Powder diffraction of a sample (P-XRD) allows the identification of crystalline phases by observing the diffraction conditions of the crystal structure at a specific x-ray wavelenght (CuKalpha) at a certain angle of irradiation. The sample is crushed and powdered to obtain diffraction condition for all crystallite orientations at different 2Theta angles. Apart from qualitatitive phase ID, we offer Rietveld refinement for the determination of the phase volume or refinement of a crystal structure. The minimum amount is around a few mg. With the standard configuration the FWHM is ~0.15° 2Theta.The Bragg-Brentano setup is illustrated here (in german): 

 xrd sketch         

       image source: Common point detector setup. modified figure

URL http://www.d2phaser.com/images/d2-phaser/images/Bilder_1-1/Bilder_1-1-1.jpg       


Our Service: 

  • qualitative phase analysis via x-ray diffraction of small amounts of material (mg-regime, comparable to very few grains of salt)
  • data evaluation via Match! Software (Crystal Impact) and ICDD® PDF 4 Minerals 2021 and  COD database.
  • each measurement includes a diffraction pattern (intensity vs. 2Theta), a table with d-values and a phase identification (if possible)
  • determination of phase volumes, atomic substition, lattice parameters via Rietveld refinement (FullProf)
  • for a reliable phase identification the knowledge of the chemical composition is sometimes needed (EDS analysis). E.g. vivianite group minerals with (M3(XO4)2 · 8H2O, where X = As, P M = Mg, Mn, Fe, Co, Ni, Cu, Zn) 
  • processing time around 1 month

picro

   Fit of sample (red) and reference picropharmacolite (green bars and blue lines)

Download: example 


How To: 

After a successfull checkout through our online shop system, you will receive an invoice with our address. Please send the samples to this address. An alternative to our ordering system is to send the samples to our address which allows to find the best working analysis method for your request.

We offer two options for the shipment of the samples:

1st option: You can order your shipment material here and isolate the material with a needle at home in a capsula. 

2nd option: It is also possible to send your sample without any preparation but with a marker indicating the material to isolate and a short note what and how we shall analyse the isolate. Previous results eg. SEM-EDS results should be sent too as they can help while the identification process.

Please choose a shipment method while checking out if you want to get a return of your samples (+5.00€ for small samples).


lab equipment: 

Analysis will be carried out on a Rigaku Miniflex Benchtop diffractometer system with 1D line detector in Bragg-Brentano geometry at 40kV and 15mA.

For a reasonable signal-noise ratio of small sample amounts we use a silicon zero background holder. For more information please follow the link : https://www.rigaku.com/en/products/xrd/miniflex/app028

For matching the data we use the COD and ICDD PDF-4 Minerals database. 

miniflex1 copy


Order [Qualitative Phase ID] (Non-EU customers, excl. VAT)

  • P-XRD measurement of sample with intensity-2Theta profile, d-value table and phase matching 
  • photo documentation is mandatory and needs to purchased one time per sample. This gives the analysis the layout to fill in the results

price/sample: 40,00€ (+3.80€ photo documentation/sample)

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Order [Qualitative Phase ID] (EU customers, incl. VAT)

  • P-XRD measurement of sample with intensity-2Theta profile, d-value table and phase matching 
  • photo documentation is mandatory and needs to purchased one time per sample. This gives the analysis the layout to fill in the results

price/sample: 40,00€ (+3.80€ photo documentation/sample)

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Order [Quantitative Phase ID - Rietveld refinement]: 

  • photo documentation is mandatory and needs to purchased one time per sample. This gives the analysis the layout to fill in the results
  • P-XRD measurement of sample with intensity-2Theta profile, d-value table and phase matching 
  • determination of the phase volume in wt% (Rietveld refinement) or internal standard, RIR method, Direct Deviation
  • substituion and/or refinement of a structure with combined SEM-EDS/EPMA-WDS data
  • Indexing of powder data (Dicvol, Treor90)

price/sample: 85,00€ (+3.80€ photo documentation/sample)

Please inquire!