logging in or signing up x ray diffraction hemumpharm Download Post to : URL : Related Presentations : Share Add to Flag Embed Email Send to Blogs and Networks Add to Channel Uploaded from authorPOINT lite Insert YouTube videos in PowerPont slides with aS Desktop Copy embed code: Embed: Flash iPad Copy Does not support media & animations WordPress Embed Customize Embed URL: Copy Thumbnail: Copy The presentation is successfully added In Your Favorites. Views: 1173 Category: Science & Tech.. License: All Rights Reserved Like it (0) Dislike it (0) Added: October 01, 2011 This Presentation is Public Favorites: 1 Presentation Description diffraction methods Comments Posting comment... Premium member Presentation Transcript X-RAY DIFFRACTION: X-RAY DIFFRACTION HEMANTH.GAMPALA, M.PHARM, PHARMACEUTICAL ANALYSIS . BYSlide 2: INTRODUCTION : ORIGIN OF X-RAYS INTERACTION OF X-RAYS WITH MATTER METHODS INSTRUMENTATION X-RAY DIFFRACTION METHODS APPLICATIONSSlide 3: INTRODUCTION: X-rays are a form of light. They are in fact more energetic than the visible light. X-radiation is part of the electromagnetic spectrum, just like visible light, radio waves, microwaves, etc. Here's a schematic of the whole spectrumSlide 4: As the wavelengths of light decrease, they increase in energy. X-rays have smaller wavelengths and therefore higher energy than ultraviolet waves .Slide 5: OUT LINE ORIGIN OF X-RAYS: study about atom and its shells INTERACTION OF X-RAYS WITH MATTER Absorption 2. Diffraction 3 MAIN METHODS : x-ray absorption method x-ray diffraction method x-ray fluorescence methodSlide 6: ORIGIN OF X RAYS: High velocity of electrons bombarded on metal target x rays are produced.Slide 7: INTERACTION OF X RAY WITH MATTER: In 3ways: ABSORPTION: x rays Matter Loss energy by scattering Absorption take place. Incoming X-rays Secondary emissionSlide 8: Follows beers law i = i o e- µ lp i 0 = intensity of incident x ray i = intensity after absorption l = thickness of material µ = mass absorption co-efficient p = density of absorption material.Slide 9: Mass absorption co-efficient: (µ ) is a measurement of how strongly a chemical species absorbs or scatters light at a given wavelength µ = CN/A λ C =Proportional constant N= Avogadro's number A= Atomic weight λ = wavelength of x rays.Slide 10: 2. Scattering and diffraction: concept: x ray beam substance Contain electrons Absorption Oscillation Emits EM radiations in form of waves Waves under go constructive interference Diffracted by crystal plane.Slide 11: Sets Electron cloud into oscillation Sets nucleus (with protons) into oscillation Small effect neglectedSlide 12: Oscillating of electrons with the incoming x-raysSlide 13: n λ = AP+PC AP = PC = l n λ = l + l =2l But triangle OPA, l = d sin θ n λ =2d sin θ = angle of incidence d = space between plans n = integer(1,2,3…etc) Millers: n λ =2d hki sin θ BRAGGS LAWSlide 14: METHODS: 1 . X-ray absorption method : imperfection of internal structure. A beam of x rays is passed Sample X ray photons absorbed by substance Measuring concentration of absorbing substance. Use : elemental analysis, thickness measurement.Slide 15: 2. X ray diffraction method: x rays fall on sample (crystal) Scattering of x rays. Use: crystal structure. 3.X ray fluorescence method: X ray fall on Sample Emits x ray beam.Slide 16: Wavelength: determine which element is present in sample. Intensity: determine how much is present. Use: qualitative and quantitative elemental analysis Above 3 methods are non destructive.Slide 17: INSTRUMENTATION: PRODUCTION OF X-RAYS COLLIMATOR MONOCHROMATOR filter crystal monochromator DETECTORSSlide 18: INSTRUMENTATION: Amplifier recorderSlide 19: Collimator: Close metal plates separated by small gap Use is to produce narrow beam(pencil rays) Monochromator : Absorbs the undesirable radiations and allows required wavelength to pass. Types: 1.filter: eg : zirconium 2.crystal: eg : sodium chloride , lithium fluoride. PRODUCTION OF X RAYS High velocity of electrons bombarded on metal target x rays are producedSlide 20: DETECTORS Photographic. Counter method: types Geiger- muller tube counter Proportional counter Scintillation counter Solid state semiconductor counter SemiconductorSlide 21: Geiger muller tube counter : :Slide 22: Scintillation detector :Slide 23: X-RAY DIFFRACTION METHODS: investigation of internal structures. Laue photographic Bragg X-ray spectrometer Rotating crystal Power metho dSlide 24: .Laue photographic: 2 types: Transmission method Back reflection method 1 Transmission method:: In this method the crystal is held stationary in a beam of x-rays , after passing through the crystal is diffracted and is recorded on a photographic plate.Slide 25: 2.Back reflection method : This method provides similar information as the transmission method.Slide 26: Bragg’s X-ray spectrometer Bragg’s x-ray spectrometer method: Using the Laue’s photograph, Bragg analyzed the structures of crystals of sodium chloride, KCl . Bragg devised a spectrometer to measure the intensity of x-ray beam. The spectra obtained in this way can be employed for crystallographic analyses. This is based on the Bragg’s equation: nλ =2d sin θ.Slide 28: For measurement of λ : Wave length of x rays can determine by following equation: 2dsin θ =n λ λ /d is lattice constant. Knowing d, wavelength λ can determined. Measurement of d: d = a∫ 2 /2 for simple cubic lattice. d = a/2 Fcc crystal lattice . d = a∫ 3 /2 for bcc crystal lattice . simple cubic lattice bcc crystal lattice Fcc crystal latticeSlide 29: Where (a) can calculated by m wt Х no.of atoms in unit cell 1/3 a = Avogadro no. Х density for Nacl crystal. d is calculated Belongs to fcc crystal Four atom in a unit cell Its density is 2.18g/cc Molecular wt is 58.5 Avogadro no is 6.02 Х 10 23Slide 30: 58.5 Х 4 1/3 a = = 5.63 Х 10 -8 cm 6.02 Х 10 23 x 2.18 For fcc lattice: a 5.63 Х 10 -8 d = 2 = 2 = 2.815 Х 10 -8 cm d = 2.815A 0Slide 31: d100:d110:d111= 1 : 1 : 1 for simple cubic lattice ∫ 2 ∫ 3 d100:d110:d111= 1 : 1 : 1 for fcc crystal ∫ 2 ∫ 3 d100:d110:d111= 1 : 1 : 1 for bcc crystal ∫ 2 ∫ 3 Light is passed at angles 5.9 0 ,8.4 o ,5.20 0 DETERMINATION OF CRYSTAL STRUCTURE BY BRAGGS LAW: Ratio of spacing for the planes can be obtained. Space will be different for different crystals. For NACL crystal:Slide 32: d100:d110:d111 = 1 1 1 sin5.9 sin8.4 sin5.2 = 1 1 1 0.1028 0.146 0.0906 = 1: 0.704 : 1.155 = 1 : 1 : 1 ∫ 2 ∫ 3Slide 33: Rotating crystal: 2 types 1.Complete rotation method: occurs in a series of complete revolutions 2.Oscillation method: oscillated through an angle 15 to 20 oSlide 34: Powder method:Slide 35: Different cones for different reflections Cone of diffracted raysSlide 36: Compared to other methods the sample used in this method is low quantity that is 1mg. By using this formula, the crystal nature can be studied Θ = 360 x 1 / π r Where , Θ = Angle of incidence 360 = scattering angle R = film radius. Used for: Cubic crystals Determination of complex structures of alloys and metals.Slide 37: APPLICATIONS: STRUCTURE OF CRYSTALS Non-destructive method Molecular structure and size of crystal. POLYMER CHARACTERISATION Powder method determines degree of crystalinity of the polymer. Non crystalline portion scatters the x ray beam gives continuous background. Crystaline portion causes diffraction lines that are not continuous Amorphous materials: causes scattering. Crystal materials : causes diffractionSlide 38: STATE OF ANNEAL IN METALS Well annealed metals-sharp diffraction lines If subjected to hammering or bending-diffused diffraction pattern PARTICLE SIZE DETERMINATION a)Spot counting method: particles above 5microns b)Broadening of diffraction lines particles of the range 30-1000A oSlide 39: APPLICATION TO COMPLEXES a)Determination of cis -trans isomerism b)Determination of linkage isomerism MISCELLANEOUS APPLICATIONS a)Soil classification based on crystallinity b)Analysis of industrial dusts c)Assessment of weathering and degradation of natural and synthetic minerals d)Study of corrosion products e)Examination of tooth enamel and dentine f)Effects of diseases on bone structure.Slide 40: THANK U You do not have the permission to view this presentation. In order to view it, please contact the author of the presentation.