ABSTRACT
A chemically modified electrode (CME) was prepared and studied as a potentiometric sensor for the end-point detection in the automatic titration of vanadium(V) with EDTA. The CME was constructed with a paste prepared by mixing spectral-grade graphite powder, Nujol oil and N-2-naphthoyl-N-p-tolylhydroxamic acid (NTHA). Buffer systems, pH effects and the concentration range were studied. Interference ions were separated by applying a liquid-liquid extraction procedure. The CME did not require any special conditioning before using. The electrode was constructed with very inexpensive materials and was easily made. It could be continuously used, at least two months without removing the paste. Automatic potentiometric titration curves were obtained for V(V) within 5 x 10(-5) to 2 x 10(-3)M with acceptable accuracy and precision. The developed method was applied to V(V) determination in alloys for hip prosthesis.
ABSTRACT
The behavior of a modified carbon paste electrode (CPE) for nickel determination by anodic adsorptive stripping voltammetry (AAdsSV) was studied. The electrode was built incorporating the Dowex 50W x 12 (H(+) form) ion exchanger to a Nujol-graphite base paste. Ni(2+) was preconcentrated on the electrode surface in open circuit conditions, with the reduction (-1300 mV)/reoxidation step carried out in HCl solution (pH 3). During deposition time (5 min), the hydrogen evolution did not present obstacle in the quantification of nickel. For 12 min of accumulation and 5 min of deposition, nickel can be quantified up to 600 mug l(-1). The detection limit was 0.005 mug l(-1) at a linear potential scan rate of 200 mV s(-1). Interferences from Hg(2+) and Ag(2+) up to a concentration of 1 and 0.6 mg l(-1), respectively, were eliminated with the aid of the anion exchanger Dowex-2 (mesh 200-400) which was added to the sample in the preconcentration step. The tolerance for some metal ions such as Cu(2+), Cd(2+), Fe(3+), Zn(2+), Co(2+) and Pb(2+) was improved in the same way. The method was applied for the determination of nickel in samples of tap and mineral water. At the concentration level of 50 mug l(-1) of Ni (2+), the results were in good agreement with those obtained using Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). For a Ni(2+) concentration of 5 mug l(-1), the results obtained showed better accuracy than those obtained by ICP-AES.
ABSTRACT
Bader indicated as the most convenient approaches for the determination of an element by atomic absorption spectrometry the (1) continuous variation of standard at constant total volume, and (2) continuous variation of the unknown analyte at constant total volume. Considering the relevance of the ease of atomization, Bader's statement were put to the test in the determination of copper, nickel, and chromiun in nodular iron by use of analysis of variance (ANOVA). The results presented here lead to the conclusion that Bader's modes (1) and (2) are not equivalent for all cases.
ABSTRACT
A chemically modified electrode (CME) was constructed and evaluated for use as an end-point indicator in the automatic titration of Ni(II) with EDTA. The CME consisted of a graphite paste prepared by mixing a strong acid ion exchanger containing 4-(3,5-dichloro-2-pyridylazo)-1,3-diaminobenzene and graphite powder-Nujol paste. This mixture showed high mechanical resistance in strongly acidic and alkaline solutions (6 M HCl-pH 12). The CME did not require any special conditioning prior to use. It could be used over long periods (5-6 months) of continuous work without renewing either the electroactive surface or paste. In buffered solutions (pH 3-4.5), automatic direct potentiometric titrations could be carried out over a wide interval of Ni(II) concentrations, ranging from 3 to 6000 ppm, with satisfactory accuracy and precision. For practical analysis, the electrode was applied to the determination of nickel in two certified composition alloys. Interferent ions were previously separated by applying an ion-exchange procedure.
ABSTRACT
A simple and sensitive potentiometric sensor for end-point detection in the automatic titration of Zn(II) with EDTA was prepared and studied. The sensor was based on a conventional carbon paste which was mixed during preparation with 4-(3,5-dichloro-2-pyridil-azo)-1,3-diaminobenzene (3,5-Cl2PADAB). pH effects, buffer concentration, reagent content into carbon paste and the presence of foreign salts on the electrode response were studied. Titration curves with sharp end-point breaks were obtained in Zn(II) concentration range from 0.5 to 6550 ppm. The electrode was easily made and with very inexpensive materials. A titrimetric method for the determination of zinc in insulin by automatic potentiometric end-point detection is described. It was applied to the determination of the metal in two commercial pharmaceutical preparations. The results were in good agreement with those obtained by the U.S. Pharmacopeia standard method.
ABSTRACT
A titrimetric method for determination of sulfide and of sulphur in steels with chloranilic acid by biamperometric and automatic potentiometric end-point detection is described. The construction of the sensor for potentiometric indication is also described. The results obtained agree with those of the iodine-thiosulfate method and with the certified values for the steels.
ABSTRACT
An indirect titrimetric method for determination of phosphate is based on precipitation with excess of bismuth, and titration of the surplus with chloranilic acid, the end-point being determined biamperometrically.
ABSTRACT
A voltammetric cell with a graphite-paste cathode and silver-wire anode was designed for dissolved oxygen determinations in water. Its most important features were evaluated in laboratory and field studies. Several advantages such as higher sensitivity, wider linear response interval, negligible interference due to carbon dioxide, and shorter response time, besides its low cost and simple construction, were found when it was compared with sensors having a platinum cathode.
