Powder X-ray Crystallography

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Presentation transcript:

Powder X-ray Crystallography

X-ray diffraction A rapid analytical technique primarily used for phase ID of a crystalline material and can provide information on unit cell dimensions The interaction of the x-ray with the sample produces a constructive interference and a diffracted ray

Characteristic States of Matter S.O.M Order (pattern repetition) Properties Notes Solid (crystalline) Long Range Anisotropic Doesn’t repeat in all directions Solid (amorphic) Short Range Isotropic Pattern repeats in all directions Liquid Gas None Diffraction = the various phenomena (bending) that are associated when the wave passes by an object that disrupts the wave Diffraction effects are MOST noticeable when the wavelength of waves is similar to the size of the diffracting objects or apertures

Principles of XRD Why crystals? Why X-rays? Challenge in focus enough x- rays into a small enough volume to “see” a single molecule Crystals have a repeating pattern on a lattice (not a single atom, but a single macromolecule) Parallel planes of atoms Spacing of atoms = 0.1 nm, x-ray wv = 0.1nm Why X-rays? To see features on the order of the distance between atoms (10-10m) X-ray wavelength = size of space between atoms X-rays are diffracted by crystals

Crystallography Divided into 7 lattice systems  all crystalline materials fit into one of these categories Determined by lengths of edges and angles Crystalline parallel rows of atoms are separated by a “unique” distance (d-spacing) Diffraction occurs when radiation enters a substance and is scattered

Bragg’s Law Angle of incident ray = angle of diffracted ray nƛ = 2dsinθ 2θ = angle between incident and reflected beams d = spacing between planes ƛ = wavelength n = order of diffraction nλ = 2d sinθ

Applications ID of unknown crystalline material Geology Environmental Science FORENSICS!!! Material science Biology Specific applications in: Characteristics of crystalline material ID of fine grained minerals (clays) Measurement of sample purity

More on xrd applications Forensic geology Environmental Science Mineral ID 1-Silicates Most common, Si-O tetrahedron group 5 configurations 2-Non-silicates CO3, SO4, S-2, O-2, OH-, Halides Wastewater precipitates Testing for: Alum, chlorides, phosphates Determine unknown substances by evaporation

How does the pxrd work? University of Washington Tutorial When X-rays hit a powdery sample during irradiation, they get diffracted by mineral crystals contained in it, and strong scattering is observed at certain incident angles to crystals, which are specific to individual minerals. Using this phenomenon, the X-ray diffractometer identifies minerals contained in samples and examines their atomic arrangements.

Safety precautions Effect of exposure Threshold Dose This machine has an x-ray; ALWAYS pay attention to SOUNDS & SMELLS *If something is funny – STOP IMMEDIATELY! GENERAL PRECAUSTIONS: Be familiar with procedure to be carried out Never expose any body part to primary x-ray beam (primary beam = 2.4 x 107 rem/hr, diffracted beam = 80rem/hr) Turn x-ray beam OFF before attempting to make any changes to experimental set up Examine system carefully for any system modifications or irregularities NEVER leave energized system unattended in an area where access is not controlled Effect of exposure Threshold Dose Erythema (skin reddening) 300-500 rem Temporary hair loss Permanent hair loss 700 rem Transepidermal injury (skin burns) 1000 rem Dermal radionecrosis (skin death 2000-3000 rem