Cloud point extraction for the determination of cadmium and lead employing sequential multi-element flame atomic absorption spectrometry

A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30?µg?L^?1 and 2.6?µg?L^?1, respectively. A precision expressed as relative standard deviation (RSD, n?=?10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10?µg?L^?1 and 30?µg?L^?1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10?µg?L^?1 and 30?µg?L^?1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.     

Determination of total antimony(III,V) by square-wave anodic stripping voltammetry with in situ plated bismuth-film electrode

A sensitive and reliable method is described for the determination of total Sb(III,?V) at traces levels by Osteryoung square-wave anodic stripping voltammery (OSWASV). This method is based on the co-deposition of Sb(III,?V) with Bi(III) onto an edge-plane pyrolytic graphite substrate at an accumulation step. OSWASV studies indicated that the co-deposited antimony was oxidised with anodic scans to give an enhanced anodic peak at about 450?mV vs. Ag/AgCl (sat. KCl). The anodic stripping peak current was directly proportional to the total concentration of antimony in the ranges of 0.01–0.10?µg?L^?1, 0.10–1.0?µg?L^?1 and 1.0–18.0?µg?L^?1 with correlation coefficient higher than 0.995 when 2.0?mol?L^?1 hydrochloric acid was used. The detection limits calculated as S/N?=?3 was 5.0?ng?L^?1 in 2.0?mol?L^?1 hydrochloric acid at 180?s deposition time. The relative standard deviation was 5% (n?=?6) at 0.10?µg?L^?1 level of antimony. The analytical results demonstrate that the proposed method is applicable to analyses of real water samples.     

Screen-printed electrodes incorporated in a flow system for the decentralized monitoring of lead,cadmium and copper in natural and wastewater samples

Mercury-based screen-printed electrodes (SPE) combined with square-wave anodic stripping voltammetry (SWASV) techniques for the analysis of copper, cadmium, lead, and zinc in different water samples have been applied. The detection system has been implemented in a flow cell and different experimental conditions have been tested in view of its application for in-situ monitoring. In particular, an acetate buffer together with a low chloride concentration (0.025?M NaCl) provided best performance and reproducible results. Additionally, the flow system was validated for the first time in terms of limits of detection, linearity, repeatability and recovery. Limits of detection of 2.8?µg?L^?1, 4.1?µg?L^?1, and 7.5?µg?L^?1 for cadmium, lead and copper respectively and repeatabilities lower than 10% (as RSD) were found. Good recoveries have been obtained for the three cations and in particular for copper, even in the presence of zinc. Finally, the method has shown its efficiency for the rapid screening of lead, cadmium and copper contained in both natural waters and wastewater samples.     

Sorbent separation and enrichment method for cobalt ions determination by graphite furnace atomic absorption spectrometry in water and urine samples using multiwall carbon nanotubes

A new cobalt ions pre-concentration method, optimised by fractional factorial design, using multiwall carbon nanotubes (MWCNTs) with further Graphite Furnace Atomic Absorption Spectrometry (GFAAS) quantification is described. The method explores the high chemical and physical stability of MWCNTs for improving the detectability of GFAAS. It is based on off-line pre-concentration of 20.0 mL of sample previously buffered (pH 8.82) on MWCNTs at a flow rate of 10.0 mL min^?1. After the pre-concentration procedure, the elution step was carried out with 500 µL of 0.524 mol L^?1 HNO₃ solution at a flow rate of 2.0 mL min^?1. Fractional factorial designs and response surface methodology were employed for optimisation of all chemical parameters involved in the pre-concentration procedure, including pre-concentration flow rate, buffer and eluent concentration, sample pH and elution volume. The method provides a linear calibration range from 0.03 up to 7.00 µg L^?1 with linear correlation coefficient higher than 0.9994 and limits of detection and quantification of 0.01 and 0.03 µg L^?1, respectively. Repeatability of the six measurements was found to be 2.38 and 1.84% for 0.3 and 4.5 µg L^?1 cobalt concentration, respectively. By pre-concentrating 20.0 mL of sample, a pre-concentration factor (PF) of 19.10-fold and a consumption index of 1.05 mL were obtained. The pre-concentration efficiency (PE) was found to be 9.55 min^?1. The proposed method was successfully applied for the pre-concentration and determination of cobalt in water and urine samples with satisfactory recovery values.     

Determination of antimony(III) and (V) in natural water by cathodic stripping voltammetry with in-situ plated bismuth film electrode

A method is described for the sequential determination of Sb(III) and Sb(V) using Osteryoung square wave cathodic stripping voltammetry. It employs an in-situ plated bismuth-film on an edge-plane graphite substrate as the working electrode. Selective electro-deposition of Sb(III)/Sb(V) is accomplished by applying a potential of ?500 mV vs. Ag/AgCl, followed by reduction to stibine at a more negative potential in the stripping step. Stripping was carried out by applying a square wave waveform between ?500 and ?1400 mV to the antimony deposited. The stripping peak current at ?1150 mV is directly proportional to the concentration of Sb( III)/Sb(V). The calibration plots for Sb (III) were linear up to 12.0?µg L^?1 depending on the time of deposition. The calibration plots for Sb (V) were linear up to 7.0?µg L^?1, also depending on the time of deposition. The relative standard deviation in the determination of 0.1?µg L^?1 of Sb(III) is 4.0% (n?=?5), and the limit of detection is as low as 2 ng L^?1. In case of 0.1?µg L^?1 Sb(V), the relative standard deviation is 3.0% (n?=?5) and the detection limit also is 2 ng L^?1. The method was applied to the analysis of river and sea water samples.     

Ligandless-ultrasound-assisted emulsification microextraction followed by inductively coupled plasma-optical emission spectrometry for simultaneous determination of heavy metals in water samples

In this study, a simple and efficient method of ligandless-ultrasound-assisted emulsification microextraction (LL-USAEME) followed by inductively coupled plasma-optical emission spectrometry (ICP-OES) has been developed for simultaneous extraction, preconcentration and determination of manganese, cadmium, cobalt and nickel in water samples. In the proposed approach, tetrachloroethylene was selected as extraction solvent. The effect of important experimental factors such as volume of extraction solvent, pH, sonication time, salt concentration, and temperature was investigated by using a fractional factorial design (2^5?1) to identify important factors and their interactions. In the next step, a Box-Behnken design (BBD) was applied for optimisation of significant factors. The obtained optimal conditions were: 30?µL for extraction solvent, 12 for pH, 5?min for sonication time, and 5% w/v for salt concentration. The limits of detections (LODs) for Cd(II), Co(II), Mn(II) and Ni(II) were 0.20, 0.13, 0.21 and 0.28?µg?L^?1, respectively. Relative standard deviations (RSD, C?=?200.0?µg?L^?1, n?=?9) were between 3.4–7.5% and the calibration graphs were linear in the range of 0.25 to 1000.0?µg?L^?1 for Mn, 0.5–1000.0?µg?L^?1 for Co and Ni and 1.0–250.0?µg?L^?1 for Cd. The determination coefficients (R ²) of the calibration curves for the analytes were in the range of 0.993 to 0.999. The proposed method was validated by using two certified reference materials, and also the method was applied successfully for the determination of heavy metals in different real water samples.     

Sequential Voltammetric Determination of Uranium,Cadmium and Lead by Using the ex situ Bismuth Film Electrode: Application to Phosphate Fertilizers

A sequential voltammetric procedure for the determination of uranium, cadmium and lead was investigated at an ex situ bismuth film electrode (BiFE). First, the adsorptive stripping voltammetry was applied to assay the U(VI)‐cupferron complex in the differential pulse mode (detection limit of 1.0 µg L^?1, 200 s accumulation time). Through the manipulation of the same aliquot of the sample, efforts were made to quantify cadmium and lead by square wave anodic stripping voltammetry. Detection limits of 2.03 µg L^?1 for Cd (II) and 2.43 µg L^?1 for Pb (II) were calculated (100 s accumulation time). The methodology was successfully applied to phosphate fertilizer samples after open vessel wet decomposition (HNO₃/H₂O₂). The following value ranges were evaluated: U (VI) 37.2–150 mg kg^?1, Pb (II) 78.3–204 mg kg^?1 and Cd (II) 44.1–71.6 mg kg^?1. Validation was performed by using the standard reference materials SRM‐695 – phosphate fertilizer – and SRM‐1643e – water.     

Rapid and sensitive determination of biphenyl and biphenyl oxide in water samples using dispersive liquid–liquid microextraction followed by gas chromatography

A rapid and sensitive method has been developed for the determination of biphenyl and biphenyl oxide in water samples using dispersive liquid–liquid microextraction followed by gas chromatography. This method involves the use of an appropriate mixture of extraction solvent (8.0?µL tetrachloroethylene) and disperser solvent (1.0?mL acetonitrile) for the formation of cloudy solution in 5.0?mL aqueous sample containing biphenyl and biphenyl oxide. After extraction, phase separation was performed by centrifugation and biphenyl and biphenyl oxide in sedimented phase (5.0?±?0.3?µL) were determined by gas chromatography-flame ionisation (GC-FID) system. Type of extraction and disperser solvents and their volumes, salt effect on the extraction recovery of biphenyl and biphenyl oxide from aqueous solution have been investigated. Under the optimum conditions and without salt addition, the enrichment factors for biphenyl and biphenyl oxide were 819 and 785, while the extraction recovery were 81.9% and 78.5%, respectively. The linear range was (0.125–100?µg L^?1) and limit of detection was (0.015?µg?L^?1) for both analytes. The relative standard deviation (RSD, n?=?4) for 5.0?µg?L^?1 of analytes were 8.4% and 6.7% for biphenyl and biphenyl oxide, respectively. The relative recoveries of biphenyl and biphenyl oxide from sea, river water and refined water (Paksan company) samples at spiking level of 5.0?µg?L^?1 were between 85.0% and 100 %.     

Enhanced Specificity and Sensitivity for the Determination of Nickel(II) by Square-wave Adsorptive Cathodic Stripping Voltammetry at Disposable Graphene-modified Pencil Graphite Electrodes

Chemical sensors relying on graphene-based materials have been widely used for electrochemical determination of metal ions and have demonstrated excellent signal amplification. This study reports an electrochemically reduced graphene oxide (ERGO)/mercury film (HgF) nanocomposite-modified pencil graphite electrode (PGE) prepared through successive electrochemical reduction of graphene oxide (GO) sheets and an in situ plated HgF. The ERGO-PG-HgFE, in combination with dimethylglyoxime (DMG) and square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV), was evaluated for the determination of Ni²⁺ in tap and natural river water samples. A single-step electrode pre-concentration approach was employed for the in situ Hg-film electroplating, metal-chelate complex formation, and non-electrolytic adsorption at –0.7 V. The current response due to nickel-dimethylglyoxime [Ni(II)-DMG₂] complex reduction was studied as a function of experimental paratmeters including the accumulation potential, accumulation time, rotation speed, frequency and amplitude, and carefully optimized for the determination of Ni²⁺ at low concentration levels (μg?L^?1) in pH 9.4 of 0.1 M NH₃–NH₄Cl buffer. The reduction peak currents were linear with the Ni²⁺ concentration between 2 and 16?μg?L^?1. The limits of detection and quantitation were 0.120?±?0.002?µg?L^?1 and 0.401?±?0.007?µg?L^?1 respectively, for the determination of Ni²⁺ at an accumulation time of 120?s. The ERGO-PG-HgFE further demonstrated a highly selective stripping response toward Ni²⁺ determination compared to Co²⁺. The electrode was found to be sufficiently sensitive to determine metal ions in water samples at 0.1?µg?L^?1, well below the World Health Organization standards.     

Speciation analysis of inorganic vanadium (V(IV)/V(V)) by graphite furnace atomic absorption spectrometry following ion-exchange separation

A sensitive and simple method of ion-exchange resin separation and graphite-furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of inorganic vanadium species. Methylene Blue (MB) was used as a chelating agent of V(V) for ion-exchange separation. The complex of V(V) and MB could be trapped by ion-exchange resin at pH 3.0 and eluted by 1.0?mol?L^?1 NaOH. The vanadium species was determined subsequently by GFAAS. The concentration of V(IV) was calculated by subtracting the V(V) concentration from the total concentration of vanadium. Under the optimized experimental conditions, the detection limit of V(V) is 0.48?µg?L^?1 with RSD of 2.6% (n?=?5, c?=?2.0?µg?L^?1). In order to verify the accuracy of the method, a certified reference soil sample was analyzed, and the results obtained were in good agreement with the certified values. The range of recovery for V(IV) and V(V) was 97.8–99.3% and 101.7–103.6%, respectively. The proposed method was applied to the speciation analysis of vanadium in lake-water samples.     

Dispersive liquid phase micro-extraction of aromatic amines in environmental water samples

A new, rapid and sensitive method for the determination of aromatic amines such as o-nitroaniline (NIT), alpha-naphtylamine (NAP), o-chloroaniline (CHL) in environmental water samples was developed with dispersive liquid phase micro-extraction coupled with high performance liquid chromatography. Preliminary experiments indicated that excellent achievements were obtained when chlorobenzene and acetonitrile were employed as the extraction solvent and dispersive solvent, respectively. Some other parameters that would have important effect on the pre-concentration of aromatic amines were investigated in detail. Under the optimal conditions, the method had excellent linear relationship between the peak area and the concentration for NIT, NAP and CHL in the concentration range of 1?～?50?µg?L^?1. The limits of detection and precisions of the proposed method were in the range of 0.1?～?0.7?µg?L^?1 and 6.3?～?9.7%, respectively. The proposed method has been validated with two real water samples, and the results showed that excellent spiked recoveries in the range of 92.8%?～?111.5% were achieved. All these demonstrated that the proposed method would be very useful and applicable for the determination of such pollutants in the future.     

Determination of trace chromium(VI) by an inhibition-based enzyme biosensor incorporating an electropolymerized aniline membrane and ferrocene as electron transfer mediator

A novel inhibition-based glucose oxidase (GOx) biosensor for environmental chromium(VI) detection is described. An electropolymerized aniline membrane has been prepared on a platinum electrode containing ferrocene as electron transfer mediator, on which GOx is cross-linked by glutaraldehyde. The mechanism of the redox reaction on the electrode and the performance of the sensor are studied. The sensor's response to glucose decreases when it is inhibited by chromium(VI), with a lower detection limit of 0.49?µg?L^?1, and the linear response range is divided into two parts, one of which is 0.49–95.73?µg?L^?1 and the other is 95.73?µg^?1 to8.05?mg?L^?1. The enzyme membrane is shown to be completely reactivated after inhibition, retaining 90% activity over more than forty days. Interference to chromium(VI) determination from lead(II), copper(II), cadmium(II), chromium(III), cobalt(II), tin(II) and nickel(II) is found to be minimal, while high concentrations of mercury(II) and silver(I) may interfere with the determination of trace chromium(VI). The sensor has been used for chromium(VI) determination in soil samples with good results.     

Synthesis of 2-mercaptobenzothiazole/magnetic nanoparticles modified multi-walled carbon nanotubes for simultaneous solid-phase microextraction of cadmium and lead

This study describes the successful sequential modification of multi-walled carbon nanotube (MWCNT) by Fe₃O₄ magnetic nanoparticles and 2-mercaptobenzothiazole (MBT) followed by its application as a novel sorbent for simultaneous magnetic solid phase microextraction of lead and cadmium. Fourier transform infrared spectroscopy and scanning electron microscopy were employed to confirm the chemical surface modification of the MWCNT. The ions retained on the 2-MBT/magnetic nanoparticles modified MWCNTs were eluted with 1.0 mL of nitric acid (0.8 mol L^?1) in methanol solution and determined by the flame atomic absorption spectrometry. All parameters affecting the extraction condition were thoroughly investigated and optimised. Under the optimised condition preconcentration factor of 150.0, enhancement factors of 149.0 and 149.2 and limits of detection of 0.21 and 0.01 µg L^?1 were achieved for lead and cadmium, respectively. Using the prepared magnetic nanocomposite, the possible interference of other common ions associated with lead and cadmium determination was effectively avoided and the method was successfully applied to the simultaneous determination of the target ions in various environmental water samples.     

Ultrasound-assisted emulsification microextraction using low density solvent for analysis of toxic nitrophenols in natural waters

An ultrasound-assisted emulsification microextraction (USAEME) based on low-density solvents was successfully applied for the extraction and pre-concentration of four toxic nitrophenols in water samples. The extracted analytes were analyzed by high-performance liquid chromatography-UV detection. The important parameters influencing the extraction efficiency were studied and optimized utilizing two different optimization methods: one variable at a time (OVAT) and central composite design (CCD). The results showed that the emulsification process can be completed in a few seconds using low-density solvents, but almost 10–20?min is necessary for high-density solvents. Under the optimum conditions (extraction solvent, 1-octanol; extraction solvent volume, 40?µL; sample pH, 3.0; salt concentration, 20% (w/v) NaCl; extraction temperature, 40 (±3)°C), limits of detection of the method were in the range of 0.25 to 1?µg?L^?1 and the repeatability and reproducibility of the proposed method, expressed as relative deviation, varied in the range of 2.2–4.2% and 4.7–6.9%, respectively. Linearity was found to be in the range of 1 to 200?µg?L^?1 and the preconcentration factors (PFs) were between 77 and 175. The relative recoveries of the four nitrophenols from water samples at spiking level of 10.0?µg?L^?1 were in the range of 92.0 to 115.0%.     

Determination of phosphate in freshwater samples by flow-injection with lucigenin chemiluminescence

Lucigenin chemiluminescence (CL) in conjunction with flow-injection analysis (FIA) is used for the determination of phosphate in freshwater samples. The procedure is based on the formation of molybdophosphoric heteropoly acid (MoP–HPA) by the reaction of phosphate and ammonium molybdate under acidic conditions. CL emission was observed as a result of oxidation of lucigenin in aqueous sodium hydroxide solution in the presence of MoP–HPA. Calibration was linear up to 500?µg?L^?1 (r ^2?=?0.9998; n?=?8), with a detection limit (S/N?=?3) of 0.95?µg?L^?1. An injection throughput of 120 h^?1, and relative standard deviation (RSD; n?=?4) of 1.3–3.2% were achieved in the concentration range studied. An on-line chelating column was used to remove interfering cations. The method was applied to freshwater samples, and the results (51?±?1.0 – 107?±?2.0?µg?L^?1) did not differ significantly from results obtained using a spectrophotometric method (52.5?±?1.0 – 102?±?2.0?µg?L^?1) at 95% confidence level (t-test).     

Solid phase extraction and diffusive gradients in thin films techniques for determination of total and labile concentrations of Cd(II), Cu(II), Ni(II) and Pb(II) in Black Sea water

Total dissolved and labile concentrations of Cd(II), Cu(II), Ni(II) and Pb(II) were determined at six locations of the Bourgas Gulf of the Bulgarian Black Sea coast. Solid phase extraction procedure based on monodisperse, submicrometer silica spheres modified with 3-aminopropyltrimethoxysilane followed by the electrothermal atomic absorption spectrometry (ETAAS) was developed and applied to quantify the total dissolved metal concentrations in sea water. Quantitative sorption of Cd, Cu, Ni and Pb was achieved in the pH range 7.5–8, for 30?min, adsorbed elements were easily eluted with 2?mL 2?mol?L^?1 HNO₃. Since the optimal pH for quantitative sorption coincides with typical pH of Black Sea water (7.9–8.2), on-site pre-concentration of the analytes without any additional treatment was possible. Detection limits achieved for total dissolved metal quantification were: Cd 0.002?µg?L^?1, Cu 0.005?µg?L^?1, Ni 0.03?µg?L^?1, Pb 0.02?µg?L^?1 and relative standard deviations varied from 5–13% for all studied elements (for typical Cd, Cu, Ni and Pb concentrations in Black Sea water). Open pore diffusive gradients in thin films (DGT) technique was employed for in-situ sampling and pre-concentration of the sea water and in combination with ETAAS was used to determine the proportion of dynamic (mobile and kinetically labile) species of Cd(II), Cu(II), Ni(II) and Pb(II) in the sea water. Obtained results showed strong complexation for Cu and Pb with sea water dissolved organic matter. The ratios between DGT-labile and total dissolved concentrations found for Cu(II) and Pb(II) were in the range 0.2–0.4. For Cd and Ni, these ratios varied from 0.6 to 0.8, suggesting higher degree of free and kinetically labile species of these metals in sea water.     

On-line separation and preconcentration of trace cadmium in environmental water samples by micro column filled with modified nanometer Si-HAP prior to FAAS determination

A novel method of on-line solid phase extraction (SPE) preconcentration has been established for the determination of cadmium in environmental water samples by flame atomic absorption spectrometry (FAAS). The method is based on the on-line retention of cadmium on a micro column of nanometer Silicon Hydroxyapatite (Si-HAP) modified with 1-phenyl-3-methyl-4-bonzoil-5-pyrazone (PMBP) and subsequent elution with 1.0?M thiourea and determination by FAAS. The effect of various parameters that could affect the performance of the system was investigated. The enrichment factor (EF) for cadmium (II) was 250. The limit of detection (LOD) obtained under optimum conditions was 0.28?µg?L^?1 and the relative standard deviation (RSD) for seven replicates at 100?µg?L^?1 Cd²⁺ concentration level was 1.4%. The method was applied to water samples and standard reference materials. The accuracy was assessed through recovery experiments and comparing the results with the accepted values of standard reference material.     

Multi‐Walled Carbon Nanotubes as Sorbent for Flow Injection On‐Line Microcolumn Preconcentration Coupled with Flame Atomic Absorption Spectrometry for Determination of Cadmium and Copper

Abstract

Multi‐walled carbon nanotubes (MWNTs) were used as sorbent for flow injection (FI) on‐line microcolumn preconcentration coupled with flame atomic absorption spectrometry (FAAS) for determination of trace cadmium and copper in environmental and biological samples. Effective preconcentration of trace cadmium and copper was achieved in a pH range of 4.5–6.5 and 5.0–7.5, respectively. The retained cadmium and copper were efficiently eluted with 0.5 mol L^?1 HCl for on‐line FAAS determination. The MWNTs packed microcolumn exhibited fairly fast kinetics for the adsorption of cadmium and copper, permitting the use of high sample flow rates up to at least 7.8 mL min^?1 for the FI on‐line microcolumn preconcentration system without loss of the retention efficiency. With a preconcentration time of 60 sec at a sample loading flow rate of 4.3 mL min^?1, the enhancement factor was 24 for cadmium and 25 for copper at a sample throughput of 45 h^?1. The detection limits (3σ) were 0.30 and 0.11 µg L^?1 for Cd and Cu, respectively. The precision (RSD) for 11 replicate measurements was 2.1% at the 10‐µg L^?1 Cd level and 2.4% at the 10‐µg L^?1 Cu level. The developed method was successfully applied to the determination of trace Cd and Cu in a variety of environmental and biological samples.     

Development of solid-phase extraction method for the determination of aromatic sensitisers in paper mill effluent

In this paper, a procedure for the determination of 11 aromatic hydrocarbon-type sensitisers and their related compounds from water samples, used in the manufacture of thermal paper, is presented. The compounds were extracted using a solid-phase extraction (SPE) cartridge with an octadecyl (C18) or a phenyl-bonded silica (PH) sorbent and then determined by gas chromatography–mass spectrometry (GC–MS). Factors affecting the performance of the extraction steps were thoroughly evaluated, and their effects on the yield of the sample preparation were discussed. Under optimised experimental conditions, SPE cartridges were conditioned with 10?mL hexane followed subsequently by 10?mL methanol, loaded with water sample at 2?mL?min^?1, and eluted with 10?mL hexane at 1.5?mL?min^?1. The limits of detection and quantification, calculated for signal-to-noise ratios of 3 and 10, were in the range of 1–5?µg?L^–1 and 2.5–10?µg?L^–1, respectively. Recovery yields of the present method using river water were in the range of 88%–112% with a C18 sorbent and 86%–116% with a PH sorbent. The repeatability, expressed as a relative standard deviation, was in the range of 2.8%–11% with a C18 sorbent and 0.7%–9.7% with a PH sorbent (n?=?4). Analysis of paper mill effluents revealed the presence of aromatic hydrocarbon-type sensitisers with maximum concentrations of up to 5.2?µg?L^?1.     

Rapid Low-Cost Determination of Lead(II) in Cassava by an iPod-Based Digital Imaging Colorimeter

An iPod-based digital image colorimeter was developed for the determination of lead(II) in cassava. The method is based on the color values of a lead(II) solution following its reaction with dithizone. Lead(II) from cassava was extracted using an ultraviolet-digestion unit followed by the color-forming reaction and image capture using the ColorConc application operated on an iPod touch. The concentration was predicted by comparing the color values with those collected in a database. The time needed for complete digestion was 30?min. The determined concentrations of lead(II) were from 0.10 to 1.00?µg mL^?1. The limits of detection and quantitation were 0.0120 and 0.0399?µg mL^?1, respectively. The recovery values were 105?±?7.07% and 109?±?6.61% at 0.2?µg mL^?1 and 0.4?µg mL^?1 lead(II) (n?=?5). The reported method was demonstrated to be simple, accurate, rapid, precise, and low cost.