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X-Ray Products By Shimadzu XRF: X-Ray Fluorescence EDXRF: Energy Dispersive XRF EDX: Energy Dispersive X-Ray XRF: Interchangeable with EDX Shimadzu EDX-720/800/900/GP Shimadzu uEDX-1200/1300/1400 WDXRF: Wavelength Dispersive XRF XRF: Wavelength Dispersive X-Ray Shimadzu XRF-1800 (Call Marketing) XRD: X-Ray Diffraction Shimadzu XRD-6000/7000 © 2007 SHIMADZU 2
XRF Analysis 1. Elements Present: Copper, Zinc, Gold, etc. 2. Quantitative: Cu: 25%, Zn: 15%, Au: 60% 3. Film Thickness of Gold on a Copper base. © 2007 SHIMADZU 3 SAMPLE (solid, liquid, film) 1.Elements Present 2.Quantitative Analysis 3.Film Thickness EDX & XRF
XRD Measures 4 Parameters © 2007 SHIMADZU 4 POLYCRYSTALLINE SAMPLE 1.Phase ID -Al 2 O 3 vs. -Al 2 O 3 2.Quantitative 3.Structural information 1.Crystallite size 2.Lattice stress & strain 4.% Crystallinity XRD Anatase Rutile Brookite Phase ID: Three of the 5 forms or Titanium (TiO2)
XRD: Quantitative Analysis & Crystal Structure Quantitative Analysis: 65% ZnO, 35% MgO Crystal Structures: © 2007 SHIMADZU 5
Crystalline vs Amorphous Solid matter is: Amorphous (random) Crystalline (regular pattern) Smallest volume is a unit cell © 2007 SHIMADZU 6 1 unit cell The Crystal Lattice – La 2 O 3 (cubic)
Percent Crystallinity of Sample Crystalline and non-crystalline (amorphous) samples scatter x-rays differently so the percent of each can be measured. Drugs in the crystalline from may be effective for the problem, but in the non- crystalline from may be ineffective. What effective does temperature have on crystallinity? High temp breaks down crystal? Room temperature vs body temp. © 2007 SHIMADZU 7
Principal of X-Rays © 2007 SHIMADZU 8
Excitation of Electrons: X-Ray vs UV-Vis-IR X-Ray: Excitation of Inner Shell Electrons UV-Vis-IR: Excitation of Outer Shell Electrons © 2007 SHIMADZU 9
Spectra: Wavelength & Electron Volts (eV) © 2007 SHIMADZU 10
Types of X-Rays for EDX © 2007 SHIMADZU 11
EDX Series © 2007 SHIMADZU 12 EDX & EDX EDX-GP
EDX Schematic © 2007 SHIMADZU 13
Components of EDX-720/800/900 © 2007 SHIMADZU 14 X-ray tube Sample Chamber Liquid N 2 Dewar (720/800) Detector and MCA
Question 1a: What Elements Need to be Measured? © 2007 SHIMADZU 15
Question 1b: What Level Need to be Measured? © 2007 SHIMADZU 16
Question 2: Will Viewing Area of Sample Change? Picture Required? Collimator: 1, 3, 5, & 10 mm Spots Shown by Green Rings CCD Camera Save Picture of Sample Area Easy Position of Sample © 2007 SHIMADZU 17
Question 3: Autosampler Required? Requires Turret Drive Unit ( ) 4 Types of Turrets 16 Sample Solid (32 mm) 16 Sample Liquid (32 mm) 8 Sample Solid (52 mm 8 Sample Solid w/Spinner for non- homogenous samples © 2007 SHIMADZU 18
Question 4: Analysis Light Elements (2 nd or 3 rd Row in Period Table) Solids Vacuum Unit Increase Sensitivity of Light Elements NOT for uses with water, oils, or powders Liquids & Powders Helium Purge Kit Increase Sensitivity of Light Elements USED with water, oils, & powders © 2007 SHIMADZU 19
Vacuum & He Purge for 6C to 17Cl © 2007 SHIMADZU 20
Questions 5-7: Other Accessories 5) Does customer need Precision stage? X-Y stage for fine positioning of sample Requires CCD Camera & Collimator 6) Liquid Nitrogen Start Up Required? Gloves, Dewar, & Transfer Tube 7) Standards Required? Mostly for RoHS Application © 2007 SHIMADZU 21
EDX Configurator to do a Quote and select “Product Gateway”, then “X-ray Instruments” and click on the “EDX Configurator” All part numbers for main body and accessories will be provided © 2007 SHIMADZU 22
Select The EDX Model © 2007 SHIMADZU 23
EDX-GP for RoHS Similar to EDX-720 (13Al to 92U) Standard: CCD and Collimator No: Vacuum, Helium Purge, or Autosampler Square Sample Compartment RoHS (Restriction of Hazardous Substances Electronics Industry Pb, Hg, Cd, Cr, Br (more to be added in future) © 2007 SHIMADZU 24
No Destructive Acceptance Test © 2007 SHIMADZU 25
EDX-GP Schematic © 2007 SHIMADZU 26
EDX-GP Includes Special RoHS Software © 2007 SHIMADZU 27
Select the Proper uEDX FeatureuEDX-1200uEDX-1300uEDX-1400 Element Range 13 Al- 92 U 11 Na- 92 U 13 Al- 92 U DetectorSi(Li) Si-Drift Detector WindowBerylliumPolycarbonateBeryllium Detector CoolingLiquid N 2 Peltier © 2007 SHIMADZU 28
Detector Types and Features Si (Li) Excellent energy resolution Good count rates Requires liquid nitrogen (or Peltier cooling) Si-drift Good energy resolution Excellent count rates No liquid nitrogen PIN Diode Poor energy resolution Good count rates No liquid nitrogen © 2007 SHIMADZU 29
Detector Signal Processing Detector current pulses Counts or “cps” Pulses are segregated into channels according to energy via the MCA (Multi- Channel Analyser). © 2007 SHIMADZU 30
No FilterAl Filter © 2007 SHIMADZU 31 5 Filters as Standard
Applications of EDX 1 © 2007 SHIMADZU 32 Electrical & Electronic Components Regulated Substances, Thin Films, Defects Chemical Industry Organic & Inorganic Material, Catalyst, Paints, Pigments, Rubbers, & Plastics Petroleum & Petrochemical Ni, V, S in Oils, Dopants & Contaminants Building & Construction Ceramic, Cements, Glasses, Bricks, & Clays
Applications of EDX 2 Agriculture & Food Products Soils, Fertilizers, Foods Iron, Steel, & Nonferrous Metals Impurities in Raw Material, Alloys, Solders, Precious Metal Machinery & Automobiles End of Life Vehicle (ELV) Environmental Analysis of Soil, Effluent, Ashes, and Filters © 2007 SHIMADZU 33
Applications of uEX Electronic Material& Components Composition & Thickness of films, plating Chemical Engineering & Chemicals Catalyst, Scale & Sediment, Cosmetic, Dyes Oil and Coal Petroleum, Oils, Coal, Coke Ceramics Pharmaceutical, Food, Agriculture Paper & Pulp (Coated Paper, Talc, Toner) © 2007 SHIMADZU 34
XRD-6000 and XRD-7000 © 2007 SHIMADZU 35
Principals of XRD © 2007 SHIMADZU 36 d hkl Bragg’s law is a simplistic model to understand what conditions are required for diffraction. Wavelength from X-Ray tube type. Angle from where peaks are located. D is space which is matched to standards or databases.
Example of XRD-6000 Design: Theta/2 Theta © 2007 SHIMADZU 37 Sample and Detector move in 1:2 ratio with respect to distance
Example of XRD-7000 Design: Theta/Theta © 2007 SHIMADZU 38 X-Ray Source and Detector move in 1:1 ratio with respect to distance
XRD-6000 & XRD-7000 Specs © 2007 SHIMADZU mm sample to detector distance XRD mm sample to detector ±0.001º degrees resolution XRD mm sample to detector ±0.0002º degrees resolution Sales 20:1 – 6K vs 7K
XRD-7000 Theta/Theta geometry Sample fixed horizontal Adjustable radius Improved resolution © 2007 SHIMADZU 40
XRD Most Commonly Used in w/RED DOT © 2007 SHIMADZU 41
X-Ray Tubes X-Ray Tube Elements: Usually Cu Other: Co, Fe, Cr, Mo, W (Substitutes Before PO) X-Ray Tube Spot Size (Substitutes Before PO) Normal Focus (NF) Long Fine Focus (LFF) Fine Focus (FF) Broad Focus (BF) © 2007 SHIMADZU 42
Qualitative Analysis: Counter Monochromator Allows only K(alpha) Rays to Detector Eliminates K(beta) and Continuous X-Rays Increase S/N ratio Sold with almost every XRD Counter Monochromator must match X-ray tube (Cu, Co, Fe, Cr) © 2007 SHIMADZU 43
Qualitative Analysis: Software Shimadzu’s Auto Search (Standard) Very Limited Database ICDD’s PDF Series (Most Popular) PDF 2: Size 219,000 records PDF 4/Organics: 371,000 PDF2 Search Software used w/PDF 2 & 4 MDI’s JADE (Not Recommend) Pattern Processing, ID, & Quantification Can Access PDF files, Training is in CA, USA only (customer pays) © 2007 SHIMADZU 44
Quantitative Analysis: Rotational Stage RS-1001 Rotates Sample Minimizes Scatter Eliminates Crystalline Orientation Improves Precision © 2007 SHIMADZU 45 No Rotation Rotation 90 Degrees Rotation 45, 90, 135 Degrees Rotation Full 360 Degrees
Quantitative Analysis: Environmental Analysis RS-2001 Environmental Stage Filter Holder Software Asbestos Analysis Similar to Rotation Stage © 2007 SHIMADZU 46
Automatic Analysis ASC-1001 Auto 5 Position Sample Changer Sample Rotation like RS-1001 Optional Environmental Stage Holders like RS © 2007 SHIMADZU 47
Thin Film Analysis THA-1101 Thin Film Sample Stage Monochromator Suction Pump to hold samples in place © 2007 SHIMADZU 48
Heating or Cooling Samples TTK-450 Heat Sample During Diffraction Observe the Crystalline Structure Heating: +450 C Cooling: - 180C Air, Inert Gas, or Vacuum © 2007 SHIMADZU 49
Sample Holders (Optional) 1.Standard with XRD – Use if need extras 2.No Metal Interference 3.No Metal Interference, Limit Sample 4.No Interferences © 2007 SHIMADZU 50
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