Application of rhodamine 800 for reversed phase liquid chromatographic detection using visible diode laser-induced fluorescence

This study reports the application of rhodamine 800, a far-red dye, suitable for excitation using visible diode laser-induced fluorescence (VDLIF) detection. A reagent synthesized from rhodamine 800 was evaluated as a precolumn reagent for derivatization with amino-containing analytes. The derivative of this reagent with primary amine analytes showed a loss of fluorescence. Rhodamine 800 was then applied as a mobile phase additive in the indirect mode for quantitation of valproic acid in plasma using reversed phase HPLC in combination with VDLIF detection. A visible diode laser (output power 8.50 mW) temperature-tuned to oscillate at 674.70 nm was used as a light source for a laboratory constructed HPLC fluorescence detector. A liquid/liquid extraction procedure was applied to human blank plasma. The selectivity of this method was validated by demonstration of a lack of interfering peaks in extracts of plasma (n = 3 sources). A calibration curve for valproic acid between 40 and 200 μg/mL was shown to be linear (r = 0.9932). The recoveries of valproic acid at concentrations of 50 and 100 μg/mL were evaluated and determined to be 73 and 72%, respectively. The precision and accuracy (n = 5) of the assay was within 7.0% RSD and 8.0% difference from the spiked concentration, respectively. The limits of detection (S/N = 3) for extracted and unextracted valproic acid were 15.0 and 11.54 μg/mL, respectively. The theoretical (C(lim)) and practical (C(det)) limits of detection in the detector flow cell for unextracted valproic acid at a S/N = 1 were found to be within 15%.     

Accurate expressions for the LP modes in a uniform circular-core curved fiber

Accurate forms for the LP(nm) modes (n = 0 and n ≧ 2) in a uniform circular-core curved fiber are given. We show that the LP(nm) modes (n ≧ 2) are composed of two spatially orthogonal components and that, to the zeroth order, there is no special polarization axis for the LP modes in a uniform circular-core curved fiber.     

Infrared microthermography of microfabricated devices

We report a new experimental apparatus for infrared microthermography applicable to a wide class of samples including semitransparent ones and perforated devices. This setup is particularly well suited for the thermography of microfabricated devices. Traditionally, temperature calibration is performed using calibration hot plates, but this is not applicable to transmissive samples. In this work a custom designed miniature calibration oven in conjunction with spatial filtering is used to obtain accurate static and transient temperature maps of actively heated devices. The procedure does not require prior knowledge of the emissivity. Calibration and image processing algorithms are discussed and analyzed. We show that relatively inexpensive uncooled bolometer arrays can be a suitable detector choice in certain radiometric applications. As an example, we apply this method in the analysis of temperature profiles of an actively heated microfabricated preconcentrator device that incorporates a perforated membrane and is used in trace detection of illicit substances.     

High performance thyratron driver with low jitter

We report the design and development of insulated gate bipolar junction transistor based high performance driver for operating thyratrons in grounded grid mode. With careful design, the driver meets the specification of trigger output pulse rise time less than 30 ns, jitter less than +/-1 ns, and time delay less than 160 ns. It produces a -600 V pulse of 500 ns duration (full width at half maximum) at repetition rate ranging from 1 Hz to 1.14 kHz. The developed module also facilitates heating and biasing units along with protection circuitry in one complete package.     

Degradation of chlorpyrifos contaminated soil by bioslurry reactor operated in sequencing batch mode: bioprocess monitoring

Bioslurry reactor (SS-SBR) was studied for the degradation of chlorpyrifos contaminated soil using native mixed microflora, by adopting sequencing batch mode (anoxic-aerobic-anoxic) operation. Reactor operation was monitored for a total cycle period of 72 h consisting of 3 h of FILL, 64 h REACT, 2 h of SETTLE, and 3 h of DECANT with chlorpyrifos concentrations of 3000 micrpg/g, 6000 microg/g and 12000 microg/g. At 3000 microg/g of chlorpyrifos concentration, 91% was degraded after 72 h of the cycle period, whereas in the case of 6000 microg/g of chlorpyrifos, 82.5% was degraded. However, for 12000 microg/g of chlorpyrifos, only 14.5% degradation was observed. The degradation rate was rapid at lower substrate concentration and 12000 microg/g of substrate concentration was found to be inhibitory. Chlorpyrifos removal rate was slow during the initial phase of the sequence operation. Half-life of chlorpyrifos degradation (t0.5) was estimated to be 6.3 h for 3000 microg/g of substrate, 17.5 h for 6000 microg/g and 732.2 h for 12000 microg/g. Process performance was assessed by monitoring chlorpyrifos concentration and biochemical process parameters viz., pH, oxidation and reduction potential (ORP), dissolved oxygen (DO), oxygen consumption rate (OCR) and microbial count (CFU) during sequence operation. From the experimental data obtained it can be concluded that the rate-limiting step with the bioslurry phase reactor in the process of chlorpyrifos degradation may be attributed to the concentration of substrate present in either soil or liquid phase. Periodic operations (SBR) by varying individual components of substrate with time in each process step place micro-organisms under nutritional changes from feast to famine and maintains a wide distribution in the population of micro-organisms resulting in high uptake of the substrate in the bioslurry reactor.     

Dynamic response analysis of pyroelectric sensitive element for thermal imaging

Temperature distributions under periodic thermal excitations and the responsivity of a pyroelectric device consisting of a cover layer, infrared absorber, metal contact, sensitive pyroelectric element, interconnecting column, and bulk silicon are found. Some results of numerical thermal modeling and analysis of exact expressions for a few extreme cases are presented. Pyroelectric responses of real structures are compared with the response of a single pyroelectric element in air as a limiting case of maximum sensitivity. The analytical approximations and numerical simulation show that the frequency response of the multilayered structure consists of different parts with simple frequency dependencies. In the region of high frequencies of light modulation, the responsivity is proportional to /spl omega//sup -1/, at low frequencies /spl sim/ /spl omega//sup -0.5/, and, in the region of intermediate frequencies, the voltage responsivity is independent of frequency.     

Determination of dehydroacetic acid and its sodium salt in food products and polymeric packing materials

HPLC method of determination of dehydroacetic acid and its sodium salt in food products and polymeric packing materials has been developed. The migration of DGA from food-contacting materials to food matrix has been investigated.     

Ultrafine particle concentrations and exposures in seven residences in northern California

Human exposures to ultrafine particles (UFP) are poorly characterized given the potential associated health risks. Residences are important sites of exposure. To characterize residential exposures to UFP in some circumstances and to investigate governing factors, seven single-family houses in California were studied during 2007-2009. During multiday periods, time-resolved particle number concentrations were monitored indoors and outdoors and information was acquired concerning occupancy, source-related activities, and building operation. On average, occupants were home for 70% of their time. The geometric mean time-average residential exposure concentration for 21 study subjects was 14,500 particles per cm(3) (GSD = 1.8; arithmetic mean ± standard deviation = 17,000 ± 10,300 particles per cm(3)). The average contribution to residential exposures from indoor episodic sources was 150% of the contribution from particles of outdoor origin. Unvented natural-gas pilot lights contributed up to 19% to exposure for the two households where present. Episodic indoor source activities, most notably cooking, caused the highest peak exposures and most of the variation in exposure among houses. Owing to the importance of indoor sources and variations in the infiltration factor, residential exposure to UFP cannot be characterized by ambient measurements alone. PRACTICAL IMPLICATIONS: Indoor and outdoor sources each contribute to residential ultrafine particle (UFP) concentrations and exposures. Under the conditions investigated, peak exposure concentrations indoors were associated with cooking, using candles, or the use of a furnace. Active particle removal systems can mitigate exposure by reducing the persistence of particles indoors. Eliminating the use of unvented gas pilot lights on cooking appliances could also be beneficial. The study results indicate that characterization of human exposure to UFP, an air pollutant of emerging public health concern, cannot be accomplished without a good understanding of conditions inside residences.