Thermal degradation of the APIs and polymers was measured using a TGA/DSC1 instrument (Mettler-Toledo, GmbH, Giessen, Germany) at a heating rate of 10 K min−1 from 25 °C to 300 °C under nitrogen gas purging (50 mL min−1) and with sample weights of 10–20 mg.
Tga dsc1 instrument
Manufactured by Mettler Toledo
Sourced in Switzerland
The TGA/DSC1 is a thermal analysis instrument that can simultaneously measure the weight change (thermogravimetry, TGA) and heat flow (differential scanning calorimetry, DSC) of a sample as a function of temperature or time. It provides quantitative information about physical and chemical changes in materials that occur as a function of temperature.
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Lab products found in correlation
Stare software, by Mettler Toledo (2 mentions)
Hq40d, by HACH (1 mentions)
Vario el cube elemental analyzer, by Elementar (1 mentions)
Av 500 nmr spectrometer, by Bruker (1 mentions)
Equinox 55 fourier transform infrared spectrometer, by Bruker (1 mentions)
Apex 2 ccd diffractometer, by Bruker (1 mentions)
Lambda 950 uv vis nir spectrometer, by PerkinElmer (1 mentions)
Ssx 550, by Shimadzu (1 mentions)
Pb 10 ph metre, by Sartorius (1 mentions)
J 720w spectropolarimeter, by Jasco (1 mentions)
Tensor 27 spectrometer, by Bruker (1 mentions)
D8 advance diffractometer, by Bruker (1 mentions)
Xrd 6000, by Shimadzu (1 mentions)
Jsm 7600f, by JEOL (1 mentions)
Icp oes, by Horiba (1 mentions)
X ray diffractometer, by Bruker (1 mentions)
Mastersizer 3000e granulometer, by Malvern Panalytical (1 mentions)
Mira3 xmu, by TESCAN (1 mentions)
Supra 55vp instrument, by Zeiss (1 mentions)
Nicolet 380 ftir spectrometer, by Thermo Fisher Scientific (1 mentions)
19 protocols using tga dsc1 instrument
1
Thermal Degradation of APIs and Polymers
2
TGA and DSC Analyses of Dry CSP Samples
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For TGA and DSC analyses, around 3 mg of dry CSP sample was scanned with a Mettler-Toledo TGA/DSC 1 instrument (Schwerzenbach, Switzerland) from 32 to 800 °C at a heating rate of 10 °C/min under nitrogen atmosphere.
3
Biochar Characterization: Thermal, pH, Conductivity
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Thermogravimetric analysis (TGA) was performed using a Mettler-Toledo TGA/DSC1 instrument to analyse ash content, fixed carbon and volatile matter according to the method described in Buss and Mašek (2014) (link). Electrical conductivity (EC) and pH were measured according to Rajkovich et al. (2012) (link) using 1 g of crushed biochar (using mortar and pestle) in 20 mL of DI water, which was shaken at 150 rpm for 1.5 h on a bench-top shaker (EC: Hach HQ40d portable meter, conductivity probe meter CDC 401; pH Mettler Toledo FE 30). These analyses were performed in duplicates.
4
Thermal Analysis of Materials
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Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were performed using a TGA/DSC1 instrument (Mettler-Toledo GMBH, S), which simultaneously measured mass loss and heat flow in the sample. The analyses were performed in the 25–950°C temperature range and at a heating rate of 10°C/min under atmospheric conditions.
5
Nanoparticle Drug Loading Analysis
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TGA was performed using a TGA/DSC1 instrument (Mettler Toledo, Greenville, SC, USA) under a nitrogen purge of 50 mL/min.
The actual drug loading of NS was also determined by extracting an accurately weighed amount of IMB16-4 nanoparticles with methanol, followed by filtration of the samples and analyzed by HPLC. The standard curve for IMB16-4 was the linear (R2 > 0.9999) over the concentration range of 0.2~50.0 μg/mL. The drug loading was calculated according to equation:
The actual drug loading of NS was also determined by extracting an accurately weighed amount of IMB16-4 nanoparticles with methanol, followed by filtration of the samples and analyzed by HPLC. The standard curve for IMB16-4 was the linear (R2 > 0.9999) over the concentration range of 0.2~50.0 μg/mL. The drug loading was calculated according to equation:
6
Water Content Analysis of Powders
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Thermogravimetric analyses performed with the TGA/DSC1 instrument (Mettler Toledo, Greifensee, Switzerland) were used to evaluate the water content of the powders based on their weight loss due to heating. Samples of about 5–8 mg were weighed in 40 µL aluminium pan and heated in the temperature range between 25 °C and 100 °C at a heating rate of 10 °C/min under nitrogen flow at 80 mL/min.
7
Thermal Stability Analysis of PLATMC Scaffolds
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TGA was used to determine the thermal stability of the PLATMC scaffolds. Samples (between 2.1 and 18.1 mg) were run under nitrogen flow with a heating rate of 10 °C min−1 from 25 °C to 500 °C using a Mettler Toledo TGA/DSC 1 instrument. The flow rate was set to 80 mL min−1. Data are reported as the temperature at which 5% mass loss (T5%) occurred.
8
Comprehensive Analytical Characterization
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13C and 1H NMR spectra were measured with AV 500 NMR spectrometer (Bruker, Switzerland). Infrared spectra were measured by an EQUINOX 55 Fourier transform Infrared spectrometer (Bruker, Germany). Elemental analyses were performed with the vario EL cube elemental analyzer (Elementar, Germany).
The thermal analysis experiments were performed with a model TGA/DSC 1 instrument (METTLER, Switzerland). Single crystal X-ray experiment was carried out on a Bruker Apex II CCD diffractometer equipped with graphite monochromatized Ga and Cu Kα radiation using ω and φ scan mode. Structures were solved by the direct method using SHELXTL and refined by means of full-matrix least-squares procedures on F2 with the programs SHELXL-97. All nonhydrogen atoms were refined with anisotropic displacement parameters. The sensitivity towards impact (IS) was determined according to BAM standards.
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13C and 1H NMR spectra were measured with AV 500 NMR spectrometer (Bruker, Switzerland). Infrared spectra were measured by an EQUINOX 55 Fourier transform Infrared spectrometer (Bruker, Germany). Elemental analyses were performed with the vario EL cube elemental analyzer (Elementar, Germany).
The thermal analysis experiments were performed with a model TGA/DSC 1 instrument (METTLER, Switzerland). Single crystal X-ray experiment was carried out on a Bruker Apex II CCD diffractometer equipped with graphite monochromatized Ga and Cu Kα radiation using ω and φ scan mode. Structures were solved by the direct method using SHELXTL and refined by means of full-matrix least-squares procedures on F2 with the programs SHELXL-97. All nonhydrogen atoms were refined with anisotropic displacement parameters. The sensitivity towards impact (IS) was determined according to BAM standards.
9
Synthesis and Characterization of Chiral Phosphonic Acid
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R- or S-(1-phenylethylamino)methylphosphonic acid (pempH2) was prepared according to methods reported in the literature38 (link). All other starting materials were of reagent grade and were used as received from commercial sources without further purification. Elemental analyses for C, H and N were carried out on a PE 240C analyser. IR spectra were recorded with a Bruker Tensor 27 spectrometer using KBr discs. The pH value was measured by a Sartorius PB-10 pH metre. Thermal analyses were performed under nitrogen in the temperature range of 25–800 °C at a heating rate of 5 °C min−1 on a METTLER TOLEDO TGA/DSC 1 instrument. PXRD data were collected using a Bruker D8 advance diffractometer. SEM measurements were performed on SHIMADZU SSX-550. The UV–Vis spectra were recorded on Perkin Elmer Lambda 950 UV–Vis/NIR Spectrometer. The circular dichroism spectra were recorded on a JASCO J-720 W spectropolarimeter at room temperature. The simultaneous CD and LD measurements were conducted forR -1 and S -1 using the multi-probe function in the J-1500 CD spectrometer. Each sample was diluted by KCl with a ratio of 1/50 and pressed into a pellet.
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R- or S-(1-phenylethylamino)methylphosphonic acid (pempH2) was prepared according to methods reported in the literature38 (link). All other starting materials were of reagent grade and were used as received from commercial sources without further purification. Elemental analyses for C, H and N were carried out on a PE 240C analyser. IR spectra were recorded with a Bruker Tensor 27 spectrometer using KBr discs. The pH value was measured by a Sartorius PB-10 pH metre. Thermal analyses were performed under nitrogen in the temperature range of 25–800 °C at a heating rate of 5 °C min−1 on a METTLER TOLEDO TGA/DSC 1 instrument. PXRD data were collected using a Bruker D8 advance diffractometer. SEM measurements were performed on SHIMADZU SSX-550. The UV–Vis spectra were recorded on Perkin Elmer Lambda 950 UV–Vis/NIR Spectrometer. The circular dichroism spectra were recorded on a JASCO J-720 W spectropolarimeter at room temperature. The simultaneous CD and LD measurements were conducted for
10
Characterization of Carbon Deposition in DRM Reactions
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To evaluate the deposited carbon during the DRM reaction, the images and amount of carbon accumulated after 10 h of the reaction were analysed. A comparative study of fresh and spent catalysts to determine carbon formation was carried out on an FESEM model JEOL JSM7600F at 20 K magnification and a transmission electron microscope (LEO 912AB).
Determination of crystal phases that appeared after the DRM reaction was conducted using XRD analysis (Shimadzu XRD-6000). Quantitative analysis of carbon formation was performed in a Mettler-Toledo TGA/DSC1 instrument. The coked catalyst was submitted to a heat treatment under 5% O2/N2 (100 cm3 min−1) with a heating rate of 10 °C min−1. Thus, the amount of carbon burned out was determined by the weight loss of CO2 and CO produced during the analysis.
Determination of crystal phases that appeared after the DRM reaction was conducted using XRD analysis (Shimadzu XRD-6000). Quantitative analysis of carbon formation was performed in a Mettler-Toledo TGA/DSC1 instrument. The coked catalyst was submitted to a heat treatment under 5% O2/N2 (100 cm3 min−1) with a heating rate of 10 °C min−1. Thus, the amount of carbon burned out was determined by the weight loss of CO2 and CO produced during the analysis.
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