An electron microscopic study of nickel sulfide inclusions in toughened glass

It has been known since the early sixties that nickel sulfide inclusions cause spontaneous fracture of toughened (thermally tempered) glass, but despite the considerable amount of work done on this problem in the last four decades, failures still occur in the field with regularity. In this study we have classified (by viewing through a 60x optical microscope) inclusions into two groups, which are classic and atypical nickel sulfides. The classics look like the nickel sulfide inclusions found at the initiation-of-fracture of windows that have broken spontaneously. We have compared the structure and composition of the atypical inclusions with the structure and composition of the classics. All of the classic and atypical nickel sulfide inclusions studied in this work were found to have a composition in the range of Ni52S48 to Ni48S52. Inclusions on the nickel rich side of stoichiometric NiS were found to be two-phase assemblies, and inclusions on the sulphur rich side of NiS were single phase. It had been proposed that the atypicals were passive, and of a different composition to the classics. However, we found that the difference between passive and dangerous nickel sulfide inclusions was not a difference in composition but rather a difference in the type of material in the internal pore space. The passive's had carbon char in their internal pore space, whereas the pore space of dangerous inclusions contained Na2O. The presence of Na2O and carbon char with the inclusions indicates that the formation of the inclusions results from a reaction of a nickel-rich phase with sodium sulphate and carbon. (C) 2001 Kluwer Academic Publishers.

Post space cleaning using a new nickel titanium endodontic drill combined with different cleaning regimens

This study compared the effect of two drills and five cleaning regimens on post space debridement. One hundred extracted premolars were instrumented and obturated with warm vertical compaction of gutta percha. The teeth were divided into two groups according to the drill used to remove gutta percha/sealer and for post space preparation: a Largo drill (Largo; Dentsply, St Quentin en Yvelines, France) or a MTwo-PF drill (Sweden&Martina, Due Carrare, Padova, Italy). The following cleaning regimens were used: EDTA, ultrasonics, ultrasonics + EDTA, phosphoric acid, and distilled water. Scanning electron microscopic images of the post spaces were taken, and the presence of debris and of open dentin tubules were evaluated. The ultrasonics + EDTA, phosphoric acid, and EDTA groups were comparable in open tubules scores for both drills and in debris scores after the use of MTwo-PF (p > 0.05). The ultrasonics and control groups performed significantly worse (p < 0.05). The MTwo-PF drill resulted as effective as the Largo drill in obtaining a good post space cleaning, especially when followed by ultrasonics + EDTA irrigant regimen.

Influence of shaft design on the shaping ability of 3 nickel-titanium rotary systems by means of spiral computerized tomography

Objective. To evaluate the influence of shaft design on the shaping ability of 3 rotary nickel-titanium (NiTi) systems. Study design. Sixty curved mesial canals of mandibular molars were used. Specimens were scanned by spiral tomography before and after canal preparation using ProTaper, ProFile, and ProSystem GT rotary instruments. One-millimeter-thick slices were scanned from the apical end point to the pulp chamber. The cross-sectional images from the slices taken earlier and after canal preparation at the apical, coronal, and midroot levels were compared. Results. The mean working time was 137.22 +/- 5.15 s. Mean transportation, mean centering ratio, and percentage of area increase were 0.022 +/- 0.131 mm, 0.21 +/- 0.11, and 76.90 +/- 42.27%, respectively, with no statistical differences (P > .05). Conclusions. All instruments were able to shape curved mesial canals in mandibular molars to size 30 without significant errors. The differences in shaft designs seemed not to affect their shaping capabilities.

New nickel catalysts supported on highly porous alumina intercalated laponite for methane reforming with CO2

Alumina intercalated laponite (Al-laponite) was prepared with a polyethylene oxide (PEO) surfactant and used as supports of nickel catalysts for the carbon dioxide reforming reaction with methane to synthesis gas. The effects of the supports of intercalated laponite and catalyst preparation on catalytic activity, stability and carbon deposition were investigated for the above reforming reaction. We found that the pore structure of the Al-laponite supports can be tailored with the surfactant and the catalyst with well-developed porosity exhibited higher catalytic activity and a longer time of catalyst stability. (C) 2001 Elsevier Science B.V. All rights reserved.

Preparation and characterization of Nickel-and cobalt-doped magnetites

Trabalho apresentado no I Simpósio Mineiro de Ciências dos Materiais, Ouro Preto, Novembro de 2001.

BASS 4: a software system for ergonomic design and evaluation of working hours

OBJECTIVE: To extend an existing computer programme for the evaluation and design of shift schedules (BASS 3) by integrating workload as well as economic aspects. METHODS: The redesigned prototype BASS 4 includes a new module with a suitable and easily applicable screening method (EBA) for the assessment of the intensity of physical, emotional and cognitive workload components and their temporal patterns. Specified criterion functions based on these ratings allow for an adjustment of shift and rest duration according to the intensity of physical and mental workload. Furthermore, with regard to interactive effects both workload and temporal conditions, e.g. time of day, are taken into account. In a second new module, important economic aspects and criteria have been implemented. Different ergonomic solutions for scheduling problems can now also be evaluated with regard to their economic costs. RESULTS: The new version of the computer programme (BASS 4) can now simultaneously take into account numerous ergonomic, legal, agreed and economic criteria for the design and evaluation of working hours. CONCLUSIONS: BASS 4 can now be used as an instrument for the design and the evaluation of working hours with regard to legal, ergonomic and economic aspects at the shop floor as well as in administrative (e.g. health and safety inspection) and research problems.

Formation of oriented nickel aggregates in rutile single crystals by Ni implantation

The magnetic and electrical properties of Ni implanted single crystalline TiO2 rutile were studied for nominal implanted fluences between 0.5 x 10(17) cm(-2) and 2.0 x 10(17) cm(-2) with 150 keV energy, corresponding to maximum atomic concentrations between 9 at% and 27 at% at 65 nm depth, in order to study the formation of metallic oriented aggregates. The results indicate that the as implanted crystals exhibit superparamagnetic behavior for the two higher fluences, which is attributed to the formation of nanosized nickel clusters with an average size related with the implanted concentration, while only paramagnetic behavior is observed for the lowest fluence. Annealing at 1073 K induces the aggregation of the implanted nickel and enhances the magnetization in all samples. The associated anisotropic behavior indicates preferred orientations of the nickel aggregates in the rutile lattice consistent with Rutherford backscattering spectrometry-channelling results. Electrical conductivity displays anisotropic behavior but no magnetoresistive effects were detected. (C) 2013 Elsevier B.V. All rights reserved.

Copper, nickel and zinc removal by peanut hulls: batch and column studies in mono, tri-component systems and with real effluent

The main goal of this research study was the removal of Cu(II), Ni(II) and Zn(II) from aqueous solutions using peanut hulls. This work was mainly focused on the following aspects: chemical characterization of the biosorbent, kinetic studies, study of the pH influence in mono-component systems, equilibrium isotherms and column studies, both in mono and tri-component systems, and with a real industrial effluent from the electroplating industry. The chemical characterization of peanut hulls showed a high cellulose (44.8%) and lignin (36.1%) content, which favours biosorption of metal cations. The kinetic studies performed indicate that most of the sorption occurs in the first 30 min for all systems. In general, a pseudo-second order kinetics was followed, both in mono and tri-component systems. The equilibrium isotherms were better described by Freundlich model in all systems. Peanut hulls showed higher affinity for copper than for nickel and zinc when they are both present. The pH value between 5 and 6 was the most favourable for all systems. The sorbent capacity in column was 0.028 and 0.025 mmol g-1 for copper, respectively in mono and tri-component systems. A decrease of capacity for copper (50%) was observed when dealing with the real effluent. The Yoon-Nelson, Thomas and Yan’s models were fitted to the experimental data, being the latter the best fit.

Synthesis, characterization and reactivity of new cobalt, palladium and nickel complexes bearing α-diimines and P, O ligands

This work describes the synthesis and characterization of a series of new α-diimine and P,O, β-keto and acetamide phosphines ligands, and their complexation to Ni(II), Co(II),Co(III) and Pd(II) to obtain a series of new compounds aiming to study their structural characteristics and to test their catalytic activity. All the compounds synthesized were characterized by the usual spectroscopic and spectrometric techniques: Elemental Analysis, MALDI-TOF-MS spectrometry, IR, UV-vis, 1H, 13C and 31P NMR spectroscopies. Some of the paramagnetic compounds were also characterized by EPR. For the majority of the compounds it was possible to solve their solid state structure by single crystal X-ray diffraction. Tests for olefin polymerization were performed in order to determine the catalytic activity of the Co(II) complexes. Chapter I presents a brief introduction to homogenous catalysis, highlighting the reactions catalyzed by the type of compounds described in this thesis, namely olefin polymerization and oligomerization and reactions catalyzed by the complexes bearing α-diimines and P,O type ligands. Chapter II is dedicated to the description of the synthesis of new α-diimines cobalt (II) complexes, of general formula [CoX2(α-diimine)], where X = Cl or I and the α-diimines are bis(aryl)acenaphthenequinonediimine) (Ar-BIAN) and 1,4-diaryl-2,3-dimethyl-1,4-diaza-1,3-butadiene (Ar-DAB). Structures solved by single crystal X-ray diffraction were obtained for all the described complexes. For some of the compounds, X-band EPR measurements were performed on polycrystalline samples, showing a high-spin Co(II) (S = 3/2) ion, in a distorted axial environment. EPR single crystal experiments on two of the compounds allowed us to determine the g tensor orientation in the molecular structure. In Chapter III we continue with the synthesis and characterization of more cobalt (II)complexes bearing α-diimines of general formula [CoX2(α-diimine)], with X = Cl or I and α-diimines are bis(aryl)acenaphthenequinonediimine) (Ar-BIAN) and 1,4-diaryl-2,3-dimethyl- 1,4-diaza-1,3-butadiene (Ar-DAB). The structures of three of the new compounds synthesized were determined by single crystal X-ray diffraction. A NMR paramagnetic characterization of all the compounds described is presented. Ethylene polymerization tests were done to determine the catalytic activity of several of the Co(II) complexes described in Chapter II and III and their results are shown. In Chapter IV a new rigid bidentate ligand, bis(1-naphthylimino)acenaphthene, and its complexes with Zn(II) and Pd(II), were synthesized. Both the ligand and its complexes show syn and anti isomers. Structures of the ligand and the anti isomer of the Pd(II) complex were solved by single crystal X-ray diffraction. All the compounds were characterized by elemental analysis, MALDI-TOF-MS spectrometry, and by IR, UV-vis, 1H, 13C, 1H-1H COSY, 1H-13C HSQC, 1H-13C HSQC-TOCSY and 1H-1H NOESY NMR when necessary. DFT studies showed that both conformers of [PdCl2(BIAN)] are isoenergetics and can be obtain experimentally. However, we can predict that the isomerization process is not available in square-planar complex, but is possible for the free ligand. The molecular geometry is very similar in both isomers, and only different orientations for naphthyl groups can be expected. Chapter V describes the synthesis of new P, O type ligands, β-keto phosphine, R2PCH2C(O)Ph, and acetamide phosphine R2PNHC(O)Me, as well as a series of new cobalt(III) complexes namely [(η5-C5H5)CoI2{Ph2PCH2C(O)Ph}], and [(η5- C5H5)CoI2{Ph2PNHC(O)Me}]. Treating these Co(III) compounds with an excess of Et3N, resulted in complexes η2-phosphinoenolate [(η5-C5H5)CoI{Ph2PCH…C(…O)Ph}] and η2- acetamide phosphine [(η5-C5H5)CoI{Ph2PN…C(…O)Me}]. Nickel (II) complexes were also obtained: cis-[Ni(Ph2PN…C(…O)Me)2] and cis-[Ni((i-Pr)2PN…C(…O)Me)2]. Their geometry and isomerism were discussed. Seven structures of the compounds described in this chapter were determined by single crystal X-ray diffraction. The general conclusions of this work can be found in Chapter VI.