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Dsc 1 differential scanning calorimeter

Manufactured by Mettler Toledo
Sourced in Switzerland

The DSC-1 is a differential scanning calorimeter (DSC) manufactured by Mettler Toledo. It is a thermal analysis instrument designed to measure heat flow in and out of a sample as it is heated or cooled. The DSC-1 provides quantitative measurements of physical and chemical changes in materials, such as melting, crystallization, glass transitions, and other thermodynamic properties.

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8 protocols using dsc 1 differential scanning calorimeter

1

Characterization of Biopolymer Properties

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Molecular-weight characteristics (Mw—molecular-weight average, Mn—molecular-number average, Зpolydispersity) of polymers were detected using a size-exclusion chromatograph (Agilent Technologies 1260 Infinity, Waldbronn, Germany) equipped with an Agilent PLgel Mixed-C column. A DSC-1 differential scanning calorimeter (Mettler Toledo, Schwerzenbac, Switzerland) was used to analyze the thermal properties of PHA. Using the STARe software, melting point (Tmelt) was determined from exothermal peaks in thermograms. Using a TGA2 thermal analysis system (Mettler Toledo, Schwerzenbac, Switzerland), the thermal degradation (Tdegr) was determined. The X-ray analysis of structure and crystallinity determination of the polymers obtained was carried out using a D8ADVANCE X-ray powder diffractometer (Bruker AXS, Karlsruhe, Germany) [77 (link)].
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2

Thermal Characterization of PLA Composites

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METTLER TOLEDO DSC1 differential scanning calorimeter was used to record glass transition temperature (Tg), crystallization temperature (Tc), cold crystallization temperature (Tcc), melting temperature (Tm), crystallization enthalpy (ΔHc), cold crystallization enthalpy (ΔHcc), and melting enthalpy (ΔHm). Samples of approximately 5–7 mg, sealed in aluminum crucible, were used.
DSC analysis was divided into five stages:

First stage (Heating 1): the samples were heated at a constant rate of 10 °C/min from 0 °C to 300 °C.

Second stage: an isothermal stage lasting 5 min.

Third stage: the samples were cooled at a rate of 10 °C/min to 0 °C.

Fourth stage: an isothermal stage lasting 5 min.

Fifth stage (Heating 2): the samples were heated at a constant rate of 10 °C/min.

The following expression was used to evaluate the room temperature crystallinity, Xc, of PLA [15 (link)]: XC=ΔHmΔHccwΔHm0·100%
where ΔHm is the fusion enthalpy (J/g), ΔHcc is the cold crystallization enthalpy (J/g),
ΔHm0 is the enthalpy of fusion of 100% crystalline PLA (93 J/g), and w is the fraction of the polymer in the composite materials. The experiment was performed in accordance with the ISO 11357-(1–3): 2016 standards [16 ]. The glass transition, crystallization, and melting temperatures were determined with accuracy of ±0.8 °C and enthalpy with ±0.5 J/g.
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3

Preparation and Characterization of Polymer Composites

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A reaction set equipped with a three-necked flask, a stirrer, a thermometer, and a reflux condenser was used to prepare the composites (Figure 1). A thermal chamber (Binder GmbH, Tuttlingen, Germany) and a hydraulic press (Skamet 54436, SKAMET, Skarzysko-Kamienna, Poland) were used for drying and shaping. The following materials were used to characterize the composites: a Zwick 1435 testing machine (Zwick/Roell, Radeberg, Germany); the Nicolet 6700 spectrophotometer (Thermo Scientific, Waltham, MA, USA); a Shore hardness tester type A with a pressure force of 12.5 N, indenter 35°Sh, spring force 806.50cN (Zwick/Roell, Herefordshire, Great Britain); an OCA 15EC goniometer (Dataphysics, Filderstadt, Germany); a DSC1 differential scanning calorimeter (Mettler Toledo, Netzsch, Switzerland); and a UV-VIS CM-3600d spectrophotometer (Konica Minolta, London, UK.). Scanning electron microscopy (SEM) Zeiss Ultra Plus Bruker, Massachusetts, USA) was used to identify structural changes in the composites. An HPP 108 climatic chamber (Memmert GmbH, Schwabach, German) was used to determine the biodegradation. The compositions of the reagents used are given in Table 1 and Table 2.
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4

Characterization of PHA polymers

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The molecular weight and molecular weight distribution of the PHAs were examined using a size-exclusion chromatograph (Agilent Technologies 1260 Infinity, Waldbronn, Germany) with a refractive index detector, and this was achieved using an Agilent PLgel Mixed-C column, where the weight average, Mw, number average, Mn and polydispersity (Ð = Mw/Mn) were determined. The thermal properties of the polymer were analyzed using a DSC-1 differential scanning calorimeter (Mettler Toledo, Schwerzenbac, Switzerland). The melting points were determined from the exothermal peaks in the thermograms using the STARe software. Thermal degradation of the samples was investigated using a TGA2 thermal analysis system (Mettler Toledo, Schwerzenbac, Switzerland). The theoretical degree of crystallinity was calculated using the following formula:
where ∆Hi is specific enthalpy of melting of the sample (J/g), and ∆H0 is the specific enthalpy of a melted 100% crystallized P(3HB) (146 J/g) [67 (link)]. The methods for analyzing the physicochemical properties of PHAs have been previously described in detail [59 (link)].
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5

Thermal Characterization of EVA/MWCNT Composites

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To study the effect of MWCNT wt.% on the thermal characteristics of the EVA/MWCNT composites, DSC measurements were carried out using a DSC 1 differential scanning calorimeter (Mettler Toledo Inc., Columbus, OH, USA). Samples weighing about 8 mg were cut from the as-received EVA/MWCNT pellets. In order to remove the thermal history, samples were first heated from 25 °C to 180 °C at 10 °C/min and held at 180 °C for 5 min, and then cooled down to 30 °C at a cooling rate of 10 °C/min to obtain the non-isothermal crystallization curves. This procedure was repeated in a second run.
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6

Thermal Characterization of PLA-PEG Blends

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Characterization of the synthesized PLA and PLA–PEG
was carried
out on a DSC1 differential scanning calorimeter (Mettler Toledo).
The temperature cycle was set as follows: heating from −35
to 200 °C (rate: 10 °C/min), then 2 min heating at 200 °C,
and cooling to −35 °C (rate: 10 °C/min); this was
repeated after 2 min of maintained temperature. This procedure for
the measurement occurred under a nitrogen atmosphere.
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7

Physicochemical Characterization of High-Purity PHAs

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The physicochemical properties of high-purity PHA specimens were determined using modern physicochemical methods, which have been described in detail elsewhere [41 (link),42 (link)]. Molecular-weight properties of the polymers (weight-average (Mw) and number-average (Mn) molecular weights and polydispersity (Ð)) were measured. Melting point (Tmelt) and thermal degradation temperature (temperature at which sample mass loss begins, Tdegr) were measured using a DSC-1 differential scanning calorimeter (Mettler Toledo, Schwerzenbac, Switzerland) and TGA (Mettler Toledo, Schwerzenbac, Switzerland), respectively. A 3–5 mg sample was heated to 200 °C at a rate of 5 °C/min; the sample was held at 200°C for 1 min, cooled to −20 °C at a rate of 5 °C/min and held for 4 min. Then, the sample was reheated at a rate of 5 °C/min (DSC). A 3–5 mg sample was heated to 450 °C at a rate of 10 °C/min (TGA). Thermograms were analyzed using the “StarE”software. X-ray examination was performed using a D8ADVANCE powder diffractometer (Bruker AXS, Karlsruhe, Germany) equipped with a VANTEC linear detector; the degree of crystallinity (Cx) was calculated as a ratio of the total area of crystalline peaks to the total area of the radiogram (the crystalline + amorphous components
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8

Comprehensive Characterization of PHAs

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Polymer was extracted with chloroform and then precipitated with hexane. The composition of PHAs was analyzed with a GC-MS (6890/5975C, Agilent Technologies, U.S.) and NMR spectrometry. 1 HNMR spectra of copolymer were recorded at room temperature inCDCl 3 on a BRUKER AVANCE III 600 spectrometer operated at 600.13 MHz.
Molecular weight and molecular-weight distribution of PHAs were examined using a gel permeation chromatograph (Agilent Technologies 1260 Infinity, U.S.) with a refractive index detector, using an Agilent PLgel Mixed-C column. Thermal analysis of PHA specimens was performed using a DSC-1 differential scanning calorimeter (Mettler Toledo, Switzerland). Samples were preheated to 60 °C and cooled to 25 °C. The specimens were heated to temperatures from -20°C to 300 °C, at 5 °C×min -1 (measurement precision 1.5 °C). The thermograms were analyzed using the STARe v11.0 software. X-Ray structure analysis and determination of crystallinity of copolymers were performed employing a D8 ADVANCE X-Ray powder diffractometer equipped with a VANTEC fast linear detector (Bruker, AXS, Germany). Calculations were done by using the Eva program of the diffractometer software.
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