Determination of zinc,cadmium, lead and copper in sea water by means of computerized potentiometric stripping analysis

Water samples from the Arctic Sea were analyzed by the potentiometric stripping technique. Lead(II) and cadmium(II) were determined after pre-electrolysis for 32 min at—1.1 V vs. Ag/AgCl, the detection limits being 0.06 and 0.04 nM, respectively. Zinc(II) was determined after the addition of gallium(III) by pre-electrolysis for 16 min at —1.4 V vs. Ag/AgCl, the detection limit being 0.25 nM. Problems in the determination of copper(II) at the very low concentrations found in oceanic waters are outlined. The average zinc(II), cadmium(II) and lead(II) concentrations in eight different samples were 2.5, 0.16 and 0.10 nM as determined by potentiometric stripping analysis and 1.9, 0.16 and 0.09 nM as determined by solvent extraction/atomic absorption spectrometry. The advantages of this computerized technique for the analysis of sea water are discussed.     

Differential pulse stripping voltammetric determination of heavy metals simultaneously using new polymer modified glassy carbon electrodes

Seven novel polymer modified glassy carbon electrodes have been developed for the analysis of metals of zinc, cadmium, lead, arsenic and copper in formulated samples of waters and industrial wastewater samples by differential pulse stripping voltammetry. Very good responses have been observed for all the metals with all the modified electrodes employed. However, the poly(3,4-ethylenedioxythiophene) modified electrode has resulted in very low detection limits. An independent atomic absorption spectroscopic analysis of the industrial wastewater sample was carried out and the results are compared.     

Determination of cadmium, lead and copper in milk and milk powder by means of flow potentiometric stripping analysis

A flow potentiometric stripping analysis procedure for the determination of cadmium, lead and copper in milk and milk powder samples is described. The instrumental arrangement consists of a glassy-carbon thin-layer cell through which six different solutions may be drawn by means of a peristaltic pump and magnetically operated valves. The glassy-carbon electrode is pre-coated with a film of mercury which can be employed for several analytical runs. The sample, diluted five-fold with Suprapur hydrochloric acid, is electrolysed for 0.5–4 min prior to stripping in Suprapur hydrochloric acid. Pump-rate, electrolysis time and potential, opening and closing of inlet valves and digital evaluation of stripping times are controlled automatically by the computer. The analytical results agree satisfactorily with the certified values for three milk powder reference samples. The detection limit for cadmium, lead and copper in milk samples after 4, 1 and 0.5 min of pre-electrolysis is 0.8, 4 and 8 μg/l., respectively. An analytical procedure for the determination of lead in samples containing high concentrations of tin is described.     

适用于改换介质的简易电解池设计及其电位溶出分析的应用研究

设计制作了用于改换介质的简易电解池,并以旋转圆盘玻碳电极为工作电极,研究了其用于电位溶出分析改换溶出介质的可行性。以同时测定Ｐｂ＾２＋、Ｃｄ＾２＋为例,试验了改换溶出介质的条件。结果表明,改换介质可消除共存离子的干扰,只要选择合适的溶出介质,可有效地提高测定方法的分辨率和灵敏度。此方法用于矿样中铅和镉的同时测定,结果满意。     

Determination of mercury in air by means of computerized flow constant-current stripping analysis with a gold fibre electrode

Mercury in air was determined after collection in potassium permanganate or sodium carbonate solution. The mercury concentration in these solutions was determined in a computerized flow potentiometric stripping analyzer with a 10-μm gold fibre working electrode, a glassy carbon reference electrode and a platinum counter electrode. After sample electrolysis for 1–10 min, stripping was done in a 1 mg l^?1 gold(III) solution in 0.01 M nitric acid/0.01 M sodium nitrate with a constant stripping current of 0.50 μA. Results obtained for flue gas samples were in good agreement with results from cold-vapor atomic absorption spectrometry.     

A flow cell with flexible depositon efficiency for a dual-detection system based on potentiometric stripping analysis and atomic absorption spectrometry

An electrochemical flow cell suitable for use with dual detection by potentiometric stripping analysis and atomic absorption spectrometry in a flow-injection system is characterized by flow pattern and dispersion measurements. The deposition efficiency can be altered from 1–2% to 24% by using a glassy carbon and a carbon felt electrode, respectively. Application to the determination of lead in water showed that after enrichment on carbon felt the sensitivity for flame atomic absorption spectrometry is increased by an order in magnitude (enrichment factor ca 5 and 30 at sample frequencies of 60 and 12 h^?1, respectively). Dual-detection allows certain errors appearing in one of the methods caused by, e.g., malfunction of the apparatus or wrong sample pretreatment, to be recognized, thus providing accuracy checks.     

The determination of trace amounts of zinc, cadmium, lead and copper in airborne particulate matter by anodic stripping voltammetry

The application of anodic stripping voltammetry, with a hanging mercury drop electrode, to the determination of zinc, cadmium, lead and copper in airborne particulate matter collected by filtration is discussed. This procedure allows for the destruction of the filter material followed by the complete dissolution (including silicates) of the collected particulate matter. A low-temperature ashing process is described and the recovery of cadmium in this procedure is studied. Analytical data obtained by anodic stripping and atomic absorption for zinc, cadmium, lead and copper are compared.     

A study of differential potentiometric stripping analysis for lead and cadmium with Nafion coated carbon fibre electrode

The differential potentiometric stripping analysis (DPSA) with Nafion coated carbon fibre electrode has been studied, and a method to determine lead and cadmium in urine directly has been attempted. The effect of various experimental parameters on the DPSA response is discussed. The experimental conditions include 0.2M sodium perchlorate, deposition potential of ?1.0 or ?1.1 V and using 20 ppm mercuric ion as oxidizing agent. The response of the signal is in linear relation with the concentrations of lead and cadmium respectively up to 0.5 ppm. The electrode coated with Nafion film alleviates the interference from organics in urine samples.     

Automated determination of cadmium and lead in whole blood by computerized flow potentiometric stripping with carbon fibre electrodes

A sample pretreatment involving only the dilution (1 + 19) of two 0.2–0.4 ml sample aliquots with 0.5 M hydrochloric acid, with a standard addition to one of the aliquots, precedes the injection of each sample. The computer-controlled flow system used automatically executes a pre-programmed number of cycles on each sample pair before presenting the final result. Each cycle, which has a duration of 80 or 135 s for lead(II) and cadmium(II), respectively, involves the display of the derivative stripping signal on a printer/plotter and integration of the stripping peaks generated. For lead(II), striping is done in 0.5 M hydrochloric acid, which eliminates interferences from copper, though at the cost of a relatively high stripping rate, compared to the 5 M calcium chloride used for cadmium(II). The flow cell consists of a silver chloride-lined silver tube which acts as both reference and counter electrode, and a disposable carbon-fibre working electrode mounted in a PVC tube, which normally will operate for 50–200 cycles. The method was verified for whole blood reference standards and by comparison with results obtained by atomic absorption spectrometry.     

Computerized potentiometric stripping analysis for the determination of cadmium,lead, copper and zinc in biological materials

Two different types of tinned mussels and a bovine liver reference sample have been analyzed for Zn, Cd, Pb and Cu by means of computerized potentiometric stripping analysis and atomic absorption spectrometry. The samples were digested by two different procedures, one employing nitric acid only and the other employing nitric and perchloric acids. It is shown that computerized stripping analysis can be used in samples containing high concentrations of electroactive organic nitro compounds, without sample deoxygenation.     

In situ electrodeposition for the determination of lead and cadmium in sea water

Electrodeposition techniques for the direct determination of lead and cadmium in sea water at the natural pH and in the presence of dissolved oxygen are examined. Anodic stripping voltammetry, at either the hanging mercury drop electrode or glassy carbon thin film electrode, is suitable for the determination of labile lead and cadmium. The presence of dissolved oxygen increases the height of the lead wave with a shift to more negative potentials. A more versatile technique is in situ deposition of labile metals on a mercury-coated graphite tube electrode. The mercury film, deposited in the laboratory, is stable on the dried tubes which are used later for field electrodeposition. The deposited metals are determined by electrothermal atomic absorption spectrometry.     

Anodic stripping voltammetry at a mercury film electrode: baseline concentrations of cadmium,lead, and copper in selected natural waters

A simple, rapid, and inexpensive anodic stripping voltammetric method with a mercury thin film electrode is reported for the establishment of baseline concentrations of cadmium, lead, and copper in natural waters. The procedure for routine surface preparation of wax-impregnated graphite mercury film electrodes requires about 30 min. Concentrations in the 0.006–6 μg l^-1 range are determined by linear d.c. voltage sweeps; the total time for a plating and stripping cycle is 6 min or less. The need for pressure-digesting samples for copper determinations is demonstrated. The a.s.v. results correlate well with corresponding analyses performed by graphite-furnace atomic absorption spectrometry.     

Multiple-scanning potentiometric stripping analysis

A computerized data acquisition technique— multichannel potentiometric monitoring—is used in conjunction with potentiometric stripping analysis. Multiple-scanning stripping potentiograms can be recorded so that the analytical signals are enhanced. A minicomputer with an internal store of4K 16-bit words suffices for experimental control and data treatment. The technique is suitable for stripping analysis with preconcentration times of 60–90 s at a mercury film electrode with linear response ranges of 1–100 μg l^-1 for cadmium(II) and lead(II). For preconcentration times of 30 min, the limit of detection is about 5 ng l^-1. Preliminary tests on continuous flow analysis are reported.     

Potentiometric stripping analysis for zinc,cadmium. lead and copper in sea water

Analytical procedures for the determination of zinc(II), cadmium (II), lead(II) and copper(II) in sea water by potentiometric stripping analysis are described. The results are compared with those obtained by a combined solvent extraction-atomic absorption method both in the laboratory and on-board ship. The detection limits for zinc, cadmium, lead and copper are 0.03, 0.03, 0.01 and 0.02 μg l^-1, respectively, for a total analysis time of about 75 min. A very thin mercury film is useful in the determination of lead and copper.     

The determination of traces of cadmium,lead and thallium in fly ash by potentiometric stripping analysis

The suitability of potentiometric stripping analysis for the determination of cadmium, lead and thallium in fly ash and in waters polluted by leaching of fly ash is assessed. By an appropriate choice of medium and of electrolysis potential and by employing a rotating working electrode, it is possible to eliminate interferences from electroactive species often found in fly ash in high concentrations. The accuracy obtained in a study of a certified coal fly ash (SRM 1633a) is satisfactory.     

Determination of mobile form contents of Zn, Cd, Pb and Cu in soil extracts by combined stripping voltammetry

The amount of mobile forms of Zn, Pb, Cd and Cu in extracts obtained by treating soil samples with ammonium nitrate were determined by an appropriate combination of anodic and cathodic stripping voltammetry with hanging mercury drop electrode. Every analysis required three mercury drops: on the first one, zinc was determined; on the second, cadmium and lead; on the third, copper was determined. Zinc, lead and cadmium were determined by conventional differential-pulse anodic stripping voltammetry. For copper determination, adsorptive differential-pulse cathodic stripping voltammetry with amalgamation using chloride ions as a complexing agent was applied. The standard deviation of the results was from 1 to 10% depending on the metal content in the sample. Voltammetric results were in good agreement with the AAS analysis. No microwave digestion of soil extracts was necessary.     

The determination of lead,copper and cadmium by anodic stripping voltammetry at a mercury thin-film electrode

The determination of lead, copper and cadmium by anodic stripping voltammetry at a wax-impregnated graphite electrode, pre-plated with mercury, has been investigated. Electrode preparation and cell design are discussed, and the effects of mercury loading and sample pH on electrode sensitivity are described. Detection limits and precision on aqueous samples are reported. Calibration graphs are linear for lead and cadmium, but non-linear for low concentrations of copper. The depression of peak current and shift of peak potential for copper in chloride media are described and an explanation is proposed. Precision and recovery of metal additions are reported for digested samples of whole blood.     

Computerized flow injection potentiometric stripping analysis with large-volume wall-jet cell

Summary A microcomputer system for flow injection potentiometric stripping analysis is presented permitting fast digital recording of potential time-curves. A large-volume wall-jet cell simple in design has been used as detector cell. Investigations about the influence of electrode pretreatment and solution delivery mode (i.e. gravity flow, pumping) reveal the strong influence of these parameters on the magnitude and precision of stripping times. The optimized system was applied to the simultaneous determination of cadmium and lead in geological samples.

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Computerisierte Potentiometrische Stripping Analyse in einem Fließinjektionssystem mit großvolumiger Wall-jet Zelle

     

Potentiometric stripping analysis and anodic stripping voltammetry with carbon fiber electrodes

High-modulus carbon fibers are used as working electrodes in differential-pulse stripping voltammetry and potentiometric stripping analysis. Different types of electrodes (particularly single-fiber and brush electrodes) are compared with regard to reproducibility, sensitivity, and practical aspects. Zinc, cadmium, and lead are determined in the 100 μg 1^?1 to 1 mg l^?1 range and optimum experimental parameters are described. The cut single-fiber electrode has the best general characteristics.     

Development of cysteine-modified screen-printed electrode for the chronopotentiometric stripping analysis of cadmium(II) in wastewater and soil extracts

Screen-printed carbon electrodes were fabricated with amino acid functionality by using in situ co-deposition of mercury and cysteine. The three-electrode configuration (graphite carbon working electrode, carbon counter electrode and silver/silver chloride reference electrode) incorporating a cysteine-modified working electrode exhibited good sensitivity towards cadmium(II). Several experimental variables affecting the sensor stripping response were characterised and optimised. These include cysteine and mercury concentrations, deposition time, deposition potential and stripping current. Surface analysis was also conducted using scanning electron microscopy (SEM) in order to characterize the electrode surface during cadmium analysis. The stripping chronopotentiometric response for cadmium(II) was linear in the concentration range 0.4–800 g L^–1 when a deposition time of 2 min was used. A detection limit of 0.4 g L^–1 was obtained using 0.025 M Tris–HCl buffer containing 0.1 M KCl (pH 7.4) as the supporting electrolyte. The analytical utility of the cysteine-modified sensor was demonstrated by applying it to cadmium analysis in various wastewater and soil samples collected from a contaminated site and extracted using acetic acid. The results obtained using the developed electrodes agreed satisfactorily with the values achieved using atomic absorption spectrometry and inductively coupled plasma mass spectrometry analysis. These results demonstrate the feasibility of using this type of sensor for cadmium analysis.