Thermal conductivity measurements for small molecule organic solid materials using modulated differential scanning calorimetry (MDSC) and data corrections for sample porosity

Lin, Yannan; Shi, Zhenqi; Wildfong, Peter L.D.

doi:10.1016/j.jpba.2009.10.022

Cited by 13 publications

(13 citation statements)

References 24 publications

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“…Additionally, the authors compared the results obtained by MDSC with those from X-ray diffraction and concluded that XRD exhibited poor detection of low amorphous content (<10%), while with MDSC it was identified at a lower percent (>1) due to the sensitivity for Tg determination. Lin et al [88] reported a method for measuring the thermal conductivity of small-molecule organic solid materials using MDSC. The experimental section involved the compaction of 18 pure small molecule compounds such as acetaminophen, aspirin, carbamazepine III, Υ-indomethacin, and ketoprofen, among others.…”

Section: Pharmaceutical Productsmentioning

confidence: 99%

Application of Differential Scanning Calorimetry (DSC) and Modulated Differential Scanning Calorimetry (MDSC) in Food and Drug Industries

et al. 2019

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Phase transition issues in the field of foods and drugs have significantly influenced these industries and consequently attracted the attention of scientists and engineers. The study of thermodynamic parameters such as the glass transition temperature (Tg), melting temperature (Tm), crystallization temperature (Tc), enthalpy (H), and heat capacity (Cp) may provide important information that can be used in the development of new products and improvement of those already in the market. The techniques most commonly employed for characterizing phase transitions are thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), thermomechanical analysis (TMA), and differential scanning calorimetry (DSC). Among these techniques, DSC is preferred because it allows the detection of transitions in a wide range of temperatures (−90 to 550 °C) and ease in the quantitative and qualitative analysis of the transitions. However, the standard DSC still presents some limitations that may reduce the accuracy and precision of measurements. The modulated differential scanning calorimetry (MDSC) has overcome some of these issues by employing sinusoidally modulated heating rates, which are used to determine the heat capacity. Another variant of the MDSC is the supercooling MDSC (SMDSC). SMDSC allows the detection of more complex thermal events such as solid–solid (Ts-s) transitions, liquid–liquid (Tl-l) transitions, and vitrification and devitrification temperatures (Tv and Tdv, respectively), which are typically found at the supercooling temperatures (Tco). The main advantage of MDSC relies on the accurate detection of complex transitions and the possibility of distinguishing reversible events (dependent on the heat capacity) from non-reversible events (dependent on kinetics).

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Section: Pharmaceutical Productsmentioning

confidence: 99%

Application of Differential Scanning Calorimetry (DSC) and Modulated Differential Scanning Calorimetry (MDSC) in Food and Drug Industries

et al. 2019

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“…Mass density was determined from the measured volumetric heat capacity. The specific heat capacity (c p ) for the IMC films was taken as 1165 J kg −1 K −1 , a value determined for crystalγ-IMC at 300 K. [46] Although it was possible that there were spatially varying crystalline or amorphous regions on the sample (Figure 1c) we assumed that the specific heat capacity of the IMC films did not change. [47][48][49] Thus, any differences in the measured volumetric heat capacity were attributed to variations in mass density.…”

Section: Thermal Characterization and Mass Density Extractionmentioning

confidence: 99%

Non‐Contact Mass Density and Thermal Conductivity Measurements of Organic Thin Films Using Frequency–Domain Thermoreflectance

Perez

Knepper

Marquez

et al. 2021

Adv Materials Inter

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in thickness, [13,14] porosity, [15] polycrystallinity, [16] and growth morphology within these materials affect critical design parameters such as mass density (ρ) and thermal conductivity (κ). For example, mass density is a primary parameter in the detonation performance of explosive materials, as it is directly proportional to the resulting propagation velocity. [17,18] The thermal conductivity on the other hand, can provide key insights into the amorphous stability of pharmaceutical ingredients that ultimately determines their bioavailability. [3,19,20] For thin-film thermal barriers, both the mass density and thermal conductivity play important roles since they are often passive and subjected to transient thermal loads. [8] Considering that the condition of engineered surfaces, [12] microscopic defects, [21] novel

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“…The thermal conductivities of glass

k_{normalg}

, stainless mesh

k_{normalm}

, and solution

k_{normall}

are 1.05, 16, and 0.137 W/m K, respectively. Because thermal conductivities of small‐molecule organic solid materials are in the range of 0.1273–0.3472 W/m K, and the crystal is immersed in the solvent, the thermal conductivity of the Aliskiren hemifumarate solid crystal layer is estimated as the same as the ethyl acetate–ethanol mixture, 0.137 W/m K. As the volumetric flow rate of the cooling liquid at 24 L/min is very high relative to the solution flow rate,

T_{1 i}

and

T_{2 o}

can be assumed equal to

T_{c 1}

and

T_{c 2}

, respectively.…”

Section: Experimental System and Parametersmentioning

confidence: 99%

Mathematical modeling and design of layer crystallization in a concentric annulus with and without recirculation

Zhou

Benyahia

et al. 2013

AIChE Journal

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A solution layer crystallization process in a concentric annulus is presented that removes the need for filtration. A dynamic model for layer crystallization with and without a recirculation loop is developed in the form of coupled partial differential equations describing the effects of mass transfer, heat transfer, and crystallization kinetics. The model predicts the variation of the temperature, concentration, and dynamic crystal thickness along the pipe length, and the concentration and temperature along the pipe radius. The model predictions are shown to closely track experimental data that were not used in the model's construction, and also compared to an analytical solution that can be used for quickly obtaining rough estimates when there is no recirculation loop. The model can be used to optimize product yield and crystal layer thickness

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Thermal conductivity measurements for small molecule organic solid materials using modulated differential scanning calorimetry (MDSC) and data corrections for sample porosity

Cited by 13 publications

References 24 publications

Application of Differential Scanning Calorimetry (DSC) and Modulated Differential Scanning Calorimetry (MDSC) in Food and Drug Industries

Application of Differential Scanning Calorimetry (DSC) and Modulated Differential Scanning Calorimetry (MDSC) in Food and Drug Industries

Non‐Contact Mass Density and Thermal Conductivity Measurements of Organic Thin Films Using Frequency–Domain Thermoreflectance

Mathematical modeling and design of layer crystallization in a concentric annulus with and without recirculation

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