x-ray presentation. x-ray products by shimadzu xrf: x-ray fluorescence edxrf: energy dispersive xrf...
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X-Ray Presentation
X-Ray Products By Shimadzu
XRF: X-Ray FluorescenceEDXRF: 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 XRFXRF: Wavelength Dispersive X-Ray
Shimadzu XRF-1800 (Call Marketing)
XRD: X-Ray DiffractionShimadzu XRD-6000/7000
© 2007 SHIMADZU2
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.
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SAMPLE(solid, liquid, film)
1. Elements Present2. Quantitative
Analysis3. Film Thickness
EDX & XRF
XRD Measures 4 Parameters
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POLYCRYSTALLINE SAMPLE
1. Phase ID1. a-Al2O3 vs. g-Al2O3
2. Quantitative3. Structural information
1. Crystallite size2. Lattice stress &
strain4. % 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:
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Crystalline vs Amorphous
Solid matter is:Amorphous (random)
Crystalline (regular pattern)
Smallest volume is a unit cell
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1 unit cell
The Crystal Lattice – La2O3 (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.
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Principal of X-Rays
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Excitation of Electrons: X-Ray vs UV-Vis-IR
X-Ray: Excitation of
Inner Shell ElectronsUV-Vis-IR: Excitation of Outer Shell Electrons
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E1 E2
Ionization
Excitation state
Light of frequency v
Electron
Atomic nuclei
E0
Spectra: Wavelength & Electron Volts (eV)
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300.0 320.0 340.0 360.0 380.0 400.06600tán28a5660
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WAVELENGTH SCALE
Wavelength (nm)
Ab-sorbance
3.10
03.
300
3.50
03.
700
3.90
04.
100
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ENERGY SCALE
RawData ...
eV
Absorbance
Types of X-Rays for EDX
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EDX Series
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EDX & mEDX
EDX-GP
EDX Schematic
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Components of EDX-720/800/900
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X-ray tube
Sample Chamber
Liquid N2 Dewar (720/800)
Detector and MCA
Question 1a: What Elements Need to be Measured?
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Question 1b: What Level Need to be Measured?
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Question 2: Will Viewing Area of Sample Change? Picture Required?
Collimator:1, 3, 5, & 10 mm Spots Shown by Green Rings
CCD CameraSave Picture of Sample Area
Easy Position of Sample
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Question 3: Autosampler Required?
Requires Turret Drive Unit (212-22685-91)
4 Types of Turrets16 Sample Solid (32 mm)
16 Sample Liquid (32 mm)
8 Sample Solid (52 mm
8 Sample Solid w/Spinner for non-homogenous samples
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Question 4: Analysis Light Elements (2nd or 3rd Row in Period Table)
Solids
Vacuum Unit
212-22460-00
Increase Sensitivity of Light Elements
NOT for uses with water, oils, or powders
Liquids & Powders
Helium Purge Kit
212-22495-01
Increase Sensitivity of Light Elements
USED with water, oils, & powders
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Vacuum & He Purge for 6C to 17Cl
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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
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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
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Select The EDX Model
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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 SubstancesElectronics Industry
Pb, Hg, Cd, Cr, Br (more to be added in future)
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No Destructive Acceptance Test
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EDX-GP Schematic
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EDX-GP Includes Special RoHS Software
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Select the Proper uEDX
Feature uEDX-1200 uEDX-1300 uEDX-1400
Element Range 13Al-92U 11Na-92U 13Al-92U
Detector Si(Li) Si(Li) Si-Drift
Detector Window Beryllium Polycarbonate Beryllium
Detector Cooling Liquid N2 Liquid N2 Peltier
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Detector Types and Features
Si (Li)Excellent energy resolutionGood count ratesRequires liquid nitrogen (or Peltier cooling)
Si-driftGood energy resolutionExcellent count ratesNo liquid nitrogen
PIN DiodePoor energy resolutionGood count ratesNo liquid nitrogen
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Detector Signal Processing
Detector current pulses Counts or “cps”Pulses are segregated into channels according to energy via the MCA (Multi-Channel Analyser).
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No Filter Al Filter
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5 Filters as Standard
Applications of EDX 1
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Electrical & Electronic ComponentsRegulated Substances, Thin Films, Defects
Chemical IndustryOrganic & Inorganic Material, Catalyst, Paints, Pigments, Rubbers, & Plastics
Petroleum & PetrochemicalNi, V, S in Oils, Dopants & Contaminants
Building & ConstructionCeramic, Cements, Glasses, Bricks, & Clays
Applications of EDX 2
Agriculture & Food ProductsSoils, Fertilizers, Foods
Iron, Steel, & Nonferrous MetalsImpurities in Raw Material, Alloys, Solders, Precious Metal
Machinery & AutomobilesEnd of Life Vehicle (ELV)
EnvironmentalAnalysis of Soil, Effluent, Ashes, and Filters
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Applications of uEX
Electronic Material& ComponentsComposition & Thickness of films, plating
Chemical Engineering & ChemicalsCatalyst, Scale & Sediment, Cosmetic, Dyes
Oil and CoalPetroleum, Oils, Coal, Coke
Ceramics
Pharmaceutical, Food, Agriculture
Paper & Pulp (Coated Paper, Talc, Toner)© 2007 SHIMADZU34
XRD-6000 and XRD-7000
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Principals of XRD
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sin2 hkldq q d
hkld
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
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Sample and Detector move in 1:2 ratio with respect to distance
Example of XRD-7000 Design: Theta/Theta
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X-Ray Source and Detector move in 1:1 ratio with respect to distance
XRD-6000 & XRD-7000 Specs
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185 mm sample to detector distance
XRD-6000
185 mm sample to detector
±0.001º degrees resolution
XRD-7000
200-275 mm sample to detector
±0.0002º degrees resolution
Sales20:1 – 6K vs 7K
XRD-7000 Theta/Theta
/q q geometry
Sample fixed horizontal
Adjustable radius
Improved resolution
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XRD Most Commonly Used in w/RED DOT
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X-Ray Tubes
X-Ray Tube Elements: Usually CuOther: 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)
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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)
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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 SHIMADZU44
Quantitative Analysis: Rotational Stage
RS-1001
Rotates Sample
Minimizes Scatter
Eliminates Crystalline Orientation
Improves Precision
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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
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Automatic Analysis
ASC-1001
Auto 5 Position Sample Changer
Sample Rotation like RS-1001
Optional Environmental Stage Holders like RS-2001
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Thin Film Analysis
THA-1101
Thin Film Sample Stage
Monochromator
Suction Pump to hold samples in place
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Heating or Cooling Samples
TTK-450
Heat Sample During Diffraction
Observe the Crystalline Structure
Heating: +450 C
Cooling: - 180C
Air, Inert Gas, or Vacuum
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Sample Holders (Optional)
1. Standard with XRD – Use if need extras
2. No Metal Interference
3. No Metal Interference, Limit Sample
4. No Interferences
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