Before starting thermal analysis, each sample was mechanically divided into three parts: a full-thickness sample (to obtain relevant thermograms) and separated peri-implant and subepidermal fragments of implantation sites (for spatial attribution of the endothermic peaks). Tissue samples of approximately 7–11 mg were excised, blotted with tissue paper to remove surface water, and placed in hermetically-sealed aluminum pans. Differential scanning calorimetry (DSC) measurements were performed using a Phoenix DSC 204 (Netzsch, Selb, Germany) differential scanning calorimeter with heating from 20 °C to 90 °C at the scanning rate of 10 °C/min. The resulting DSC curves were analyzed using Proteus® Thermal Analysis software. The heat of collagen denaturation was normalized to dry weight of the tissue. Deconvolution of the data in the 40–85 °C region into Gaussian peaks was performed by multi-peaks fitting using Origin 8.0 software. The fraction of the corresponding collagen population in the mixture was estimated via the area under each peak (estimated by peak deconvolution).
Dsc 204 phoenix
Manufactured by Netzsch
Sourced in Germany
The DSC 204 Phoenix is a differential scanning calorimeter (DSC) manufactured by Netzsch. It is a thermal analysis instrument designed to measure the heat flow associated with phase transitions and other thermal events in materials. The DSC 204 Phoenix provides precise temperature control and measurement capabilities, allowing for the analysis of a wide range of materials.
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10 protocols using dsc 204 phoenix
1
Thermal Analysis of Collagen Denaturation
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Differential Scanning Calorimetry of Meropenem
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Differential scanning calorimetry (DSC) data were collected by the use of a Phoenix DSC-204 (Netzsch) system at a scanning rate of 5 °C·min−1. The samples of about 3 mg of non- irradiated and irradiated meropenem samples were sealed in aluminium cells with pierced lids. The measurements were performed in a helium atmosphere within the temperature range from 25 °C to 200 °C. The results were processed using the TAA (Netzsch) software. The peak area was evaluated using linear baseline corrections.
3
Thermal Properties of Native and HHP-Treated Starch
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The thermal properties of native and HHP-treated starch samples were evaluated in a differential scanning calorimeter (DSC) instrument (DSC 204 Phoenix, Netzsch, Wittelsbacherstraße, Germany). Prior to experiments, DSC was calibrated for temperature and enthalpy using indium as a standard (Tm: 156.6 °C and ΔHm: 28.45 J/g). For the analysis, 20 ± 0.01 mg of HHP-treated samples were placed in a 25 µL aluminum pan. Pans were hermetically sealed, and an empty pan was used as a reference. DSC measurements were carried out through an isothermal phase (25 °C for 3 min) and then scanned at a dynamic phase at 5 °C/min from 25 to 90 °C. Denaturation temperature (Td) and denaturation enthalpy (ΔHd) were estimated by measuring the area under the DSC transition curve with the manufacturer software Proteus Analysis Software (Version 4.2/3, Netzsch, Wittelsbacherstraße, Germany). All the DSC measurements were done in triplicate.
% of gelatinization was calculated using Equation (6) reported by Blaszczak et al. [51 (link)]:
where ΔHns and ΔHts were the gelatinization enthalpies of native and HHP-treated potato starch, respectively.
% of gelatinization was calculated using Equation (6) reported by Blaszczak et al. [51 (link)]:
where ΔHns and ΔHts were the gelatinization enthalpies of native and HHP-treated potato starch, respectively.
4
Thermal Behavior Analysis of MP Particles
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To investigate the thermal behavior of MP particles, differential scanning calorimetry (DSC) was performed (DSC 204 Phoenix, Netzsch, Selb, Germany). Ten samples of about 10 mg were weighed and sealed in aluminum DSC crucibles and placed in the DSC cell. The samples were heated from -50 °C to 170 °C at a rate of 10 °C min-1 under nitrogen atmosphere running two cycles for each sample. The crystallinity of the materials was calculated using a heat of fusion of 293 J g-1 for 100% crystalline PE.
5
Thermal Transitions of Polyols and TPUs
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The thermal transitions of the polyols and TPUs were determined by differential scanning calorimetry (DSC, Netzsch DSC 204 Phoenix, Selb, Germany) under nitrogen atmosphere (50 mL.min−1). Samples of 9–10 mg were used. The melting temperature and enthalpy were calibrated with indium, tin, bismuth, and zinc standards. The samples were analyzed from −80 to 240 °C at a heating rate of 20 °C.min−1. The value of the Tg is given at the onset point, and the variation of heat capacity ΔCp is calculated at the ΔTg midpoint. To determine the specific transition temperatures of the rigid phase, model reactions were carried out with the MDI-BDO and MDI-DPG at 80 °C under mechanical stirring for 1 h.
6
Thermal Analysis of cPEVA Copolymers
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DSC measurements were performed on DSC 204 Phoenix (NETZSCH, Selb, Germany) including a heating-cooling-heating cycle. The first heating process was performed from ambient temperature to 200 °C with a heating rate of 20 °C·min−1 followed by cooling to −100 °C at varied cooling rate (100 °C·min−1, 50 °C·min−1, 20 °C·min−1, 10 °C·min−1, 5 °C·min−1 and 1 °C·min−1) for determination of the temperature, where crystallization occurred. The melting temperature and the glass transition temperature of cPEVAs were obtained from the second heating run from −100 °C to 200 °C. Furthremore, the crystallinity index (χc) of PE segments in cPEVAs can be calculated from DSC exothermic curves according to Equation (3) [37 (link)]: where ΔHm is the integrated melting enthalpy, representing the area of the melting peak [38 ], and ΔH100 is the specific melting enthalpy for a 100% crystalline PE segment (287.3 J·g−1) [39 (link),40 (link),41 (link)]
7
Thermal Characterization of Compounds
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The results from the DSC made it possible to determine the melting temperatures of the tested compounds including the onset melting temperatures (Tonset) and the maximum melting temperatures (Tmelt) as well as the melting enthalpy (ΔH). The DSC analyses with a use of a DSC 204 Phoenix apparatus (Netzsch, Selb, Germany) were applied. The tested compounds (a sample mass of approx. 10 mg) in the aluminium crucible with a pierced lid were heated from 20 °C to 250 °C. The heating rate was 10 °C min−1. The course of melting was studied in inert and oxidative atmospheres. For an inert atmosphere, helium with a flow rate of 40 mL min−1 was used. For an oxidative atmosphere, a synthetic air with a flow rate of 40 mL min−1 was applied.
8
Thermal Analysis of Polylactic Acid
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The thermal properties of the samples were analyzed by differential scanning calorimetry (DSC) on a DSC 204 Phoenix from Netzsch (Selb, Germany). Samples of about 10 mg were weighed and then sealed in DSC crucibles and placed in the DSC cell. The measurements were performed under nitrogen atmosphere. First, they were heated from 20 to 200 °C at 10 K/min. Subsequently, they were cooled down from 200 to 20 °C with 10 K/min. and then heated up again from 20 to 200 °C at 10 K/min. Additional experiments with elevated heating rates of 20 K/min. were also carried out. It is well known that the crystallization of PLA is very slow. Hence, measurements were also performed at a lower cooling rate of 2 K/min to further investigate the crystallization process. The crystallinity of the materials was calculated by the use of heat of fusion of 93.1 J/g for 100% crystalline PLA homopolymers [22 (link)].
9
Thermal Analysis of PCL Scaffolds
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Differential scanning calorimetry (DSC) measurements were carried out on a Netzsch DSC204 Phoenix connected to Netzsch TASC 414/3A controller equipped with CC-200 cooling controller from Netzsch (Selb, Germany). PCL scaffolds were sealed in alumina pans with pierced lid and exposed to a double heating cycle: Samples were heated up from room temperature to 120 °C with a heating rate of 10 °C/min. Subsequently, samples were cooled down to -100 °C with a cooling rate of 10 °C/min and heated up again to 120 °C with a heating rate of 10 °C/ min. Proteus thermal analysis software (Netzsch) was used to quantify melting temperature as peak temperature (T m ), enthalpy of fusion (H F ), glass transition temperature (T g ) and change in heat capacity at glass transition (Δc p ). Both heating cycles were evaluated. For quality control reasons, another set of thermograms was recorded on a TA Q2000 by TA instruments (New Castle, USA). Heating cycles and sample preparation are identical to the ones performed on Netzsch DSC. Universal Analysis software (TA Instruments) was used to quantify melting temperature (T m ), enthalpy of fusion (H F ), glass transition temperature (T g ) and change in heat capacity at glass transition (Δc p ). Data was merged by averaging for a comprehensive overall median value, since all measured sets were identical.
10
DSC Analysis of L-Cys-g-PCL Crystallinity
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The crystallinity of the 1 h L-Cys-g-PCL was further investigated with differential scanning calorimetry (DSC) (DSC 204 Phoenix (Netzsch, Germany)) with samples completely filled in small aluminum containers. Nonisothermal scans were carried out from 30ºC to 300ºC at a heating rate of 2ºC per minute, with a nitrogenreplacing atmosphere. The melting point (T m ) and enthalpy of fusion (ΔH m ) were obtained.
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