Solid State Characterization of Organic Compounds

Gain a sound understanding of solid state characterization of organic molecules.

About the Course

This course is an introduction to solid state characterization of organic molecules. Techniques include x-ray powder diffraction (XRPD), thermal methods spectroscopic methods, and water uptake.

For each technique, basic theory is presented along with its application to organic molecules. Information on instrumentation, sample preparation, and data analysis is included in the modules. Use of the technique to differentiate and quantitate solid forms (polymorphs) is discussed and case studies are presented to show how the measurements were used in real life situations.

  • XRPD theory and best practices
  • Thermal analysis methods and how they are used together
  • Spectrometric methods overview and when to use them
  • Water sorption measurements and how to determine when water may be an issue
  • Case studies to show how the techniques were used to solve real world problems

What You Will Learn

  • Learn about a variety of analytical techniques and gain information that you can apply directly to your job
  • Understand how solid forms can affect your project and how to spot them early before they become a major issue
  • Help your company put the best data in your patent and regulatory documents

Who Should Attend

Anyone who works with organic molecules, such as synthesis, crystallization, characterization, analysis, use, formulation, physical and chemical stability.

Organic chemists, process chemists, materials scientists, analytical chemists, pharmaceutical scientists, formulation scientists, patent attorneys.

Managers and supervisors who need a basic understanding of solid form characterization and how it will affect their ultimate goals will also find this course useful.

Course Outline

Module 1. X-Ray Powder Diffraction (XRPD) 

  • Diffraction basics
  • Instrumentation (geometry, detectors, data collection modes)
  • Sampling issues (preferred orientation, particle size)
  • Variable temperature XRPD
  • Data Analysis
  • Quantitation
  • Case study

Module 2. Thermal Methods

  • Differential scanning calorimetry (DSC)
    • Overview
    • Calibration
    • Sample preparation
    • Measurements and data analysis (enthalpy of fusion, glass transition temperature)
  • Hot stage microscopy
    • Instrumentation
    • Use
  • Thermogravimetry (TG)
    • Instrumentation
    • Use
    • Thermogravimetry-infrared (TG-IR) measurements
  • Determination of thermodynamic stability
  • Monotropic vs enantiotropic systems
    • Energy temperature diagrams
    • Quantitation
    • Case study

Module 3. Infrared (IR) Spectroscopy

  • Theory
  • Instrumentation
  • Sampling Techniques (DRIFTS, ATR, imaging)
  • Variable temperature IR
  • Near- IR (NIR)
  • Data Analysis
  • Quantitation
  • Case Study

Module 4. Raman Spectroscopy

  • Theory
  • Instrumentation
  • Sample preparation
  • In-situ measurements (crystallization studies, RH, hot and cold stage microscopy)
  • Applications (form identification, form conversion, interactions, processing, stability, screening)
  • Imaging
  • Quantitation
  • Case Study

Module 5. NMR Spectroscopy

  • Theory
  • Solid state NMR
  • Solution NMR
  • Applications (solvent identification, interactions, salts/cocrystal identification, mixture analysis, suspensions, reactions)
  • Quantitation
  • Case Study

Module 6. Water Sorption

  • Water-solid interactions (absorption, adsorption, deliquescence)
  • Automated instrumentation
  • Data collection, analysis, and interpretation
  • Relative humidity chambers
  • Hygroscopicity flow chart, how to determine if water will be an issue, strategies to deal with problematic materials
  • Case studies included in the various sections

About the Instructor(s)


Ann Newman

Pharmaceutical Consultant, Seventh Street Development Group

Dr. Ann Newman is currently a pharmaceutical consultant at Seventh Street Development Group with more than 20 years of large pharma and contract research experience. She teaches Polymorphism in Organic/Pharmaceutical Systems.

 


Cost per Module: $199.00


 

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Module 1. X-Ray Powder Diffraction (XRPD) 

  • Diffraction basics
  • Instrumentation (geometry, detectors, data collection modes)
  • Sampling issues (preferred orientation, particle size)
  • Variable temperature XRPD
  • Data Analysis
  • Quantitation
  • Case study


Module 2. Thermal Methods

  • Differential scanning calorimetry (DSC)
    • Overview
    • Calibration
    • Sample preparation
    • Measurements and data analysis (enthalpy of fusion, glass transition temperature)
  • Hot stage microscopy
    • Instrumentation
    • Use
  • Thermogravimetry (TG)
    • Instrumentation
    • Use
    • Thermogravimetry-infrared (TG-IR) measurements
  • Determination of thermodynamic stability
  • Monotropic vs enantiotropic systems
    • Energy temperature diagrams
    • Quantitation
    • Case study


Module 3. Infrared (IR) Spectroscopy

  • Theory
  • Instrumentation
  • Sampling Techniques (DRIFTS, ATR, imaging)
  • Variable temperature IR
  • Near- IR (NIR)
  • Data Analysis
  • Quantitation
  • Case Study


Module 4. Raman Spectroscopy

  • Theory
  • Instrumentation
  • Sample preparation
  • In-situ measurements (crystallization studies, RH, hot and cold stage microscopy)
  • Applications (form identification, form conversion, interactions, processing, stability, screening)
  • Imaging
  • Quantitation
  • Case Study


Module 5. NMR Spectroscopy

  • Theory
  • Solid state NMR
  • Solution NMR
  • Applications (solvent identification, interactions, salts/cocrystal identification, mixture analysis, suspensions, reactions)
  • Quantitation
  • Case Study


Module 6. Water Sorption

  • Water-solid interactions (absorption, adsorption, deliquescence)
  • Automated instrumentation
  • Data collection, analysis, and interpretation
  • Relative humidity chambers
  • Hygroscopicity flow chart, how to determine if water will be an issue, strategies to deal with problematic materials
  • Case studies included in the various sections