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PubMed1995

Inhibition of cellobiohydrolase I from Trichoderma reesei by palladium.

Cellulase from Trichoderma reesei is a multienzyme mixture that hydrolyzes cellulose to glucose. Two enzymes in this mixture, cellobiohydrolase (CBH) and endoglucanase (EG), possess a common structure comprising a distinct cellulose-binding domain (CBD) and catalytic domain. Inhibition of the catalytic domain of cellulases without affecting their CBD function might be useful for structure/function studies of these enzymes. Complexes of the platinum group metals were tested for their ability to inhibit the major cellulase enzyme from T. reesei, cellobiohydrolase I (CBH I). Only palladium complexes inhibited CBH I, inhibition being dependent upon the molar ratio of palladium to CBH I with 1 microM CBH I retaining only 10% of its activity in the presence of 100 microM ammonium hexachloropalladate(IV) and after the incorporation of 28 mol Pd/mol CBH I. Inhibition was irreversible and could be completely prevented by including histidine, cysteine, and cystine in the assay mixture. Although the primary mechanism of inhibition of CBH I by palladium remains to be elucidated, it could involve the binding of palladium to sulfur or cystine residues resulting in their degradation. This is based on the findings that (i) palladium-inhibited CBH I was less thermally stable than native CBH I; (ii) CBH I, chemically modified by the attachment of pentaammine ruthenium(III) to the imidazole-N of either H206 or H228, showed greater sensitivity to inhibition by palladium compared to native CBH I; and (iii) ammonium hexachloropalladate cleaved 5,5'-dithiobis(2-nitrobenzoic acid)--Ellman's reagent. Binding of CBH I to crystalline cotton linters was not affected by palladium.

Amino Acids↗
PubMed2003

Evaluation of the long-term corrosion behavior of dental amalgams: influence of palladium addition and particle morphology.

OBJECTIVES: The purpose of this investigation was to evaluate the long-term corrosion behavior of experimental amalgams as a function of particle morphology and palladium content. METHODS: Samples of four experimental high copper amalgams were prepared according to ADA specifications. Two of them had the same chemical composition but one had lathe cut particles (LCP) and the other had spherical particles (SP). The two others had spherical powders with an addition of 0.5 wt% of palladium (SP 0.5) and 1 wt% of palladium(SP 1) for the other. Corrosion resistance was evaluated by electrochemical techniques in Ringer's solution in a thermostated cell at 37 degrees C for samples aged 5, 8, 12, 16 months and 10 years. Potentiokinetic curves were drawn and the potential and the current density corresponding to the first anodic peak were registered. RESULTS: For all the amalgam samples the corrosion behavior improves over the 10-year period. SP samples exhibit a better behavior than LCP. Palladium addition improves corrosion behavior as compared to samples without palladium. No real difference is found regarding the amount of palladium between 0.5 and 1%. The potentials progress from a range between 0 and 20 mV/SCE to a range of 60-80 after 10 years. The stabilization of the potential begins after only 16 months. Except for the LCP, all the values converge to the same level of 80 mV/SCE. SIGNIFICANCE: The addition of no more than 0.5 wt% Palladium in a high copper amalgam powder improves the corrosion behavior of the amalgam up to a period of 10 years. The potential of the first anodic peak increases for each amalgam, probably in relation to the evolution of the structure of the material. Clinically, it is of interest to consider the good electrochemical behavior of older restorations when contemplating the repair or replacement of such fillings. At the same time, galvanic current can occur when a new amalgam restoration is placed in contact with an old one even if the same amalgam is used. In this situation, the new filling will be anodic and its degradation will be accelerated. The evaluation of the corrosion behavior of dental amalgams has to take into account the age of the samples.

Copper↗
PubMed1999

Effects of palladium addition on emission of mercury vapor from dental amalgam.

OBJECTIVES: The purpose of this investigation was to test the hypothesis that palladium causes a reduction in mercury emission when added to dental amalgam during condensation. METHODS: Mercury vapor release was measured in a closed bottle system and an Intraoral Flow device(IOF). Conventional amalgam restorations were modified by addition of various palladium pellets. 1.57 mm diameter palladium pellets with different porosities were fabricated. These pellets were then placed in amalgam restoration using typical condensation and carving procedures. The samples were stored in a closed bottle and mercury measurements were taken from the bottles at 30 min, 1, 3, 5, 24 and 48 h and 7 days after trituration using a Jerome 411 Mercury Vapor Analyzer (Arizona Instrument Corp., Jerome, AZ). The palladium pellets identified as the most effective in mercury vapor reduction were further tested in an IOF device. Data were analyzed by two-way ANOVA followed by Tukey HSD pairwise analysis for significant findings (alpha = 0.05). RESULTS: The palladium containing amalgams when tested in the closed bottle system yielded significantly lower (p < 0.05) mercury vapor release than the controls. Pellets fabricated with the highest porosity yielded the greatest reduction in overall mercury vapor release. In the IOF device the overall amount of mercury vapor released from the palladium containing amalgams was also significantly less than the control (p < 0.05). SIGNIFICANCE: Mercury vapor emission from dental amalgam was greatly reduced by adding palladium pellets to amalgam during condensation. These techniques require only slight modifications of the standard operative procedures.

Air Pollutants, Occupational↗
PubMed1978

Palladium chloride as a stain for elastin at the ultrastructural level.

Palladium chloride in aqueous solution stains elastic fibers in thin sections of Epon-embedded tissues. When palladium chloride is used with a lead citrate counterstain, high contrast sections with gray to black elastic fibers are obtained. The stain was tested on newborn and adult mammalian tissues and on adult tissues from lower animals. Sections were mounted on stainless steel grids, stained with 1% palladium chloride solution for 5 to 15 min, rinsed thoroughly, and counterstained with lead citrate for 7 min. Palladium chloride staining solution is stable for several months at room temperature and if the stain is filtered immediately before use, contamination of sections is not a problem. Chemical studies indicate that palladium binds directly to purified bovine ligamentum nuchae elastin and that this binding is not affected by glutaraldehyde fixation or by sodium borohydride reduction of elastin. Osmium post-fixation of glutaraldehyde-fixed elastin did significantly lower the amount of palladium bound. Palladium was shown to be chemically bound to sites on the elastin and not weakly associated. The nature of these sites is discussed.

Air Sacs↗
PubMed2003

Second and first-derivative spectrophotometry for efficient simultaneous and individual determination of palladium and cobalt using 1-(2-pyridylazo)-2-naphthol in sodium dodecylsulfate micellar media.

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous and individual determination of palladium and cobalt at trace levels. PAN complexes of palladium and cobalt at neutral pH form green-color neutral complexes, which are soluble in aqueous SDS micellar media. Under optimum conditions, calibration graphs for individual determinations by zero and first-derivative spectrophotometry, and also for simultaneous determinations by second-derivative spectrophotometry were obtained. A zero-crossing method using second-derivative spectrophotometry at 628 or 578 and 614 nm, respectively, for cobalt and palladium was used for simultaneous determinations. The method is able to determine the cobalt-to-palladium ratio, 5:1 to 1:10 (Wt/Wt), accurately. The accuracy and reproducibility of the determination method for various known amounts of cobalt and palladium in their binary mixtures were tested. The effects of diverse ions on the determination of cobalt and palladium to investigate the selectivity of the method were also studied. The recommended procedures were applied to a synthetic binary alloy, cobalt in vitamin B12 and B-complex ampoules, a Co2O3-Co3O4 laboratorial chemical mixture, some synthetic cobalt-alloy samples, a Pd-charcoal catalyst, and some synthetic palladium alloys.

Alloys↗
PubMed1990

[Studies on the allergenic potential of palladium alloys].

Epicutaneous tests with test solutions of the European standard series and palladium chloride (1%) were performed in 486 patients of the University Hospital for Dermatology in Aachen. 17.9% of the patients exhibited Ni, 8.6% Co, 7.4% Pd and 4.1% Cr allergy. In 18 of 36 patients with a positive patch test reaction a further epicutaneous and epimucosal testing with metallic plates of pure palladium and a palladium alloy was performed. In 34 cases a positive skin reaction to palladium chloride was combined with a positive skin reaction to nickel sulphate. Only in one case was it possible to demonstrate an allergic reaction to a palladium metallic plate, which was tested additionally in artificial saliva. The results show that a dental alloy envisaged for use should be tested in an epicutaneous test, if the patient shows a positive reaction to the metallic salt solution. In case of positive patch tests to nickel sulphate, dental palladium alloys should not be used as an alternative unless sensitivity to palladium has been tested.

Dental Alloys↗
PubMed2001

Palladium-catalyzed cyclization of allylsilanes with nucleophilic displacement of the silyl group.

Allylsilanes containing hydroxy or tosylamide groups undergo palladium(II)catalyzed cyclization to afford derivatives of tetrahydrofuran, piperidine, and pyrrolidine. This catalytic reaction proceeds through an (eta3-allyl)palladium intermediate that is generated by allylic displacement of the silyl group of the allylsilane precursors. The internal nucleophilic attack on the (eta3-allyl)palladium intermediates proceeds with high chemo- and regioselectivity. Benzoquinone and copper(II) chloride can be used for regeneration of the palladium(II) catalyst precursor. Mechanistic studies revealed that the copper(II) chloride reoxidant also activates the (eta3-allyl)palladium intermediate towards nucleophilic attack. Kinetic studies on the formation of the (eta3-allyl)palladium intermediates showed that the reaction rate is highly dependent on the concentration of chloride ligand and the solvent. The structure and reactivity of the key intermediates of the palladadesilylation process were studied by density functional theory (DFT) calculations, which showed that coordination of the electrophilic palladium(II) catalyst precursor to allylsilanes leads to a relatively weak beta-silicon effect. The DFT studies also indicate that the cleavage of the carbon-silicon bond takes place by coordination of a chloride ion to the silicon atom.

Journal Article↗
PubMed1999

Synthesis, Characterization, and Reactivity of Palladium(II) Salen and Oxazoline Complexes.

Two methods for the syntheses of palladium(II) salen complexes are described. The first involves template synthesis of the ligand in which bis(salicylaldehydato)palladium(II), 2, is initially synthesized and reacted with the appropriate diamine bridge to yield the desired palladium salen. The template synthesis approach suffers, however, from low overall yields (17-30%). Alternatively, treatment of bis(acetonitrile)palladium(II) chloride with the appropriate salen ligand under inert atmosphere yields the palladium salen complex in high yields (80-85%). [2-(2'-Hydroxyphenyl)-2-oxazolinato]palladium(II), 7, was also synthesized. All the palladium complexes were fully characterized spectroscopically. A single-crystal X-ray structure of 7 has been solved. In contrast to previous reports, complex 2 was found to be stable over weeks and remained suitable for the template syntheses. The catalytic activity of complex 2 in cyclopropanation of alkenes with ethyl diazoacetate (EDA) was investigated. The catalyst is not functional group tolerant and works best for styrene; turnover numbers (TON's) of 45 were achieved. The availability of an open coordination site seems to be a prerequisite for catalytic decomposition of EDA.

Journal Article↗
PubMed2006

Experimental and theoretical investigations of new dinuclear palladium complexes as precatalysts for the amination of aryl chlorides.

A series of new palladium dinuclear species with general formula [Pd2X(mu-X)[mu-P(t)Bu2(Bph-R)]] (X = Cl, Br; Bph = biphenyl; R = H, Me, NMe2) have been prepared. The two palladium centers in these species are bridged by one of the aromatic rings of the biphenyl group present in the corresponding phosphine. The X-ray crystal structure of one of these complexes has been obtained, providing a clear picture of the bonding pattern. The stability of these dimers in solution is shown to be highly dependent on the nature of the phosphine R group and also on the bridging halide. When R = NMe2, the dimers dissociate, yielding the palladium(II) compounds PdX2[P(t)Bu2(BPh-NMe2)] (X = Cl, Br), and the X-ray crystal structure of one of them (X = Br) has shown that the biphenyl group from the phosphine interacts directly with the metal center. This interaction seems to play an important role in stabilizing the otherwise coordinatively unsaturated palladium(II) complex. In contrast, when R = H or Me, the analogous monomeric palladium(II) complexes are unstable and undergo cyclometalation to generate a palladium(II) dinuclear species in which each of the two phosphines cyclometalates with the palladium centers forming a strained four-membered ring. In addition to their unusual structures, these aryl-bridged dimers have also proven to be excellent precatalysts for the amination of aryl chlorides. To rationalize some of the experimental results, a detailed DFT computational study has been carried out and is presented herein.

Journal Article↗
PubMed2004

Palladium-catalyzed enantioselective allylic alkylation of thiocarboxylate ions: asymmetric synthesis of allylic thioesters and memory effect/dynamic kinetic resolution of allylic esters.

The palladium-catalyzed allylic alkylation of KSAc and KSBz with racemic cyclic and acyclic allylic esters by using N,N'-(1R,2R)-1,2-cyclohexandiylbis[2-(diphenylphosphino)-benzamide] as ligand frequently gave the corresponding allylic thioesters with high ee values and yields. The reaction of the cyclic allylic carbonates with KSAc in the presence of H(2)O was accompanied by a partial palladium-catalyzed enantioselective "hydrolysis" of the substrates with formation of the corresponding enantioenriched allylic alcohols. The degree of the "hydrolysis" was strongly dependent on the solvent and the thiocarboxylate ion. Highly selective kinetic resolutions (KRs) were observed in the palladium-catalyzed reaction of the racemic cyclohexenyl and cycloheptenyl acetates with KSAc. While the KR of the cyclohexenyl acetate is characterized by a selectivity factor S = 72 +/- 19, that of the cycloheptenyl acetate afforded (R)-cycloheptenyl acetate of >or=99% ee in 48% yield and (S)-cycloheptenyl thioacetate of 98% ee in 50% yield. The palladium-catalyzed reaction of the racemic cyclopentenyl acetate with KSAc showed a strong "memory effect" (ME), that is, both enantiomers reacted with different enantioselectivities. The ME was probed by studying the palladium-catalyzed reactions of both the matched acetate of >or=99% ee and the mismatched acetate of >or=99% ee with KSAc. The acetates not only reacted with different enantioselectivities and rates but also suffered an unexpected and concomitant palladium-catalyzed racemization in the presence of the chiral ligand. This led in the case of the mismatched acetate to a temporary dynamic kinetic resolution (DKR) that featured a racemization of the mismatched acetate by the chiral catalyst. Studies of the palladium-catalyzed reaction of the racemic cyclopentenyl acetate, carbonate, and naphthoate with KSAc in the presence of the chiral ligand also showed the ME to be strongly dependent on the nucleofuge. This also allowed the synthesis of (S)-cyclopentenyl thioacetate of 92% ee in high yield from the racemic cyclopentenyl naphthoate.

Journal Article↗
PubMed2006

Hydrogen capacity of palladium-loaded carbon materials.

Several samples of palladium-loaded single-wall carbon nanotubes and palladium-loaded MAXSORB activated carbon were prepared by means of the reaction of the raw carbon support with Pd2(dba)3.CHCl3. When carbon nanotubes were used as the support, the palladium content in the samples reached 13-31 wt % and fine particles of 5-7 nm average size were obtained. In the case of the samples with MAXSORB as the support, the palladium content was higher (30-50 wt %) and the particle size larger (32-42 nm) than in the nanotube samples. At 1 atm and room temperature, the hydrogen capacity of the palladium-loaded samples exceeds 0.1 wt % and is much higher than the capacity of the raw carbon supports (less than 0.01 wt %). The maximum hydrogen capacity at 1 atm and room temperature was found to be 0.5 wt %. A maximum hydrogen capacity of 0.7 wt % was obtained at 90 bar in a palladium-loaded MAXSORB sample, while the capacities for the raw carbon nanotubes and MAXSORB at the same pressure were 0.21 and 0.42 wt %, respectively. At low pressure, it was observed that the H/Pd atomic ratios in the palladium-loaded samples were always higher than in the bulk Pd. The spillover effect is considered as a possible cause of the high H/Pd atomic ratios. On the other hand, the effect of the pressure increase on the spillover was observed to be very low at high pressure and room temperature.

Journal Article↗
PubMed2002

Electrochemical impedance spectroscopy study of high-palladium dental alloys. Part I: behavior at open-circuit potential.

Electrochemical impedance spectroscopy (EIS) was used to study the in vitro corrosion of three representative high-palladium alloys and a gold-palladium alloy for comparison. The corrosion resistances (measured as the charge transfer resistance R(CT) from an equivalent circuit) of the high-palladium alloys and the gold-palladium alloy were comparable in simulated body fluid and oral environments, and under simulated dental plaque. The great similarity in corrosion behavior for the three high-palladium alloys is largely attributed to their substantial palladium content and passivity in the laboratory test media, and possibly to their similar structure at the submicron level. Differences in composition and microstructure at the micron level and greater, including the effects of heat treatment simulating the firing cycles for dental porcelain, do not have noteworthy effects on the in vitro corrosion of the three high-palladium alloys. Good accuracy and convenience of extracting corrosion characteristics from equivalent circuit modeling, along with the capability of providing intrinsic information about the corrosion mechanism, enable EIS to be an excellent alternative method to conventional potentiodynamic polarization for evaluating the corrosion behavior of noble dental alloys.

Journal Article↗
PubMedDate not supplied

Zero-crossing second derivative spectrophotometry for simultaneous determination of palladium and nickel using 1-(2-pyridylazo)-2-naphthol in mixed micellar solutions.

1-(2-Pyridylazo)-2-naphthol (PAN) has been used for the simultaneous determination of nickel and palladium at trace levels. PAN complexes of nickel and palladium in the pH 1.98 form red and green colored complexes, respectively, which are soluble in aqueous 4:1 Triton X-100 to sodium dodecylsulfate (SDS) micellar media with total detergent concentration of 3.2%. Under optimum conditions, calibration graphs for the simultaneous determination by second derivative spectrophotometry were obtained. Zero crossing second derivative spectrophotometry at 668 and 572 nm, respectively for palladium and nickel was used for the simultaneous determination. The method is able to determine palladium to nickel ratio 70:1 to 1:6 (Wt/Wt), accurately. Accuracy and reproducibility of the determination method on the known various amounts of palladium and nickel in their binary mixtures were tested. Effects of diverse ions on the determination of palladium and nickel to investigate selectivity of the method also were studied.

Detergents↗
PubMed2004

In vitro toxicity of palladium(II) and gold(III) porphyrins and their aqueous metal ion counterparts on Trypanosoma brucei brucei growth.

The trypanocidal effects of aqueous gold(III) and palladium(II) and their metalloporphyrin derivatives on Trypanosoma brucei brucei growth in culture have been studied using an Alamar Blue indicator assay. All the experiments were conducted in the dark. As previously described for mercury(II), cadmium(II) and lead(II) porphyrins [Chem.-Biol. Interact. 139 (2002) 177], the toxicity of the metalloporphyrin complex of palladium(II) to T. b. brucei parasites was much higher compared to the aqueous free palladium(II) and free base porphyrin. Palladium(II) porphyrin, free palladium(II), and the free base porphyrin were trypanocidal to T. b. brucei at concentrations >1.5 x 10(-6), >6.1 x 10(-6) and >1.9 x 10(-5) M, respectively. While gold(III) porphyrin was effective against the parasites at concentrations >4.8 x 10(-6) M, its aqueous gold(III) was toxic at concentrations as low as 2.0 x 10(-7) M due to the generation of free radicals in the presence of this metal ion which enhanced its toxicity to the T. b. brucei parasites. Although some cell division was observed in some of the cells treated with palladium(II) porphyrin, some dividing cells had no nucleus due to unequal division and delivery of the nuclei into the daughter cells. As a result, the rate of cell division decreased with time and cell death occurred within 24 h. Interestingly, trypanosomes treated with metalloporphyrin complexes displayed different morphological features from those cells treated with free base porphyrin or metal ions. Of all the porphyrins and free metal ions tested, only mercury(II) porphyrin and aqueous gold(III) ion were toxic to the trypanosomes in the 10(-7) M range. The chemotherapeutic potential of these observations is discussed.

Animals↗
PubMed2004

An in vitro model to evaluate cell adhesion to metals used in implantation shows significant differences between palladium and gold or platinum.

Adhesion of tissue cells to metallic implants is a major factor that is important for proper tissue integration. Adhesion of Swiss mouse 3T3 fibroblasts to gold, platinum and palladium surfaces was investigated. Immunofluorescence staining for the integrin subunits alphav and beta1 and the focal contact protein vinculin revealed that cells growing on gold and platinum expressed many focal contacts. In contrast, cells on palladium surfaces had reduced numbers of focal contacts shown by vinculin staining and failed to demonstrate expression of alphav and beta1 in focal contacts. Spread cell area was also significantly reduced on palladium than on other surfaces suggesting that cells on palladium were more weakly attached. This may be due to either a different molecular composition of focal contacts in cells grown on palladium surfaces or unusual microstructural properties of the palladium surface. This model is useful to evaluate adhesion of cells to different metal surfaces.

3T3 Cells↗
PubMed1997

Effect of addition of palladium on properties of Ag2Hg3 (gamma 1) phase.

The effect of palladium addition on the microstructure, compressive strength, creep rate and mercury release rate of Ag2Hg3 (gamma 1) phase was evaluated. Experimental results indicated that fairly pure gamma 1 phase could be fabricated using the present trituration method. The heat treatment of gamma 1 at 90 degrees C increased porosity level, increased dimensional shrinkage, increased mercury vapour release and enhanced the formation of beta1 phase. Addition of palladium in gamma 1 slowed down the amalgamation reaction, largely suppressed the phase transition to beta1 and caused a slight shift in open circuit potential toward the anodic direction. Although the overall anodic polarization profiles did not show a significant effect of palladium, scanning electron microscopy revealed morphological differences between pure and palladium-containing gamma 1. Addition of palladium in gamma 1 also increased compressive strength, increased creep resistance, and largely reduced both mercury vapour and ion release rates. Considering overall performance, the optimal palladium content in gamma 1 seems to be in the range between 0.50 and 0.75 wt%.

Dental Amalgam↗
PubMed2002

Self-assembled monolayers of alkanethiolates on palladium are good etch resists.

This paper describes microcontact printing (muCP) of long-chain alkanethiolates on palladium, followed by solution-phase etching with an iron(III)-based etchant, to make patterned structures. The commonly used soft-lithographic procedure for fabricating microstructures-muCP of SAMs on gold-has three shortcomings: a significant surface density of pinhole defects, substantial edge roughness, and incompatibility with processes used in CMOS fabrication. Microcontact printing on palladium gives fewer defects and smaller edge roughness than on gold, and is compatible with CMOS. The mechanism by which etch-resistant patterns are formed is different for palladium and gold. The Pd/S interfacial layer formed by the reaction of palladium films with sulfur-containing compounds provides good resistance to etches independently of the barrier to access the surface provided by the film of (CH2)n groups in the long-chain SAMs. This barrier is the basis of the etch resistance of SAMs on gold, but only supplements the etch resistance of the sulfur-containing interfacial layer on palladium. Characterization of the SAM formed from hexadecanethiol on palladium is described.

Microscopy, Electron, Scanning↗
PubMed2005

Direct synthesis of palladium porphyrins from acyldipyrromethanes.

[reaction: see text] Palladium porphyrins are valuable photosensitizers and luminescent agents in biology and materials chemistry. New methodology is described wherein a 1-acyldipyrromethane is converted into the palladium chelate of a trans-A(2)B(2) porphyrin via a one-flask reaction. The reaction entails self-condensation of the 1-acyldipyrromethane in refluxing ethanol containing KOH (5-10 mol equiv) and Pd(CH(3)CN)(2)Cl(2) (0.6 mol equiv) exposed to air. This direct route to palladium porphyrins is more expedient than the four steps of the traditional synthesis: (1) reduction of the 1-acyldipyrromethane; (2) acid-catalyzed condensation; (3) oxidation of the porphyrinogen intermediate; and (4) metal insertion. The new synthesis requires neither acid nor DDQ and formally entails only a 2e(-) + 2H(+) oxidation overall versus the traditional multistep synthesis which requires a 2e(-) + 2H(+) reduction per each 1-acyldipyrromethane (4e(-) + 4H(+) overall) followed by a 6e(-) + 6H(+) oxidation. The analogous reaction of a 1,9-diacyldipyrromethane and a dipyrromethane also gives the palladium porphyrin. Seven palladium porphyrins have been prepared in yields of 25-57%. The direct route also can be used with Cu(OAc)(2).H(2)O to give the copper porphyrin albeit in low yield. In summary, this methodology readily affords palladium porphyrins directly from acyldipyrromethanes.

Catalysis↗