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.
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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
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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.
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 | ||
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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 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.
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| 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 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 - XRF Suppression (for iron-containing materials including pharmaceuticals) - Click here for our App Note |
We have 4 Powder X-ray Diffractometers -
See below for More info and FAQS
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| 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.
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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)
Speak to one of our Subject Matter Experts about Powder X-Ray Diffraction:
Micro crystal Electron Diffraction Analysis (MicroED)-
Routinely solve high-resolution crystal structures without the need to grow large single crystals..
| Application AND Technique Description | ||
|---|---|---|
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Micro crystalline Electron Diffraction (MicroED) can extract structural information from crystals
that are orders of magnitude smaller than the size required for X-ray diffraction. This technique
is designed to overcome single crystal growth challenges or the inability to grow crystals of
suitable diffraction size. MicroED has the ability to diffract and extract high-resolution
structural information from samples that resist forming large crystals while using significantly
less material. Micro ED can utilize crystallite sizes in the range of 10-1000nm (for comparison
Single Crystal XRD requires 1-100um). With minimal sample preparation and reduced radiation
damage, Triclinic's MicroED approach is not only efficient but also gentle on your samples.
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| Lab Instrumentation | Model | Notes: |
| ELDICO | ED-1 |
Ideal for: Structure determination and absolute configuration.
• Routinely solve high-resolution crystal structures without the need to grow large single crystals.
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Speak to one of our Subject Matter Experts about MicroED:
Single Crystal X-Ray Diffraction (SCXRD) -
Absolute Structure Elucidation
| Application AND Technique Description | ||
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SCXRD is a method of determining the arrangement of atoms within a crystal. The mean positions of the atoms in the crystal can be determined, as well as their chemical bonds, their disorder, and various other information using additional software analysis. A single crystal of the material is required. We provide services for growth of diffraction quality single crystals (if necessary and you don't already have one), structure elucidation, and unit cell determination, and electronic searching. |
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| Lab Instrumentation | Model | Notes: |
| Bruker | AXS D8 Quest |
Structure determination, absolute configuration |
Synchrotron X-Ray Source
High Energy Structure Elucidation and Enhanced Sensitivity
| Application AND Technique Description | ||
|---|---|---|
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Triclinic Labs is an approved U.S. Department of Energy user at the Advanced Photon Source (APS)
located at Argonne National Laboratory in Chicago, IL. Accessing the X-ray sources/beamlines at
the APS allows us to determine crystalline phases and probe materials by generating a higher
resolution data set than we can get using our in-house powder diffractometers.
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| Lab Instrumentation | Model | Notes: |
| Advanced Photon Source, Argonne National Labs | Beamline 11-BM and Beamline 6-ID-D |
Confidentiality agreements are in place to assure ownership of data by the study sponsor.
Please contact us to discuss sample costs and submission |
SAXS (Small Angle X-Ray Scattering) -
Determine Nanoscale or Microscale Structure
| Application AND Technique Description | ||
|---|---|---|
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Small angle X-ray scattering (SAXS) is a nondestructive measurement and is a very versatile technique
able to measure various samples such as powders, solutions, thin films, and coatings. SAXS is
preferable to other methods because it is nondestructive and rapid measurements can be performed on a
variety of sample materials including bulk samples, powders and solutions.
Triclinic offers the new SAXS services utilizing its Rigaku SmartLab X-ray Diffractometer and SAXS (NanoSolver) analysis software. Of particular use are SAXS applications for nanoparticle analysis. Nanoparticles are widely utilized in a large number of applications, including light emitting devices, catalysts, fuel cells, covering materials, adhesion bonds, abrasives, inks and dyes, drug substances in drug delivery system (DDS), and real-time PCR kits. SAXS techniques can be used to determine size distributions of various nanoparticles in bulk, powders, and liquids. SAXS can be readily applied to particles in the range from 1 to 100 nm, although measurements outside this range are also possible. Particles from 1 to 10 nm can be analyzed with higher accuracy compared to other techniques (e.g. particle size analysis (PSA) and transmission electron microscopy (TEM)). The method is accurate, non-destructive and usually requires only a minimum of sample preparation. Applications are very broad and include colloids of all types, metals, cement, oil, polymers, plastics, proteins, foods, and pharmaceuticals. |
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| Lab Instrumentation | Model | Notes: |
| Rigaku | Nonius |
Wiki Reference for SAXS
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Elemental analysis -
Detection, identification, and quantification:
Elemental analysis and testing includes identification and quantification of elements, elemental compounds and molecular species. Sample types and matrices tested for trace elements include organic and non-organic, aqueous and non-aqueous materials. Elemental trace and ultra-trace analysis detection ranges from parts per million (ppm), to parts per billion (ppb) and parts per trillion (ppt) levels, using proven techniques.| Application AND Technique Description | ||
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Elemental analysis is a qualitative and quantitative process for identifying the elemental composition
of materials (e.g., chemical compounds, minerals, metals, fluids). Certain elemental techniques can
even identify the isotopes of a given element.
We offer several X-ray elemental analysis techniques: Energy Dispersive X-ray - (EDX) is a rapid technique for identifying the elements from beryllium to uranium in solid materials. EDX uses an electron beam to stimulate the emission of characteristic x-rays of the elements from the sample surface. The elemental results are presented in an x-ray spectrum. EDX can be used to analyze localized areas or generate chemical maps. Both qualitative and quantitative analyses can be performed. (Triclinic Labs typically uses EDX for the identification of contaminants.) Proton Induced X-Ray Emission (PIXE) is a non-destructive technique that can identify elements from sodium to uranium in solids, liquids, and aerosol filters. It uses a proton beam to excite an electron shell change to force the emission of detectable X-rays. PIXE can be used to analyze multi-element samples because each element's X-rays are characteristic of the element and do not overlap with each other.
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| Lab Instrumentation | Model | Notes: |
| Various | Various |
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