The Determination Of Sub Part-Per-Billion Levels Of Volatile Organic Compounds In Air By Pre-Concentration From Small Sample Volumes

Abstract

Trace level Volatile Organic Compounds (VOCs) in ambient air are normally determined according to EPA Method TO-14. This method describes the analysis in ambient air of 41 VOCs, ranging in boiling point from -29 to 215°C. It covers a concentration range from 0.2 to 20 parts per billion, volume/volume (ppb), and specifies sample enrichment of a 400 mL air sample on glass beads at -160°C. While this sample volume provides sub-ppb levels of VOC detection for target analytes when using a quadrupole mass spectrometer detector in SIM mode or when using GC detectors, the identification of non-target analytes may only be done in full scan mode for higher concentrations. Also with this sample volume a Nafion dryer is needed for water removal thereby lowering the recovery of polar VOCs.

Because of the very high sensitivity of the ion trap MS, relatively small air volumes (60 mL) are adequate to obtain the required or lower detection levels. An integrated air analysis system based on a GC-ion-trap MS has been investigated and is described. This system has a built-in cryogenic trap and necessary valving, internal standard gas sampling loop, and is controlled from the GC-MS workstation. The linearity, precision, and method detection levels obtainable with this system when using small volumes are reported. In addition, examples of the quantitative and qualitative analysis of ambient air samples are shown.     

Synthesis of Iridium Oxide Nanotubes by Electrodeposition into Polycarbonate Template: Fabrication of Chromium(III) and Arsenic(III) Electrochemical Sensor

For the first time iridium oxide (IrO₂) nanotubes are synthesized by electrodeposition in a polycarbonate (PC) template. Potential cycling (90 cycles) between 0.0 and 0.9 V is used for the preparation of IrO_x nanotubes onto the PC template with a pore diameter of 100 nm. Field‐emission scanning electron microscopy (FESEM) images show, that IrO₂ nanotubes with uniform diameters of 110±10 nm and an estimated length of 1–3 µm are formed. The electrochemical properties and the electrocatalytic activity of a glassy carbon‐IrO_x nanotube modified electrode toward Cr³⁺ and As³⁺ oxidation are investigated. Finally, the modified electrode is used for micromolar detection of the proposed analytes using differential pulse voltammetry.     

Comparison and Evaluation of Three Diagnostic Methods for Detection of Beet Curly Top Virus in Sugar Beet Using Different Visualizing Systems

To diminish the time required for some diagnostic assays including polymerase chain reaction (PCR), loop-mediated isothermal amplification (LAMP; due to mainly DNA extraction step) and also triple antibody sandwich enzyme-linked immunosorbent assay (TAS-ELISA) into a minimum level, an innovative immunocapture LAMP (IC-LAMP) and immunocapture PCR (IC-PCR) protocol on the basis of beet curly top virus (BCTV) genome was used and optimized. TAS-ELISA was employed first to validate the existence of the virus. All six IC-LAMP primers (i.e. forward outer primer (F3), backward outer primer (B3), forward inner primer (FIP), backward inner primer (BIP), loop forward (LF) and loop backward (LB)) together with IC-PCR primers were designed on the basis of the replication-associated protein (rep) gene (GenBank accession AF379637.1) of BCTV genome. Also, a novel colorimetric IC-LAMP assay for rapid and easy detection of BCTV was developed here, its potential compared with TAS-ELISA and IC-PCR assays. The method, on the whole, had the following advantages over the two mentioned procedures: (i) fascinatingly, no need of DNA extraction; (ii) no requirement of expensive and sophisticated tools for amplification and detection; (iii) no post-amplification treatment of the amplicons and (iv) a flexible and easy detection approach, which is visually detected by naked eyes using diverse visual dyes.     

Über heteroorganische Verbindungen, 39. Mitt.: Neue Darstellungsmethoden für Bis-(dialkylthiophosphinyl)-trisulfide. Reaktionsmechanismus

Zusammenfassung Dialkyl-dithiophosphinsäuren reagieren mit Morpholinoschwefelchlorid zu Bis-(dialkyl-thiophosphinyl)-trisulfiden. In Anwesenheit von Triäthylamin bilden sich die bisher unbekannten S-Morpholino-dialkyl-mercapto-dithiophosphinate, die, dem angenommenen Reaktionsmechanismus entsprechend, mit Chlorwasserstoff und Dithiophosphinsäuren die Bis-(dialkyl-thiophosphinyl)-trisulfide liefern. S-Morpholino-diäthyl-mercapto-dithiophosphinat und Diäthyldithiophosphinsäure setzen sich zu Bis-(diäthyl-thiophosphinyl)-trisulfid um.

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Heteroorganic compounds, XXXIX.: New methods for the preparation of bis-(dialkylthiophosphinyl)-trisulfides, and a reaction mechanism

Dialkyldithiophosphinic acids react with morpholinosulfenyl chloride to give bis-(dialkylthiophosphinyl)-trisulfides. In the presence of triethylamine the hitherto not described S-morpholino-dialkyl-mercapto-dithiophosphinates are formed. According to an assumed reaction mechanism the latter react with HCl and dithiophosphinic acids to give bis-(dialkyl-thiophosphinyl)-trisulfides. S-Morpholino-diethylmercapto-dithiophosphinate and diethyldithiophosphinic acid yield bis-(diethylthiophosphinyl)-trisulfide.

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38. Mitt.:L. Almasi undA. Hantz, Mh. Chem.100, 798 (1969).     

Die Säuredissoziationskonstanten von O,O-Dialkyl-Estern der Aroylamido-thiophosphorsäuren in Äthanol—Wasser-Mischungen

Zusammenfassung Die Säuredissoziationskonstanten von O,O-Dialkyl-ester der Aroylamido-thiophosphorsäuren wurden in Äthanol-Wasser-Mischungen potentiometrisch bestimmt. Die experimentellen Angaben bestätigen bei einigen Vertretern dieser Verbindungsgruppe die Gleichung I^*, bei anderen die Gleichung II^**. Die charakteristischen Konstanten dieser Gleichungen werden ermittelt.

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Ionization Constants of O,O-Dialkyl aroylamido-thiophosphonates in ethanol—Water mixtures

The dissociation constants of O,O-dialkyl esters of aroylamido-thiophosphoric acids have been determined potentiometrically in ethanol-water mixtures. Some compounds of this group obey equation I^*, others equation II^**. The constants of these equations have been determined.

     

Electrical investigation and ultraviolet detection of ZnO nanorods encapsulated with ZnO and Fe-doped ZnO layer

Encapsulated ZnO nanorod arrays were fabricated using a two-step method; hydrothermal followed by dip-coating. Intensity of X-ray diffraction peaks of ZnO nanorod films increased by encapsulation with ZnO and Fe doped ZnO layer. Encapsulation process increased diameter of the rods in a range of 20–40 nm. The optical studies indicated that the band-gap decreased with increment of the nanorod diameter, and increased with Fe doping in the ZnO layer. The electrical resistance of the samples demonstrated a remarkable reduction due to encapsulation, especially in the sample encapsulated with Fe doped-ZnO layer. The photoresponse behavior of ZnO nanorod films was investigated under different powers of ultraviolet illumination. The photoresponsivity was improved for encapsulated nanorods as compared to bare nanorods.     

Crystallinity and magnetic properties of electrodeposited Co nanowires in porous alumina

Crystalline Co nanowires were pulse electrodeposited into nanoporous aluminum oxide template having an ultra-thinned barrier layer. The effects of off-time between pulses and electrolyte acidity on the microstructure and magnetic properties of the nanowires were investigated. Increasing the off time between pulses increased the crystallinity and the alignment of easy axis with the wire axis. The rate of these increments was seen to depend on the electrolyte acidity and reached its maximum at pH=5.25 electrolyte acidity. Optimizing the crystallinity and crystal orientation, a coercivity value of 3320 Oe and a squareness of>90% were obtained for pure Co nanowires. A 10% increase in coercivity was found after annealing the samples.     

Analysis of structural and UV photodetecting properties of ZnO nanorod arrays grown on rotating substrate

Journal of Sol-Gel Science and Technology - ZnO nanorods (NRs) were successfully synthesized on seed layered substrate by a novel rotational hydrothermal method. The effect of substrate rotational...