Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole and their determination by ICP-OES

A fast, sensitive, and simple method using magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole, as an adsorbent has been successfully developed for extraction, preconcentration, and determination of trace amounts of Ag, Cd, Cu, and Zn from environmental samples. The prepared nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). These magnetic nanoparticles can be easily dispersed in aqueous samples and retrieved by the application of external magnetic field via a piece of permanent magnet. The main factors affecting the extraction efficiency such as pH value, sample volume, eluent concentration and volume, ultrasonication time, and coexisting ions have been investigated and established. Under the optimal conditions, high concentration factors (194, 190, 170, and 182) were achieved for Ag, Cd, Cu, and Zn with relative standard deviations of 5.31%, 4.03%, 3.62%, and 4.20%, respectively. The limits of detection for Ag, Cd, Cu, and Zn were as low as 0.12, 0.12, 0.13 and 0.11 ng mL(-1). The prepared sorbent was applied for preconcentration of trace amounts of Ag, Cd, Cu, and Zn in the various water samples with satisfactory results.     

An ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique combined with a sol-gel process for selective solid-phase extraction of cadmium(II)

A new ion-imprinted thiol-functionalized silica gel sorbent was synthesized by a surface imprinting technique in combination with a sol-gel process for selective on-line, solid-phase extraction of Cd(II). The Cd(II)-imprinted thiol-functionalized silica sorbent was characterized by FT-IR, the static adsorption-desorption experiment, and the dynamic adsorption-desorption method. The maximum static adsorption capacity of the ion-imprinted functionalized sorbent was 284 micromol g(-1). The largest selectivity coefficient for Cd(II) in the presence of Pb(II) was over 220. The static uptake capacity and selectivity coefficient of the ion-imprinted functionalized sorbent are higher than those of the nonimprinted sorbent. The breakthrough capacity and dynamic capacity of the imprinted functionalized silica gel sorbent for 4 mg L(-1) of Cd(II) at 5.2 mL min(-1) of sample flow rate were 11.7 and 64.3 micromol g(-1), respectively. No remarkable effect of sample flow rate on the dynamic capacity was observed as the sample flow rate increased from 1.7 to 6.8 mL min(-1). The imprinted functionalized silica gel sorbent offered a fast kinetics for the adsorption and desorption of Cd(II). The prepared ion-imprinted functionalized sorbent was shown to be promising for on-line, solid-phase extraction coupled with flame atomic absorption spectrometry for the determination of trace cadmium in environmental and biological samples. All competitive ions studied did not interfere with the determination of Cd(II). With a sample loading flow rate of 8.8 mL min(-1) for 45-s preconcentration, an enhancement factor of 56, and a detection limit (3sigma) of 0.07 microg L(-1) were achieved at a sampling frequency of 55 h(-1). The precision (RSD) for 11 replicate on-line sorbent extractions of 8 mug L(-1) Cd(II) was 0.9%. The sorbent also offered good linearity (r = 0.9997) for on-line, solid-phase extraction of trace Cd(II).     

Tris(2-aminoethyl) amine functionalized silica gel for solid-phase extraction and preconcentration of Cr(III), Cd(II) and Pb(II) from waters

A new tris(2-aminoethyl) amine (TREN) functionalized silica gel (SG-TREN) was prepared and investigated for selective solid-phase extraction (SPE) of trace Cr(III), Cd(II) and Pb(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Identification of the surface modification was characterized and performed on the basis of FT-IR. The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III), Cd(II) and Pb(II) onto the SG-TREN were 32.72, 36.42 and 64.61 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 5 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of International Union of Pure and Applied Chemistry, the detection limits (3sigma) of this method for Cr(III), Cd(II) and Pb(II) were 0.61, 0.14 and 0.55 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=11). The application of this modified silica gel to preconcentration trace Cr(III), Cd(II) and Pb(II) of two water samples gave high accurate and precise results.     

On-line preconcentration using a resin functionalized with 3,4-dihydroxybenzoic acid for the determination of trace elements in biological samples by thermospray flame furnace atomic absorption spectrometry

In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L(-1) (Zn) for 60s preconcentration time, at a sample flow rate of 7.0 mL min(-1). Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials.     

Multielemental determination of GEOTRACES key trace metals in seawater by ICPMS after preconcentration using an ethylenediaminetriacetic acid chelating resin

GEOTRACES is an international research project on marine biogeochemical cycles of trace elements and their isotopes. GEOTRACES key trace metals in seawater are Al (8-1000 ng/kg), Mn (4-300 ng/kg), Fe (1-100 ng/kg), Cu (30-300 ng/kg), Zn (3-600 ng/kg), and Cd (0.1-100 ng/kg), of which global oceanic distribution will be determined on a number of research cruises. This work introduces a novel method of solid-phase extraction to determine Al, Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb in seawater by adjusting the pH of the sample to 6 and carrying out a single preconcentration step. The trace metals were collected from approximately 120 mL of seawater using a column of a chelating resin containing the ethylenediaminetriacetic acid functional group and eluted with approximately 15 mL of 1 M HNO3. Mn and Fe in the eluate were measured by inductively coupled plasma mass spectrometry (ICPMS) using the dynamic reaction cell mode, and the other metals were measured using the standard mode. Using this procedure, the trace metals were collected quantitatively, while >99.9% of alkali and alkaline earth metals in seawater were removed. The procedural blank was <7% of the mean concentration in deep ocean waters, except 16% for Pb. The overall detection limit was <14% of the mean concentration in deep ocean waters. The RSD was <9%. Our values for the trace metals in the certified reference materials of seawater NASS-5 and nearshore seawater CASS-4 agreed with the certified values (except that there is no certified value for Al). This method was also successfully applied to the reference materials of open-ocean seawater produced by the SAFe program. Our Fe concentrations were 5.9 +/- 0.7 ng/kg for surface water (S1) and 50.4 +/- 2.9 ng/kg for deep water (D2), which are in agreement with the interlaboratory averages of 5.4 +/- 2.4 and 50.8 +/- 9.5 ng/L, respectively. The data for other metals were oceanographically consistent.     

Determination of trace metals in drinking water using solid-phase extraction disks and X-ray fluorescence spectrometry

A convenient method is described for monitoring Cd, Ni, Cu, and Pb at trace levels in drinking water samples. These metals are preconcentrated on a chelating solid-phase extraction disk and then determined by X-ray fluorescence spectrometry. The method tolerates a wide pH range (pH 6-14) and a large amount of alkaline and alkaline earth elements. The preconcentration factor is well over 1600, assuming a 1 L water sample volume. The limits of detection for Cd, Ni, Cu, and Pb are 3.8, 0.6, 0.4, and 0.3 ng/mL, respectively. These are well below the federal maximum contaminant level values, which are 5, 100, 1300, and 15 ng/mL, respectively. The proposed method has many advantages including ease of operation, multielement capability, nondestructiveness, high sensitivity, and relative cost efficiency. The solid-phase extraction step can be conducted in the field and then the disks can be mailed to a laboratory for the analysis, eliminating the cost of transporting large volumes of water samples. Furthermore, the color of the used extraction disk provides an initial estimate of the degree of contamination for some transition metals (for example, Ni and Cu). Thus, the overall cost for analysis of metals in drinking water can be minimized by implementing the method, and small water supply companies with limited budgets will be better able to comply with the Safe Drinking Water Act.     

Biosorption and preconcentration of lead and cadmium on waste Chinese herb Pang Da Hai

The biosorption behavior of the solid waste Chinese herb Pang Da Hai (seeds of Sterculia lychnophera Hance) was studied as a sorbent for trace lead and cadmium. The solid waste Chinese herb Pang Da Hai has good sorption and desorption properties for Pb and Cd. The sorbed waste Chinese herb Pang Da Hai was both easily eluted with 0.1 mol l(-1) HNO(3) and easily digested with concentrated HNO(3). The extent of adsorption depends on pH, metal concentration, substrate concentration and the presence of interfering ions. The adsorption capacities were found to be 27.1 and 17.5 mg g(-1) for Pb and Cd. The relative standard deviation of the metal uptake experiment was found to be less than 10% for Pb(II) and Cd(II) using 100 microg l(-1) of metal ions and 20 mg substrate. Based on above, an ecofriend and low cost method for Cd and Pb preconcentration and determination with flame atomic absorption spectrophotometry was developed. The method was validated by the analysis of a standard reference material (GBW 08301). The results agree with those quoted by manufactures. It was used for 90-fold preconcentration of Cd and Pb from tap water and river water samples followed by flame atomic absorption spectroscopic (FAAS) determination with satisfactory results.     

A solid phase extraction procedure for Fe3+, Cu2+ and Zn2+ ions on 2-phenyl-1H-benzo[d] imidazole loaded on Triton X-100-coated polyvinyl chloride

A new and efficient solid phase extraction method is described for the preconcentration of trace heavy metal ions. The method is based on the adsorption of Fe(3+), Cu(2+) and Zn(2+) on 2-phenyl-1H-benzo[d] imidazole (PHBI) loaded on Triton X-100-coated polyvinyl chloride (PVC). The influences of the analytical parameters including pH and sample volume were investigated. Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 5 mL of 4 mol L(-1) nitric acid. The preconcentration factor is 90. The detection limits (3 sigma) were in the range of 0.95-1 microg L(-1). The sorbent exhibited excellent stability and its sorption capacity under optimum conditions has been found to be more than 2.7 mg of ions per gram of sorbent. The recoveries of analytes were generally higher than 95%. The relative standard deviations (R.S.D.s) were generally lower than 4%. The method has been successfully applied to some real samples.     

Selective measurement of ultratrace methylmercury in fish by flow injection on-line microcolumn displacement sorption preconcentration and separation coupled with electrothermal atomic absorption spectrometry

A novel nonchromatographic speciation technique for ultratrace methylmercury in biological materials was developed by flow injection microcolumn displacement sorption preconcentration and separation coupled on-line with electrothermal atomic absorption spectrometry (ETAAS). In the developed technique, Cu(II) was first on-line complexed with diethyldithiocarbamate (DDTC), and the resultant Cu-DDTC was presorbed onto a microcolumn packed with the sorbent from a cigarette filter. Selective preconcentration of methylmercury (MeHg) in the presence of Hg(II), ethylmercury (EtHg), and phenylmercury (PhHg) was achieved at pH 6.8 through loading the sample solution onto the microcolumn due to a displacement reaction between MeHg and the presorbed Cu-DDTC. The retained MeHg was subsequently eluted with 50 microL of ethanol and on-line determined by ETAAS. Interferences from coexisting heavy metal ions with lower stability of their DDTC complexes relative to Cu-DDTC were minimized without the need of any masking reagents. No interferences from 5.5 mg L(-1) Cu(II), 4.5 mg L(-1) Cd(II), 2.5 mg L(-1) Cr(III), 3 mg L(-1) Fe(III), 10 mg L(-1) Ni(II), 10 mg L(-1) Pb(II), and at least 25 mg L(-1) Zn(II) were observed for the determination of MeHg at the 50 ng L(-1) level (as Hg). With the consumption of only 3.4 mL of sample solution, an enhancement factor of 75, a detection limit of 6.8 ng L(-1) (as Hg) in the digest (corresponding to 3.4 ng g(-1) in original solid sample for a final 50 mL of digest of 0.1 g of solid material), and a precision (RSD, n = 13) of 2.3% for the determination of methylmercury at the 50 ng L(-1) (as Hg) level were achieved at a sample throughput of 30 samples h(-1). The recoveries of methylmercury spike in real fish samples ranged from 97 to 108%. The developed technique was validated by determination of methylmercury in a certified reference material (DORM-2, dogfish muscle), and was shown to be useful for the determination of methylmercury in real fish samples.     

Synthesis and application of chloromethylated polystyrene modified with 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new sorbent for the on-line preconcentration and determination of copper in water, soil, and food samples by FAAS

In this paper, we report a simple and sensitive on-line solid phase extraction system for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry (FAAS). This method is based upon the on-line retention of copper at pH 5.0 on a minicolumn packed with chloromethylated polystyrene modified by 1-phenyl-1,2-propanedione-2-oxime thiosemicarbazone (PPDOT) as a new solid-phase extraction (SPE) sorbent. The retained Cu(II) ions were eluted with 1.0 M HNO₃, and transported directly to FAAS for determination. Several chemical and flow variables were studied and optimized for a quantitative preconcentration and determination of copper(II). At the optimized conditions, for preconcentration of 10.0 mL of a sample solution, a linear calibration graph was obtained over the concentration range of 3.00-120.0 μg L⁻¹ for Cu(II). The limit of detection (3σ), limit of quantification (10σ), and enrichment factor are 0.56 μg L⁻¹, 2.0 μg L⁻¹ and 41, respectively. The relative standard deviation (n = 6) at 20 μg L⁻¹ of Cu(II) is 2.0%. This method could be applied for determination of trace amounts of Cu(II) in water, soil, and food samples with satisfactory results.     

Membrane solid phase microextraction with alumina hollow fiber on line coupled with ICP-OES for the determination of trace copper, manganese and nickel in environmental water samples

A novel alumina hollow fiber was synthesized by sol-gel template method and was characterized by scanning electron microscopy, N(2) adsorption technique and X-ray diffraction. With the use of prepared alumina hollow fiber as extraction membrane, a new method of flow injection (FI)-membrane solid phase microextraction (MSPME) on-line coupled to inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for simultaneous determination of trace metals (Cu, Mn and Ni) in environmental water samples. The adsorption capacities of the alumina hollow fiber for Cu, Mn and Ni were found to be 6.6, 8.7 and 13.3 mg g(-1), respectively. With a preconcentration factor of 10, the limits of detection (LODs) for Cu, Mn and Ni were found to be 0.88, 0.61 and 0.38 ng mL(-1), respectively, and the relative standard deviations (RSDs) were ranging from 6.2 to 7.9% (n = 7, c = 10 ng mL(-1)). To validate the accuracy, the proposed method was applied to the analysis of certified reference material GSBZ50009-88 environmental water and the determined values are in good agreement with the certified values. The developed method was also employed for the analysis of Yangtze River water and East Lake water, and the recoveries for the spiked samples were in the range of 87.4-110.2%.     

On-line solid phase selective separation and preconcentration of Cd(II) by solid-phase extraction using carbon active modified with methyl thymol blue

An on-line flow system was used to develop a selective and efficient on-line sorbent extraction preconcentration system for cadmium. The method is based on adsorption of cadmium ions onto the activated carbon modified with methyl thymol blue. Then the adsorbed ions were washed using 0.5M HNO(3) and the eluent was used to determine the Cd(II) ions using flame atomic absorption spectrometry. The results obtained show that the modified activated carbon has the greatest adsorption capacity of 80 microg of Cd(II) per 1.0 g of the solid phase. The optimal pH value for the quantitative preconcentration was 9.0 and full desorption is achieved by using 0.5M HNO(3) solution. It is established that the solid phase can be used repeatedly without a considerable adsorption capacity loss. The detection limit was less than 1 ngmL(-1) Cd(II), with an enrichment factor of 1000. The calibration graph was linear in the range of 1-2000 ngmL(-1) Cd(II). The developed method has been applied to the determination of trace cadmium (II) in water samples and in the following reference materials: sewage sludge (CRM144R), and sea water (CASS.4) with satisfactory results. The accuracy was assessed through recovery experiments.     

Separation, preconcentration and determination of silver ion from water samples using silica gel modified with 2,4,6-trimorpholino-1,3,5-triazin

A new modified silica gel using 2,4,6-trimorpholino-1,3,5-triazin was used for separation, preconcentration and determination of silver ion in natural water by atomic absorption spectrometry (AAS). This new bonded silica gel was used as an effective sorbent for the solid-phase extraction (SPE) of silver ion from aqueous solutions. Experimental conditions for effective adsorption of trace levels of silver ion were optimized with respect to different experimental parameters in column process. Common coexisting ions did not interfere with the separation and determination of silver at pH 3.5 so that silver ion completely adsorbed on the column. The preconcentration factor is 130 (1 mL elution volume for a 130 mL sample volume). The relative standard deviation (R.S.D.) under optimum conditions is 3.03% (n=5). The accuracy of the method was estimated by using spring and tap water samples that were spiked with different amounts of silver ion. The adsorption isotherm of silver ion was obtained. The capacity of the sorbent at optimum conditions has been found to be 384 microg of silver per gram of sorbent.     

Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni2+ with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni2+ with 10 mL solution. Under the optimal conditions, the detection limit of Ni2+ is 0.12 ng mL(-1) with R.S.D. of 4.3% (n = 10, c = 100 ng mL(-1)). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.     

Cloud-point preconcentration and spectrophotometric determination of trace amounts of molybdenum(VI) in steels and water samples

A cloud-point extraction process using micelle of the cationic surfactant CTAB to extract Mo(VI) from aqueous solutions was investigated. The method is based on the color reaction of molybdenum with bromopyrogallol red in the presence of potassium iodide at pH 1.0 glycine/HCl buffer media and micelle-mediated extraction of complex. The optimal extraction and reaction conditions (e.g., surfactant concentration, reagent concentration and effect of time) were studied and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration and improvement factors) were obtained. Linearity was obeyed in the range of 0.3-320.0 ng mL(-1) of molybdenum(VI) ion and the detection limit of the method was 0.1 ng mL(-1). The relative standard deviation (R.S.D.) and relative error for five replicate measurements of 65.0 ng mL(-1) Mo(VI) were 1.1% and 1.9%, respectively. The interference effect of some anions and cations was also tested. The method was applied to the determination of molybdenum(VI) in steels and tap water and well water samples.     

Determination of trace aluminum in biological and water samples by cloud point extraction preconcentration and graphite furnace atomic absorption spectrometry detection

A cloud point extraction (CPE) method for the preconcentration of trace aluminum prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. The CPE method is based on the complex of Al(III) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), and then entrapped in non-ionic surfactant Triton X-114. PMBP was used not only as chelating reagent in CPE preconcentration, but also as chemical modifier in GFAAS determination. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PMBP and Triton X-114, equilibration temperature and time, were investigated in detail. An enrichment factor of 37 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of this method for Al(III) is 0.09 ng mL(-1), and the relative standard deviation is 4.7% at 10 ng mL(-1) Al(III) level (n=7). The proposed method has been applied for determination of trace amount of aluminum in biological and water samples with satisfactory results.     

Solid phase extraction using silica gel modified with murexide for preconcentration of uranium (VI) ions from water samples

Murexide was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane (APMS) to produce the new sorbent. A solid phase extraction method using the new sorbent has been developed to separate and concentrate trace amount of uranium (VI) from aqueous samples for the measurement by spectrophotometry method using Arsenazo III reagent. The influences of some analytical parameters on the quantitative recoveries of the analyte were investigated both in batch and column methods. Quantitative recovery of U(VI) was achieved by stripping with 0.1 mol L(-1) HCl. The maximum sorption capacity of the modified silica gel was 1.13 mmol g(-1) U(VI). A high preconcentration factor value of 400 with a lower limit of detection of 1 microg L(-1) was obtained for U(VI). The practical applicability of the developed sorbent was examined using synthetic and real samples such as sea/ground water samples.     

Determination of heavy metals by ICP-OES and F-AAS after preconcentration with 2,2'-bipyridyl and erythrosine

The applicability of 2,2'-bipyridyl and erythrosine co-precipitation method for the separation and preconcentration of some heavy metals, such as Cd, Co, Cu, Ni, Pb and Zn in actual samples for their determination by ICP-OES and F-AAS was studied. Experimental conditions influencing the recovery of the investigated metals, such as pH, molar ratio of 2,2'-bipyridyl to erythrosine, the effect of time on co-precipitation were optimized. The analytical characteristics of the method (e.g. limit of detection, sensitivity, linear range and preconcentration factor) were obtained. The limits of detection LOD (ng mL(-1)) of the ICP-OES (F-AAS) method were: Cd: 4.0 (7.75), Co: 3.1 (57.2), Cu: 18 (10.3), Ni 21.3 (32.8), Pb: 35.9 (29.2) and Zn: 10.2 (6.90). The recovery of all the elements tested was more than 93%. The influence of inorganic matrix was examined. The proposed method was applied to determination of Cd, Co, Cu, Ni, Pb and Zn in vegetables and certified reference material (NCS ZC85006 Tomato).     

Determination of Cd, Co, Ni and Pb in biological samples by microcolumn packed with black stone (Pierre noire) online coupled with ICP-OES

A simple and sensitive method using microcolumn (20-mm length x 2.0-mm i.d.) packed with black stone (Pierre noire) for the separation/preconcentration of Cd, Co, Ni and Pb in biological samples prior to their online determination by inductively coupled plasma optical emission spectrometry (ICP-OES) has been developed. Optimal experimental conditions including pH, eluent concentration and volume, sample volume and sample flow rate were investigated and established. The adsorption capacity of black stone for Cd, Co, Ni and Pb were found to be 23.4, 21.2, 18.1 and 22.2 mg g(-1), respectively. With a preconcentration time of 72 s and an elution time of 4s, an enrichment factor of 20 and a sampling frequency of 25 h(-1) were obtained. The detection limits corresponding to three times the standard deviations of the blank for Cd, Co, Ni and Pb were found to be 0.3, 0.4, 0.4 and 1.1 ng mL(-1). The precision for seven replicate determinations of Cd, Co, Ni and Pb gave relative standard deviations (RSDs) of 5.9, 4.8, 2.7 and 1.1%, respectively (n=7, C=10 ng mL(-1)). The method was validated with certified reference material GBW09103 human urine and the results obtained were in good agreement with the certified values. The method was also applied to the determination of the target analytes in biological samples with satisfactory results.     

Preconcentration and Voltammetric Determination of Mercury(II) at a Chemically Modified Glassy Carbon Electrode

In this work, the organic compound 2-mercaptobenzimidazole was covalently bound on the surface of a glassy carbon rod, via silanization, yielding a material capable of selectively complexing Hg(2+) ions. This material was applied as an electrode for voltammetric determination of mercury(II) following its nonelectrolytic preconcentration. After exchanging the medium, the voltammetric measurements were carried out by anodic stripping in the differential pulse mode (pulse amplitude, 50 mV; scan rate, 1.25 mV s(-)(1)) using 10(-)(2) mol L(-)(1) NaSCN solution as supporting electrolyte. An anodic stripping peak was obtained at 0.06 V (vs SCE) by scanning the potential from -0.3 to +0.3 V. After a 5 min preconcentration period in a pH 4.0 Hg(2+) solution, this electrode shows increasing voltammetric response in the range 0.1-2.2 μg mL(-)(1), with a relative standard deviation of 5% and a practical detection limit of 0.1 μg mL(-)(1) (5.0 × 10(-)(7) mol dm(-)(3)). Compared with the conventional stripping approach, this chemically modified glassy carbon electrode procedure presented good discrimination against interference from Cu(II) in up to 10-fold molar excess.