Application of inductively coupled plasma mass spectrometry in biological samples analysis

Recent important applications of inductively coupled plasma mass spectrometry in biological samples analysis are reviewed. The sample preparation, sample introduction techniques, interference correction and typical applications are introduced in detail with 154 references.

Magnetic microsphere and its use in biochemical separation and analysis

Magnetic microsphere comprises a magnetically responsive metal or metal oxide core surrounded by a polymer shell with active groups. Nowadays, methods of directly coating polymer, monomer polymerazation, impregnation, extrusion and biological synthesis are generally used to prepare magnetic particles. This kind of superparamagnetic microspheres can be attached to chemical, biochemical and biological substances by their active groups, then applying a magnetic field to separate from the media. Preparation and utilization of magnetic microspheres in immunoassay, nucleic acid hybrization assay, gene sequencing, cell isolation, enzyme immoblization, receptor isolation and other Gelds are reviewed with 44 references in this paper. Also, the further development is outlooked.

Preparation, charactreization, and catalytic properties of Co-M-Al (M = transition metal) mixed oxides derived from hydrotalcite-like compound

Hydrotalcite-like compounds (HTLcs) CoMAlCO3, where M stands for Cr, Mn, Ni, Cu, or Fe, were synthesized by coprecipitation. After calcination at 450 degrees C, they became mixed oxides with spinel-like structure. The mixed oxides were characterized by XRD, BET, chemical analysis and the adsorption of NO. The catalytic decomposition of NO and its reduction by CO were studied over these mixed oxides. The study showed that the catalytic activity for removal of NO, was very high. The reaction mechanism is proposed and the effects of d-electrons of the transition metals on catalytic activity are elucidated.

Electrospray ionization multiple-stage tandem mass spectrometric analysis of diglycosyldiacylglycerol glycolipids from the bacteria Bacillus pumilus

Electrospray ionization (ESI) combined with multiple-stage tandem mass spectrometry (MSn) was used to directly analyze the glycolipid mixture from bacteria Bacillus pumilus without preliminary separation. Full scan ESI-MS revealed the composition of picomole quantities of glycerolglycolipid species containing C-14-C-19 fatty acids, some of which were monounsaturated, Two main components were identified from their molecular masses and fragmentation pathways. The fragmentation pathway of the known compound compared with the investigated compound verified the proposed structure as 1(3)-acyl-2-pentadecanoyl-3(1)-O-[beta-D-glucopyranosyl-(1-->6)-O-beta-D-glucopyranosyl]-sn-glycerols. A comparison of the multiple tandem mass spectra of the different alkali-metal cation adducts indicates that the intensity of fragments and the dissociation pathways are dependent on the alkali-metal type, The basic structures of glycerolglycolipids were reflected clearly from the fragmentation patterns of the sodium cations, The intense fragments of the sugar residue from the precursor ions were obtained from the lithiated adduct ions. ESI-MSn spectra of [M + K](+) ions did not provide as much fragmentation as [M + Na](+) and [M + Li](+) adducts, but their spectra allow the position of glycerol acylation to be determined. On the basis of MS2 spectra of[M + K](+) ions, it was established that all components have a C-15:0 fatty acid at the sn-2 position of the glycerol backbone and C-14-C-19 acids at the sn-1 position of the glycerol backbone. Copyright (C) 1999 John Wiley & Sons, Ltd.

Investigation on molecular and crystal structures of metal complexes with aminopolycarboxylic acids .1. Synthesis and structure of Na-2[Fe-III(ida)(2)](2)center dot 3H(2)O

The crystal structure of the title complex salt has been determined by single-crystal X-ray structure analysis. The crystal data areas follows; Monoclinic, P2(1)/c, a=15.6480(10)Angstrom, b=16.7870(10)Angstrom, c=10.347(2)Angstrom, beta=90.790(10), V=2717.7(6)Angstrom(3), Z=3, and R=0.0333 for 4789 unique reflections. The complex anion has a pseudo-octahedral structure distorted more than the Cr-III and Co-III analogs, in which each, iminodiacetato ligand (ida(2-)) is coordinated in a facial fashion with the two N atoms in a cis configuration, resulting in an unsym-fac structure.

TRACE ANALYSIS AT A MERCAPTOACETIC ACID-MODIFIED ELECTRODE

The strong chelating ability of mercaptoacetic acid for certain metal ions is exploited for a new; kind of voltammetric sensor. Specifically, a glassy carbon electrode (GCE) surface was covalently covered br; mercaptoacetic acid. The preparation of mercap

STUDIES ON THE REACTIONS OF TRANSITION-METAL HYDRIDES WITH HETEROCUMULENES .6. REACTION OF CP2ZR(H)CL WITH RNCS (R=C6H5, 2-C10H7, C-C6H11 AND N-C4H9)

The novel NS-containing zirconacycle complexes Cp2ZrCl[SC(H)NR] (1a, R = C6H5; 1b, R = 2-C10H7; 1c, R= C-C6H11; 1d; R = n-C4H9) were obtained by insertion reactions of Cp2Zr(H)Cl with RNCS. 1(a-d) could react further with Cp2Zr(H)Cl to yield a sulphur-bridging compleX (Cp2ZrCl)2S (2) and a Schiff base RN=CH2. The crystal structure of la has been determined by X-ray analysis.

MULTIVARIATE CLASSIFICATION BASED ON METAL CONTENTS IN HUMAN SENILE CATARACT LENSES

Multivariate classification methods were used to evaluate data on the concentrations of eight metals in human senile lenses measured by atomic absorption spectrometry. Principal components analysis and hierarchical clustering separated senile cataract lenses, nuclei from cataract lenses, and normal lenses into three classes on the basis of the eight elements. Stepwise discriminant analysis was applied to give discriminant functions with five selected variables. Results provided by the linear learning machine method were also satisfactory; the k-nearest neighbour method was less useful.

Assessment of metal contamination in surface sediments of Jiaozhou Bay, Qingdao, China

An assessment of metal contamination in surface sediments of the Jiaozhou Bay, Qingdao, one of the rapidly developing coastal economic zones in China, is provided. Sediments were collected from 10 stations and a total of 15 heavy metals were analyzed. Concentrations of metals show significant variability and range from 210 to 620 ppm for Ti, 2.7 to 23 ppm for Ni, 4.2 to 28 ppm for Cu, 5.2 to 18 ppm for Pb, 12 to 58 ppm for Zn, 0.03 to 0.11 ppm for Cd, 5 to 51 ppm for Cr, 1.5 to 9.9 ppm for Co, 5.3 to 19 ppm for As, 12 to 32 ppm for Se, and 19 to 97 ppm for Sr. Based on concentration relationships and enrichment factor (EF) analyses, the results indicate that sediment grain size and organic matter played important roles in controlling the distribution of the heavy metals in surface sediments of the Jiaozhou Bay. The study shows that the sediment of the Jiaozhou Bay has been contaminated by heavy metals to various degrees, with prominent arsenic contributing the most to the contamination. The analysis suggests that the major sources of metal contamination in the Jiaozhou Bay are land-based anthropogenic ones, such as discharge of industrial waste water and municipal sewage and run-off. Notably, the elevated heavy metal concentrations of the Jiaozhou Bay sediments could have a significant impact on the bay's ecosystem. With the rapid economic development and urbanization around the Jiaozhou Bay, coastal management and pollution control should focus on these contaminant sources, as well as provide ongoing monitoring studies of heavy metal contamination within the bay.

Partial oxidation of ethane to syngas over nickel-based catalysts modified by alkali metal oxide and rare earth metal oxide

The catalytic activity, thermal stability and carbon deposition of various modified NiO/gamma-Al2O3 and unmodified NiO/gamma-Al2O3 catalysts were investigated with a flow reactor, XRD, TG and UVRRS analysis. The activity and selectivity of the NiO/gamma-Al2O3 catalyst showed little difference from those of the modified nickel-based catalysts. However, modification with alkali metal oxide (Li, Na, K) and rare earth metal oxide (La, Ce, Y, Sm) can improve the thermal stability of the NiO/gamma-Al2O3 and enhance its ability to suppress carbon deposition during the partial oxidation of ethane (POE). The carbon deposition contains graphite-like species that were detected by UVRRS. The nickel-based catalysts modified by alkali metal oxide and rare earth metal oxide have excellent catalytic activities (C2H6 conversion of similar to 100%, CO selectivity of similar to 94%, 7x 10(4) l/(kg h), 1123 K), good thermal stability and carbon-deposition resistance.

On-line concentration of peptides and proteins with the hyphenation of polymer monolithic immobilized metal affinity chromatography and capillary electrophoresis

An iminodiacetic acid (IDA)-type adsorbent is prepared at the one end of a capillary by covalently bonding IDA to the monolithic rods of macroporous poly(glycidyl methacrylate-co-ethylene dimethacrylate). Cu(II) is later introduced to the support via the interaction with IDA. By this means, polymer monolithic immobilized metal affinity chromatography (IMAC) materials are prepared. With such a column, IMAC for on-line concentration and capillary electrophoresis (CE) for the subsequent analysis are hyphenated for the analysis of peptides and proteins. The reproducibility of such a column has been proved good with relative standard deviations (RSDs) of dead time of less than 5% for injection-to-injection and 12% for column-to-column (n = 3). Through application on the analysis of standard peptides and real protein samples, such a technique has shown promising in proteome study.

Invertebrates of ancient heavy metal spoil and smelting tip sites in southern Jordan: Thier distribution and use as bioindicators of metalliferous pollution derived from ancient sources

Pyatt, B. Amos, D. Grattan, J. Pyatt, A. Terrell-Nield, C. Invertebrates of ancient heavy metal spoil and smelting tip sites in southern Jordan: Thier distribution and use as bioindicators of metalliferous pollution derived from ancient sources. Journal of Arid Environments. 2002. 52 pp 53-62

Fabrication and characterisation of semiconductor nanowires and metal interconnects

One-dimensional semiconductor nanowires are considered to be promising materials for future nanoelectronic applications. However, before these nanowires can be integrated into such applications, a thorough understanding of their growth behaviour is necessary. In particular, methods that allow the control over nanowire growth are deemed especially important as it is these methods that will enable the control of nanowire dimensions such as length and diameter (high aspect ratios). The production of nanowires with high-aspect ratios is vital in order to take advantage of the unique properties experienced at the nanoscale, thus allowing us to maximise their use in devices. Additionally, the development of low-resistivity interconnects is desirable in order to connect such nanowires in multi-nanowire components. Consequently, this thesis aims to discuss the synthesis and characterisation of germanium (Ge) nanowires and platinum (Pt) interconnects. Particular emphasis is placed on manipulating the nanowire growth kinetics to produce high aspect ratio structures. The discussion of Pt interconnects focuses on the development of low-resistivity devices and the electrical and structural analysis of those devices. Chapter 1 reviews the most critical aspects of Ge nanowire growth which must be understood before they can be integrated into future nanodevices. These features include the synthetic methods employed to grow Ge nanowires, the kinetic and thermodynamic aspects of their growth and nanowire morphology control. Chapter 2 outlines the experimental methods used to synthesise and characterise Ge nanowires as well as the methods used to fabricate and analyse Pt interconnects. Chapter 3 discusses the control of Ge nanowire growth kinetics via the manipulation of the supersaturation of Ge in the Au/Ge binary alloy system. This is accomplished through the use of bi-layer films, which pre-form Au/Ge alloy catalysts before the introduction of the Ge precursor. The growth from these catalysts is then compared with Ge nanowire growth from standard elemental Au seeds. Nanowires grown from pre-formed Au/Ge alloy seeds demonstrate longer lengths and higher growth rates than those grown from standard Au seeds. In-situ TEM heating on the Au/Ge bi-layer films is used to support the growth characteristics observed. Chapter 4 extends the work of chapter 3 by utilising Au/Ag/Ge tri-layer films to enhance the growth rates and lengths of Ge nanowires. These nanowires are grown from Au/Ag/Ge ternary alloy catalysts. Once again, the supersaturation is influenced, only this time it is through the simultaneous manipulation of both the solute concentration and equilibrium concentration of Ge in the Au/Ag/Ge ternary alloy system. The introduction of Ag to the Au/Ge binary alloy lowers the equilibrium concentration, thus increasing the nanowire growth rate and length. Nanowires with uniform diameters were obtained via synthesis from AuxAg1-x alloy nanoparticles. Manifestation of the Gibbs-Thomson effect, resulting from the dependence of the mean nanowire length as a function of diameter, was observed for all of the nanowires grown from the AuxAg1-x nanoparticles. Finally, in-situ TEM heating was used to support the nanowire growth characteristics. Chapter 5 details the fabrication and characterisation of Pt interconnects deposited by electron beam induced deposition of two different precursors. The fabrication is conducted inside a dual beam FIB. The electrical and structural characteristics of interconnects deposited from a standard organometallic precursor and a novel carbon-free precursor are compared. The electrical performance of the carbon-free interconnects is shown to be superior to that of the organometallic devices and this is correlated to the structural composition of both interconnects via in-situ TEM heating and HAADF-STEM analysis. Annealing of the interconnects is carried out under two different atmospheres in order to reduce the electrical resistivity even further. Finally, chapter 6 presents some important conclusions and summarises each of the previous chapters.

Engineering of metal oxide interfaces for renewable energy applications

Diminishing non-renewable energy resources and planet-wide de-pollution on our planet are among the major problems which mankind faces into the future. To solve these problems, renewable energy sources such as readily available and inexhaustible sunlight will have to be used. There are however no readily available photocatalysts that are photocatalytically active under visible light; it is well established that the band gap of the prototypical photocatalyst, titanium dioxide, is the UV region with the consequence that only 4% of sun light is utilized. For this reason, this PhD project focused on developing new materials, based on titanium dioxide, which can be used in visible light activated photocatalytic hydrogen production and destruction of pollutant molecules. The main goal of this project is to use simulations based on first principles to engineer and understand rationally, materials based on modifying TiO2 that will have the following properties: (1) a suitable band gap in order to increase the efficiency of visible light absorption, with a gap around 2 – 2.5 eV considered optimum. (2). The second key aspect in the photocatalytic process is electron and hole separation after photoexcitation, which enable oxidation/reduction reactions necessary to i.e. decompose pollutants. (3) Enhanced activity over unmodified TiO2. In this thesis I present results on new materials based on modifying TiO2 with supported metal oxide nanoclusters, from two classes, namely: transition metal oxides (Ti, Ni, Cu) and p-block metal oxides (Sn, Pb, Bi). We find that the deposited metal oxide nanoclusters are stable at rutile and anatase TiO2 surfaces and present an analysis of changes to the band gap of TiO2, identifying those modifiers that can change the band gap to the desirable range and the origin of this. A successful collaboration with experimental researchers in Japan confirms many of the simulation results where the origin of improved visible light photocatalytic activity of oxide nanocluster-modified TiO2 is now well understood. The work presented in this thesis, creates a road map for the design of materials with desired photocatalytic properties and contributes to better understanding these properties which are of great application in renewable energy utilization.