Investigation into accurate mass capability of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, with respect to radical ion species

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) has been shown to be an effective technique for the characterization of organometallic, coordination, and highly conjugated compounds. The preferred matrix is 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB), with radical ions observed. However, MALDI-TOFMS is generally not favored for accurate mass measurement. A specific method had to be developed for such compounds to assure the quality of our accurate mass results. Therefore, in this preliminary study, two methods of data acquisition, and both even-electron (EE+) ion and odd-electron (OE+.) radical ion mass calibration standards, have been investigated to establish the basic measurement technique. The benefit of this technique is demonstrated for a copper compound for which ions were observed by MALDI, but not by electrospray (ESI) or liquid secondary ion mass spectrometry (LSIMS); a mean mass accuracy error of -1.2 ppm was obtained.     

The Existence of Latin Squares without Orthogonal Mates

A latin square is a bachelor square if it does not possess an orthogonal mate; equivalently, it does not have a decomposition into disjoint transversals. We define a latin square to be a confirmed bachelor square if it contains an entry through which there is no transversal. We prove the existence of confirmed bachelor squares for all orders greater than three. This resolves the existence question for bachelor squares.     

An improved holey carbon film for cryo-electron microscopy.

Two issues that often impact the cryo-electron microscopy (cryoEM) specimen preparation process are agglomeration of particles near hole edges in holey carbon films and variations in vitreous ice thickness. In many cases, the source of these issues was identified to be the residues and topography often seen in commercially available films. To study and minimize their impact during specimen preparation, an improved holey carbon film has been developed. Rather than using a consumable template based on soft materials that must be removed prior to grid assembly, a method was developed that uses a hard template and a water-soluble release layer to replicate the template pattern into the carbon films. The advantages of this method are the improved purity and flatness of the carbon films, and these attributes are shown to have a dramatic improvement on the distribution of single particles embedded in vitreous ice suspended across the holes. Improving particle distribution is an enabling factor toward increasing the throughput of data collection for cryoEM.     

What is an infinite design?

It is usually assumed that an infinite design is a design with infinitely many points. This encompasses a myriad of structures, some nice and others not. In this paper we consider examples of structures that we would not like to call designs, and investigate additional conditions that exclude such anomalous structures. In particular, we expect a design to be regular, the complement of a design to be a design, and a t‐design to be an s‐design, for all 0 < s ≤ t. These are all properties that can be taken for granted with finite designs, and for infinite Steiner systems. We present a new definition of an infinite t‐design, and give examples of structures that satisfy this definition. We note that infinite designs considered in the literature to date satisfy our definition. We show that infinite design theory does not always mirror finite design theory, for example there are examples of designs with υ > b. © 2002 Wiley Periodicals, Inc. J Combin Designs 10: 79–91, 2002; DOI 10.1002/jcd.10005     

DuPont qualicon BAX system real-time PCR assay for Escherichia coli O157:H7

Evaluations were conducted to test the performance of the BAX System Real-Time PCR assay, which was certified as Performance Tested Method 031002 for screening E. coli O157:H7 in ground beef, beef trim, spinach, and lettuce. Method comparison studies performed on samples with low-level inoculates showed that the BAX System demonstrates a sensitivity equivalent or superior to the FDA-BAM and the USDA-FSIS culture methods, but with a significantly shorter time to result. Tests to evaluate inclusivity and exclusivity returned no false-negative and no false-positive results on a diverse panel of isolates, and tests for lot-to-lot variability and tablet stability demonstrated consistent performance. Ruggedness studies determined that none of the factors examined affect the performance of the assay. An accelerated shelf life study determined an initial 36 month shelf life for the test kit.     

Poly(perfluoroalkylation) of metallic nitride fullerenes reveals addition-pattern guidelines: synthesis and characterization of a family of Sc3N@C80(CF3)n (n = 2-16) and their radical anions

A family of highly stable (poly)perfluoroalkylated metallic nitride cluster fullerenes was prepared in high-temperature reactions and characterized by spectroscopic (MS, (19)F NMR, UV-vis/NIR, ESR), structural and electrochemical methods. For two new compounds, Sc(3)N@C(80)(CF(3))(10) and Sc(3)N@C(80)(CF(3))(12,) single crystal X-ray structures are determined. Addition pattern guidelines for endohedral fullerene derivatives with bulky functional groups are formulated as a result of experimental ((19)F NMR spectroscopy and single crystal X-ray diffraction) studies and exhaustive quantum chemical calculations of the structures of Sc(3)N@C(80)(CF(3))(n) (n = 2-16). Electrochemical studies revealed that Sc(3)N@C(80)(CF(3))(n) derivatives are easier to reduce than Sc(3)N@C(80), the shift of E(1/2) potentials ranging from +0.11 V (n = 2) to +0.42 V (n = 10). Stable radical anions of Sc(3)N@C(80)(CF(3))(n) were generated in solution and characterized by ESR spectroscopy, revealing their (45)Sc hyperfine structure. Facile further functionalizations via cycloadditions or radical additions were achieved for trifluoromethylated Sc(3)N@C(80) making them attractive versatile platforms for the design of molecular and supramolecular materials of fundamental and practical importance.     

Microtubule‐Templated Cadmium Sulfide Nanotube Assemblies

This paper describes the use of microtubules (MTs) as nanoscale templates for the biologically directed growth and assembly of cadmium sulfide (CdS) nanotubes. CdS is a wide bandgap semiconductor with valuable optical, electronic, and chemical properties, and the organization of CdS nanostructures is critical to their widespread utility. The present work explores a bioinspired, biomediated approach to the formation and assembly of CdS nanotubes. In particular, a biomimetic synthetic strategy is used to control the uniform growth of cubic zinc blende CdS nanocrystals on MT templates, replicating the MTs' tubular morphology with dense CdS only a single nanocrystal thick. Furthermore, specific interactions between MTs and functional microtubule‐associated proteins (MAPs) are exploited to manipulate the secondary organization of these MT templates. The subsequent directed growth of CdS nanotubes on these structures produces specific biomediated architectures including linear arrays, 3D asters, and rings. Finally, cathodoluminescence from MT‐templated CdS structures verifies that the valuable semiconducting character of these materials is exhibited. These demonstrations of nanoscale materials synthesis and assembly illustrate a new level of complexity and control over materials synthesis that may be achieved using such biological tools and processes.     

Electrochemical template synthesis of multisegment nanowires: fabrication and protein functionalization

Multisegment nanowires represent a unique platform for engineering multifunctional nanoparticles for a wide range of applications. For example, the optical and magnetic properties of nanowires can be tailored by modifying the size, shape, and composition of each segment. Similarly, surface modification can be used to tailor chemical and biological properties. In this article, we report on recent work on electrochemical template synthesis of nanogap electrodes, the fabrication of multisegment nanowires with embedded catalysts, and the selective functionalization of multisegment nanowires with proteins.     

Characterizing the topography of membrane receptors and signaling molecules from spatial patterns obtained using nanometer-scale electron-dense probes and electron microscopy

The flow of information through a cell requires the constant remodeling of cell signaling networks. Thus, spatially and temporally resolved microscopy of signaling components is needed to understand the behavior of normal cells as well as to uncover abnormal behavior leading to human disease. Nanoprobe labeling and transmission electron microscopy of cytoplasmic face-up sheets of cell membrane have been developed as a high-resolution approach to map the interactions of proteins and lipid during cell signaling. Membrane sheets are labeled with 3-15 nm electron-dense probes for receptors, signaling proteins and lipids and micrographs record the distributions of the probes relative to each other and to surface features. Here, we establish computational methods to extract spatial coordinates of probes from micrographs, to analyze and statistically validate the clustering and co-clustering of these probes and to integrate results between experiments in order to establish the relative spatial distributions of single and multiple probes. Our analyses, and the resulting programs for automating data collection and for carrying out statistical and clustering analyses provide toolboxes specialized for the spatiotemporal analysis and modeling of signal transduction pathways.     

The effects of environmental and classroom noise on the academic attainments of primary school children

While at school children are exposed to various types of noise including external, environmental noise and noise generated within the classroom. Previous research has shown that noise has detrimental effects upon children's performance at school, including reduced memory, motivation, and reading ability. In England and Wales, children's academic performance is assessed using standardized tests of literacy, mathematics, and science. A study has been conducted to examine the impact, if any, of chronic exposure to external and internal noise on the test results of children aged 7 and 11 in London (UK) primary schools. External noise was found to have a significant negative impact upon performance, the effect being greater for the older children. The analysis suggested that children are particularly affected by the noise of individual external events. Test scores were also affected by internal classroom noise, background levels being significantly related to test results. Negative relationships between performance and noise levels were maintained when the data were corrected for socio-economic factors relating to social deprivation, language, and special educational needs. Linear regression analysis has been used to estimate the maximum levels of external and internal noise which allow the schools surveyed to achieve required standards of literacy and numeracy.