Organic Process Research & Development · 2019 · 42 citations · 10 references
Natural SciencesChemistryMaterials ScienceAnalytical ChemistryMaterials CharacterizationThermal AnalysisCalorimetryChemical Hazard AssessmentDifferential Scanning CalorimetryMaterial SafetyOxidation AnalysisSafety EvaluationContainersDevice CalibrationDifferential CalorimetryExperimental Thermal AnalysisStandard Operating Procedure DevelopmentThermal Hazard EvaluationThermal StabilityThermal Test Methodology
Differential scanning calorimetry (DSC) is a common industry tool used in the assessment of thermal stability of materials. Despite widespread use of DSC for thermal stability hazard evaluation, mistakes in testing methodology or interpretations of data are common. To avoid these issues, a standard operating procedure and list of common practices utilized within our Corteva Agriscience Reactive Chemicals (RC) group is presented in this manuscript. Emphasis within our RC program is placed on device calibration and maintenance, selection of the appropriate sample container, and a unique sample preparation methodology. The use of glass capillary and glass ampoule sample containers for DSC testing is outlined, along with the unique flame-sealing procedure utilized to protect the sample. The results of the glass sample containers using di-tert-butyl-peroxide in toluene compared to gold pan are presented showing the effects that sample containers can have on results. Additionally, glass ampoule sample containers, containing ethylene glycol, are used in DSC testing to show their effectiveness for examining a sample’s oxidative nature. A discussion of the issues and shortcomings of the commonly used aluminum pans, for use with organic samples particularly, is also presented. All this DSC testing information provides insight into our group’s ability to work on a diverse array of samples and generate quality data for understanding the thermal stability hazards present within our company.
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