Um3 ultramicrobalance

Manufactured by Mettler Toledo

Sourced in Switzerland

The UM3 ultramicrobalance is a highly precise laboratory weighing instrument designed for the measurement of minute sample masses. It features advanced technology to provide accurate and reliable results for delicate weighing applications.

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Lab products found in correlation

Dsc 7, by PerkinElmer (9 mentions) Tga7 system, by PerkinElmer (2 mentions) Curie point standards, by PerkinElmer (2 mentions) Dp71 digital camera, by Olympus (2 mentions) Diamond dsc, by PerkinElmer (2 mentions) Tam 3 nanocalorimeter unit, by TA Instruments (2 mentions) Alumel and ni, by PerkinElmer (1 mentions) Dsc 7 instrument, by PerkinElmer (1 mentions) Dsc 214 polyma, by Netzsch (1 mentions)

14 protocols using um3 ultramicrobalance

Differential Scanning Calorimetry of Solid Samples

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DSC thermograms were recorded on a DSC
7 (PerkinElmer Norwalk,
Ct., USA) controlled by the Pyris 2.0 software. Using a UM3 ultramicrobalance
(Mettler, Greifensee, CH), samples of approximately 5–15 mg
were weighed into perforated or sealed aluminum pans or hermetically
sealed (high pressure) capsules. The samples were heated using rates
in between 1 and 20 °C min^–1 with dry nitrogen
as the purge gas (purge: 20 mL min^–1). The instrument
was calibrated for temperature with pure benzophenone (mp 48.0 °C)
and caffeine (236.2 °C), and the energy calibration was performed
with indium (mp 156.6 °C, heat of fusion 28.45 J g^–1). The errors on the stated temperatures (extrapolated onset temperatures)
and enthalpy values were calculated at the 95% confidence intervals
(CI) and are based on at least five measurements.

Braun D.E, & Griesser U.J. (2016). Stoichiometric and Nonstoichiometric Hydrates of Brucine. Crystal Growth & Design, 16(10), 6111-6121.

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Differential Scanning Calorimetry of Novel Compound

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Example 3

Differential scanning calorimetry (DSC) was performed with a DSC 7 (Perkin-Elmer, Norwalk, Conn., USA) using a Pyris 2.0 software. 4.7307±0.0005 mg sample (using a UM3 ultramicrobalance, Mettler, Greifensee, CH) were weighed into Al-Pans (25 microliter) and sealed with a cover, which was perforated by a needle. The sample was heated at a rate of 10 K/min. Dry nitrogen was used as the purge gas (purge rate: 20 mL/min).

The corresponding DSC curve is displayed in FIG. 2 of the present invention and displays a first endothermic peak having an onset temperature of about 131° C. and a peak temperature of about 148° C. Thereafter an exothermic peak having an onset temperature of about 196° C. and a peak temperature of about 211° C. appears immediately followed by a second endothermic peak having an onset temperature of about 231° C. and a peak temperature of about 238° C. The DSC curve may be interpreted in that the first endothermic peak corresponds to a dehydration/melting event, the exothermic peak is a crystallization peak and the second endothermic peak corresponds to a melting event.

US10954235B2. Crystalline forms of valbenazine salts (2021-03-23). Sandoz AG [CH]. Inventors: Christoph Langes [AT], Ulrich Griesser [AT], Erwin Schreiner [AT], Marijan Stefinovic [AT].

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Thermal Analysis of Hy1/Water Mixtures

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DSC thermograms were recorded on a DSC 7 or Diamond DSC (PerkinElmer
Norwalk, CT, USA) controlled by the Pyris 7.0 software. Using a UM3
ultramicrobalance (Mettler, Greifensee, Switzerland), samples of approximately
2–25 mg were weighed into open/closed aluminum pans or hermetically
sealed (high-pressure) pans. For the construction of the temperature/composition
phase diagram, Hy1/AH_s1 mixtures were prepared by gently
mixing the two phases. The Hy1/water mixtures were prepared by placing
precisely weighed amounts of Hy1 and pure water (with the aid of a
Hamiltion syringe) into high-pressure DSC pans followed by a second
accurate weight measurement. The sealed sample pans were stored for
24 h before the DSC runs were started to equilibrate the mixtures.
For low temperature measurements the samples were frozen (liquid N₂) before the DSC runs. The samples were heated using rates
ranging from 2 to 20 °C min^–1, with dry nitrogen
as the purge gas (purge: 20 mL min^–1). The two instruments
were calibrated for temperature with pure benzophenone (mp 48.0 °C)
and caffeine (236.2 °C), and the energy calibration was performed
with indium (mp 156.6 °C, heat of fusion 28.45 J g^–1). The errors on the stated desolvation temperatures (extrapolated
onset temperatures) and enthalpy values were calculated at the 95%
confidence intervals (CI) and are based on at least five measurements.

Braun D.E., Nartowski K.P., Khimyak Y.Z., Morris K.R., Byrn S.R, & Griesser U.J. (2016). Structural Properties, Order–Disorder Phenomena, and Phase Stability of Orotic Acid Crystal Forms. Molecular Pharmaceutics, 13(3), 1012-1029.

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Thermal Characterization of Materials

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For hot-stage thermomicroscopic
(HSM) investigations a Reichert Thermovar polarization microscope,
equipped with a Kofler hot-stage (Reichert, A), was used. Photographs
were taken with an Olympus DP71 digital camera.
Differential
scanning calorimetry (DSC) thermograms were recorded on a DSC 7 (PerkinElmer
Norwalk, Ct., USA) and Diamond DSC controlled by the Pyris software.
Using a UM3 ultramicrobalance (Mettler, Greifensee, CH), samples of
approximately 3–10 mg were weighed into perforated aluminum
pans or high pressure capsules. The samples were heated using rates
of 1, 2, 5 (perforated), and 10 (high pressure capsules) °C min^–1 with dry nitrogen as the purge gas (purge: 20 mL
min^–1). The instruments were calibrated for temperature
with pure benzophenone (mp 48.0 °C) and caffeine (236.2 °C),
and the energy calibration was performed with indium (mp 156.6 °C,
heat of fusion 28.45 J g^–1).
Thermogravimetric
analysis (TGA) was carried out with a TGA7 system
(PerkinElmer, Norwalk, CT, USA) using the Pyris 2.0 Software. Approximately
5–8 mg of sample was weighed into a platinum pan. Two-point
calibration of the temperature was performed with ferromagnetic materials
(Alumel and Ni, Curie-point standards, PerkinElmer). A heating rate
of 2, 5, or 10 °C min^–1 was applied, and dry
nitrogen was used as a purge gas (sample purge: 20 mL min^–1, balance purge: 40 mL min^–1).

Braun D.E., Gelbrich T., Kahlenberg V, & Griesser U.J. (2020). The Eight Hydrates of Strychnine Sulfate. Crystal Growth & Design, 20(9), 6069-6083.

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Differential Scanning Calorimetry of Samples

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DSC thermograms were recorded on a DSC 7 or Diamond DSC
(Perkin-Elmer Norwalk, Ct., USA) controlled by the Pyris 7.0 software. Using
a UM3 ultramicrobalance (Mettler, Greifensee, CH), samples of approximately
2 - 5 mg were weighed into perforated/sealed aluminium pans. The samples
were heated using rates starting from 0.5 to and 20 °C
min^–1, with dry nitrogen as the purge gas (purge: 20
ml min^–1). The two instruments were calibrated for
temperature with pure benzophenone (mp 48.0 °C) and caffeine (236.2
°C), and the energy calibration was performed with indium (mp 156.6
°C, heat of fusion 28.45 J g^–1). The errors on the
stated temperatures (extrapolated onset temperatures) and enthalpy values
were calculated at the 95% confidence intervals (CI) and are based on at
least three measurements.

Braun D.E., Schneeberger A, & Griesser U.J. (2017). Understanding the Role of Water in 1,10-Phenanthroline Monohydrate. CrystEngComm, 19(41), 6133-6145.

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Differential Scanning Calorimetry Protocol

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DSC measurements were performed using a DSC7 (Perkin-Elmer, Norwalk,
Connecticut, USA), controlled by the Pyris 8.0 software. Approx. 2–3
mg of sample was weighed into sealed aluminum pans using a UM3 ultramicrobalance
(Mettler, Greifensee, Switzerland). Heating rates of 5 and 10 °C
min^–1 were applied, and dry nitrogen was used as
a purge gas (20 mL min^–1). The instrument was calibrated
for temperature with pure benzophenone (mp 48.0 °C) and caffeine
(236.2 °C), and the energy calibration was performed with indium
(mp 156.6 °C, heat of fusion 28.45 J g^–1).
The stated (extrapolated onset) temperatures and enthalpy values have
an error calculated at 95% CI and are based on at least three measurements.

Racher F., Petrick T.L, & Braun D.E. (2023). Exploring the Supramolecular Interactions and Thermal Stability of Dapsone:Bipyridine Cocrystals by Combining Computational Chemistry with Experimentation. Crystal Growth & Design, 23(6), 4638-4654.

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Differential Scanning Calorimetry of Valbenazine Ditosylate

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Example 7

Differential scanning calorimetry (DSC) was performed with a DSC 7 (Perkin-Elmer, Norwalk, Conn., USA) using a Pyris 2.0 software. 7.115±0.0005 mg sample (using a UM3 ultramicrobalance, Mettler, Greifensee, CH) were weighed into Al-Pans (25 microliter) and sealed with a cover, which was perforated by a needle. The sample was heated at a rate of 10 K/min. Dry nitrogen was used as the purge gas (purge rate: 20 mL/min).

The corresponding DSC curve of the crystalline anhydrous form of valbenazine ditosylate of the present invention is shown in FIG. 5 and displays a single endothermic peak having an onset temperature of 239.4° C., a peak temperature of 242.4° C. and a heat of fusion of 54.1 kJ/mol. The DSC curve may be interpreted in that the endothermic peak corresponds to a melting event.

US10954235B2. Crystalline forms of valbenazine salts (2021-03-23). Sandoz AG [CH]. Inventors: Christoph Langes [AT], Ulrich Griesser [AT], Erwin Schreiner [AT], Marijan Stefinovic [AT].

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Differential Scanning Calorimetry Analysis

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A DSC7 instrument (PerkinElmer, Norwalk, Connecticut) in conjunction
with the Pyris 8.0 Software was used to analyze the samples. The samples
were precisely weighed using a UM3 ultramicrobalance (Mettler, Greifensee,
Switzerland). Approximately 2–5 mg of the sample were used,
and the analysis employed a heating rate of 10 °C min^–1, with a N₂ purge gas flow of 20 mL min^–1. Enthalpies were derived from hermetically sealed capsules with
a minimum of three measurements, and error estimation was performed
at a 95% confidence interval. The solvates were additionally measured
with pierced lids. The calorimeter underwent calibration using benzophenone
(48.0 °C) and caffeine (236.2 °C) for temperature calibration
and indium (28.45 J g^–1) for enthalpy calibration.

Petrick T.L., Grünwald A, & Braun D.E. (2024). Flavone Cocrystals: A Comprehensive Approach Integrating Experimental and Virtual Methods. Crystal Growth & Design, 24(10), 4195-4212.

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Thermal Analysis of Samples

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The analyses were carried out using a DSC7 instrument (PerkinElmer,
Norwalk, Connecticut, USA) in combination with the Pyris 8.0 Software.
Precise sample weighing was performed with a UM3 ultramicrobalance
(Mettler, Greifensee, Switzerland). Approximately 2–5 mg of
each sample was utilized, and the analyses involved heating rates
of 1, 2, 5, or 10 °C min^–1, with a nitrogen
purge gas flow of 20 mL min^–1. Temperature (onset)
and enthalpy values were determined based on a minimum of three measurements,
and error estimation was conducted with a 95% confidence interval.
The calorimeter was calibrated using benzophenone (48.0 °C) and
caffeine (236.2 °C) for temperature calibration and indium (28.45
J g^–1) for enthalpy calibration.

Widauer A., Petrick T.L, & Braun D.E. (2024). Comprehensive Insights into Sulfaguanidine in the Solid State: An Experimental and Computational Study. Crystal Growth & Design, 24(3), 1438-1457.

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Solution Calorimetry of Organic Compounds

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The experiments were performed with a TAM III nanocalorimeter unit
(TA Instruments, US). Solution calorimetry data were recorded using
a 20 mL micro solution ampule. The experiments were performed at 25
°C in 15 mL of DMSO. Approximately 7–12 mg of the sample
were accurately weighed into reusable stainless-steel capsules using
a UM3 ultramicrobalance (Mettler, CH). Once the baseline had stabilized
to ±50 nW, the capsule was dropped into the calorimeter. The
heat flow into or out of the calorimeter was recorded, and data analysis
was performed using TAM Assistant software. The heat flow of the empty
RH capsule was subtracted from the heat flow of the sample measurements.
The errors on the stated enthalpy values are calculated at 95% confidence
intervals and are based on at least three measurements. The calorimeter
was calibrated periodically using the electrical substitution method
as well as with reference materials (KCl and sucrose).

Dyba A.J., Wiącek E., Nowak M., Janczak J., Nartowski K.P, & Braun D.E. (2023). Metronidazole Cocrystal Polymorphs with Gallic and Gentisic Acid Accessed through Slurry, Atomization Techniques, and Thermal Methods. Crystal Growth & Design, 23(11), 8241-8260.

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