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    A study of lead uptake and distribution in horns from lead-dosed goats using synchrotron radiation-induced micro X-ray fluorescence elemental imaging
    ( 2019) Tehrani,MW ; Huang,R ; Diana Filipa Guimarães ; Smieska,L ; Woll,A ; Parsons,PJ ; 6888
    Objective: The principal goal of this study was to investigate the uptake and distribution of lead (Pb) in the horns of Pb-dosed goats, and to explore possible links to their historical Pb dosing records. Horn is a keratinized material that grows in discrete increments with the potential to preserve the historical record of past environmental exposures. While previous studies have leveraged this potential to examine environmental and biological phenomena in horns, Pb uptake has never been explored. Methods: Horns were collected post-mortem from three goats that had been previously used to produce blood lead reference materials for the New York State proficiency testing program. The animals were periodically dosed with lead acetate, administered orally in a capsule, over a 5 to 8-year period. Horn cross sections were taken from each animal and analyzed using synchrotron radiation-induced micro X-ray fluorescence spectrometry (SR-µXRF) at the Cornell High Energy Synchrotron Source (CHESS). Results: Elemental distribution maps were obtained by SR-µXRF for Pb, Ca, S, Se, and three other elements (Br, Zn and Cu), with values reported quantitatively as a mass fraction (µg/g for trace elements and mg/g for Ca and S). Accumulations of Pb were clearly visible as a series of narrow “rings” in each of the horn samples analyzed. The elements Ca, S, Br, Zn, and Cu were also detected as discrete rings within each cross-section, with Br strongly correlated with S in the samples examined. A marginal increase in Se may coincide with Pb accumulation in horn cross-sections. Annual mineralization estimates based on the relative distribution of Ca and S were used to establish a tentative timeline for horn growth, with each timeline linked to the pattern of Pb accumulation in the corresponding horn cross-section sample. Conclusions: Following ingestion, absorbed Pb is eventually deposited into caprine horns, resulting in discrete accumulations or “rings.” Elemental mapping by SR-µXRF clearly show Ca-rich layers that vary with annual periodicity, consistent with previous reports of horn mineralization. Localized enrichment of Cu, Zn, Br and S appear to coincide with the keratinized regions related to the annual growth ring pattern in horns. Spatial analysis of horns for Pb accumulation may be useful as a qualitative marker of time-resolved exposures that may reflect specific periods of acute Pb absorption. © 2019 Elsevier GmbH
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    Characterization of arsenic in dried baby shrimp (Acetes sp.) using synchrotron-based X-ray spectrometry and LC coupled to ICP-MS/MS
    ( 2018) Diana Filipa Guimarães ; Roberts,AA ; Tehrani,MW ; Huang,R ; Smieska,L ; Woll,AR ; Lin,S ; Parsons,PJ ; 6888
    The arsenic content of dried baby shrimp (Acetes sp.) was investigated as part of an independent field study of human exposure to toxic metals/metalloids among the ethnic Chinese community located in Upstate New York. The dried baby shrimp were analyzed in a home environment using a portable X-Ray Fluorescence (XRF) instrument based on monochromatic excitation. Study participants had obtained their dried baby shrimp either from a local Chinese market or prepared them at home. The shrimp are typically between 10-20 mm in size and are consumed whole, without separating the tail from the head. Elevated levels of As were detected using portable XRF, ranging between 5-30 µg g-1. Shrimp samples were taken to the Cornell High Energy Synchrotron Source (CHESS) for Synchrotron Radiation µXRF (SR-µXRF) elemental mapping using a 384-pixel Maia detector system. The Maia detector provided high resolution trace element images for As, Ca, and Br, (among others) and showed localized accumulation of As within the shrimp's cephalothorax (head), and various abdominal segments. As quantification by SR-µXRF was performed using a lobster hepatopancreas reference material pellet (NRC-CNRC TORT-2), with results in good agreement with both portable XRF and ICP-MS. Additional As characterization using µX-ray Absorption Near Edge Spectroscopy (µXANES) with the Maia XRF detector at CHESS identified arsenobetaine and/or arsenocholine as the possible As species present. Further arsenic speciation analysis by LC-ICP-MS/MS confirmed that the majority of As (>95%) is present as the largely non-toxic arsenobetaine species with trace amounts of arsenocholine, methylated As and inorganic As species detected. © The Royal Society of Chemistry.
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    Femtosecond laser micromachining of suspended silica-core liquid-cladding waveguides inside a microfluidic channel
    ( 2022) João Miguel Maia ; Carlos Duarte Viveiros ; Amorim,VA ; Paulo Vicente Marques ; 4287 ; 5872 ; 6596
    This work addresses the fabrication of straight silica-core liquid-cladding suspended waveguides inside a microfluidic channel through fs-laser micromachining. These structures enable the reconfiguration of the waveguide's mode profile and enhance the evanescent interaction between light and analyte. Further, their geometry resembles a tapered optical fiber with the added advantage of being monolithically integrated within a microfluidic platform. The fabrication process includes an additional post-processing thermal treatment responsible for smoothening the waveguide surface and reshaping it into a circular cross-section. Suspended waveguides with a minimum core diameter of 3.8 µm were fabricated. Their insertion losses can be tuned and are mainly affected by mode mismatch between the coupling and suspended waveguides. The transmission spectrum was studied and it was numerically confirmed that it consists of interference between the guided LP01 mode and uncoupled light and of modal interference between the LP01 and LP02 modes. © 2022 Elsevier Ltd
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    Turn Around Point Long Period Fiber Gratings With Coupling to Asymmetric Cladding Modes Fabricated by a Femtosecond Laser and Coated With Titanium Dioxide
    ( 2021) Carlos Duarte Viveiros ; José Almeida ; Luís Carlos Coelho ; Vasconcelos,H ; João Miguel Maia ; Amorim,VA ; Pedro Jorge ; Paulo Vicente Marques ; 3565 ; 4287 ; 5256 ; 5799 ; 5872 ; 6596
    A detailed study of turn around point (TAP) long period fiber gratings (LPFGs) with coupling to the asymmetric cladding modes of a standard single-mode fiber (SMF-28e), fabricated by femtosecond (fs) laser direct writing was realized. The entire fabrication process, including the coating with different titanium dioxide (TiO2) film thicknesses of LPFGs and the corrections needed to achieve coated devices operating precisely in the TAP condition with coupling to the asymmetric cladding modes, was addressed. The significant fabrication details are also given, such as inscription periods, shape and localization of the refractive index modifications across the core. The fabrication process described allows the optimization of the LPFGs sensitivity in regards to the surrounding refractive index (SRI). Optimization of the writing parameters to obtain gratings working at the TAP for two different media surrounding the fiber (water and air) was achieved. It was demonstrated that for a grating period of 191.8 mu m, the LP1,12 mode exhibits a TAP at 1442.7 nm in air, and for a period of 192.5 mu m, the same mode exhibits a TAP at 1448.6 nm in water. The LPFGs operating at the TAP in air and water were coated with 10, 20, and 30 nm thin TiO2 film thicknesses and the spectral behavior characterized. The wavelength sensitivity to the surrounding refractive index (SRI) was assessed in the range between 1.3700 to 1.4120, and a maximum sensitivity of similar to 8051.4 nm/RIU was measured for the 192.5 mu m LPFG coated with a 30 nm thick TiO2 film.
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    Femtosecond laser micromachining of an optofluidics-based monolithic whispering-gallery mode resonator coupled to a suspended waveguide
    ( 2021) João Miguel Maia ; Amorim,VA ; Carlos Duarte Viveiros ; Paulo Vicente Marques ; 4287 ; 5872 ; 6596
    A monolithic lab-on-a-chip fabricated by femtosecond laser micromachining capable of label-free biosensing is reported. The device is entirely made of fused silica, and consists of a microdisk resonator integrated inside a microfluidic channel. Whispering gallery modes are excited by the evanescent field of a circular suspended waveguide, also incorporated within the channel. Thermal annealing is performed to decrease the surface roughness of the microstructures to a nanometric scale, thereby reducing intrinsic losses and maximizing the Q-factor. Further, thermally-induced morphing is used to position, with submicrometric precision, the suspended waveguide tangent to the microresonator to enhance the spatial overlap between the evanescent field of both optical modes. With this fabrication method and geometry, the alignment between the waveguide and the resonator is robust and guaranteed at all instances. A maximum sensitivity of 121.5 nm/RIU was obtained at a refractive index of 1.363, whereas near the refractive index range of water-based solutions the sensitivity is 40 nm/RIU. A high Q-factor of 10(5) is kept throughout the entire measurement range.