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Determination of solidus and liquidus temperatures by means of a Perkin-Elmer 1B differential scanning calorimeter

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Abstract

A Perkin-Elmer 1B DSC apparatus was used to test the O'Neill expression for the melting interval of pure compounds on samples of organic compounds 1–10 mg in weight. On the basis of O'Neill's model, an expression for the melting interval of solid solutions,ΔT, has been derived. The difference betweenΔT andT 1 − T s (T 1 andT s = =liquidus and solidus temperatures) is discussed. A simple procedure for the determination of solidus and liquidus temperatures from DSC data is proposed.

Zusammenfassung

Ein Perkin-Elmer DSC-Gerät 1B wurde zur Prüfung des O'Neillschen Ausdruckes für den Schmelzbereich reiner Verbindungen an Proben organischer Verbindungen von 1–10 mg eingesetzt. Auf Grund des O'Neill-schen Modells wurde ein Ausdruck für den Schmelzbereich fester Lösungen,ΔT, abgeleitet. Der Unterschied zwischenΔT undT 1 − T s (T 1,T s =Flüssig- und Fest-Temperaturen) wird erörtert. Eine einfache Methode zur Bestimmung von Fest- und Flüssigphasentemperaturen aus DSC-Daten wird vorgeschlagen.

Резюме

Дифференциальный ск анирующий калоримет р типа 1В фирмы Перкин—Э льмер был использован для п роверки выражения О'Н ейлля, установленного для и нтервала плавления чистых сое динений на примере ор ганических веществ взятых по вес у 1–10 мг. На основании модели О'Не йлля было выведено ΔТ для интервала плавления твердых растворов. Обсуждено различие м ежду ΔТ иT π-T с, гдеT π и Тc — температуры ликв идуса и солидуса. Предложен п ростой метод определ ения температур ликвидус а и солидуса из данных ДСК.

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Abbreviations

T :

temperature of solidus-liquidus interface, K

T s,T 1 :

solidus and liquidus temperature, respectively, K

T i,T f :

initial and final transition temperature, respectively, in a DSC curve, K

T 0 :

temperature of sample container bottom, K

T p :

temperature of thermal energy source, K

ΔT :

temperature interval of non-isothermal or “complex” transition in a DSC curve, K

ΔT iso :

temperature interval of isothermal transition in a DSC curve (temperature resolution of “sharp” transition), K

\(\dot T_p \) :

scanning rate, K. min−1

ΔH :

transition energy, J

W :

heat flow rate, J min−1

R 0 :

thermal resistance between sample and sample holder, K min J−1

r :

sample thermal resistivity, K. cm.min.J−1

η :

specific transition energy, J. g−1

ρ :

sample density, g.cm−3

m :

sample weight, g

A :

area of contact between sample and sample pan, cm2

x :

thickness of liquid layer, cm

t :

time, min

Δt :

time interval of transition (peak width), min

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Authors and Affiliations

  1. Institute of Organic and Physical Chemistry, Technical University, 50 370, Wrocław, Poland

    R. Radomski & M. Radomska

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  1. R. Radomski
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  2. M. Radomska
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Radomski, R., Radomska, M. Determination of solidus and liquidus temperatures by means of a Perkin-Elmer 1B differential scanning calorimeter. Journal of Thermal Analysis 24, 101–109 (1982). https://doi.org/10.1007/BF01914805

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  • DOI: https://doi.org/10.1007/BF01914805

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