Morphology and kinetics of asphalt binder microstructure at gas, liquid and solid interfaces.

We combined optical and atomic force microscopy to observe morphology and kinetics of microstructures (typically referred to as bees) that formed at free surfaces of unmodified Performance Graded (PG) 64-22 asphalt binders upon cooling from 150°C to room temperature (RT) at 5°C min-1 , and changes in these microstructures when the surface was terminated with a transparent solid (glass) or liquid (glycerol) overlayer. The main findings are: (1) at free binder surfaces, wrinkled microstructures started to form near the crystallization temperature (∼45°C) of saturates such as wax observed by differential scanning calorimetry, then grew to ∼5 µm diameter, ∼25 nm wrinkle amplitude and 10-30% surface area coverage upon cooling to RT, where they persisted indefinitely without observable change in shape or density. (2) Glycerol coverage of the binder surface during cooling reduced wrinkled area and wrinkle amplitude three-fold compared to free binder surfaces upon initial cooling to RT; continued glycerol coverage at RT eliminated most surface microstructures within ∼4 h. (3) No surface microstructures were observed to form at binder surfaces covered with glass. (4) Submicron bulk microstructures were observed by near-infrared microscopy beneath the surfaces of all binder samples, with size, shape and density independent of surface coverage. No tendency of such structures to float to the top or sink to the bottom of mm-thick samples was observed. (5) We attribute the dependence of surface wrinkling on surface coverage to variation in interface tension, based on a thin-film continuum mechanics model. LAY DESCRIPTION: Asphalt binder, or bitumen, is the glue that holds aggregate particles together to form a road surface. It is derived from the heavy residue that remains after distilling gasoline, diesel and other lighter products out of crude oil. Nevertheless, bitumen varies widely in composition and mechanical properties. To avoid expensive road failures, bitumen must be processed after distillation so that its mechanical properties satisfy diverse climate and load requirements. International standards now guide these mechanical properties, but yield varying long-term performance as local source composition and preparation methods vary. In situ diagnostic methods that can predict bitumen performance independently of processing history are therefore needed. The present work focuses on one promising diagnostic candidate: microscopic observation of internal bitumen structure. Past bitumen microscopy has revealed microstructures of widely varying composition, size, shape and density. A challenge is distinguishing bulk microstructures, which directly influence a binder's mechanical properties, from surface microstructures, which often dominate optical microscopy because of bitumen's opacity and scanning-probe microscopy because of its inherent surface specificity. In previously published work, we used infrared microscopy to enhance visibility of bulk microstructure. Here, as a foil to this work, we use visible-wavelength microscopy together with atomic-force microscopy (AFM) specifically to isolate surface microstructure, to understand its distinct origin and morphology, and to demonstrate its unique sensitivity to surface alterations. To this end, optical microscopy complements AFM by enabling us to observe surface microstructures form at temperatures (50°C-70°C) at which bitumen's fluidity prevents AFM, and to observe surface microstructure beneath transparent, but chemically inert, liquid (glycerol) and solid (glass) overlayers, which alter surface tension compared to free surfaces. From this study, we learned, first, that, as bitumen cools, distinctly wrinkled surface microstructures form at the same temperature at which independent calorimetric studies showed crystallization in bitumen, causing it to release latent heat of crystallization. This shows that surface microstructures are likely precipitates of the crystallizable component(s). Second, a glycerol overlayer on the cooling bitumen results in smaller, less wrinkled, sparser microstructures, whereas a glass overlayer suppresses them altogether. In contrast, underlying smaller bulk microstructures are unaffected. This shows that surface tension is the driving force behind formation and wrinkling of surface precipitates. Taken together, the work advances our ability to diagnose bitumen samples noninvasively by clearly distinguishing surface from bulk microstructure.

Correlated time-variation of bulk microstructure and rheology in asphalt binders.

We use near-infrared dark-field optical microscopy to probe isothermal time variation of the volume fraction of naturally-occurring, subsurface microstructures in PG 64-22 asphalt binders at temperature T=30∘C, following a rapid heating (cooling) increment |ΔT|=20∘C from initial temperature T0=10∘C(50∘C). We compare these microstructure variations with isothermal time variations of the magnitude |G30∗(t)| of the bulk complex shear modulus measured for identical sample conditions with a Dynamic Shear Rheometer. The main findings are: (1) Microstructure volume fraction (inferred from intensity I(t) of near-infrared optical scatter) and |G∗(t)| both continue to change appreciably long after measurable changes of binder temperature cease. Moreover, delayed time variations in I(t) and |G∗(t)| (2) correlate closely with each other; (3) evolve on three distinct time scales - several minutes, ∼1 h, >1 day; (4) depend on binder aging; (5) are more pronounced after a cooling step (ΔT=-20∘C) than after a heating step (ΔT=+20∘C); and (6) account for hysteresis in I(t) and |G∗(t)| curves observed during heating-cooling cycles.

Optical characterization of temperature- and composition-dependent microstructure in asphalt binders.

We introduce noncontact optical microscopy and optical scattering to characterize asphalt binder microstructure at temperatures ranging from 15°C to 85°C for two compositionally different asphalt binders. We benchmark optical measurements against rheometric measurements of the magnitude of the temperature-dependent bulk complex shear modulus |G*(T)|. The main findings are: (1) Elongated (∼5 × 1 µm), striped microstructures (known from AFM studies as 'bees' because they resemble bumble-bees) are resolved optically, found to reside primarily at the surface and do not reappear immediately after a single heating-cooling cycle. (2) Smaller (∼1 µm(2) ) microstructures with no observable internal structure (hereafter dubbed 'ants'), are found to reside primarily in the bulk, to persist after multiple thermal cycles and to scatter light strongly. Optical scattering from 'ants' decreases to zero with heating from 15°C to 65°C, but recovers completely upon cooling back to 15°C, albeit with distinct hysteresis. (3) Rheometric measurements of |G*(T)| reveal hysteresis that closely resembles that observed by optical scatter, suggesting that thermally driven changes in microstructure volume fraction cause corresponding changes in |G*(T)|.

Development of a hematite nanotube and tyramine-based drug carrier against drug-resistant bacteria Klebsiella pneumoniae.

In this study, hematite nanotube (HNT) and tyramine-based advanced nano-drug carriers were developed for inhibiting the growth of Klebsiella pneumoniae (K. pneumoniae). The HNT was synthesized by following the Teflon line autoclaved assisted hydrothermal process and tyramine was incorporated on the surface of the HNT to fabricate the formulated nano-drug. The nano-drug was prepared by conjugating meropenem (MP) on the surface of Tyramine-HNT and characterized using different techniques, such as scanning electron microscopy (SEM), attenuated total reflection Fourier transform infrared (ATR-FTIR), etc. Furthermore, the drug-loading efficiency and loading capacity were measured using a UV-vis spectrometer. The pH, amount of Tyr, and HNT required for drug loading were optimized. A controlled and gradual manner of pH-sensitive release profiles was found after investigating the release profile of MP from the carrier drug. The antibacterial activity of MP@Tyramine-HNT and MP was compared through the agar disc diffusion method which indicates that antibacterial properties of antibiotics are enhanced after conjugating. Surprisingly, the MP@Tyramine-HNT exhibits a minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of K. pneumoniae lower than MP itself. These results indicate the nanocarrier can reduce the amount of MP dosed to eradicate K. pneumoniae.

Isolation of Acinetobacter species from Clinical Specimens with Detection of Their Antimicrobial Susceptibility Pattern from a Tertiary Care Hospital, Bangladesh.

Acinetobacter species are important opportunistic and nosocomial pathogens capable of causing both community and health care-associated infections. The aim of this study was to determine the prevalence of Acinetobacter species and determination of the antibiotic susceptibility patterns of Acinetobacter. A total of 341 specimens were collected over a period of one year from January 2017 to January 2018 from ICU and Surgery unit of Mymensingh Medical College Hospital, Mymensingh, Bangladesh. Antimicrobial susceptibility testing of all Acinetobacter isolates was done using Kirby Bauer's disc diffusion technique as per recommendations of Clinical Laboratory Standards Institute (CLSI). MIC of commonly used Imipenem and newly introduced Tigecycline by agar dilution method was done and was compared it with disc diffusion method. From total 341 specimens, 119(34.8%) pathogen were isolated. Among 119 isolates total 46(38.6%) Acinetobacter were isolated. Maximum number of Acinetobacter was isolated from respiratory samples- endotracheal secretions. Regarding antimicrobial resistance, 42(91.3%), 33(71.7%), 20(43.5%), 28(60.9%) and 1(2.2%) were resistant to Piperacillin-Tazobactam, Doxycycline, Imipenem, Colistin and Tigecycline. Regarding, MIC of Imipenem, 41.3% was resistant, 32.6% was intermediate and 26.1% was sensitive. Regarding MIC of Tigecycline none was resistant, 39.1% was intermediate and 60.9% was sensitive. Acinetobacter species is emerging as a predominant healthcare associated multidrug resistant pathogen. The findings of this study will help our clinicians to apply appropriate antibiotics for treatment of patients.