Trace Analysis on Capillary Columns. Selected Practical Applications: Insecticides in Raw Butter Extract; Aroma Head Space from Liquors; Auto Exhaust Gas

Trace analysis on capillary columns becomes feasible provided appropriate injection techniques without stream splitting are used. To demonstrate potentialities and limitations of the methods, we investigated practical applications, the conditions of which were as dissimilar as possible. Insecticides in dairy products can be estimated by direct analysis of the raw petrol ether extract, without previous purification by column chromatography. 2-4 µl of extract are injected without splitting on a short inlet capillary fitted in a separate injection bloc. The inlet capillary is then connected to the capillary column mounted in the column oven with electron capture detector. Analysis is started by rapid heating to a constant temperature or by temperature programming resp. Head space analysis is another case in which trace components are important. Whereas several workers reported trapping of head space vapors in capillaries at low temperatures, we emphasize avoiding candensation, e.g. of water vapor, in the capillary. All sampling is done, therefore, near the original temperature of the head space material, i.e. at room temperature. In the case of coqnac aroma analysis in which most of the water and ethanol vapor are vented through the inlet capillary, the influences of most sampling variables—gas volume, length of inlet capillary—are studied. In the analysis of auto exhaust gas, again, bypassing of water is an important detail. In addition to hydrocarbons originating directly from the fuel as investigated by several authors, we found many combustion and conversion products, primarily naphthaline derivatives and phenol

Separation Efficiency Versus Column Length. An Experimental Study With Capillary Columns

The columns of different length used for studying the relation between HETP and column length are supposed to exhibit identical characteristics per meter. In the laboratory this condition cannot be rigorously fulfilled. The best approximation probably consists in starting the work with a relatively long capillary column followed by running shorter parts obtained by progressive cutting of the original column. Based on this procedure a marked increase of HETP with increasing column length is observe

Splitless Injection on Capillary Columns, Part II. Conditions and Limits, Practical Realization

Our procedure of direct splitless injection on capillary columns is based on the choice of column temperature for injection. Under appropriate conditions a marked concentration effect is observed, i.e. the eluted band is more concentrated than the injected one. The dependence of this effect on column temperature, injection time, sample size, and other variables has been studied experimentally. A solvent bypassing technique has been developed which allows the performance of trace analysis on capillary column

Splitless Injection on Capillary Columns, Part I. The Basic Technique; Steroid Analysis as an Example

A very simple procedure for splitless injection on capillary columns is discussed. In contrast to more sophisticated devices recently developed for the same purpose, the method described requires no additional equipment. The advantages of the method which broadens the use of capillary columns are discussed. Steroid analysis serves as an example of the application

A procedure model for evaluating IT-security investments

The security of information systems is a vital factor for companies nowadays. In order to achieve an adequate level of security, a variety of distinct measures is available, ranging from technical meas-ures to organizational measures. In near past suitable methods for decision support especially for the assessment of the profitability of IT-security investments have been developed. But integrated procedure models for a complete it-security controlling can neither be found in literature nor in practice. With this article, we propose a method framework that enables the analysis of the results of alternative security investments from a process-oriented perspective. As a basis, we have conducted an in-deep analysis of the state-of-the-art in the fields of IT-Business-Alignment and IT-security management in order to identify suitable concepts for the framework. A special focus lies on the requirements of IT-security controlling of critical business processes.Безпека інформаційних систем у теперішній час є життєво важливим фактором для компаній. Багато різних вимірів, від технічних до організаційних, є доступними для досягнення прийнятного рівня безпеки. У недалекому минулому було розроблено методи підтримки прийняття рішень при оцінюванні прибутковості інвестицій у IT-безпеку. Проте інтегральні процедурні моделі для повного управління IT-безпекою до цього часу не знайдені – ані у літературі, ані на практиці. У цієї статті ми пропонуємо середовище, яке дає можливість аналізувати результати альтернативних інвестицій у безпеку з точки зору, орієнтованої на процеси. Ми здійснили поглиблений аналіз сучасного стану справ у галузях синхронізації IT та бізнесу та управління IT-безпекою з метою ідентифікувати прийнятні концепції для цього середовища. Спеціальну увагу приділено вимогам до IT-безпеки критичних бізнес-процесів

Contribution of picoplankton to the total particulate organic carbon (POC) concentration in the eastern South Pacific

International audienceProchlorococcus, Synechococcus, picophytoeukaryotes and bacterioplankton abundances and contributions to the total particulate organic carbon concentration (POC), derived from the total particle beam attenuation coefficient (cp), were determined across the eastern South Pacific between the Marquesas Islands and the coast of Chile. All flow cytometrically derived abundances decreased towards the hyper-oligotrophic centre of the gyre and were highest at the coast, except for Prochlorococcus, which is not detected under eutrophic conditions. Temperature and nutrient availability appeared important in modulating picophytoplankton abundance, according to the prevailing trophic conditions. Although the non-vegetal particles tended to dominate the cp signal everywhere along the transect (50 to 83%), this dominance seemed to weaken from oligo- to eutrophic conditions, the contributions by vegetal and non-vegetal particles being about equal under mature upwelling conditions. Spatial variability in the vegetal compartment was more important than the non-vegetal one in shaping the water column particulate attenuation coefficient. Spatial variability in picophytoplankton biomass could be traced by changes in both Tchla and cp. Finally, picophytoeukaryotes contributed with ~38% on average to the total integrated phytoplankton carbon biomass or vegetal attenuation signal along the transect, as determined by direct size measurements on cells sorted by flow cytometry and optical theory. The role of picophytoeukaryotes in carbon and energy flow would therefore be very important, even under hyper-oligotrophic conditions

Early results in the treatment of proximal humeral fractures with a polyaxial locking plate

Objectives: We report early results using a second generation locking plate, non-contact bridging plate (NCB PH®, Zimmer Inc. Warsaw, IN, USA), for the treatment of proximal humeral fractures. The NCB PH® combines conventional plating technique with polyaxial screw placement and angular stability. Design: Prospective case series. Setting: A single level-1 trauma center. Patients: A total of 50 patients with proximal humeral fractures were treated from May 2004 to December 2005. Intervention: Surgery was performed in open technique in all cases. Main outcome measures: Implant-related complications, clinical parameters (duration of surgery, range of motion, Constant-Murley Score, subjective patient satisfaction, complications) and radiographic evaluation [union, implant loosening, implant-related complications and avascular necrosis (AVN) of the humeral head] at 6, 12 and 24weeks. Results: All fractures available to follow-up (48 of 50) went to union within the follow-up period of 6months. One patient was lost to follow-up, one patient died of a cause unrelated to the trauma, four patients developed AVN with cutout, one patient had implant loosening, three patients experienced cutout and one patient had an axillary nerve lesion (onset unknown). The average age- and gender-related Constant Score (n=35) was 76. Conclusions: The NCB PH® combines conventional plating technique with polyaxial screw placement and angular stability. Although the complication rate was 19%, with a reoperation rate of 12%, the early results show that the NCB PH® is a safe implant for the treatment of proximal humeral fracture

PULSED ELECTRON BEAM ANNEALING OF As AND B IMPLANTED SILICON

p-type (100) silicon wafers have been implanted either by As or B ions at 20 and 200 keV energies and doses of 1016cm-2. Pulsed electron beam annealing has been performed with fluences of 1.1 and 1.4 J/cm2 using a mean electron energy of 15 keV. The pulse duration was 50 ns. The annealed layers have been investigated by Rutherford backscattering under random and channeling conditions and by S.I.M.S. profiling. Good crystal regrowth and high dopant activation occur in all cases except for the 200 keV Boron implant. Impurities redistribution is observed but no significant segregation effects appear. The experimental profiles are in good agreement with a diffusion model using a modified green function solution and taking into account dopant diffusion in liquid phase and the computed melt front location. The deduced diffusion coefficient are in the 5.10-5cm2/s range for boron and 2.10-4cm2/s range for arsenic

Probing two topological surface bands of Sb2Te3 by spin-polarized photoemission spectroscopy

Using high resolution spin- and angle-resolved photoemission spectroscopy, we map the electronic structure and spin texture of the surface states of the topological insulator Sb2Te3. In combination with density functional calculations (DFT), we directly show that Sb2Te3 exhibits a partially occupied, single spin-Dirac cone around the Fermi energy, which is topologically protected. DFT obtains a spin polarization of the occupied Dirac cone states of 80-90%, which is in reasonable agreement with the experimental data after careful background subtraction. Furthermore, we observe a strongly spin-orbit split surface band at lower energy. This state is found at 0.8eV below the Fermi level at the gamma-point, disperses upwards, and disappears at about 0.4eV below the Fermi level into two different bulk bands. Along the gamma-K direction, the band is located within a spin-orbit gap. According to an argument given by Pendry and Gurman in 1975, such a gap must contain a surface state, if it is located away from the high symmetry points of the Brillouin zone. Thus, the novel spin-split state is protected by symmetry, too.Comment: 8 pages, 10 figure

Contribution of picoplankton to the total particulate organic carbon concentration in the eastern South Pacific

International audienceProchlorococcus, Synechococcus, picophytoeukaryotes and bacterioplankton abundances and contributions to the total particulate organic carbon concentration, derived from the total particle beam attenuation coefficient (cp), were determined across the eastern South Pacific between the Marquesas Islands and the coast of Chile. All flow cytometrically derived abundances decreased towards the hyper-oligotrophic centre of the gyre and were highest at the coast, except for Prochlorococcus, which was not detected under eutrophic conditions. Temperature and nutrient availability appeared important in modulating picophytoplankton abundance, according to the prevailing trophic conditions. Although the non-vegetal particles tended to dominate the cp signal everywhere along the transect (50 to 83%), this dominance seemed to weaken from oligo- to eutrophic conditions, the contributions by vegetal and non-vegetal particles being about equal under mature upwelling conditions. Spatial variability in the vegetal compartment was more important than the non-vegetal one in shaping the water column particle beam attenuation coefficient. Spatial variability in picophytoplankton biomass could be traced by changes in both total chlorophyll a (i.e. mono + divinyl chlorophyll a) concentration and cp. Finally, picophytoeukaryotes contributed ~38% on average to the total integrated phytoplankton carbon biomass or vegetal attenuation signal along the transect, as determined by size measurements (i.e. equivalent spherical diameter) on cells sorted by flow cytometry and optical theory. Although there are some uncertainties associated with these estimates, the new approach used in this work further supports the idea that picophytoeukaryotes play a dominant role in carbon cycling in the upper open ocean, even under hyper-oligotrophic conditions