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PubMed2004

(2,2'-bipyridine-kappa(2)N,N')(2,3-naphthalenediolato-kappa(2)O,O')palladium(II) and (2,2'-biquinoline-kappa(2)N,N')(2,3-naphthalenediolato-kappa(2)O,O')palladium(II).

In the title compounds, [Pd(C(10)H(6)O(2))(C(10)H(8)N(2))], (I), and [Pd(C(10)H(6)O(2))(C(18)H(12)N(2))], (II), each Pd(II) atom has a similar distorted cis-planar four-coordination geometry involving two O atoms of the 2,3-naphthalenediolate dianion and two N atoms of the 2,2'-bipyridine or 2,2'-biquinoline ligand. The overall structure of (I) is essentially planar, but that of (II) is not, as a result of intramolecular overcrowding leading to bowing of the biquinoline ligand.

Journal Article↗
PubMed2005

The mechanism of corrosion of palladium-silver binary alloys in artificial saliva.

Palladium dental casting alloys are alternatives to gold alloys. The aim of this study was to determine the electrochemical behaviour and the corrosion mechanism of binary silver-palladium alloys. Seven binary silver-palladium alloys and pure palladium and silver were tested in a model saliva solution. Electrochemical tests included corrosion potential, polarization resistance, and potentiodynamic polarization measurements. The corrosion products, which may be theoretically formed, were determined by thermodynamic calculation. The behaviour of silver and silver-rich alloys was dominated by the preferential formation of a thiocyanate surface layer, which controlled the free corrosion potential. Palladium dissolved in the form of a thiocyanate complex, but the surface became passivated by either palladium oxide or solid palladium thiocyanate layer, the thermodynamic calculations indicating preference for the oxide. Palladium-rich alloys showed evidence of silver depletion of the surface, resulting in behaviour similar to palladium. Examination of binary silver-palladium alloys has made possible determination of the role of the components of the alloys and model saliva in the corrosion behaviour. The findings are applicable to the more complex commercial dental alloys containing silver and palladium as major components.

Biocompatible Materials↗
PubMed1995

Interaction of palladium ions with the skin.

87 subjects sensitive to both nickel sulfate and palladium-chloride pet., were contemporaneously patch retested to nickel sulfate 5% pet., metallic palladium chloride 1% pet. and to palladium chloride 1% aq. Whilst all subjects reacted to nickel sulfate and palladium chloride pet., only 3 reacted to palladium chloride aq. No positive reactions were found to metallic palladium. The negative results to palladium chloride aq. are probably due to the formation of a new palladium ion (PdCl4)2-, achieved on adding an amount of hydrocloric acid to the aqueous solution of PdCl2. The findings seem to demonstrate that the allergic reaction to palladium depends on the arrangement of the metal electrons. The sensitization to palladium does not seem to be dependent on the element itself but on the complexes formed by the different compounds. The concomitant reactions to nickel and palladium ions could be dependent on the generation of similar complexes between the ions and the skin proteins.

Dermatitis, Allergic Contact↗
PubMed2004

Improved separation of palladium species in biological matrices by using a combination of gel permeation chromatography and isotachophoresis.

The binding of palladium to high-molecular-mass compounds in palladium-treated lettuce is investigated as an example for a biological matrix. The total palladium concentration in lettuce leaves is 10.3 ng/g wet weight. After homogenization, high-molecular-mass compounds (> 10 kDa) are isolated by ultrafiltration. For separation of these palladium species a combination of preparative gel permeation chromatography (GPC) and preparative isotachophoresis (ITP) is used. Palladium is determined in separated fractions by using a highly sensitive total reflection X-ray fluorescence (TXRF) method after preconcentration. After GPC separation, four main fractions of palladium species are collected, each containing palladium in ng quantities (3-10 ng). Two of these fractions are further separated by ITP, yielding at least three main peaks per GPC fraction, each containing palladium in the range of 0.3-3 ng. These palladium containing peaks are characterized by high-performance size exclusion chromatography (HPSEC) and capillary isotachophoresis (cITP) in parallel. HPSEC enables the estimation of the molecular mass of six main palladium peaks, covering a molecular mass range of 69-200 kDa. It is also shown that the estimation of molecular mass after separation is more reliable than the respective estimation directly in the first GPC run. However, cITP reveals that each of the separated peaks is still a mixture of at least five different compounds.

Chromatography, Gel↗
PubMed1996

Allergic patch test reactions to palladium chloride in schoolchildren.

A study of the prevalence of allergic patch test reactions to palladium chloride compared to nickel sulfate was performed in a group of Finnish schoolchildren. All adolescents 14-18 years of age in a Finnish town with 40,000 inhabitants, who had received orthodontic treatment with metallic appliances at a municipal dental clinic, were included in the study. The selection of patients was based on patient records. A non-treatment control group was randomly selected from the same age groups of the town population. A total of 700 subjects (77% of those invited), 417 (60%) girls and 283 (40%) boys, participated. The majority (91%) of the girls had pierced ears. Orthodontic treatment was equally common (67-70%) in the boys and the girls. The girls had a much higher frequency of allergic patch test reactions to both nickel sulfate and palladium chloride. Of the 700 adolescents tested, 48 (7%) had an allergic patch test reaction to palladium chloride. Of the 417 girls, 44 (11%) were palladium-chloride-positive, whereas only 4 of the 283 boys tested (1%) had an allergic patch test reaction to palladium chloride. 3 patients reacted to palladium chloride only, whereas all other patients with allergic patch test reactions to palladium chloride also had an allergic patch test reaction to nickel sulfate. The results support the concept of cross-reactivity between nickel sulfate and palladium chloride. The clinical significance of the allergic patch test reactions caused by palladium chloride remains unclear.

Adolescent↗
PubMed1992

Cross-reactivity to palladium and nickel studied in the guinea pig.

In recent years there have been several reports on concomitant patch test reactions to palladium and nickel, which belong to the same group in the periodic table. Exposure to palladium mainly takes place via dental alloys and jewelry. However, the clinical relevance of simultaneous reactivity to these metals is unknown. To elucidate the question of cross-reactivity, guinea pigs were induced with palladium or nickel and simultaneously challenged with palladium and nickel. Animals sensitized to palladium according to the guinea pig maximization test method (GPMT) or to a new method by van Hoogstraten & Scheper (H&S) reacted to palladium as well as to nickel. On the other hand, animals sensitized to nickel according to H&S reacted to nickel but not to palladium. The GPMT shows that palladium is a more potent sensitizer than nickel: could palladium be the primary sensitizer in humans?

Animals↗
PubMed2006

Pore surface fractal analysis of palladium-alumina ceramic membrane using Frenkel-Halsey-Hill (FHH) model.

The alumina ceramic membrane has been modified by the addition of palladium in order to improve the H(2) permeability and selectivity. Palladium-alumina ceramic membrane was prepared via a sol-gel method and subjected to thermal treatment in the temperature range 500-1100 degrees C. Fractal analysis from nitrogen adsorption isotherm is used to study the pore surface roughness of palladium-alumina ceramic membrane with different chemical composition (nitric acid, PVA and palladium) and calcinations process in terms of surface fractal dimension, D. Frenkel-Halsey-Hill (FHH) model was used to determine the D value of palladium-alumina membrane. Following FHH model, the D value of palladium-alumina membrane increased as the calcinations temperature increased from 500 to 700 degrees C but decreased after calcined at 900 and 1100 degrees C. With increasing palladium concentration from 0.5 g Pd/100 ml H(2)O to 2 g Pd/100 ml H(2)O, D value of membrane decreased, indicating to the smoother surface. Addition of higher amount of PVA and palladium reduced the surface fractal of the membrane due to the heterogeneous distribution of pores. However, the D value increased when nitric acid concentration was increased from 1 to 15 M. The effect of calcinations temperature, PVA ratio, palladium and acid concentration on membrane surface area, pore size and pore distribution also studied.

Journal Article↗
PubMed2006

H-point standard addition method--first derivative spectrophotometry for simultaneous determination of palladium and cobalt.

H-point standard addition method (HPSAM) has been applied for simultaneous determination of palladium and cobalt in trace levels, using disodium 1-nitroso-2-naphthol-3, 6-disulphonate (nitroso-R salt) as a selective chromogenic reagent. Palladium and cobalt in the neutral pHs form red color complexes with nitroso-R in aqueous solutions and making spectrophotometric monitoring possible. Simultaneous determination of palladium and cobalt were performed by HPSAM--first derivative spectrophotometry. First derivative signals at the two pairs of wavelengths, 523 and 589 nm or 513 and 554 nm were monitored with the addition of standard solutions of palladium or cobalt, respectively. The method is able to accurately determine palladium/cobalt ratio 1:10 to 15:1 (wt/wt). Accuracy and reproducibility of the determination method on the various amounts of palladium and cobalt known were evaluated in their binary mixtures. To investigate selectivity of the method and to ensure that no serious interferences were observed the effects of diverse ions on the determination of palladium and cobalt were also studied. The recommended procedure was successfully applied to real and synthetic cobalt or palladium alloys, B-complex ampoules, a palladium-charcoal mixture and real water matrices.

Alloys↗
PubMed2001

Competitive sorption of platinum and palladium on chitosan derivatives.

Glutaraldehyde-cross-linked chitosan (GCC), thiourea derivative of chitosan (TGC) and rubeanic acid derivative of chitosan (RADC) have previously been shown to be very efficient at removing platinum and palladium from single component dilute acidic solutions. This study examines the competitive sorption of these metal anions in bi-component mixtures for GCC, TGC and RADC. Palladium sorption is less sensitive to the presence of platinum than the reverse: the maximum sorption capacity decreases less for palladium than for platinum in the presence of the competitor anion (the metals being in their chloro-metal forms). Moreover, the Langmuir-shape of the sorption isotherm for palladium is unaffected (with the usual plateau reached at low residual palladium), while in the case of platinum sorption, the isotherms exhibit a significant decrease of the sorption capacity at high residual platinum concentration which increases with increasing concentrations of palladium. RADC is more selective for palladium over platinum than the other chitosan derivatives. A preliminary study of the competitive sorption kinetics in both batch and fixed bed systems is presented for RADC and confirms the higher affinity of the sorbent for palladium than for platinum.

Adsorption↗
PubMed2001

Palladium-catalyzed synthesis of 2,3-dihydro-2-ylidene-1,4-benzodioxins.

Palladium-catalyzed condensation of benzene-1,2-diol with various propargylic carbonates afforded regio- and stereoselectively 2,3-dihydro-2-ylidene-1,4-benzodioxins. The reaction is suggested to proceed by the formation of a (sigma-allenyl)palladium complex, followed by the intermolecular attack of the phenoxide ion on this complex to generate a new (sigma-allyl)palladium complex in equilibrium with the corresponding (eta(3)-allyl)palladium complex. Intramolecular attack of the phenoxide ion afforded the corresponding benzodioxan compound. This last attack occurs predominantly at the more electrophilic end of the (eta(3)-allyl)palladium intermediate. The Z- or E-stereochemistry of the products was established by (1)H NMR and proton NOE measurements and also by X-ray analysis on an example. The Z-stereochemistry generally observed is in agreement with the formation of this (eta(3)-allyl)palladium intermediate. However, in the case of tertiary propargylic carbonates, the E-stereochemistry generally observed could be explained by an intramolecular attack of the phenoxide ion on the intermediate (sigma-allyl)palladium complex, in slow equilibrium with the (eta(3)-allyl)palladium complex.

Adrenergic Antagonists↗
PubMed2003

Sensitization to palladium chloride: a 10-year evaluation.

BACKGROUND: Palladium is increasingly used in industry, jewelry, and dentistry and is becoming more common since the European directive restricting the use of nickel in all products placed in direct and prolonged contact with the skin. OBJECTIVE: The role of palladium sensitization is still unclear, and the aim of our study is to evaluate the trend of sensitization in a contact dermatitis clinic population during a 10-year period. METHODS: We report our experience with 4,446 patients (3,077 female, 1,369 male; mean age, 40.1 +/-13.7 years) with suspected contact dermatitis patch-tested during the period of 1991 to 2000. RESULTS: A positive patch-test result to palladium chloride 1% was indicated in 236 patients (5.3%), with a higher percentage in females (6.7%) than in males (2.3%), and the sensitization to this metal has increased over the specified period, to a maximum in the year 2000 (9.7%). In the majority of cases, subjects were polysensitized (92.8%), but 7.2% of subjects were patch-test positive only to palladium. Of palladium-sensitized patients, 40.5% complained of hand dermatitis, 47.4% complained of body dermatitis, and 1.7% complained of burning mouth syndrome. Palladium sensitization is significantly related to female sex (OR = 3.08; 95% CI, 2.07-4.61) and to sensitization to other metals, with a maximum for nickel sulfate (OR = 32.9; 95% CI, 21.3-51.5). CONCLUSION: Sensitization to palladium is increasing by the year, reaching high values, but its role in reducing sensitization and symptoms is still unclear because of the frequent cosensitization with nickel and the low number of monosensitized patients with relevant sensitizations. We need to follow palladium sensitization in future years to verify an increase of sensitization due to the increasing use of this metal.

Adult↗
PubMed2004

Preparation of thin films comprising palladium nanoparticles by a solid-liquid interface reaction technique.

A new approach to the formation of palladium nanoparticulate films with diameter between 6 and 50 nm by the solid-liquid interface reaction technique (SLIRT) has been presented. A solid film of palladium nitrate was formed by the modified spin coating method. This film is subsequently immersed in a reducing solution to initiate a reaction at the interface and ultimately transforms it to a palladium metal film. The kinetics of palladium reduction has been studied by UV-visible spectroscopy. The characterization of the palladium film has been performed by various physicochemical techniques such as XRD, ED, XPS, SEM, EDX, TEM, and UV-visible spectroscopy. The texture and morphology of the materials has been investigated by atomic force microscopy (AFM). At a constant palladium nitrate concentration, the average diameter of palladium nanoparticles decreases with an increase of hydrazine concentration. The effect of concentration of hydrazine on the particle size has been discussed. The palladium film formation mechanism has been proposed for the SLIRT.

Journal Article↗
PubMed2006

Interaction of CO with palladium supported on oxidized tungsten.

A model catalyst system, palladium on tungsten oxide, has been examined by temperature-programmed desorption and photoemission spectroscopy. The samples were prepared by evaporation of palladium onto an oxidized tungsten foil under ultrahigh vacuum conditions. Mostly three-dimensional (3-D) palladium (Pd) clusters were found to be present on oxidized tungsten (WOx) surfaces at room temperature. Upon annealing to 670 K, the palladium clusters are redispersed and decorated by the WOx surface layer. The nature of the WOx phase on top of the palladium clusters is dependent on the mode of oxidation of the tungsten foil prior to palladium deposition. Mainly W(2+) species decorate palladium deposits on tungsten oxidized at room temperature, while mainly W(4+) species are on top of palladium deposits on the surface oxidized at 1300 K. The appearance of a Pd(n+)-O-W(4+) mixed oxide phase with n < 2 was observed on the oxidized tungsten surface. The substantial reduction (relative to nonannealed samples) of molecular CO coverage induced by annealing is discussed in terms of the changes in chemical composition and morphology of the outermost surface.

Journal Article↗
PubMed2006

Palladium nanostructures and nanoparticles from molecular precursors on highly ordered pyrolytic graphite.

Nanostructures and nanoparticles of palladium assembled on highly ordered pyrolytic graphite (HOPG) by the adsorption of palladium molecular precursors (MPs), in dichloromethane solutions, have been prepared. Self-assemblies of palladium nanostructures on HOPG were characterized by scanning electron microscopy (SEM), Auger electron spectroscopy (AES), transmission electron microscopy (TEM), and atomic force microscopy (AFM) techniques. In this work, palladium rings had a wide variety of sizes in the nanometer range, and the ring/tube structures were preserved after a reductive process in which palladium metallic nanoparticles were formed. Noncircular structures were observed at HOPG defects and atomic step sites, as well. It is proposed that the observed ring formation of the palladium molecular precursors on HOPG substrates is related to the functional groups in the MPs, van der Waals interactions between particles and between particle-substrate, as well as the wetting properties of the solvent. In the present work, we illustrate several examples of the formation and characterization of palladium complex tubes and the resulting palladium rings, via the reduction process.

Journal Article↗