Solid-state materials characterization and development expertise

Comprehensive Crystallography:

Experts in organic and inorganic materials diffraction analysis, crystallography, structure determination, data interpretation, and monitoring of crystalline phases.

X-ray (PXRD, XRD, SCXRD) and micro crystal electron diffraction (MicroED) are nondestructive techniques that provide detailed information about the crystallographic structure, chemical composition, and physical properties of materials. XRD relies on the dual wave/particle nature of X-rays to obtain information about the structure of crystalline and non-crystalline materials. A primary use of the technique is the identification and characterization of compounds based on their diffraction pattern. MicroED was developed as a hybrid method that exploits the advantages of both electron microscopy and crystallography. The crystals required for MicroED can often be one-billionth the size of those needed for X-ray diffraction.

We have experience applying diffraction techniques in the following applications:

• Materials Science and Engineering: Characterizing the crystal structure, phase identification, and defect analysis of metals, ceramics, polymers, and composites.
• Semiconductor and Electronics: Studying thin films, nanostructures, and the microstructure of semiconductor materials, aiding in the development of electronic devices.
• Pharmaceuticals: Determining the molecular structure of complex organic compounds, Phase Analysis, Degree of Crystallinity, and Quantitiative and Qualitiative Method Development , Validation and Release
• Chemicals: Analyzing catalysts, nanomaterials, and other chemical substances, understanding their crystalline structure and properties.
• Nanotechnology: Structural characterization of nanoparticles, nanowires, and other nanomaterials, crucial for developing new nanotechnologies.
  
  

Trust Triclinic for your crystallography and diffraction needs:

• More than four decades of crystallization and solid-form development expertise
• In house crystallographers, systems, and latest generation software
• Access to Single Crystal, Powder, Electron Diffraction,and Synchrotron systems
• The only North American lab with ELDICO ED-1 MicroED Systems
  
  We offer both cGMP and non GMP structure analysis services as well as crystal growth and crystallographic refinement in house. Please see below for more detail about the services we offer.
  
  
  

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XRPD/PXRD - X-ray Powder Diffraction -

Identification, quantification, and characterization of solid and liquid materials and mixtures

• Crystal Structure Analysis
• Phase Identification
• Quantitative Phase Analysis
• Lattice Parameter Measurements
  
  

Application AND Technique Description
X-ray powder diffraction or powder X-ray diffraction (a.k.a. XRPD, PXRD, XRD) is most widely used for the identification of unknown crystalline materials (e.g. minerals, inorganic compounds). Determination of unknown solids is critical to studies in pharmaceuticals, geology, environmental science, material science, engineering, and polymer sciences. In addition to routine crystalline phase identification, we are able to develop specific methods for quantitative and semi-quantitative analysis depending on the system of interest. Solid state materials are often more than just a sum of individual phases, often requiring characterization of the complete sample matrix (micro-structure, texture, crystalline/non-crystalline, solid-solution) in order to isolate key material characteristics and to determine the relationship between the matrix and key material properties. Triclinic labs has developed a number of unique analytical methods for the characterization of the solid-state matrix. These techniques can be used for more complex materials and to determine the matrix variability under controlled environmental conditions. Each chemical molecule (or phase) reflects X-rays slightly differently and have different diffraction patterns. A mixture of compounds gives a pattern that is made up of the patterns of all the individual components. To identify the components present in a mixture the XRD pattern obtained is compared to a large database of patterns. Often the spectra are overlapping so experience and judgment are important. When phase identification is complete the components (phases) are classified as major, minor, or trace.
Lab Instrumentation	Model	Notes:
Rigaku	SmartLab Instruments (Quadruple redundant) 1D and 2D, Reflection and Transmission Orientation Capable Used for Powders, Tablets, Thin Films, Drug Product Mapping Transmission and Reflection Geometries Minimal Sample Req.(<5mg) Cu Source and Co Sources available. HyPix-3000 Detector is a single photon counting X-ray detector with a high count rate of greater than 10⁶ cps/pixel, a fast readout speed and essentially no noise. - Variable Temperature, Variable Humidity Stage - - Glancing Angle - Small Angle X-ray Scattering (SAXS) experimental configurations are available. See below for more info on SAXS.	We have 4 Diffractometers - 3 are cGMP and 1 (non-cGMP) offers a 2D detector for advanced materials studies including SAXS and Variable Temperature / Variable Relative Humidity (VT/VRH) PXRD See below for More info and FAQS
Anton Paar	CHCplus Cryo and Humidity Chamber with Liquid Nitrogen Cooling Often referred to as Variable Temperature - Variable Relative Humidity Powder X-ray Diffraction (VT/VRH/PXRD) . This new addition supports investigations into pharmaceuticals, fine chemicals, and clays or zeolites in humid air, inert gasses, or vacuum. Due to its versatility, the new VT/VRH/PXRD setup opens new dimensions in analysis for materials science. The VT/VRH/PXRD system at Triclinic Labs offers the following features: 2% to 95% relative humidity with variable temperature from 10 to 80 °C, -5 °C to +300 °C in air or dry nitrogen, -120 °C to +300 °C using liquid nitrogen cooling system, -180 °C to +400 °C using liquid nitrogen cooling system and vacuum, Atmospheres: vacuum (< 10-2 mbar), air, inert gasses, Reflection-geometry PXRD in 2θ range of 0°-164°, Data collection strategies include program-controlled VT/VRH points or continuous scanning modes.	This system offers a unique combination of temperature and humidity control for real time observation of structural changes in materials under non-ambient conditions using Powder X-ray diffraction. See Figure 1 below for an example.

XRPD Applications include: 

• Characterization of crystalline materials (identification, quantification, micro-structure, texture, micro-crystalline, nano-crystalline ..) EXPERTS IN SOLID MIXTURE ANALYSIS
• Characterization of non-crystalline materials (meso-phase [ i.e. liquid crystals], glassy and amorphous)
• Characterization of the solid-state matrix (micro-structure, texture, solid-solution, segregation, micro-absorption ..)
• Determination of unit cell dimensions through indexing and crystal structure determination from X-ray powder patterns
• Semi-quantitative and quantitative determination of crystalline and non-crystalline phase composition and variance under controlled environmental conditions.
• Solid Mixture Method Development for Validation and Lot Release (CoA Issuance) - Click here for more info on Method Development
• Ability to handle large (<~10cm) and small (>~0.5mm) solid samples, liquids, suspensions, powders, and thin films.

By integrating the precision of advanced equipment with the expertise of our specialized team, our XRPD services offer unparalleled advantages for pharmaceutical analysis, ensuring detailed insights and reliable data for all your analytical needs.

Figure 1. Use of Variable Temperature Variable Humidity Powder X-ray Diffraction for determination of polymorphic conversion: Theophylline was heated from 5 to 80 °C under constant relative humidities of 5%, 50%, and 75%. PXRD patterns were collected in the 2θ range of 5° to 20° every seven minutes. The animation shows a waterfall plot of the heating experiment at 5% RH. The onset temperature at which each form was first observed is indicated on the right. The experiment started with pure Theophylline. At 10 °C a set of peaks was observed to emerge at 2θ angles of 9.4°, 12.5°, 13.7°, and 15.3°. This set of peaks matches the dehydrated-hydrate form I. At 30 °C, a new set of peaks emerged that could be attributed to form III. At 50 °C, the peaks attributed to the stable anhydrous form II started to appear. Before the final temperature of 80 °C was reached, the peaks of form I had completely diminished, resulting in a mixture of forms II and III at the end of the experiment. This approach is useful for time-course studies under normal and modified conditions (e.g. stability, scale-up, formulation) to determine if polymorphic change arises. Infringement determination cases and process control experiments benefit from this approach as well.

Frequently Asked Questions about Triclinic's XRPD Services
(click here)

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