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Mercury Sulfide and Silver Sulfide Based Hg(II) Sensitive Solid State Ion Selective Electrode

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Mercury Sulfide and Silver Sulfide Based Hg(II) Sensitive Solid State Ion Selective Electrode Mercury Sulfide and Silver Sulfide Based Hg(II) Sensitive Solid State Ion Selective Electrode Mustafa Ta§tekin* and Eren Qantay Department of Chemistry, Science Faculty, Ankara University, Tandogan 06100 Ankara Turkey ABSTRACT This study is related to the development of a new solid state membrane ion-selective electrode for Hg(II) ions. The membrane was prepared by the amalgamation of metallic mercury with metallic silver powder and this solid amalgam was finely ground, mixed with Na2C03, K2C03 and elemental sulfur and was burned in nitrogen atmosphere in a glass container with a strong burner flame for six hours. The resulting mercury and silver sulfides were pressed into a 10 mm diameter and 0.2 mm thick membrane. The Hg (II) sensitive electrode prepared was found to have a slope of 29.5 ± 0.6 mV/pHg, detection range of 1.0 χ 10"1 -1.0 χ 10"6, response time of 15-30 s and electrode lifetime of 18 months. Among the ten cations studied (Ag+, Al3+, Cd2+, Cu2+, Co2+, Fe3+, K+, Ni2+, Ca2+, Mg2+, Ba2+, Pb2+), only Ag+ was observed to have a disruptive effect upon the performance of the electrode. The electrode was used in the determination of mercury in various dental filling materials titrating with EDTA and the results were compared with the spectral data. Keywords: Ion-selective electrodes; Mercury(II); Solid-state; 1. INTRODUCTION The literature related to Hg(II) sensitive ion selective electrodes reports mainly neutral carrier polymer- based membrane /1-15/, carbon paste /16-17/ and chalcogenide electrodes /18-20/. However, these electrodes have certain disadvantages such as relatively shorter electrode lifetime, leakage from the membrane and membrane rupture during the usage. Also, since they have internal filling solution, there are problems associated with surface contamination and cleaning when they are in continuous use /21/. There are relatively few studies related to the Hg(II)-selective metal sulfide based solid membrane electrodes. This is mainly due to the fact that Hg(II) sulfide is present as black colored cubic HgS * Corresponding author. Tel.: +90-312-2126720/1281; Fax: +90-312-2232395 E-mail address: [email protected] 331 Vol. 31, No. 6, 2009 Mercury Sulfide and Silver Sulfide Based Hg(ll) Sensitive Solid State Ion Selective Electrode (metacinnabar) and red colored hexagonal HgS (cinnabar) structures and cinnabar is difficult to press and has an inferior sensitivity to Hg(II) ions /21, 22/. Therefore, cinnabar must not be present in the structure of the membrane to be used in the construction of the solid-state membrane for ion-selective electrodes. That is why the precipitation of HgS in cubic structure, in other words its particle structure, is very important. There are various methods proposed in literature for the precipitation of Hg(II) ions /21, 22/. This study involves the preparation of a new material formed by the mixture of Ag2S-HgS and its use in the development of an ion-selective electrode sensitive to Hg(II) ions. The performance of the electrode prepared with the use of this material was investigated. 2. EXPERIMENTAL 2.1. Apparatus All Potentiometrie and pH measurements were made at 25±1°C using a Consort pH/mV meter (model C863) and an Ingold U402-S7/120 glass electrode was used for pH measurement .All the spectrometric measurements were performed with the use of a Digilab Hitachi U-2800 UV-VIS spectrophotometer. 2.2. Reagents and materials All the chemicals used in the study were of analytical grade and were not subjected to any further purification. The stock solutions of the metal ions were prepared in 0.1 M. The experimental solutions were prepared by dilution of the stock solutions with deionized water obtained from Elgestat-prima 2 and Elgestat- maxima UF water purification apparatus. The conductivity of the deionized water was 2.5 χ 10"6 Siemens. Hg(N03)2 (99.0 %), AgN03 (99.8 %), A1(N03)3 (99.8 %), Cr(N03)3 (99.0 %), Ni(N03)2 (97.0 %), Pb(N03)2 (98.5 %), CO(N03)2 (99.0 %), Cu(N03)2 (97.0 %), NaOH (97.0 %), HN03 (65 %; d = 1.42 kg/L), EDTA (98.0 %), KN03 (99.0 %), Ca(N03)2 (98.0 %), Fe(N03)3 (99.0 %), NaN03 (99.9 %), Mg(N03)2 (98.0 %) and standard mercury solution (0.05 M) were obtained from Merck, HCl (37 %; d = 1.19 kg/L) from Riedel-De- Haen, dithizone (99.0 %) from Fluka and mercury amalgam (=99.0 %) used in dentistry from Sdi ultracaps+ firms. The pH values of the experimental solution were set to 2.5 with the use of HN03 and NaOH. The ionic strengths of the solutions were adjusted to contain 0.1 Μ NaN03. 2.3. Preparation of the electrode Metallic silver powder obtained by the electrolysis of silver nitrate was gradually added to metallic mercury by constant stirring until solid amalgam structure was obtained (there was 2.5 g of silver powder used for each 5.0 g of mercury). The mercury-silver amalgam was finely ground in a mortar. Then approximately 100 g of this grounded amalgam was homogenously mixed with 15.0 g sulfur, 2.0 g Na2C03 and 10.0 g K2C03 and this mixture was placed in a fusion column and fused under nitrogen atmosphere at 332 Tastekin and Cantay Main Group Metal Chemistry elevated temperatures. The fusion was started at low Bunsen flame until the material turned completely black then the temperature was increased to elevated values. Care was taken for the homogeneity of heating process. When the heating was not homogenous it was observed that HgS and elemental sulfur rapidly sublimated and recrystallized on the walls of the cooling system. The membrane material obtained after six hours of fusing process was treated with dilute HN03 to eliminate its alkalinity and washed with abundant amounts of water and alcohol in order to remove the residual sulfur. The resulting black Ag(I)-Hg(II) sulfide mixture had a very homogenous appearance with very small sized particles. 1 g of this finely powdered membrane material was taken, subjected to 9 tons of total pressure gradually applied in ten minutes, and kept under this pressure for 20 minutes to obtain 1 cm diameter and 0.3 mm thick membrane disks. The disc shape membrane was attached to a helical copper wire with silver adhesive. It was then mounted on the electrode with a suitable binder. 2.4. Potential measurements The Potentiometrie cell was formed using Ag/AgCl reference electrode and Hg(II) sensitive electrode . The schematic representation of the cell is given below: Ag/AgCl, KCl(saturated)//test solution /AgS.HgS (membrane)/ Cu The cell potential was measured after stirring the solution with a magnetic stirrer and waiting for the potential to reach a steady value. To test the analytical application of the ion-selective electrode prepared, the determination of mercury in dental filling materials was tried. For this purpose, the sample of the material was dissolved in 6.0 Μ HN03 and diluted to an appropriate volume so as to adjust the mercury concentration to fall into a range suitable for the electrode working range. Any trace of mercury (I) ions was oxidized to mercury (II) by the addition of KMn04; the excess of which was removed by H202, and the remaining H202 was expelled by boiling. The accompanying silver ions were removed by precipitation as AgCl with HCl and the final solution was diluted with water to the mark of volumetric flask. This solution was used for analysis. 3. RESULT AND DISCUSSION Performance characteristics and optimum working condutions of the mercury (Il)-selective electrode were investigated. Working conditions involved were suitable pH-range, linear working range and response lifetime, and selectivity coefficients for the proposed electrode. The performance of the electrode for the analysis of real samples was also investigated by comparison with a well-established spectrophotometric method. 333 Vol. 31, No. 6, 2009 Mercury Sulfide and Silver Sulfide Based Hg(ll) Sensitive Solid State Ion Selective Electrode 3.1. Effect of pH The accurate detection of Hg(II) ions was performed by measuring the potential of the ion-selective electrode at lower pH values /2, 8, 21/. This is due to the fact that at high pH values free Hg(II) ion forms the hydroxyl complex (HgOH+), which causes a decrease in the Potentiometrie response of the electrode. On the other hand, at extremely low pH values the interference of hydrogen ions partly affects the solubility of the membrane and results in variation in potential. In order to determine the optimum pH range at which the electrode is least affected, 50 mL of a ΙχΙΟ"1 Μ Hg(N03)2 was taken and its pH value was adjusted to 1.5 with HN03 solution. Then the pH value was increased by 0.1 unit with 0.5 Μ NaOH solutions. The potential values recorded were plotted against pH values. This procedure was repeated till pH = 9.0. The pH value where the potential did not show a significant variation was found to be 1.5 - 3.0. Therefore all the measurements were taken at a pH value of 2.5 (Figure 1). 800 700 1 600 LU 500 1 400 0 2 4 6 8 10 pH Fig. 1: The effect of pH on the response of Hg(II)-selective electrode. 3.2. Determination of working range and lower detection limit The calibration curve of Hg(II) ion selective electrode was constructed by the use of mercury(II) nitrate standard solutions with concentrations ranging from 1 χ 10"' Μ to 1 χ ΙΟ'7 Μ.
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