DSC studies of PEG 20,000, protein powder, and protein-loaded extrudates were performed with a DSC 2 (Mettler Toledo, Gießen, Germany) equipped with an auto sampler, nitrogen cooling and nitrogen as purge gas (30 mL/min). The system was calibrated with indium and zinc standards. Extrudates were milled with a mortar and pestle. At least three samples of ∼10 mg were accurately weighed in 40 μL aluminum crucibles with a pierced lid. DSC scans were recorded from 25 °C to 230 °C using a heating rate of 10 °C/min. STARe software (Mettler Toledo, Gießen, Germany) was employed for acquiring thermograms. Thermograms were normalized for sample weight. The heat capacity (input parameter for simulation) of PEG 20,000, pure BSA and Lysozyme, and protein-PEG 20,000 mixtures were determined using a multi-frequency temperature modulation (TOPEM® mode) with an underlying heating rate of 2 °C/min, a pulse height of 1 °C, from 25 °C to 100 °C and a constant nitrogen purge (30 mL/min).
Dsc 2
Manufactured by Mettler Toledo
Sourced in Germany, Switzerland, United States
The Mettler Toledo DSC 2 is a differential scanning calorimeter that measures the heat flow associated with phase transitions and chemical reactions in materials as a function of temperature and time. It provides accurate and reliable data on thermal properties of substances.
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20 protocols using dsc 2
1
Thermal Analysis of PEG, Protein Powders, and Extrudates
2
Thermal Analysis of Amorphous Solid Dispersions
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DSC measurements were performed using a Mettler-Toledo DSC 2 (Gießen, Germany) equipped with a nitrogen cooling system and nitrogen as purge gas (30 ml/min). Both extruded ASDs were weighed (8–15 mg) into aluminum pans with a pierced lid. The determination of the glass transition temperatures was carried out in TOPEM-mode (DSC measurements with multi-frequency temperature modulation) with a constantly heating rate of 2 K/min using a scanning range from 2 °C to 180 °C.
3
Thermal Properties of HDPE Blends
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Thermal properties were determined using a DSC 2 (Mettler Toledo, Greifensee, Switzerland) calorimeter in 40 µL aluminium crucibles. Samples were tested in a temperature range of 20 °C to 170 °C, with a heating/cooling rate of 10 K/min in a nitrogen (N2) atmosphere (20 mL/min). Isothermal segments before heating and cooling segments were set to 5 min. The degree of crystallinity (Xc) was calculated according to the following equation:
where ΔHm is the sample melting enthalpy, wPE is the mass fraction of HDPE and HDPE-g-MA in the sample, and ΔH0 is the melting enthalpy of 100% crystalline HDPE (293 J/g) [29 (link)].
where ΔHm is the sample melting enthalpy, wPE is the mass fraction of HDPE and HDPE-g-MA in the sample, and ΔH0 is the melting enthalpy of 100% crystalline HDPE (293 J/g) [29 (link)].
4
Thermal Characterization by DSC
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5
Thermal Properties of PA6 and TPU
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Thermal properties were determined using a DSC 2 (Mettler-Toledo GmbH, Greifensee, Switzerland) calorimeter in 40 µL aluminium crucibles. Specimens were prepared from tensile test specimens. The samples were tested in the N2 atmosphere (20 mL/min), with a temperature range of 25 °C to 240 °C and −70 °C to 240 °C for the PA6 and TPU, respectively. The heating and cooling rates were 10 K/min, and the isothermal segments were set to 5 min and 1 min before the heating and cooling runs, respectively. The degree of crystallinity (Xc) of the PA6 was calculated according to the following equation:
where ΔHm is the sample melting enthalpy, and ΔH0 is the melting enthalpy of 100% crystalline PA6 (230 J/g) [20 ].
where ΔHm is the sample melting enthalpy, and ΔH0 is the melting enthalpy of 100% crystalline PA6 (230 J/g) [20 ].
6
Thermal Analysis of Perylene Derivative
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DSC measurements were carried out with a Mettler Toledo DSC2 equipped with a Gas controller GC 200 system. The perylene derivative was dissolved in DCM with a concentration of 10 g liter−1, dried, and collected with tissue paper into a 40-μl Al crucible. Samples were first cooled down to −50°C at a rate of −10°C min−1 and kept isothermal for 30 min, followed by two heating/cooling cycles between −50° and 150°C at 10°C min−1. Melting temperatures were extracted from the first heating scan, while the glass transition temperatures and the reference fictive temperatures were extracted from the second heating scan.
7
Thermal Analysis of Protein Powders
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DSC studies of protein powder, physical mixture and extrudates were performed with a DSC 2 (Mettler Toledo, Gießen, Germany) equipped with an auto sampler, nitrogen cooling and nitrogen as purge gas (30 mL/min). The system was calibrated with indium and zinc standards. At least three samples of ∼10 mg were accurately weighed in 40 μL aluminum crucibles with a pierced lid. DSC scans were recorded from 25 °C to 230 °C using a heating rate of 10 K/min. STARe software (Mettler Toledo, Gießen, Germany) was employed for acquiring thermograms. Thermograms were normalized for sample weight and the peak minimum was designated as unfolding temperature of the protein.
8
Thermal analysis of PHB-based polymer blends
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DSC experiments were conducted on a DSC2 (Mettler Toledo, Columbus, OH, USA), equipped with an intracooler (Julabo FT900, Seelbach, Germany) calibrated with an Indium standard before use. The weight of the DSC samples was around 5 mg. Samples were first heated from −20 °C to 190 °C at 10 °C/min and kept for 1 min at 190 °C, then cooled to −20 °C at 10 °C/min, kept for 1 min at −20 °C, and finally heated to 190 °C at 10 °C/min. Melting temperatures (Tm) and enthalpies (ΔHm), as well as crystallization temperatures (Tc) and enthalpies (ΔHc), were calculated from the second heating and cooling curves, respectively. Crystallinity (Xc) of the PHB phase in the blends was determined by applying the following expression:
where ΔHm (J/g) is the melting enthalpy of the polymer matrix, ΔH0m is the melting enthalpy of 100% crystalline PHB (146 J/g) [33 (link)], and wPHB is the polymer weight fraction of PHB in the blend.
where ΔHm (J/g) is the melting enthalpy of the polymer matrix, ΔH0m is the melting enthalpy of 100% crystalline PHB (146 J/g) [33 (link)], and wPHB is the polymer weight fraction of PHB in the blend.
9
Thermal Analysis of PA6 Composite Materials
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Thermal properties were determined using a DSC 2 (Mettler Toledo, Greifensee, Switzerland) calorimeter in 40 µL aluminium crucibles. Specimens were prepared from tensile test specimens and had a mass of 3.5–5.0 mg. The samples were tested in the temperature range of 25 °C to 240 °C, with a heating/cooling rate of 10 K/min in the N2 atmosphere (20 mL/min). The isothermal segments before the heating and cooling segments were set to 1 min to minimise CeF degradation during the measurement. The results are average values of two measurements. The degree of crystallinity (Xc) was calculated according to the following equation:
where ΔHm is the sample melting enthalpy, wPA is the mass fraction of PA6 in the sample, and ΔH0 is the melting enthalpy of 100% crystalline PA6 (230 J/g) [21 ].
where ΔHm is the sample melting enthalpy, wPA is the mass fraction of PA6 in the sample, and ΔH0 is the melting enthalpy of 100% crystalline PA6 (230 J/g) [21 ].
10
Thermal Analysis of Polymer Films
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DSC measurements were conducted using a Mettler-Toledo DSC 2 (Gießen, Germany) that was equipped with a nitrogen cooling system using nitrogen as the purge gas (30 mL/min). Samples were weighed on aluminum pans at 5–15 mg and closed with a pierced lid. The glass transition temperature and melting point for neat BFZ were determined using a heat–cool–heat cycle (25 °C to 170 °C to −50 °C to 170 °C) with a heat rate of 10 K/min. The glass transition temperatures and melting points for the polymer films and patch matrices were investigated using TOPEM mode with a heat rate of 2 K/min from −70 °C to 170 °C with a pulse height of 1 K.
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