1. X-Ray Presentation

2. 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

3. XRF Analysis 1. Elements Present: Copper, Zinc, Gold, etc.
SAMPLE
(solid, liquid, film)
Elements Present
Quantitative Analysis
Film Thickness
EDX & XRF
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

4. XRD Measures 4 Parameters
POLYCRYSTALLINE SAMPLE
Phase ID
a-Al2O3 vs. g-Al2O3
Quantitative
Structural information
Crystallite size
Lattice stress & strain
% Crystallinity
XRD
Phase ID: Three of the 5 forms or Titanium (TiO2)
Anatase
Brookite
Rutile
© 2007 SHIMADZU

5. XRD: Quantitative Analysis & Crystal Structure
65% ZnO, 35% MgO
Crystal Structures:
© 2007 SHIMADZU

6. Crystalline vs Amorphous
Solid matter is:
Amorphous (random)
Crystalline (regular pattern)
Smallest volume is a unit cell
The Crystal Lattice – La2O3 (cubic)
1 unit cell
© 2007 SHIMADZU

7. 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

8. Principal of X-Rays
X-rays are an electromagnetic wave. Also known as light or energy.
© 2007 SHIMADZU

9. 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

10. Spectra: Wavelength & Electron Volts (eV)
© 2007 SHIMADZU

11. Types of X-Rays for EDX
© 2007 SHIMADZU

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

13. EDX Schematic
© 2007 SHIMADZU

14. Components of EDX-720/800/900 Liquid N2 Dewar (720/800) Sample Chamber
Detector and MCA
X-ray tube
© 2007 SHIMADZU

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

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

17. 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

18. 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

19. Question 4: Analysis Light Elements (2nd or 3rd 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

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

21. 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

22. 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

23. Select The EDX Model
© 2007 SHIMADZU

24. 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

25. No Destructive Acceptance Test
© 2007 SHIMADZU

26. EDX-GP Schematic
© 2007 SHIMADZU

27. EDX-GP Includes Special RoHS Software
© 2007 SHIMADZU

28. Select the Proper uEDX Feature uEDX-1200 uEDX-1300 uEDX-1400
Element Range
13Al-92U
11Na-92U
Detector
Si(Li)
Si-Drift
Detector Window
Beryllium
Polycarbonate
Detector Cooling
Liquid N2
Peltier
Add about 500 on to EDX to get uEDX version - EDX-800 - uEDX-1300
© 2007 SHIMADZU

29. 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
© 2007 SHIMADZU

30. 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

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

32. Electrical & Electronic Components Chemical Industry
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
© 2007 SHIMADZU

33. Agriculture & Food Products Iron, Steel, & Nonferrous Metals
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

34. Electronic Material& Components Chemical Engineering & Chemicals
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

35. XRD-6000 and XRD-7000
© 2007 SHIMADZU

36. Principals of XRD
Bragg’s law is a simplistic model to understand what conditions are required for diffraction. 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

37. Example of XRD-6000 Design: Theta/2 Theta
Think of a goniometer as the equivalent of a monochromator for UV-Vis
Sample and Detector move in 1:2 ratio with respect to distance
© 2007 SHIMADZU

38. Example of XRD-7000 Design: Theta/Theta
X-Ray Source and Detector move in 1:1 ratio with respect to distance
© 2007 SHIMADZU

39. XRD-6000 & XRD-7000 Specs XRD-6000 185 mm sample to detector
±0.001º degrees resolution
XRD-7000
mm sample to detector
±0.0002º degrees resolution
Sales
20:1 – 6K vs 7K
185 mm sample to detector distance
Also, sample can fall off sample stage as XRD-6000 rotates if not packed tight.
© 2007 SHIMADZU

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

41. XRD Most Commonly Used in w/RED DOT
Many, many option but only going to cover the 7 most sold items
© 2007 SHIMADZU

42. 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)
Tubes are $6-$10K so no exchanges after the order
© 2007 SHIMADZU

43. 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

44. 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

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

46. Quantitative Analysis: Environmental Analysis
RS-2001
Environmental Stage
Filter Holder
Software
Asbestos Analysis
Similar to Rotation Stage
© 2007 SHIMADZU

47. Automatic Analysis ASC-1001 Auto 5 Position Sample Changer
Sample Rotation like RS-1001
Optional Environmental Stage Holders like RS-2001
© 2007 SHIMADZU

48. Thin Film Analysis THA-1101 Thin Film Sample Stage Monochromator
Suction Pump to hold samples in place
© 2007 SHIMADZU

49. 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

50. Sample Holders (Optional)
Standard with XRD – Use if need extras
No Metal Interference
No Metal Interference, Limit Sample
No Interferences
© 2007 SHIMADZU