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Obnovit | RAW
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Obnovit | RAW

Laboratory of X-ray Diffractometry and Spectrometry

Performed in lab

  • XRF elemental analysis of compacts(including layers), powder and liquid samples
  • XRD phase analysis ov compacts(including layers), powder and liquid samples
  • Element distribution (maps) from circle with Ø (20mm) even for NO-CONDUCTIVITY SAMPLES
  • Determination of thickness, elemental and phase composition of layers and multilayers
  • Determination of amorphous content in sample by XRD
  • Determination of average crystallite size in range 1-500nm by XRD
  • Phase transformation by XRD – range 278K - 1693K
  • Cell parameters and stechiometrie by XRD
  • Micro and macro strain by XRD
  • Crystals orientation by XRD
  • Determination of 3D molecular and crystal structure of small moleculs from single crystals
  • Structure or quantitative analysis by Rietveld method
  • Non-destructive determination of minerals even in jewels

Performed outside of lab

  • XRF elemental analysis of compact, powder and liquid samples
  • Determination of thickness, elemental composition of layers and multilayers

Instruments for XRF (elemental, chemical) analysis:

The measurement can be done with WD spectrometr or ED spectrometer. WD spectrometer have better resolution, lower detection limits, but restrictions on sample size.

In the case of WD spectrometers, sample must fit in cylindrical cassette – inner diameter 52mm, height 25mm (resp. up to 40mm). Circle in the CENTRE OF THE SAMPLE is analysed. The diameter of measuring circle could be changed.

IF THE SAMPLE CANNOT  FIT IN CASETTE, it is possible to use portable ED spectrometer Niton XL5, only elements Mg-U and size of sample IS NOT IMPORTANT!!!,

WD XRF spectrometers: ARL 9400, Axios, PERFORM‘X

Elements F-U. Standart measurement for concentration in range 0.005%(50ppm)-100%.

ARL9400 – calibration for mask with diameter 29mm ( 9mm and 15mm without calibration).

Axios  – calibration for mask with diameter 6mm, 10mm, 20mm, 25mm, 38mm.

Performix- calibration for mask with diameter 15mm, 29mm (1.5 a 3mm without  calibration)

 

Standardless software – Uniquant 4(ARL9400- intensity measurement for 110 channels-83 elements F-U), Omnian (Axios - 11 scans-84 elementsO-U), Integrated Uniquant UQi (PERFORM‘X – intensity mesurement for 122 channels - 83 prvků F-U),

Price for standard analysis (sample preparation, data collection and evaluation) is 1000 Kč + DPH. 10 samples and more, discount 10%, discount 10% for universities and academic institutions.

Low concentrations in range 1ppm-100ppm is better consult before measurement.

Be-O determination in concentration from 2% possible, is better consult before measurement.

Determination of thickness of multilayers from 10 nm up to 100mikrometrs by XRF.

 

ED XRF spektrometr: Niton XL5

Niton XL5 – calibration for circle, diameter 8mm and 3mm for General Metals(GM), 8mm for Mining(M)), Plastics, Soil, Coating – measurement of thickness up to 4 layers (layers must include different elements)

 

Range Mg-U. Worse resolution than WD spectrometrs, possible overlap of elements (meziprvkové ovlivnění koncentrace, minoritní prvek je překryt majoritními prvky a nejen s protonovým číslem Z+-1. Standard measurement for concentrations range 0.01%-100%. Sitable for compacts, which do not fit in cassette for WD spectrometer or the measured area is small (circle diameter 8mm,  or smaller 3mm) or measured area  is in centre of sample Suitable for  screening liquids, pH 1-14!!!

Price for standard analysis (sample preparation, data collection and evaluation) is 400 Kč + DPH. 10 samples and more, discount 10%, discount 10% for universities and academic institutions.

Instruments for XRD (phase, powder, mineralogical) analysis:

Vertical diffractometrs:                                                                 

X´pert Pro (2002) – Co tube, rotational transmission/reflextion stage, sample changer for 15 samples

X'Pert3 Powder  (2015) – Cu tube, rotational transmission/reflextion stage, sample changer for 15 samples eliptical focus mirror, capillary spiner, colimator for thin layers 

Bruker - D8 Advance (2001) – Co tube ( Cu or Mo tube), sample changer  for 7 samples          

Evaluation software – Panalytical HighScore Plus 4.0

Powder samples and compact samples of different size ( preferably suitable for standard holders) can be analysed by XRD. Size of analysed place 0.1x0.1mm2 až 15x20mm2. Minimum quantity of powder sample is 1mg, standard quantity is 200mg.

Price for for standard qualitative analysis (sample preparation-100Kč, data collection-500Kč and evaluation 400Kč) is 1000 Kč + DPH. 10 samples and more, discount 10%, discount 10% for universities and academic institutions.

Instrument for microXRD analysis:

microXRD – microdiffraction system D8 Discover with 2D detector Vantec 500, laser focusing and camera – spot measurement diameter 0.1-2mm.

Price for measurement 1 spot and standard qualitative phase analysis ( data collection-500Kč and evaluation 500Kč) is 1000 Kč+DPH. 10 samples and more, discount 10%, discount 10% for universities and academic institutions.

Instrument for microXRF analysis and elemental distribution(maps):

microXRF–spot analysis with spectrometr PERFORM’X, spot diameter 1.5mm, camera system, element distribution within the circle diameter 20mm -MAPS.

Instrument for  powder structure (3D- atomic positions) analysis:

Vertical difractometr:          

X'Pert3 Powder ( 2015) – Cu tube, eliptical focus mirror, capillary spiner 

Evaluation software – Fox, Dash, Mercury 3.0, Discovery Studio 4.0

Instrument for single crystal structure analysis:

4-cicle difractometr: XcaliburTMPX – (2004), single crystals size 0. 1 – 1mm

Evaluation software – Jana 2006, Sir 2004,Ortep, Mercury 3.0, Diamond, Platon,

 

Databases, regularly yearly update:

Database CSD – structures of  organic substances

Databáze PDF-4+ – database d, I values of reference measured and calculated inorganic substances ( x,y,z atomic coordinates)  

Databáze PDF-4/Organics – databasee d, I values of reference organic substances calculated from CSD  (NO x,y,z ATOMIC COORDINATES)

Updated: 19.7.2018 11:07, Author: Jan Prchal


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Copyright: UCT Prague 2015
Information provided by the Department of International Relations and the Department of R&D. Technical support by the Computing Centre.
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