FTIR imaging measurements were carried out using a Thermo Scientific Nicolet iN10 Infrared Microscope. This IR microscope is equipped with a liquid nitrogen cooled mercury-cadmium-tellurium (MCT) detector and a 10 × objective. The instrument was purged by gas nitrogen overnight before scanning. Spectral images were recorded in reflectance mode with 4 cm −1 spectral resolution in the 4000–675 cm−1 range, taking the average of 4 scans per pixel. The aperture size and step size were 200 × 200 µm and 200 µm. The full bacterial drop was imaged with the actual drop size ranging from 3.4 mm × 3.4 mm to 6.4 mm × 6.0 mm. The background spectrum was collected every 10 min from a gold disc integrated into the standard sample plate.
Nicolet in10 infrared microscope
Manufactured by Thermo Fisher Scientific
Sourced in United States, Italy
The Nicolet iN10 Infrared Microscope is a laboratory instrument designed for the analysis of small samples. It utilizes infrared spectroscopy to provide detailed information about the chemical composition and molecular structure of materials. The core function of the Nicolet iN10 is to enable the non-destructive examination of microscopic samples.
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Lab products found in correlation
Avaspec 3648 spectrophotometer, by Avantes (1 mentions)
Slide on microtip ge atr crystal, by Thermo Fisher Scientific (1 mentions)
Originpro, by OriginLab (1 mentions)
Avalight dh s bal, by Avantes (1 mentions)
Omnic 9, by Thermo Fisher Scientific (1 mentions)
Omnicpicta software, by Thermo Fisher Scientific (1 mentions)
Picoview software, by Agilent Technologies (1 mentions)
Nova nanosem 200, by Thermo Fisher Scientific (1 mentions)
Lext ols3000, by Olympus (1 mentions)
Escalab 250 x ray photoelectron spectrometer, by Thermo Fisher Scientific (1 mentions)
Omnic software, by Thermo Fisher Scientific (1 mentions)
12 protocols using nicolet in10 infrared microscope
1
FTIR Imaging of Bacterial Samples
2
Spectroscopic Characterization of Photoactive Materials
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To characterize the photoexcitation and photodynamic properties of these materials, spectroscopic examinations were conducted by the AvaSpec-3648 spectrophotometer with 2 nm spectral resolution (Avantes Inc., Apeldoorn, The Netherlands) in the transmission mode with deuterium-halogen lamp (AvaLight-DH-S-BAL Avantes Inc., Apeldoorn, The Netherlands). The ATR-FTIR spectra of photoactive materials deposited on the slide glass were obtained using a Nicolet iN10 infrared microscope (Thermo Fisher Scientific, Waltham, MA, USA) equipped with liquid nitrogen-cooled mercury cadmium telluride (MCT-A) detector and Slide-On MicroTip Ge ATR crystal. The microscope was continuously purged with dry air. All spectra were collected in the range of 3750–675 cm−1 with a spectral resolution of 4 cm−1, averaging 128 scans. Directly before sampling, the background spectrum of germanium/air was recorded as a reference (256 scans, 4 cm−1). All spectra were registered at room temperature. Each sample was measured three times and then averaged to cover variation in material thickness. All spectra were analyzed using OriginPro (ver. 2019, OriginLab Corporation, Northampton, MA, USA).
3
Microplastic Identification and Sizing via FTIR Spectroscopy
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We analyzed 667 potential microplastic particles with our FTIR spectroscopy setup described below. Of these particles, 647 particles were analyzed with FTIR spectroscopy while the remaining 20 particles were only measured for size because they did not return usable spectra. In January, February, and June 2018, we used an FTIR microscope (Nicolet iN 10 Infrared Microscope, Thermo Scientific, Waltham, Massachusetts, USA) in attenuated total reflectance (ATR) mode, equipped with a liquid nitrogen-cooled mercury cadmium telluride (MCT) detector at the Korean Institute of Ocean Science and Technology for our spectroscopy measurements. We used a diamond tip, and the spectra were recorded as 64 scans in the spectral range of 650–4000 cm−1.
Plastic polymer types were identified by matching the sample’s IR spectrum with the spectra stored in an FTIR polymer spectrum library which is already integrated into the measuring program of the FTIR microscope68 (link). To measure the size of each particle, a ruler built into the measuring program of the FTIR microscope was adjusted to measure the maximum dimension of the particle. This equipment has been used for various studies of microplastics before (e.g., refs5 (link),56 (link)).
The results of our spectroscopy analyses are available in the Supplementary Appendix S1.
Plastic polymer types were identified by matching the sample’s IR spectrum with the spectra stored in an FTIR polymer spectrum library which is already integrated into the measuring program of the FTIR microscope68 (link). To measure the size of each particle, a ruler built into the measuring program of the FTIR microscope was adjusted to measure the maximum dimension of the particle. This equipment has been used for various studies of microplastics before (e.g., refs5 (link),56 (link)).
The results of our spectroscopy analyses are available in the Supplementary Appendix S1.
4
Analyzing Inhibited Polymer Film Composition
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The molecular behavior of the ingredients of the inhibited polymer films made by different methods was analyzed using ATR-FTIR spectroscopy. For this aim, we used a Nicolet iN10 infrared microscope (Thermo Fisher Scientific, Waltham, MA, USA) using the ATR mode with Ge-crystal, a research range of 675 to 4000 cm−1, the transmission mode (a resolution of 4 cm−1 by accumulating 128 scans), and a subsequent processing of spectra in the software Omnic 9 (Thermo Fisher Scientific, Waltham, MA, USA).
5
Characterizing Thin Film Morphology and Composition
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AFM
amplitude micrographs were obtained in tapping mode using a Pico Plus
AFM instrument (Molecular Imaging) with aluminum-coated silicon tips
(BudgetSensors) and a spring constant of 40 N m–1. A sample area of 3 μm by 3 μm was scanned at a rate
of 1 Hz while collecting data in topographic, phase, and amplitude
modes. Morphological changes are captured in micrographs using PicoView
software (Agilent) and postprocessed using Gwyddion.30 (link)FTIR imaging was performed with a Nicolet iN10 infrared
microscope (Thermo Scientific) after mounting the optical windows
on a motorized stage for scanning the infrared map in an XY pattern. OMNIC Picta software (Thermo Scientific) was utilized for
FTIR microscopy and spectral mapping. Individual spectra corresponding
to an average of 64 scans were collected over the range of 800–4000
cm–1 with 4 cm–1 resolution. All
samples were background-subtracted using an empty optical window.
Control experiments ensured that films exposed to humid air in the
absence of O3(g) correspond to the spectral features of
catechol despite any loss by sublimation, which was carefully monitored
to remain below 5%. Data processing to obtain the CD line (or corrected
peak heights after local baseline correction) was performed10 (link) to collect kinetic data from the average of
duplicate experiments with error bars corresponding to one standard
deviation.
amplitude micrographs were obtained in tapping mode using a Pico Plus
AFM instrument (Molecular Imaging) with aluminum-coated silicon tips
(BudgetSensors) and a spring constant of 40 N m–1. A sample area of 3 μm by 3 μm was scanned at a rate
of 1 Hz while collecting data in topographic, phase, and amplitude
modes. Morphological changes are captured in micrographs using PicoView
software (Agilent) and postprocessed using Gwyddion.30 (link)FTIR imaging was performed with a Nicolet iN10 infrared
microscope (Thermo Scientific) after mounting the optical windows
on a motorized stage for scanning the infrared map in an XY pattern. OMNIC Picta software (Thermo Scientific) was utilized for
FTIR microscopy and spectral mapping. Individual spectra corresponding
to an average of 64 scans were collected over the range of 800–4000
cm–1 with 4 cm–1 resolution. All
samples were background-subtracted using an empty optical window.
Control experiments ensured that films exposed to humid air in the
absence of O3(g) correspond to the spectral features of
catechol despite any loss by sublimation, which was carefully monitored
to remain below 5%. Data processing to obtain the CD line (or corrected
peak heights after local baseline correction) was performed10 (link) to collect kinetic data from the average of
duplicate experiments with error bars corresponding to one standard
deviation.
6
In Vitro Bioactivity Evaluation of Materials
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Bioactivity was evaluated upon immersion in SBF, following the standard procedure described by the International Standard ISO 23317:2014 [34 ]. Samples were placed in sterilized tubes filled with SBF which were then sealed and placed in a thermostatic bath at 37 °C for 8 days. Samples were then thoroughly rinsed with DI water and air dried prior to subsequent analysis. The formation of calcium-phosphate species (CaPs) was assessed by EDS analysis, while identification of their type was obtained by Fourier transformed infrared (FT-IR) microspectroscopy, using a Nicolet iN10 infrared microscope (Thermo Fisher Scientific IT, Milano, Italy) equipped with a mercury-cadmium-telluride (MCT-A) nitrogen-cooled detector in ATR mode. The FTIR spectra were collected in the 4000–650 cm−1 range as an average of 64 scans, with 8 cm−1 resolution. At least five measurements were acquired from different areas for each sample. OmnicPicta software version 2.03 (Thermo Fischer Scientific, Milano, Italy) was used for post elaboration of the spectra.
7
Characterization of DVS-BCB Bonding Layer
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The shape of the coated DVS-BCB pattern layer was observed, using an optical microscope (BX-41, Olympus, Tokyo, Japan). Raman spectroscopy (Raman, DXR, Thermo Fisher Scientific, Waltham, MA, USA) was performed to confirm the removal of the DVS-BCB material during the DVS-BCB pattern formation process. To determine the voids and pattern deformation of the DVS-BCB bonding layer, a non-destructive analysis was performed, using a near-infrared confocal laser microscope (LEXT OLS-3000, Olympus, Tokyo, Japan). Scanning electron microscopy (SEM, Nova Nano SEM200, FEI, Hillsborough, OR, USA) was performed to observe changes in the thickness of the DVS-BCB bonding layer with respect to the compressive pressure. FT-IR microscopy (Nicolet iN10 Infrared Microscope, Thermo Fisher Scientific, MA, USA) was performed to observe the chemical bonding properties of the DVS-BCB bonding layer produced, according to the compressive pressure.
8
FT-IR Analysis of Carbonated Materials
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The Nicolet iN10 Infrared Microscope (ThermoFisher Scientific, Milan, Italy) was used to perform FT-IR analysis on the selected starting materials and corresponding carbonated products (AOD_1, LF_2, EAF_3 + SiO2, CKD) in transmittance mode using a barium fluoride (BaF2) window. Each spectrum was collected with a spectral resolution of 8 cm−1 over 16 scans. The obtained spectra were analyzed using OMNIC software version 9.11.475 (ThermoFisher Scientific, Milan, Italy) to interpret the results.
9
Synthesis and Characterization of Graphdiyne Oxide
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Graphdiyne (GDY) was synthesized as described previously. 22 GDYO was synthesized by the oxidation of GDY powder using a mixture of H 2 O 2 and H 2 SO 4 as a complex oxidant. Briefly, 50 mg of GDY was gradually stirred into 30% H 2 O 2 solution (1 mL) and 98% H 2 SO 4 (2.5 mL) under an ice-water bath for 1 h. The oxidization was stopped by adding 50 mL double-distilled water, followed by dialysis (cutoff, 3000) for seven days to remove mixed acid. GDYO samples were obtained by sonication for 4 h in water. The physicochemical characterization of GDYO was performed using atomic force microscope (AFM), X-ray photoelectron spectroscopy (XPS), and Fourier-transform infrared spectroscopy (FTIR). AFM images were captured using the Bruker MultiMode V8-SPM (Bruker, Germany) with a ScanAsyst mode. XPS survey scans were measured by an ESCALAB 250 X-ray photoelectron spectrometer (Thermo Scientific). FTIR spectra were collected using a Nicolet™ iN™10 Infrared Microscope (ThermoFisher Scientific). One droplet of the GDYO solution was transferred onto the 15 × 15 × 0.5 mm CaF 2 infrared window, and dried and the trans-mission spectrum of GDYO was obtained by subtracting the CAF 2 background spectrum.
10
FT-IR Analysis of Silver Nanoparticles Coated with Oleic Acid
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FT-IR spectra were obtained using a Thermo Scientific Nicolet iN10 Infrared Microscope operating between 500 and 4000 cm -1 with a resolution of 4 cm -1 . AgNP-OA sample was deposited and dried onto a AgBr disk. FT-IR spectra confirmed that AgNP-OA were under protection of a single layer of OA 34, 36 , where the carboxylate group was interacting with the silver surface and the hydrocarbon chains were pointing towards the exterior, leading to the NP hydrophobic properties. FT-IR spectra of AgNP-OA and OA are shown in Figure S1.
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