X-ray Diffraction Powder Method

X-ray diffraction is a method which has long been used in industry for the rapid and accurate identification of crystalline substances.

The method uses x-ray diffraction patterns which act as unique "fingerprints" for every known crystalline substance.  An unknown substance (as little as a few milligrams of a powdered sample) produces a pattern which is then compared with standard reference patterns from a file of tens of thousands of compounds compiled by the National Bureau of Standards, American Society for Testing Materials, the American Crystallographic Association and the British Institute of Physics.

EMS has the ICDD diffraction files on computer; it uses PDF-2 data base on a CD-ROM.  This database has accompanying search-match software where unknown materials are identified using the diffraction pattern and element matching techniques.

If several substances are present in a mixture, their characteristic patterns are recorded in the unknown pattern, so that each material present can be identified.  Depending on the material, quantities greater than one to five percent can be detected with confidence. Since it is the crystal structure and not the chemical composition which is being analyzed, this method will distinguish between distinctly different materials which have identical compositions, for instance, between graphite and diamond (forms of carbon), quartz and cristobalite (forms of silicon oxide), calcite and aragonite (calcium carbonate), hematite and magnetite (alpha and gamma forms of iron oxide).

Where a quantitative analysis of the amount of a known substance in a mixture is desired, accurate standard mixtures of the substance in question are prepared and then analyzed along with the unknown mixture.  The relative intensities of the x-ray patterns derived are measured and the weight percentage of the substances in the mixture computed.  An accuracy better than 5% is possible with many substances.

EMS Laboratories has the facilities and expertise necessary to analyze any crystalline material, in quantities as small as a few milligrams (more is required for quantitative analysis). In addition, we provide valuable additional information regarding particle shape and size, composition and crystal habit.

 

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