Knowledge one the conformations and packing of PLA macrochains was gained via Raman spectroscopy. These experiments were performed in the Raman Micro-Spectroscopy Laboratory of the Characterization Service at ICTP-CSIC by using a Renishaw InVia Reflex Raman system (Renishaw plc, Wotton-under-Edge, UK), provided with a grating spectrometer coupled to a confocal microscope, as well as a Peltier-cooled charge-coupled device (CCD) detector. A diode laser (wavelength of 785 nm) was used for exciting the Raman scattering. The laser beam, with a power of 160 mW, was focused at the sample with the aid of a 0.85 × 100 microscope objective. An exposure time of 1 s and 200 accumulations were employed in these Raman measurements. After a baseline correction, the Raman spectra were normalized to the intensity of C=O stretching vibration of ester groups at 1772 cm−1 [32 (link)].
Invia reflex raman system
Manufactured by Renishaw
Sourced in United Kingdom
The InVia Reflex Raman system is a high-performance Raman spectrometer designed for a wide range of analytical applications. It features advanced optics and a high-sensitivity detector to provide high-quality Raman spectra. The system is capable of performing Raman microscopy, mapping, and imaging.
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Lab products found in correlation
Wire 3, by Renishaw (2 mentions)
Zetasizer nano, by Malvern Panalytical (1 mentions)
Asap 2460 3, by Micromeritics (1 mentions)
Tg 209 f1, by Netzsch (1 mentions)
Uatr two spectrometer, by PerkinElmer (1 mentions)
Zetasizer 3000 hs particle size analyzer, by Malvern Panalytical (1 mentions)
Biospin nmr spectrometer, by Bruker (1 mentions)
Escalab 250xi spectrometer, by Thermo Fisher Scientific (1 mentions)
Vertex 70 ftir spectrometer, by Bruker (1 mentions)
7 protocols using invia reflex raman system
1
Raman Spectroscopy Analysis of PLA Macrochains
2
Comprehensive Characterization of Nanomaterial Samples
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TEM images and high resolution TEM (HRTEM) were obtained on an electron microscope (Tecnai F30, the Netherlands) at 300 keV. SEM images and EDX analysis were carried out on environmental scanning electron microscopy (FEI QUANTA FEG 650). X-ray diffraction (XRD) was conducted on an AXS D8 Advance diffractometer with Cu-Kα radiation (λ = 1.5418 Å). X-ray photoelectron spectroscopy (XPS) was performed on an AXIS ULTARDLD spectroscope. The binding energy was calibrated by C 1s as reference energy (C 1s = 284.6 eV). Fourier transform infrared spectroscopy (FTIR, FTIR6500; Tianjin Gangdong Sci. & Tech. Co., Ltd) was used to analyze component changes before and after preparation. The Pd(ii ) concentration in the solution were analyzed by the atomic absorption spectrophotometer (AAS, TAS-990AFG, PERSEE, China). Raman spectra was measured with an Invia-reflex Raman system (RENISHAW PLC, UK). Thermogravimetric (TG) analysis was carried out on a Netzsch TG209F1 thermobalance under flowing N2 atmosphere at a heating rate of 10 K min−1 from 300 to 1073 K. Zeta potential was performed on Malvern Zetasizer Nano. BET analysis was conducted on Micromeritics ASAP 2460 3.01 using N2 as analysis adsorptive.
3
Analyzing Materials via FTIR and Raman
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Fourier transform infrared (FTIR) spectroscopy measurements were done in a Perkin Elmer UATR TWO spectrometer (PerkinElmer limited, Seer Greeb, UK), employing a resolution of 4 cm−1. Measurements were carried out in attenuated total reflectance modes (with ATR accessory) from 400 to 4000 cm−1, performing 16 scans per sample over the surface in a dried state.
Raman spectra were taken in a Renishaw InVia Reflex Raman system (Renishaw plc, Old Town, Wotton-under-Edge, UK). It was used by employing a grating spectrometer with a Peltier-cooled charge-coupled device (CCD) detector, coupled to a confocal microscope. All spectra were processed using Renishaw WiRE 3.3 software. The scans were obtained from the surface of the samples and the depth profiles were carried out positioning the laser each 2 μm.
Raman spectra were taken in a Renishaw InVia Reflex Raman system (Renishaw plc, Old Town, Wotton-under-Edge, UK). It was used by employing a grating spectrometer with a Peltier-cooled charge-coupled device (CCD) detector, coupled to a confocal microscope. All spectra were processed using Renishaw WiRE 3.3 software. The scans were obtained from the surface of the samples and the depth profiles were carried out positioning the laser each 2 μm.
4
Characterization of SERS Nanotags by TEM, Raman, and DLS
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Transmission electron microscopy (TEM) images were obtained in a field-emission high-resolution Philips JEOL JEM-2100F electron microscope, at an acceleration voltage of 200 kV. Samples for TEM analysis were prepared by drop-casting the diluted solutions of SERS nanotags on holey carbon-coated Cu mesh grids (400 mesh) and air-dried at room temperature. SERS measurements were performed by means of an InVia Reflex Raman system (Renishaw) comprising a microscope (Leica), a 785 nm laser excitation source (nominal output 260 mW) and a spectrometer equipped with a 1200 grooves/mm diffraction grating and a front-illuminated Peltier-cooled CCD detector (1024 pixels × 512 pixels). Dynamic light scattering (DLS) measurements were performed in a Malvern Zetasizer 3000 HS particle size analyzer (Malvern Instruments, UK). UV-vis absorption spectra were recorded at room temperature, using a Beckman Coulter DU 800 spectrometer.
5
Raman Microspectroscopy Analysis Protocol
6
Characterization of Grafted PCL in MCC-g-PCL Copolymers
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The contents of grafted PCL in MCC-g-PCL copolymers were characterized by 1H nuclear magnetic resonance (NMR) spectroscopy. 1H NMR spectra were recorded at 400 MHz using a Bruker BioSpin NMR spectrometer (Bruker Company, Germany) in dimethyl sulfoxide-d6 (DMSO-d6) solvent. The chemical shifts were calibrated against the internal standard signals of tetramethysilane (TMS). 13C NMR spectra were acquired on a Bruker BioSpin NMR apparatus at 100 MHz, at ambient temperature, using TMS as the internal standard and DMSO-d6 as solvent.
Raman spectroscopy was conducted on a Renishaw InVia Reflex Raman system. The Raman scattering was excited using a diode laser at a wavelength of 785 nm. The laser beam was focused on the sample with a 100 an0.85 microscope objective. The laser power at the sample was 320 mW. The exposure was 10 s and two accumulations of Raman measurements were carried out. In addition, an optical microscope was coupled to the system.
The molecular weight and molecular weight distribution of prepared MCC-g-PCL were measured on a Waters 5510 gel permeation chromatograph (U.S.A.). DMSO was used as eluent at a flow rate of 0.5 mL min−1 at 50 °C. The SEC system was calibrated with linear polystyrene standards.
Raman spectroscopy was conducted on a Renishaw InVia Reflex Raman system. The Raman scattering was excited using a diode laser at a wavelength of 785 nm. The laser beam was focused on the sample with a 100 an0.85 microscope objective. The laser power at the sample was 320 mW. The exposure was 10 s and two accumulations of Raman measurements were carried out. In addition, an optical microscope was coupled to the system.
The molecular weight and molecular weight distribution of prepared MCC-g-PCL were measured on a Waters 5510 gel permeation chromatograph (U.S.A.). DMSO was used as eluent at a flow rate of 0.5 mL min−1 at 50 °C. The SEC system was calibrated with linear polystyrene standards.
7
Comprehensive Characterization of Material Properties
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Zeta potential measurement was performed by dynamic light scattering (DLS; NanoBrook Omni, U.S.) for evaluating surface charge and dispersion stability of the samples in aqueous solution. A Renishaw InVia Reflex Raman system with 512 nm IR-diode laser coupled to an optical microscope was used to record spectra from the samples. X-Ray Photoelectron Spectroscopy (XPS) measurement was carried out using a Thermo ESCALAB 250Xi spectrometer. Fourier transform infrared spectroscopy (FTIR) was recorded by a Bruker Vertex 70 FT-IR spectrometer with the scan range of 400–4000 cm−1 in ATR mode. Thermogravimetric analysis (TGA) was carried out under nitrogen flow with a heating rate of 10 °C min−1 by using an TG209F1 instrument. Electrical conductivity of the samples was measured on a RTS-9 four-point probe resistivity measurement system. Measurements were taken in five different spots of the same sample, and the conductivity was averaged. Samples were prepared by compressing weighted amount of powder in a piston cylinder apparatus at 10 MPa for 5 min.
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