The hydrogen bonds were characterized using a Fourier transform infrared (FT-IR) spectrometer (IR 200, Thermo Nicolet, USA). Polarized optical microscopy (POM) images were obtained using a Caikon microscope (XPF-500C) equipped with polarization filters. A CK-400 hot stage was used to conduct the thermo-controlled experiments. Differential scanning calorimetry (DSC) was performed using a TA instruments Q2000 calorimeter. The samples were heated or cooled at a rate of 10 °C min−1 with an isothermal equilibration of 2 min after each heating or cooling ramp. The thermogravimetric analyses (TGA) of samples were performed using a STA-449C (Germany). The samples were heated from 30 to 800 °C at a rate of 10 °C min−1 under a nitrogen atmosphere. The XRD patterns were collected on an Anton Paar Saxsess mc2 apparatus attached to an ID 3003 laboratory X-ray generator (General Electric) equipped with a sealed X-ray tube (PANalytical, λ (Cu-Kα) = 0.1542 nm, 40 kV, 50 mA). Adsorption kinetics were studied by UV-vis spectroscopy using a UV-vis spectrometer (Spectrum lab 752s, Shanghai). Other UV-vis spectroscopy experiments were performed using a UV-vis spectrophotometer (UV-1800PC, Mapada Instruments, Shanghai).
Q2000 calorimeter
Manufactured by TA Instruments
Sourced in United States
The Q2000 calorimeter is a thermal analysis instrument manufactured by TA Instruments. It is designed to measure the heat flow in and out of a sample as a function of temperature or time. The Q2000 can be used to analyze a wide range of materials, including polymers, metals, and biological samples.
Automatically generated - may contain errors
Lab products found in correlation
Ta universal analysis software version 4, by TA Instruments (2 mentions)
Id 3003 laboratory x ray generator, by GE Healthcare (1 mentions)
Ir 200, by Thermo Fisher Scientific (1 mentions)
Uv 1800pc, by MAPADA (1 mentions)
Uv 3102 pc spectrophotometer, by Shimadzu (1 mentions)
Alpha 300r, by WITec (1 mentions)
670 ftir spectrometer, by Agilent Technologies (1 mentions)
Lambda 750, by PerkinElmer (1 mentions)
Originpro 2021, by OriginLab (1 mentions)
Tga q50, by TA Instruments (1 mentions)
Sdt q600, by TA Instruments (1 mentions)
Universal analysis software, by TA Instruments (1 mentions)
Hanna hi 8424, by Hanna Instruments (1 mentions)
Spectrum 100 spectrometer, by PerkinElmer (1 mentions)
25 protocols using q2000 calorimeter
1
Characterization of Hydrogen Bonds and Thermal Properties
2
Thermal Analysis of Electrospun Drug-Polymer Fibers
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Modulated temperature differential scanning calorimetry (MTDSC)
thermograms of pure drug, polymer, physical mixture, and electrospun
fibers were recorded using a TA Instruments Q2000 calorimeter (TA
Instruments, New Castle, Delaware, USA). Sample weights ranged from
4 to 8 mg and were sealed in a 40 μL aluminum PerkinElmer standard
pan. A pinhole was manually formed in the lids to allow for solvent
evaporation. Samples were heated under nitrogen gas (flow rate 50
mL/min) at a heating rate of 2 °C/min ramped up to 150 °C,
amplitude ±0.212 °C, and a period of 40 s. Data analysis
was carried out with TA Universal Analysis software, version 4.5A.
thermograms of pure drug, polymer, physical mixture, and electrospun
fibers were recorded using a TA Instruments Q2000 calorimeter (TA
Instruments, New Castle, Delaware, USA). Sample weights ranged from
4 to 8 mg and were sealed in a 40 μL aluminum PerkinElmer standard
pan. A pinhole was manually formed in the lids to allow for solvent
evaporation. Samples were heated under nitrogen gas (flow rate 50
mL/min) at a heating rate of 2 °C/min ramped up to 150 °C,
amplitude ±0.212 °C, and a period of 40 s. Data analysis
was carried out with TA Universal Analysis software, version 4.5A.
3
Thermal Analysis of Phase Change Materials
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DSC was performed to measure the most important thermal properties
of a PCM, such as the phase transition enthalpies and temperatures,
and to evaluate their changes after the coating process. Powder samples
of approx. 5 mg were placed in standard aluminum DSC pans and analyzed
with a TA Instruments Q2000 calorimeter (New Castle, DE). Each sample
was subjected to a heating/cooling/heating cycle at 10 °C/min
from −20 to 80 °C, under a nitrogen atmosphere. The test
allowed the measurement of the peak temperature and enthalpy of each
phase transition and an evaluation of the variation in the core-to-shell
mass ratio after the coating.
of a PCM, such as the phase transition enthalpies and temperatures,
and to evaluate their changes after the coating process. Powder samples
of approx. 5 mg were placed in standard aluminum DSC pans and analyzed
with a TA Instruments Q2000 calorimeter (New Castle, DE). Each sample
was subjected to a heating/cooling/heating cycle at 10 °C/min
from −20 to 80 °C, under a nitrogen atmosphere. The test
allowed the measurement of the peak temperature and enthalpy of each
phase transition and an evaluation of the variation in the core-to-shell
mass ratio after the coating.
4
Tensile and Thermal Properties of Polymers
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Uniaxial tensile testing was carried out on electromechanical universal tester machine (MTS, CMT4304) with 50 N sensor at a strain rate of 2 mm/min (for PMMA based materials) or 20 mm/min (for PMA based materials) and a temperature of 25 °C. The 3.5 cm length dog bone-shaped specimens were prepared by cut-off knife followed by precise machining. The stress at break and elongation at break were obtained from the stress-strain experiment with at least three identical specimens and reported as averaged values. The stress relaxation experiments were carried out on electromechanical universal tester machine (MTS, CMT4304). Samples were first loaded uniaxially at a strain rate of 20 mm/min or 2 mm/min to a strain of 80% or 10%. Load and strain are measured with time at constant grip displacement. DSC measurements were carried out on a TA Instruments Q2000 calorimeter. Samples were sealed into a standard aluminum pan. A sealed empty pan was used as reference. The scan was carried out in nitrogen atmosphere at a flow rate of 200 ml/min at a scanning rate of 10 °C /min. Final data were collected for three full cycles which were identical. The inflection points of the DSC traces were used for the determination of the glass transition temperatures, Tg.
5
Quantifying Polymer Crystallinity by DSC
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The crystallinity of type B samples was investigated by DSC with a TA Instruments Q2000 calorimeter calibrated with indium. Xc values were determined from the first heating scan from 25 °C to 300 °C at a rate of 50 °C/min. The enthalpy of fusion of 100% crystalline PPO used to calculate Xc was set at 5.95 kJ/mol (49.5 J/g).50
The Xc value of type A samples was validated to be ∼0% using the same procedures.
The Xc value of type A samples was validated to be ∼0% using the same procedures.
6
Characterizing Paracetamol Crystallization and Melting
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The crystallization
and melting dynamics were further evaluated with DSC. Two scans were
performed. The first scan was used to determine the actual polymorph
of the crystalline paracetamol measured by THz-TDS at room temperature.
Five milligrams of crystalline sample was loaded into an aluminum
pan and crimped (closed with a lid). The calorimetric measurement
was performed with a TA Instruments Q2000 calorimeter from room temperature
to 470 K at 10 K min–1.
The second scan was
used to accurately determine the onset of crystallization in amorphous
paracetamol. For this purpose, 5 mg of crystalline sample was loaded
into an aluminum pan and crimped. The sample was then heated to 453
K, melted, quenched down to 298 K, heated to 320 K, equilibrated for
15 min, and measured from 323 to 373 K at a rate of 0.4 K min–1, which matches the heating rate of the variable temperature
THz-TDS experiment described above.
and melting dynamics were further evaluated with DSC. Two scans were
performed. The first scan was used to determine the actual polymorph
of the crystalline paracetamol measured by THz-TDS at room temperature.
Five milligrams of crystalline sample was loaded into an aluminum
pan and crimped (closed with a lid). The calorimetric measurement
was performed with a TA Instruments Q2000 calorimeter from room temperature
to 470 K at 10 K min–1.
The second scan was
used to accurately determine the onset of crystallization in amorphous
paracetamol. For this purpose, 5 mg of crystalline sample was loaded
into an aluminum pan and crimped. The sample was then heated to 453
K, melted, quenched down to 298 K, heated to 320 K, equilibrated for
15 min, and measured from 323 to 373 K at a rate of 0.4 K min–1, which matches the heating rate of the variable temperature
THz-TDS experiment described above.
7
Optical and Thermal Characterization of Thin Films
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The surface
microstructure and roughness of the films were characterized by optical
microscopy (Leica DM 2700M) and an Interferometer (FOGALE Nanotech
Incorporated, France). The polarized transmittance of samples was
measured in the range of 0–180° at 550 nm on a Shimadzu
(Japan) UV-3102 PC spectrophotometer with a 1° interval. During
UV–vis measurement, the samples were sandwiched between two
glass slides and coated with a few drops of paraffin oil to reduce
the surface scattering of the samples.16 (link) Small-angle light scattering (SALS) patterns were measured using
a He–Ne gas laser (wavelength: 632 nm) and Vv patterns were
obtained with the polarizer and analyzer parallel. Differential scanning
calorimetry (DSC) experiments were performed on a TA Instruments Q2000
calorimeter at a rate of 10 °C/min between 25 to 180 °C.
Wide-angle X-ray scattering (WAXS) measurements were performed on
a Ganesha lab instrument equipped with a Genix-Cu ultralow divergence
source producing X-ray with a wavelength of 1.54 Å. Raman spectra
were performed to characterize the crystallinity and chain orientation
on a Raman Microscope (Witec Alpha 300 R). Thermal conductivity was
measured by a setup based on the Angstrom method as previously reported.16 (link)
microstructure and roughness of the films were characterized by optical
microscopy (Leica DM 2700M) and an Interferometer (FOGALE Nanotech
Incorporated, France). The polarized transmittance of samples was
measured in the range of 0–180° at 550 nm on a Shimadzu
(Japan) UV-3102 PC spectrophotometer with a 1° interval. During
UV–vis measurement, the samples were sandwiched between two
glass slides and coated with a few drops of paraffin oil to reduce
the surface scattering of the samples.16 (link) Small-angle light scattering (SALS) patterns were measured using
a He–Ne gas laser (wavelength: 632 nm) and Vv patterns were
obtained with the polarizer and analyzer parallel. Differential scanning
calorimetry (DSC) experiments were performed on a TA Instruments Q2000
calorimeter at a rate of 10 °C/min between 25 to 180 °C.
Wide-angle X-ray scattering (WAXS) measurements were performed on
a Ganesha lab instrument equipped with a Genix-Cu ultralow divergence
source producing X-ray with a wavelength of 1.54 Å. Raman spectra
were performed to characterize the crystallinity and chain orientation
on a Raman Microscope (Witec Alpha 300 R). Thermal conductivity was
measured by a setup based on the Angstrom method as previously reported.16 (link)
8
Optical and Thermal Analysis of CLC Polymers
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The reflection of the CLC polymers
was measured through ultraviolet–visible spectroscopy using
a PerkinElmer LAMBDA 750 with a 150 mm integrating sphere over a range
of 400–750 nm. A Varian 670 FT-IR spectrometer with slide-on
ATR (Ge) was used to record IR spectra. Thermogravimetric analysis
was performed in a TA TGA Q500 with a constant heating rate of 5 °C/min.
Thermal transitions of the liquid-crystalline polymers were analyzed
by differential scanning calorimetry using a TA Instruments Q2000
calorimeter with constant heating and cooling rates of 10 °C/min.
was measured through ultraviolet–visible spectroscopy using
a PerkinElmer LAMBDA 750 with a 150 mm integrating sphere over a range
of 400–750 nm. A Varian 670 FT-IR spectrometer with slide-on
ATR (Ge) was used to record IR spectra. Thermogravimetric analysis
was performed in a TA TGA Q500 with a constant heating rate of 5 °C/min.
Thermal transitions of the liquid-crystalline polymers were analyzed
by differential scanning calorimetry using a TA Instruments Q2000
calorimeter with constant heating and cooling rates of 10 °C/min.
9
Thermal Analysis of Drug-Loaded ODMTs
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DSC thermal analyses were conducted in the drug-loaded ODMTs (crushed into fine powders with a mortar and a pestle). Circa. 5 mg samples were mounted in T130425 Tzero hermetic aluminium pans and were sealed with pin-holed aluminium hermetic lids (TA instruments, New Castle, UK). DSC analysis was performed using a Q2000 calorimeter (TA Instruments), with a nitrogen gas (flow rate at 50 mL/min). The DSC method started from 25 °C and increased at a rate of 10 °C/min up until 250 °C. The data were collected and processed via the TA Universal Analysis software version 4.5 (TA Instruments). Exported data were plotted using the OriginPro 2021(OriginLab Corporation, Northampton, MA, USA).
10
Differential Scanning Calorimetry Analysis
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DSC was carried out using a Q2000 calorimeter (TA Instruments), using a heating rate of 15 °C/min and a Ni/Ar (50 ml/min) controlled environment, measuring the heat flow from 40 to 500 °C.
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