Center for advanced solid state analysis (CPHarma)

DSC measures the temperatures and heat flows associated with transitions in materials as a function of time and temperature in a controlled environment These measurements provide quantitative and qualitative information about physical and chemical changes that involve endothermic or exothermic processes, or changes in heat capacity:

• Glass transition (Tg)
• Melting points
• Crystallization time and temperature
• Percent crystallinity
• Heats of fusion and reactions
• Specific heat capacity
• Reaction kinetics
• Purity
• Relaxation kinetics

Technical Details:

• TA instruments Discovery DSC (high-end DSC)
• Tzero™ technology
• Modulated DSC (MDSC)
• Temp. range from -180 to 725°C
• Direct measurement of heat capacity (Cp)
• Baseline repeatability: ±5µW (-50° C to

TGA measures the amount and rate of change in the weight of a material as a function of temperature or time in a controlled atmosphere. The technique characterizes the weight loss or gain due to:

• Decomposition
• Oxidation
• Dehydration
• Moisture and volatile content

Technical Details:

• TA instruments Discovery TGA (high-end TGA)
• Infrared (IR) furnace technology (up to 500° C controlled heating rate and 2000° C ballistic)
• TGA Punching (for environmental sensitive samples)

Microcalorimetry is measuring all physical and chemical processes associated with a heat flow, e.g.:

• Stability (physical, chemical)
• Compatibility
• Amorphicity
• Polymorphism
• Reaction kinetics
• Dissolution kinetics
• Microorganism detection and discrimination

Technical Details:

• TA instruments
• Thermal Activity Monitor (TAM III)
• Nanocalorimeter and multicalorimeter
• SolCal (Solution Calorimetry)
• Relative Humidity RH Perfusion Setup
• Precisely controlled temperature within 0.0001° C
• Temperature range of operation is from 15 to 150° C
• Isothermal, step-isothermal, and temperature-scanning operation.

DMA measures the sample response on mechanical deformation (sinusoidally, constant or step fashion, or under a fixed rate). The technique can characterize the response to the deformation as a function of temperature and time and give information on:

• Tg
• Secondary relaxations
• Crystallinity
• Molecular Weight/cross linking
• Phase separation (polymer blends, co-polymers)
• Aging (physical and chemical)
• Orientation
• Curing
• Effect of additives

Technical Details:

• TA instruments DMA Q800
• Temperature range: -150 to 600° C
• Frequency range: 0.01 to 200 Hz
• Force range: 0.0001 to 18 N
• Amplitude range: 0.5 to 10,000 microns
• Film & Fiber clamp
• 3-point-bending clamp
• Powder characterization kit.

TMA measures sample dimensional changes under conditions of controlled temperature, time, force and atmosphere. The technique can characterize intrinsic material properties and processing/product performance, e.g.:

• Expansion or contraction
• Coefficient of thermal expansion
• Glass transition
• Softening and melting points
• Multilayer Film Analysis
• Young's Modulus

Technical Details:

• TA instruments Q400 TMA
• Temperature range: -150 to 1000° C
• Standard expansion probe
• Penetration probe
• Macro-expansion probe
• Standard operation modes (temperature ramp, isostrain, force ramp)
• Advanced modes (stress ramp, strain ramp, isostrain)
• Dynamic TMA and modulated TMATM modes.

XRPD measures the solid form and/or the amorphous nature of the sample. This technique can also be used to verify the structural changes observed during thermal analysis. XRPD can characterize structure of matter, and specifically:

• Qualitative and quantitative analysis of polymorphic forms
• Identification of amorphous matter
• Other solid forms (salt, co-crystal, solvates)
• High-throughput (HTS) polymorph/solid form screening
• Variable-Temperature measurements

Technical Details:

• PANalytical X’Pert Pro diffractometer
• PIXcel detector CuKα radiation (λ=1.5418 Å)
• Temperature measurements with Anton Parr CHC-Plus chamber: -120°C to 300° C
• 15-sample autosampler (larger sample size)
• High-throughput screening with programmable XYZ stage for 96-well plate.

Raman spectroscopy is useful for characterizing and monitoring of solid form changes. Raman can characterize sample characteristics, especially:

• Solid form analysis (polymorphic forms, amorphous matter, salt, co-crystal, solvates)
• Non-contact measurements without sample preparation in process environment
• Support for polymorph/solid form screening
• Interfacing with dissolution testing

Technical Details:

• RamanRxn1 with CCD detector (Kaiser Optical Systems)
• 785-nm Invictus TM NIR diode laser
• In situ Raman analysis with MR probe
• PhAT probe with a spot size of 1-6 mm.

IR spectroscopy is useful for identification purposes, as well as characterizing solid form. IR can be used for:

• Identification of chemical compounds
• Identification of foreign matter and impurities Solid form analysis (polymorphic forms, amorphous matter, salt, co-crystal, solvates)
• Support for polymorph/solid form screening
• Molecular interactions, especially polymer-API interactions 

Technical Details:

• ABB MB3000 FTIR
• Spectral range 485 to 8,500 cm^-1
• Resolution better than 0.7 cm^-1
• Apodized resolution, adjustable 1 to 64 cm^-1
• Temperature controlled liquid cell (Peltier cooling and heating 5-130° C)
• ZnSe crystal-ATR.

Scanning electron microscopy (SEM) is ideal tool for visualization of a sample. SEM can be used for imaging of different solid state properties:

• Visualization of surface structure
• Providing 3D view into sample  appearance
• Particle size and shape visualization

Technical Details:

• Hitachi TM3030 Tabletop SEM
• Magnification 15 to 30,000 x
• Max. sample size 70 mm (diameter), max. sample height 50 mm
• Image output BMP, JPEG, TIFF.