XRay Presentation XRay Products By Shimadzu XRF XRay

X-Ray Presentation

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 u. EDX-1200/1300/1400 WDXRF: Wavelength Dispersive X-Ray Shimadzu XRF-1800 (Call Marketing) XRD: X-Ray Diffraction 2 Shimadzu XRD-6000/7000 © 2007 SHIMADZU

XRF Analysis EDX & XRF SAMPLE (solid, liquid, film) 1. Elements Present 2. Quantitative Analysis 3. Film Thickness 1. Elements Present: Copper, Zinc, Gold, etc. 2. Quantitative: Cu: 25%, Zn: 15%, Au: 60% 3. Film Thickness of Gold on a Copper base. 3 © 2007 SHIMADZU

XRD Measures 4 Parameters 1. Phase ID 1. a-Al 2 O 3 vs. g-Al 2 O 3 2. Quantitative 3. Structural information 1. Crystallite size 2. Lattice stress & strain 4. % Crystallinity XRD POLYCRYSTALLINE SAMPLE Phase ID: Three of the 5 forms or Titanium (Ti. O 2) 4 Anatase Rutile Brookite © 2007 SHIMADZU

XRD: Quantitative Analysis & Crystal Structure Quantitative Analysis: 65% Zn. O, 35% Mg. O

Crystalline vs Amorphous Solid matter is: Amorphous (random) Crystalline (regular pattern) Smallest volume is

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 noncrystalline from may be ineffective. What effective does temperature have on crystallinity? High temp breaks down crystal? Room temperature vs body temp. 7 © 2007 SHIMADZU

Excitation of Electrons: X-Ray vs UV-Vis-IR X-Ray: Excitation of Inner Shell Electrons 9 UV-Vis-IR:

Spectra: Wavelength & Electron Volts (e. V) WAVELENGTH SCALE ENERGY SCALE Estándar Estándar Absorbance Estándar Estándar 300. 0 320. 0 340. 0 360. 0 380. 0 Wavelength (nm) 10 400. 0 Raw. Data. . . Estándar 3. 100 3. 300 3. 500 3. 700 3. 900 4. 100 e. V © 2007 SHIMADZU

Types of X-Rays for EDX 11 © 2007 SHIMADZU

EDX Series EDX-GP EDX & m. EDX 12 © 2007 SHIMADZU

Components of EDX-720/800/900 Liquid N 2 Dewar (720/800) Sample Chamber Detector and MCA X-ray

Question 1 a: What Elements Need to be Measured? 15 © 2007 SHIMADZU

Question 1 b: What Level Need to be Measured? 16 © 2007 SHIMADZU

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 17 © 2007 SHIMADZU

Question 3: Autosampler Required? Requires Turret Drive Unit (212 -22685 -91) 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 nonhomogenous samples 18 © 2007 SHIMADZU

Question 4: Analysis Light Elements (2 nd or 3 rd Row in Period Table) Solids Vacuum Unit 212 -22460 -00 Increase Sensitivity of Light Elements NOT for uses with water, oils, or powders 19 Liquids & Powders Helium Purge Kit 212 -22495 -01 Increase Sensitivity of Light Elements USED with water, oils, & powders © 2007 SHIMADZU

Vacuum & He Purge for 6 C to 17 Cl 20 © 2007 SHIMADZU

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 Ro. HS Application 21 © 2007 SHIMADZU

EDX Configurator to do a Quote www. ssi. shimadzu. com 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 22 © 2007 SHIMADZU

EDX-GP for Ro. HS Similar to EDX-720 (13 Al to 92 U) Standard: CCD and Collimator No: Vacuum, Helium Purge, or Autosampler Square Sample Compartment Ro. HS (Restriction of Hazardous Substances Electronics Industry Pb, Hg, Cd, Cr, Br (more to be added in future) 24 © 2007 SHIMADZU

No Destructive Acceptance Test 25 © 2007 SHIMADZU

EDX-GP Includes Special Ro. HS Software 27 © 2007 SHIMADZU

Select the Proper u. EDX Feature u. EDX-1200 u. EDX-1300 u. EDX-1400 Element Range 13 Al-92 U 11 Na-92 U 13 Al-92 U Detector Si(Li) Si-Drift Detector Window Beryllium Polycarbonate Beryllium Detector Cooling Liquid N 2 Peltier 28 © 2007 SHIMADZU

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 29 © 2007 SHIMADZU

Detector Signal Processing Detector current pulses Counts or “cps” Pulses are segregated into channels

5 Filters as Standard No Filter 31 Al Filter © 2007 SHIMADZU

Applications of EDX 1 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 32 © 2007 SHIMADZU

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 33 © 2007 SHIMADZU

Applications of u. EX 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) 34 © 2007 SHIMADZU

XRD-6000 and XRD-7000 35 © 2007 SHIMADZU

Principals of XRD Bragg’s law is a simplistic model to understand what conditions are required for diffraction. 36 q q dhkl Wavelength from X-Ray tube type. Angle from where peaks are located. D is space which is matched to standards or databases. © 2007 SHIMADZU

Example of XRD-6000 Design: Theta/2 Theta Sample and Detector move in 1: 2 ratio

Example of XRD-7000 Design: Theta/Theta X-Ray Source and Detector move in 1: 1 ratio

XRD-6000 & XRD-7000 Specs XRD-6000 185 mm sample to detector ± 0. 001º degrees resolution XRD-7000 200 -275 mm sample to detector ± 0. 0002º degrees resolution Sales 39 185 mm sample to detec distance 20: 1 – 6 K vs 7 K © 2007 SHIMADZU

XRD-7000 Theta/Theta q/q geometry Sample fixed horizontal Adjustable radius Improved resolution 40 © 2007

XRD Most Commonly Used in w/RED DOT 41 © 2007 SHIMADZU

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) 42 © 2007 SHIMADZU

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) 43 © 2007 SHIMADZU

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 PDF 2 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) 44 © 2007 SHIMADZU

Quantitative Analysis: Rotational Stage RS-1001 Rotates Sample Minimizes Scatter Eliminates Crystalline Orientation Improves Precision No Rotation 90 Degrees Rotation 45, 90, 135 Degrees Rotation Full 360 Degrees 45 © 2007 SHIMADZU

Quantitative Analysis: Environmental Analysis RS-2001 Environmental Stage Filter Holder Software Asbestos Analysis Similar to

Automatic Analysis ASC-1001 Auto 5 Position Sample Changer Sample Rotation like RS-1001 Optional Environmental

Thin Film Analysis THA-1101 Thin Film Sample Stage Monochromator Suction Pump to hold samples

$Heating or Cooling Samples TTK-450 Heat Sample During Diffraction Observe the Crystalline Structure Heating:$