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Institut für Geo- und Umweltnaturwissenschaften

Mineralogie - Petrologie 

Albertstr. 23b   

79104 Freiburg         

Tel.: +49 (0)761 -203-6396  

Fax: +49 (0)761 -203-6407

info@minpet.uni-freiburg.de

 

 

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Electron microprobe: Cameca SX100

Albertstr. 23c (lab building), ground floor, room 01 009-01 010
Tel.: 0761 203 6392
Contact: Dr. Hiltrud Müller-Sigmund, Tel.: 0761 203 6388, E-mail: hiltrud.mueller-sigmund(at)minpet.uni-freiburg.de

We operate Cameca SX100 electron microprobe with five WD spectrometers and an ED detector. The system allows for full spatially resolved chemical microanalysis of solid materials (2-3 um resolution). Suitable for analysis are mineral grain mounts rock sections, synthetic materials including oxides, metals or medical and organic products. The accuracy allows for measurements in tenths of one percent. The element distribution patterns can be mapped, concentration profiles can be measured for a range of geological, gemological, technical, forensic or medical applications.

Detailed technical information

Cameca SX100 electron microprobe provides highly accurate, automated elemental analysis in the microresolution (um). Our instrument was installed in 1995.

Principles of microprobe analytics
• physical principle: registration of characteristic X-ray emission spectra produced by electron bombardment
• minimum spacial resolution: micrometer scale, depending on acceleration voltage and resulting penetration depth of the electron beam
• detection limits: element and matrix dependent, some tens to some hundreds ppm
• accuracy: element and matrix dependent, 1 - 3 relative percent (for Z < 11 much worse)
• reproducability: concentration and measuring time dependent: ~ 1 relative percent
• analysis time: concentration and necessary accuracy dependent: some ten to some hundred seconds per element (WDS)

Sample requirements:
• For quantitative work all samples must be flat and mounted perpendicular to the electron beam.
• Materials must be stable under electron bombardment and vacuum conditions.
• Standard geological applications require uncovered thin sections with 0.5
µm diamond powder polishing.
• Samples have to be electronically conductive or coated with some conductive material (typically carbon).
• In general samples have to be regarded as being homogeneous on the micrometer scale. Special correction procedures are needed for thin films and single particles.

Features of our SX100:
• 50 kV electron gun, W-filament 
• Spectrometers:

Five vertical wavelength-dispersive spectrometers (PC0 - PC3 = synthetic multilayers):

No. Crystals Special features
1 TAP, PCO --
2 LIF, PET "high pressure" proportional counte
3 LIF, PET "high pressure" proportional counte
4 TAP, PET, PC1, PC3 --
5 TAP, PET, LIF, PC2 extended 2theta range, allowing O Ka to be measured on the TAP xtal

 

 

 

Element range covered (theoretically, element specific inconveniences occur):

Crystal Formula 2d [Å] K shell L shell
PC3 Mo/B4C Multilayer 200 Be-B  
PC2 Ni/C Multilayer 95 B-O  
PC1 W/Si Multilayer 60 C-F  
PC0 W/Si Multilayer 45 O-F  
TAP C8H5O4Tl 27.745 F-P Mn-Nb
PET C5H12O4 8.742 Si-Mn Sr-Tb
LIF LiF 4.027 Sc-Rb Te-U

 

 

 

 

The system is integrated with a Link (Oxford) nitrogen cooled ED-system, specified resolution 138 eV, standard Be-window, element range Na-U.

• Specimen stage: The minimum step size is 0.5 µm. Accommodation of a wide range of samples sizes, including 40mm round, 48*28mm, 30*30mm, but the standard size being either 1 inch (25.4mm) round or 28 x 48 mm sized thin sections; maximum specimen size 75*50*25 mm. A maximum of 6 samples/standards of the standard size (1in) can be loaded at the same time.

• Optical microscope: reflected and transmitted light optics and polariser. The magnification is fixed to 400. An attached color CCD camera provides an image on the computer screen.

• Vacuum system: Cameca standard vacuum system. 

• Anticontamination: Equipment comprising a liquid nitrogen cold finger near the point of impact of the electron beam, and an oxygen jet to burn off carbon contamination.

• Instrument control via a Windows PC running under Windows XP, Cameca EPMA automation and analysis software "Peaksight". The instrument is fully automated for unattended overnight operation, including a Z-axis autofocus system.
• Edwards Auto 306 sputter-coater for carbon coating of non-conductive specimens to facilitate a stable electron beam.

A variety of standard materials that cover most geological and materials science applications is available. The original file format of analysis data is ASCII, which is easily converted to Excel 5. Possible image formats are "Cameca" (ASCII), Sun Raster or TIFF. Only the Cameca format contains information about analysis conditions.

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