Determination of Nitrobenzene in Wastewater Using a Hanging Mercury Drop Electrode

The determination of trace amount nitrobenzene in wastewater on a hanging mercury drop electrode was studied. The determination conditions of pH, supporting electrolyte, accumulation potential, accumulation time, and voltammetric response were optimized. The sharp peak of the nitrobenzene was appeared at 0.05 V. The peak electric current was proportional to the concentration of nitrobenzene in the range of 1.47 × 10⁻⁵ ∼ 1.0 × 10⁻³ mol/l with relative standard deviations of 3.99 ∼ 8.94%. The detection limit of the nitrobenzene in water was 5 × 10⁻⁶ mol/l. The proposed method offered low limit of determination, easy operation, the use of simple instrumentation, high sensitivity and good reproducibility. It was applied to the determination of nitrobenzene in wastewater with an average recovery of 94.0% ∼ 105%. The proposed method provided fast, sensitive and sometimes real time detection of nitrobenzene.     

Facile and Sensitive Spectrophotometric Determination of Carbosulfan in Formulations and Environmental Samples

Facile, selective and sensitive spectrophotometric method has been developed for the determination of carbosulfan in insecticidal formulations, fortified water, food grains, agriculture wastewater and soil samples with newly synthesized reagents. The method was based on acid and alkaline hydrolysis of the carbosulfan pesticide, and the resultant hydrolysis product of carbosulfan was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with λ _max of 464 nm or interaction with 2,6-dibromo-4-nitroaniline to produce yellow colored product with λ _max of 408 nm or coupling with 2,4,6-tribromoaniline to form red colored product has a λ _max of 471 nm. Under optimal conditions, Beer’s law range for 2,6-dibromo-4-methylaniline (DBMA) was found to be 0.2–12.0 μg ml⁻¹, 0.6–16.0 μg ml⁻¹ for 2,6-dibromo-4-nitroaniline (DBNA) and 0.4–15.0 μg ml⁻¹ for 2,4,6-tribromoaniline (TBA). The molar absorptivity of the color systems were found to be 3.112 × 10⁴ l mol⁻¹ cm⁻¹ for DBMA, 3.214 × 10⁴ l mol⁻¹ cm⁻¹ for DBNA and 3.881 × 10⁴ l mol⁻¹ cm⁻¹ for TBA. Sandell’s of the color reactions are 0.013 μg cm⁻² (DBMA), 0.012 μg cm⁻² (DBNA) and 0.011 μg cm⁻² (TBA) respectively. The effect of the non-target species on the determination of carbosulfan was studied to enhance the selectivity of the proposed methods. The formation of colored derivatives with the coupling agents is instantaneous and stable for 28, 30, and 26 h. Performance of the proposed methods were compared statistically in terms Student’s F and t-tests with the reported methods. An erratum to this article can be found at     

Selective and sensitive extractive spectrophotometric determination of micro amounts of palladium(II) in spiked samples: using a new reagent N-ethyl-3-carbazolecarbaxaledehydethiosemicarbazone

N-Ethyl-3-cabazolecarboxaldehydethiosemicarbazone (ECCT) is proposed as a new, sensitive and selective complexing reagent for the separation and extractive spectrophotometric determination of palladium(II) at pH: 4.0 to form a yellowish orange colored 1:1 chelate complex, which is very well extracted in to n-butanol. The absorbance was measured at a maximum wavelength, 410 nm. This method obeys Beer’s law in the concentration range 0.0–6.6 μg mL⁻¹ and the correlation coefficient of Pd(II)-ECCT complex is 0.998, which indicates an excellent linearity between the two variables with good molar absorptivity and Sandell’s sensitivity, 1.647 × 10⁴ l mol⁻¹cm⁻¹, 6.49 × 10⁻³ μg cm⁻², respectively. The instability constant of complex calculated from Edmond’s method, 2.724 × 10⁻⁵ was in good agreement with the value calculated from Asmus’ method 2.624 × 10⁻⁵, at room temperature. The precision and accuracy of the method is checked with calculation of relative standard deviation (n = 5), 0.839. Edmond’s method was observed to be a more selective method in the presence of EDTA, oxalate and phosphate ions. The method was successfully applied for the determination of Pd(II) in water samples, synthetic mixtures and hydrogenation catalysts, employing an atomic absorption spectrometer for comparing these results.     

Differential pulse adsorptive stripping voltammetric determination of simeton in its formulations and vegetables

A sensitive adsorptive stripping voltammetric method for the determination of simeton with universal buffer solution has been described. The method was based on the adsorption accumulation of simeton at a hanging mercury drop electrode. The overall reduction process is under controlled diffusion. The adsorptive peak was observed at ?0.8 V vs SCE in acidic solution 2 < pH < 6. The peak response was characterized with respect to pH, accumulation potential, time, and scan rate. The calibration plot was found to be linear from 1.13 × 10^???5 to 3.5 × 10^???8 M with a limit of detection of 2.0 × 10^???8 M. Finally, the method has been applied for the determination of simeton in its formulations and vegetable samples.     

Concentrations of cadmium and lead heavy metals in Dardanelles seawater

Cadmium and lead were determined simultaneously in seawater by differential pulse stripping voltammetry (DPSV) preceded by adsoptive collection of complexes with 8-hydroxyquinoline (oxine) on to a hanging mercury drop electrode (HMDE). In preliminary experiments the optimal analytical condition for oxine concentration was found to be 2.10⁻⁵ M, at pH 7.7, the accumulation potential was −1.1 V, and the initial scannig potential was −0.8 V. The peak potentials were found −0.652 V for Cd and −0.463 V for Pb At the 60 s accumalation time. The limit of detection (LOD) and limit of quantitatification (LOQ) were found to be by voltammetry as 0.588 and 1.959 μg l⁻¹ (RSD, 5.50%) for Cd and 0.931 and 3.104 μg l⁻¹ (RSD, 4.10%) for Pb at 60 s stirred accumulation time respectively. In these conditions the most of the seawater samples are amenable for direct voltammetric determination of cadmium and lead using a HMDE. An adsorptive stripping mechanism of the electrode reaction was proposed. For the comparison, seawater samples were also analysed by ICP-atomic emission spectrometry method (ICP-AES). The applied voltammetric technique was validated and good recoveries were obtained.     

Development of simple and sensitive spectrophotometric method for the determination of bendiocarb in its formulations and environmental samples

Facile, selective and sensitive spectrophotometric method has been developed for the determination of bendiocarb in its insecticidal formulations, fortified water, food grains, agriculture wastewater and agriculture soil samples with prepared reagents. The method was based on alkaline hydrolysis of the bendiocarb pesticide, and the resultant hydrolysis product of bendiocarb was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with λmaxof457 nmorcouplingwith2, 6−dibromo−4−nitroanilinetoproducearedcoloredproductwithλ_max of474~nmorcouplingwith2, 4, 6−tribromoanilinetoformorangeredcoloredproducthasaλ_max of465 nm.Underoptimalconditions, Beer'slawrangefor2, 6−dibromo−4−methylaniline(DBMA)wasfoundtobe0.6−−14.0~μgmL ^-1, 0.8−−10.0 μgmL ^-1 for2, 6−dibromo−4−nitroaniline(DBNA)and0.4−−10.0 μgmL ^-1 for2, 4, 6−tribromoaniline(TBA).Themolarabsorptivityofthecolorsystemswerefoundtobe4.126~×~10⁴ lmol ^-1 cm ^-1 forDBMA, 3.254×10⁴ l~mol ^-1 cm ^-1 forDBNAand2.812×10⁴ lmol ^-1 cm ^-1 forTBA.Sandell'softhecolorreactionsare0.018 μgcm ^-2(DBMA), 0.052 μgcm ^-2(DBNA)and0.065 μgcm ^-2$ (TBA) respectively. The effect of the non-target species on the determination of bendiocarb was studied. The formation of colored derivatives with the coupling agents is instantaneous and stable for 18 h, 30 h, and 12 h. Performance of the proposed methods were compared statistically in terms Student's F and t-tests with the reported methods.     

Water quality assessment: surface water sources used for drinking and irrigation in Zaria,Nigeria are a public health hazard

We assessed the quality and pollution status of source surface waters in Zaria, Nigeria by monitoring the nature, cause and extent of pollution in Samaru stream, Kubanni River and Kubanni dam over a period of 10 months, between March and December 2002. A total of 228 water samples was collected from 12 sites and analysed for a total of ten physicochemical and one bacteriological quality indicators, using standard methods. Aesthetic water quality impairment parameters were also observed. The mean values of most water quality parameters were significantly higher (P < 0.05) in both the stream and river than in the dam. There was no significant correlation between faecal coliform counts (FCC) and water temperature (in the range 15–33°C); pH (5.77–7.32); and turbidity (1.4–567 NTU). The high FCC ranged from 2.0 × 10¹ to 1.6 × 10⁶ MPN/100 ml and exceeded the WHO standards for drinking water and water used for fresh-produce irrigation, and correlated positively (P < 0.05) with conductivity (in the range 68–1,029 μS/cm); TDS (10.0–70.0 mg/l); TSS (10.0–70.0 mg/l); Cl (7.5–181 mg/l); PO₄⁻P (0.01–0.41 mg/l); NO₃⁻N (0.6–3.8 mg/l) and BOD₅ (0.1–14.9 mg/l). The main pollution sources were municipal wastewater, stormwater runoffs, the ABU sewage treatment plant, abattoir effluents and irrigation farms treated with chemical fertilisers. We conclude that these water bodies are potentially hazardous to public health and that proper sewage treatment and river quality monitoring are needed to warn against hazards to public health.     

Biofilms coating Schoenoplectus californicus as indicators of water quality in the Río de la Plata Estuary (Argentina)

N-ethyl-3-carbazolecarboxaldehyde-3-thio- semicarbazone (ECCT) as an new analytical reagent used for the development of a highly sensitive extractive spectrophotometric method for the determination of copper(II). The ECCT forms a greenish-yellow colored 1:1 (M:L) complex with copper(II) at pH 3.0, which is well extracted into n-butanol and shows maximum absorbance at 380nm. The color of the complex is stable for more than forty eight hours. The system obey Beer's law in the range 0.4–3.6 with 2.243 × 10⁴lmol⁻¹cm⁻¹, 2.83 × 10^-3μgcm⁻² molar absorptivity and Sandell's sensitivity respectively. The regression coefficient is 0.412 with 0.99 correlation coefficient. The precision and accuracy of the method was checked by finding the relative standard deviation (0.422%). This developed method has been successfully employed for the determination of copper(II) in environmental and pharmaceutical samples. The method is evaluated by analyzing samples from the bureau of analyzed samples (BCS 233, 266, 216/1, 207 and 179) and by inter comparison of experimental values using AAS.     

Spatio-Temporal Fluxes in Particulate Organic Carbon in a Tropical Coastal Lagoon

Temporal and spatial variations in particulate organic carbon (POC) in relation to primary production, chlorophyll a, phaeophytin, plankton abundance, secondary production and suspended particulate matter (SPM) were studied monthly for 1 year from April 1996 to March 1997 in a shallow tropical coastal lagoon on the southwest coast of India. Though temporal variations in all components were significant, spatial variabilities were not statistically significant. POC values range from 200 to 5690 mg C m³ h⁻¹, while primary production, chlorophyll a, and phaeophytin varied between 0.02 and 14.53 mg C m⁻³ h⁻¹, 0.87 and 23.11 mg m⁻³ and 3.02 and 30.581 mg m⁻³, respectively. Phytoplankton and zooplankton abundance varied from 0.01 to 655.5×10⁵ no m⁻³ and negligible to 7.08×10⁵ no m⁻³ respectively; secondary production from 10 to 490 mg C m⁻³ and SPM between 0.38 and 74.43×10⁴ mg m⁻³ during this study. Temporally, postmonsoon months were observed to have the highest concentrations of POC in the lagoon waters. The bulk of the POC pool in the lagoon was composed of secondary producers (72%), followed by chlorophyll a (21%), phaeophytin (7%) and suspended particulate matter of inorganic origin (< 0.1%).     

Application of a Larval Medaka Assay to Evaluate the Fish Safety Level in Sagami River, Japan

Physico-chemical characteristics of some river and hand-dug well waters used for drinking and domestic purposes in the oil rich Niger Delta area of Nigeria were assessed using standard methods. The concentrations of the parameters in the river water samples ranged in the following order: pH (5.6–6.9), temperature (26.90–28.60°C), turbidity (23–63 NTU), electrical conductivity (52–184 μs/cm), DO (5.4–7.2 mg/l), BOD (21–57 mg/l), TDS (6.0–217 mg/l), PO₄ ³⁻ (0.19–1.72 mg/l), SO₄ ²⁻ (25–36.8 mg/l), NO₃ ⁻ (20.3–28 mg/l), Fe (6.07–15.71 mg/l), Zn (0.04–0.24 mg/l), Pb (0.01–0.17 mg/l), Ni (0.01–0.13 mg/l), Vn (0.01–0.20 mg/l) and Hg (0.001–0.002 mg/l). The concentrations of these parameters in the hand-dug well water ranged in the following order: pH (5.7–6.8) temperature (26–30°C), turbidity (134–171 NTU), electrical conductivity (160–340 μs/cm), DO (5.4–6.4 mg/l), BOD (13–34 mg/l), TDS (110–190 mg/l), PO₄ ³⁻ (0.84–1.84 mg/l), SO₄ ²⁻ (10.6–28.1 mg/l), NO₃ ⁻ (11.3–23 mg/l), Fe (13.17–16.31 mg/l), Ni (0.01–0.02 mg/l), Vn (0.01–0.04 mg/l) and Hg (0.001–0.004 mg/l). The concentrations of BOD, turbidity, NO₃ ⁻ and Fe in the water samples were above WHO and FMENV permissible limits for safe drinking water. The results suggest that the use of such waters for drinking and domestic purposes pose a serious threat to the health of the users and calls for the intervention of government agencies.