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

6600tán28a5660

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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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