a precolumn

A continuous flow liquid membrane extraction (CFLME)-C₁₈ precolumn-liquid chromatography system was developed for preconcentration and determination of chlorinated phenols (CPs). After preconcentration by CFLME, which is based on the combination of continuous flow liquid-liquid extraction and supported liquid membrane, CPs were enriched in 960 μl of 0.5 mol l⁻¹ NaOH used as acceptor. This acceptor was on-line neutralized and transported onto the C₁₈ precolumn where analytes were absorbed and focused. Then the focused analytes were injected onto the C₁₈ analytical column for separation and detected at 215 nm with a diode array detector. CFLME related parameters such as flow rates, pH of donor and acceptor concentration were optimized. The proposed method presents detection limits of 0.02-0.09 μg l⁻¹ (S/N=3) when 100 ml samples were enriched. The proposed method was successfully applied to determine CPs in tap water and river water samples with spiked recoveries in the range of 70-121%.     

Sequential flow injection analysis of ammonium and nitrate using gas phase molecular absorption spectrometry

A flow injection method on the basis of gas phase molecular absorption is described for the sequential determination of ammonium and nitrate. Two hundred microliters of sample solution is injected into the flow line. For ammonium determination, the sample zone is directed to a line in which reacts with NaOH (13 M) and produces ammonia. But for nitrate determination, the sample zone is passed through the on-line copperized zinc (Zn/Cu) reduction column and produces ammonium ion and in the follows ammonia. The produced ammonia in both cases is purged into the stream of N₂ carrier gas. The gaseous phase is separated from the liquid phase using a gas-liquid separator and then is swept into a flow through cell, which has been positioned in the cell compartment of an UV-Vis spectrophotometer. The absorbance of the gaseous phase is measured at 194 nm. Under selected conditions for sequential analysis of ammonium and nitrate, linear relations were found between the peak heights of absorption signals and concentrations of ammonium (10-650 μg ml⁻¹) and nitrate (20-800 μg ml⁻¹). The limit of detections for ammonium and nitrate analysis were 8 and 10 μg ml⁻¹, respectively. The relative standard deviations of repeated measurements of 50 μg ml⁻¹ of ammonium and nitrate were 2.0, 2.9%, respectively. Maximum sampling rate was about 40 samples/h. The method was applied to the determination of ammonium in pharmaceutical products and the sequential determination of ammonium and nitrate in spiked water samples.     

On-line electrochemical preconcentration and flame atomic absorption spectrometric determination of manganese in urine samples

A sensitive and selective method was developed for the determination of traces of manganese in urine using on-line electrochemical preconcentration followed by flame atomic absorption spectrometry detection. A home made flow-through polypropylene cell (4.5 cm long × 0.8 cm diameter filled with glass marbles) with an effective inner volume of 0.5 ml containing a working and a counter electrode, both of glassy carbon and a Pt pseudo reference electrode was located in a flow injection manifold specially designed for the purpose of this work. The manganese was deposited from buffer solution of NH₃/NH₄Cl at pH 9.00 through an oxidizing process at a current of 400 mA during 7 min. A flow of HCl 0.1 mol l⁻¹ at 4 ml min⁻¹ through the cell, chemically dissolved the deposit. A small portion (15 μl) of the concentrate was introduced in a continuously flowing system by means of a timing device and was then carried to the detector for the manganese quantification. All electrochemical and spectroscopic variables as well as possible interferences in both systems were systematically studied. The relative standard deviations for ten consecutive measurements of manganese solutions of 2.0 and 20 μg l⁻¹ were of 2.3 and 1.5%, respectively, while for a sample processed five times was less then 5%. The accuracy of the developed procedure was evaluated by adding known amounts of manganese standard to urine samples and following the whole procedure. Recoveries within the range 97.2-102.8% were obtained. To further prove the accuracy, a Seronorm Trace Elements in Urine, Batch 403125 sample with a reported concentration of 13 μg Mn l⁻¹ was also analyzed. The experimental value obtained was of 12.7 ± 0.1 μg l⁻¹, which does not differ significantly from the reported amount (p < 0.05). A preconcentration factor of 40, a linear range between 0.015 and 60 μg l⁻¹ and a limit of detection of 15 ng l⁻¹ permitted the determination of manganese in real urine samples from non-exposed subjects in the range 0.5-2.8 μg l⁻¹.     

Development of a voltammetric sensor for diospyrin determination in nanomolar concentrations

A sensor based on glassy carbon (GC) electrode modified with cobalt tetrasulfonated phthalocyanine (CoTSPc) and a poly-l-lysine (PLL) film is proposed for diospyrin determination in nanomolar concentrations with differential pulse voltammetry (DPV) technique. The modified electrode showed excellent catalytic activity presenting much higher peak currents than those measured on a bare GC electrode. Linear response range, sensitivity and limit of detection (LOD) were of 1-120 nmol l⁻¹, 220.46 nA l nmol⁻¹ cm⁻² and 0.3 nmol l⁻¹, respectively. The repeatability of the proposed sensor, evaluated in term of relative standard deviation (R.S.D.), was measured as 4.4% for 10 experiments in 50 μmol l⁻¹ diospyrin samples. The developed sensor was applied for the determination of diospyrin in the crude extracts of the stem-bark of Diospyros montana Roxb. and the average recovery for these samples was 101.9 (±3.1)%.     

Development of an enzymeless biosensor for the determination of phenolic compounds

The construction of amperometric enzymeless biosensors for phenolic compounds determination, using carbon paste electrode modified with copper phtalocyanine (CuPc) and histidine (His), based on the chemistry of the dopamine β-monooxygenase (DβM) enzyme that catalyzes the hydroxylation of the dopamine and its analogs is shown. The modified carbon paste was evaluated on electrodes constructed in two ways: putting the paste into a cavity of a rotating disk electrode and a platinum slide electrode fixed into a glass tube. The sensor in hydrodynamic conditions presented a linear response range between 30 and 250 μmol l⁻¹, with a sensitivity of 4.6±0.1 nA l μmol⁻¹ cm⁻² for catechol, response time of 3 s and lifetime of about 50 days when stored at room temperature. The sensor in static conditions showed a linear response range from 40 to 250 μmol l⁻¹, with a sensitivity of 0.30±0.01 nA l μmol⁻¹ cm⁻² for catechol. The sensors presented the following relative response order for dopamine and some analog species: catechol>dopamine>guaiacol>serotonin>phenol.     

Direct and simultaneous determination of arsenic, manganese, cobalt and nickel in urine with a multielement graphite furnace atomic absorption spectrometer

A simple method was developed for the direct and simultaneous determination of arsenic (As), manganese (Mn), cobalt (Co), and nickel (Ni) in urine by a multi-element graphite furnace atomic absorption spectrometer (Perkin-Elmer SIMAA 6000) equipped with the transversely heated graphite atomizer and longitudinal Zeeman-effect background correction. Pd was used as the chemical modifier along with either the internal furnace gas or a internal furnace gas containing hydrogen and a double stage pyrolysis process. A standard reference material (SRM) of Seronorm™ Trace Elements in urine was used to confirm the accuracy of the method. The optimum conditions for the analysis of urine samples are pyrolysis at 1350 °C (using 5% H₂ v/v in Ar as the inter furnace gas during the first pyrolysis stage and pure Ar during the second pyrolysis stage) and atomization at 2100 °C. The use of Ar and matrix-free standards resulted in concentrations for all the analytes within 85% (As) to 110% (Ni) of the certified values. The recovery for As was improved when mixture of 5% H₂ and 95% Ar (v/v) internal furnace gas was applied during the first step of a two-stage pyrolysis at 1350 °C, and the found values of the analytes were within 91-110% of the certified value. The recoveries for real urine samples were in the range 88-95% for these four elements. The detection limits were 0.78 μg l⁻¹ for As, 0.054 μg l⁻¹ for Mn, 0.22 μg l⁻¹ for Co, and 0.35 μg l⁻¹ for Ni. The upper limits of the linear calibration curve are 60 μg l⁻¹ (As); 12 μg l⁻¹ (Mn); 12 μg l⁻¹ (Co) and 25 μg l⁻¹ (Ni), respectively. The relative standard deviations (R.S.D.s) for the analysis of SRM were 2% or less. The R.S.D.s of a real urine sample are 1.6% (As), 6.3% (Mn), 7.0% (Ni) and 8.0% (Co), respectively.     

Flow analysis-hydride generation-gas phase derivative molecular absorption spectrophotometric determination of antimony in oral homeopathic products ("AntimoniumTartaricum") formulated under alcoholic medium

In this work, a flow analysis-hydride generation-gas phase derivative molecular absorption-(UV) spectrophotometric method has been developed for the direct determination of antimony in aqueous and hydro-alcoholic samples. Antimony (III) from undiluted samples is directly transformed into the gaseous stibine (SbH₃) form by on-line reaction with sodium tetrahydroborate (NaBH₄) in acidic medium (HCl). The gaseous phase generated is separated from the liquid phase using a commercial gas-liquid separator, and swept - with the help of a carrier gas (N₂) stream - into a quartz gas cell (10 cm pathlength); where the corresponding absorption spectrum is acquired in a continuous mode over the 190-300 nm wavelength range, using a conventional spectrophotometer. A derivative strategy was selected in order to avoid the strong spectral interference of the ethanol vapor on the gaseous SbH₃ absorption spectrum. In this way, the peak height at 223 nm of the second order derivative spectrum appears as a clear, clean and interference free analytical signal, which allows the direct determination of antimony. The recovery values obtained from homeopathic formulations (prepared in alcoholic medium) spiked with know amounts of antimony ranged between 97.5 and 103%. The method provides a dynamic range from 0.20 to 30 mg Sb l⁻¹. The precision (RDS), evaluated by replicate analysis (n = 5) of samples and standard solution containing between 2.5 and 15 mg Sb l⁻¹ was in all cases lower than 1.2%. The proposed method was applied to the determination of antimony in commercial homeopathic products (“Antimonium Tartaricum”) prepared in hydro-alcoholic medium; and showed to be simple, precise, and accurate.     

Thermal modified Kaolinite as useful material for separation and preconcentration of trace amounts of manganese ions

This work assesses for the first time the potential of natural Kaolinite as adsorptive material for preconcentration of metal traces. Manganese is quantitatively retained by 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) on thermal modified Kaolinite by column method in pH range of 8.5-10.0 at flow rate of 2 ml min⁻¹. Manganese was removed from column with 5.0 ml of H₂SO₄ 4 mol l⁻¹ and determined by flame atomic absorption spectrometric at 279.5 nm. In this case, 0.l μg of manganese can be concentrated from 800 ml of aqueous sample (where concentration is as low as 0.125 μg l⁻¹). Detection limit is 4.3 μg l⁻¹ (3 δ_bl m⁻¹) and analytical curve is linear in the 0.02-10 mg l⁻¹ in final solution with correlation coefficient 0.9997 and relative standard deviation for eight replicate determination of 5 μg of manganese in final solution is 0.71%. The interference of a large number of anions and cations has been studied in detail to optimize the conditions and method was successfully applied for determination of manganese in complex materials.     

Flow system to gas capture from a nebulized solution

The use of aerosol produced in a nebulization chamber is proposed as an alternative to gas sample capture in flow systems. This paper describes the coupling of a sampling interface with a flow system, for in situ gas monitoring. Aspects related with the behavior of aerosol formation and gas solubilization in liquid drops are discussed. The method is applied to the determination of residual lime in acidic soils. Aliquots of 5.0 ml of 1.0 mol l⁻¹ HCl were mixed with soil samples (1 g). The CO₂ released from these samples was captured by a nebulized aerosol and determined conductivity. The analytical curve from 1.0×10⁻² to 5.0×10⁻² mol kg⁻¹ CaCO₃ was ploted applying the matrix matching approach. This proposition, allowed an increase in the sensibility with detection limit of 6.0×10⁻³ mol kg⁻¹. The precision was good (R.S.D. <3%) for an analytical frequency of 22 determinations per hour. A fair agreement, at 95% confidence level, was found between the results from the proposed method and certified values of the investigated samples.     

Voltammetric determination of chloramphenicol in milk at electrochemically activated carbon fibre microelectrodes

Electrochemical activation of cylindrical carbon fibre microelectrodes (CFMEs) by repetitive square-wave (SW) voltammetric scans between 0.0 and +2.6 V has shown to increase dramatically the cathodic current of chloramphenicol (CAP). This is attributed to the increase of the carbon fibre surface area due to its fracture and the appearance of deep fissures along the main fibre axis. Cyclic voltammograms of CAP suggested a contribution to the total current from most likely thin-layer electrolysis. The current density:concentration ratio calculated for the reduction of CAP at an activated fibre was 6.5×10⁷ μA cm⁻² mol⁻¹ l. A method for the determination of CAP at low concentrations levels, using SW voltammetry at electrochemically activated cylindrical microelectrodes, was developed. Different chemical and electrochemical variables involved in the activation step were optimised. Calibration graphs were linear (r=0.9990) in the 1.0×10⁻⁷ to 1.0×10⁻⁵ mol l⁻¹ concentration range, with a slope of (2.69+0.03) × 10⁵ μA mol⁻¹ l. A limit of detection of 4.7×10⁻⁸ mol l⁻¹ (15 ng ml⁻¹) was found. The SWV method was applied for the determination of CAP in milk samples spiked with the antibiotic at two concentration levels: 64 and 320 ng ml⁻¹. Recoveries >97% were obtained in all cases by following a very simple experimental procedure.     

Electrochemical studies and square wave stripping voltammetry of five common pesticides on poly 3,4-ethylenedioxythiophene modified wall-jet electrode

The cyclic voltammetric behavior of five common pesticides such as dicofol (DCF), cypermethrin (CYP), monocrotophos (MCP), chlorpyrifos (CPF) and phosalone (PAS) was investigated at a poly 3,4-ethylenedioxythiophene modified glassy carbon electrode (PEDOT/GCE). A method was developed for the detection and determination of these pesticides in trace level flowing stream, based on their redox behavior. The square wave stripping voltammetric principle was used to analyze the selected pesticides on PEDOT/GCE. Varying the accumulation potential and accumulation time, the best accumulation conditions were found out. Effects of initial scan potential, square wave pulse amplitude, step potential and frequency were examined for the optimization of stripping conditions. The peak current responses of analyte under optimum conditions were correlated over flow rate by using wall-jet PEDOT/GCE assembly. The calibration plots were linear over the pesticide's concentration range 0.10-72.60 μg l⁻¹ for DCF, 0.41-198.24 μg l⁻¹ for CYP, 0.22-220.95 μg l⁻¹ for MCP, 0.35-259.69 μg l⁻¹ for CPF and 1.07-141.46 μg l⁻¹ for PAS. The limit of detection was obtained between <0.09 and <1.0 μg l⁻¹ for five pesticides. It is low enough for trace pesticide determination in real samples. This method is applied for the determination of the five pesticides in soil samples. The recovery values obtained in spiked soil samples are 95.4 ± 5.4% for DCF, 93.7 ± 4.2% for CYP, 85.3 ± 8.4% for MCP, 94.6 ± 6.6% for CPF and 93.5 ± 4.9% for PAS.