Calorimetric measurement of the SBL bulk films was performed on a Phoenix 204 F1 (Netzsch, Selb, Germany) instrument using aluminium crucibles (pierced lid) and nitrogen as carrier gas. The temperature range was selected from −150 °C to 200 °C (liquid N2 cooling) with scanning rates of 10 K min−1.
204 f1 phoenix
Manufactured by Netzsch
Sourced in Germany
The 204 F1 Phoenix is a thermogravimetric analyzer (TGA) designed for precise and reliable analysis of material properties. It measures the weight changes of a sample during heating or cooling in a controlled atmosphere. The 204 F1 Phoenix provides accurate data on thermal stability, decomposition, and moisture content of a wide range of materials.
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10 protocols using 204 f1 phoenix
1
Calorimetric Measurement of SBL Films
2
Thermal Analysis of PLGA/TG Mixtures
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The DSC thermograms of the PLGA/TG mixtures differing in composition were obtained with a Phoenix 204F1 (NETZSCH, Waldkraiburg, Germany) differential scanning calorimeter (temperature scanning speed 10 °C/min, mass of the samples sealed into crucibles 3–7 mg, standard calibration). Experiments were performed as follows. Samples of various PLGA/TG mixtures, as well as of pure PLGA and TG, sealed into crucibles, were cooled to −70 °C, heated to 120 °C, cooled once more to −70 °C, and heated again to 120 °C, with the crucibles with samples being kept for 5 min at each of the temperatures indicated above.
3
Differential Scanning Calorimetry for UHMWPE
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Differential scanning calorimetry (DSC) thermograms of the initial films, their blends with o-xylene, and the prepared membranes were recorded using a Phoenix 204F1 instrument (NETZSCH, Selb, Germany). The measurement protocol is shown in Figure 1 .
The crystallinity degree of the polymer was calculated using the following equation:
where ∆Hm is the melting enthalpy of the sample determined in DSC experiments, and ∆Hm100% = 293 J/g [44 (link)] is the melting enthalpy of the hypothetical 100% crystalline UHMWPE sample.
Taking into account the fact that melting enthalpy was calculated per unit of the full sample mass, for the mixtures of UHMWPE with o-xylene, Equation (1) was modified as follows:
where w2 is the polymer mass fraction in the mixture.
The crystallinity degree of the polymer was calculated using the following equation:
where ∆Hm is the melting enthalpy of the sample determined in DSC experiments, and ∆Hm100% = 293 J/g [44 (link)] is the melting enthalpy of the hypothetical 100% crystalline UHMWPE sample.
Taking into account the fact that melting enthalpy was calculated per unit of the full sample mass, for the mixtures of UHMWPE with o-xylene, Equation (1) was modified as follows:
where w2 is the polymer mass fraction in the mixture.
4
Photoreactive LC-crosslinker Characterization
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The photo-reactivity of LC-crosslinkers was characterised using photo-DSC (Netzsch Phoenix 204 F1, μ-sensor). In curing experiments, 2-10 mg samples containing 2% of Irgacure369 ™ (note BA740 could not initiate the samples curing under UV irradiation) were loaded in open aluminum crucibles and cured for 10 min at 30 °C, 50 °C and 70 °C using S2000 UV-lamp (Omni Cure). Samples were kept for 10 min at each temperature before application of UV.
The data of interest from photo-DSC measurements were the time of maximal heat production, t max , measured in seconds, determined by the position of the peak maximum and the heat of polymerization, ΔH P , measured in Joule per gram as a part of the reaction rate equation [45] (link);
and determined by peak integration. Measurements of the molar heat of polymerization (J mol -1 ) were calculated on the basis of the molecular weight and degree of methacrylation determination of NMRanalysis. The heat of the samples ΔH sample (t) was calculated as follows, where 2 is the theoretical number of methacryl groups with respect to the methacrylation degree % MA multiplied with the theoretical heat of a methacryl group ΔH MA (55 kJ mol -1 ) [46] (link), divided by the molecular weight of the sample M sample .
The degree of double bond conversion was then calculated with equation ( 3):
The data of interest from photo-DSC measurements were the time of maximal heat production, t max , measured in seconds, determined by the position of the peak maximum and the heat of polymerization, ΔH P , measured in Joule per gram as a part of the reaction rate equation [45] (link);
and determined by peak integration. Measurements of the molar heat of polymerization (J mol -1 ) were calculated on the basis of the molecular weight and degree of methacrylation determination of NMRanalysis. The heat of the samples ΔH sample (t) was calculated as follows, where 2 is the theoretical number of methacryl groups with respect to the methacrylation degree % MA multiplied with the theoretical heat of a methacryl group ΔH MA (55 kJ mol -1 ) [46] (link), divided by the molecular weight of the sample M sample .
The degree of double bond conversion was then calculated with equation ( 3):
5
Thermal Characterization of PLA Samples
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DSC measurements were performed using a DSC calorimeter (204 F1 Phoenix, NETZSCH, Selb, Germany) in a temperature range from −25 °C to 210 °C at φ = 5 °C/min, performing two heating and one cooling scans. Melting and cold crystallization temperatures and enthalpies (Tm, Tc, ΔHm, ΔHc) were determined from the second heating scan and glass transition temperatures (Tg) were also measured. The crystallinity degree (χ) was calculated according to the following Equation:
where ΔHm is the enthalpy for melting, ΔHm0 is enthalpy of melting for a 100% crystalline PLA sample (taken as 93 J/g) and W is weight fraction of PLA in the sample [16 (link)].
All the experiments were carried out under nitrogen flow. The results were visualized and analyzed using NETZSCH Proteus Software (v6.0, NETZSCH-Gerätebau GmbH, Selb, Germany).
where ΔHm is the enthalpy for melting, ΔHm0 is enthalpy of melting for a 100% crystalline PLA sample (taken as 93 J/g) and W is weight fraction of PLA in the sample [16 (link)].
All the experiments were carried out under nitrogen flow. The results were visualized and analyzed using NETZSCH Proteus Software (v6.0, NETZSCH-Gerätebau GmbH, Selb, Germany).
6
Thermal Analysis of Poly(hydroxybutyrate) (PHB)
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A 10 mg sample of PHB was encapsulated in an aluminum sample vessel and placed in the sample holding chamber of the differential scanning calorimetry (DSC) apparatus (204 F1 Phoenix, NETZSCH-Gerätebau GmbH Büro Rheinbach, Bonn, Germany). The previous thermal history of the sample was removed before the thermal analysis by heating the sample from ambient temperature to 230°C at 20°C/min. Next, the temperature was cooled down at 20°C/min to 50°C/min. The sample was then thermally cycled at 20°C/min to 230°C/min. The melting peak temperature, denoted by TM, was given by the intersection of the tangent to the furthest point of an endothermic peak and the extrapolated sample baseline. The glass transition temperature, denoted by Tg, could be estimated by extrapolating the midpoint of the heat capacity difference between glassy and viscous states after heating the quenched sample.
7
Thermal Analysis of Polymer Samples
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Differential scanning calorimetry (DSC) analyses were performed using the calorimeter 204 F1 Phoenix (NETZSCH). The samples (~10 mg) were cooled to −100 °C and heated up to 160 °C with a rate of 36 °C min−1 under argon atmosphere (50 mL min−1) [39 (link)]. Thermogravimetric analysis (TGA) was performed using an STA 449 F3 Jupiter balance (NETZSCH). The samples (~10 mg) were heated from room temperature to 500 °C with a heating rate of 20 °C min−1 under argon atmosphere (50 mL min−1). The glass transition temperature (Tg) and the degradation temperature (Td) were determined following ASTM E1356 and ASTM E473 standards.
8
Differential Scanning Calorimetry (DSC) of Samples
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A Netzsch 204 F1 Phoenix (Netzsch Group, Selb, Germany) apparatus was used for the DSC analysis of the above-mentioned samples. The analysis conditions were the same as those used for TG (temperature range and rate of 25–500 °C and 10 °C/min, nitrogen purge and protective flow of 40 mL/min), as well as the software used for the acquisition and handling of the DSC data.
9
Thermal Characterization of Flavonoid Complexes
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The differential scanning calorimetry (DSC, Netzsch, 204 F1 Phoenix) was used for recording DSC thermograms of the free hesperetin and naringenin and the inclusion complexes with β-CD and RAMEB. The thermal behavior was studied by heating samples (2–5 mg) in closed aluminum crimped pans at a rate of 10 °C min−1 between a temperature range of 25 to 250 °C for both hesperetin and naringenin [42 (link)].
10
Thermal Analysis of PACA Films
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PACA films for thermal analysis were prepared by casting PEG1000 at 40 °C in a Petri dish (diameter 3.5 cm), followed by 16 repeats of deposition of 160 µL of CA monomer solution (1% v/v in hexane) on the solidified PEG (compare Section 2.3 ). After immersion in water, PACA films were detached and floated, allowing collection in a tube, three repeats of washing with water and centrifugation (8500 rpm, Biofuge Stratos, Heraeus Instruments, Hanau, Germany), and finally freeze drying (Alpha 1-2LD plus, Christ, Osterode, Germany).
PACA films (≈5 mg) were analyzed using DSC (204 F1 Phoenix, Netzsch, Selb, Germany) in a temperature range of −100 to +150 °C for determining the glass transition temperature. Heating and cooling rates were 10 K·min−1 for PMCA, PECA and PBCA and 20 K·min−1 for PMECA and PEECA (as no signals were detectable at 10 K·min−1). The Tg was determined at the inflection point of the thermograms from the second heating run.
PACA films (≈5 mg) were analyzed using DSC (204 F1 Phoenix, Netzsch, Selb, Germany) in a temperature range of −100 to +150 °C for determining the glass transition temperature. Heating and cooling rates were 10 K·min−1 for PMCA, PECA and PBCA and 20 K·min−1 for PMECA and PEECA (as no signals were detectable at 10 K·min−1). The Tg was determined at the inflection point of the thermograms from the second heating run.
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