Characterization Tools - Mineral Synthesis

GFZ Helmholtz Centre for Geosciences

last updated: February 7, 2025

About the Laboratory

Characterization Tools - Mineral Synthesis

GFZ Helmholtz Centre for Geosciences

@ Section 3.5 Interface Geochemistry

This Laboratory is part of:

Environmental Mineralogy Labs laboratory complex
Networks: Geo.X

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Description

The Environmental Mineralogy Labs are equipped with a very diverse suite of spectroscopic and scattering instruments to determine material chemical composition, structure, surface area and grain size of both synthetic and natural samples. For instance,

Our powder X-ray diffractometer (XRD) consists of two individual instruments capable of X-ray scattering analysis using both Cu (λ=1.54 Å) and Ag radiation (λ=0.56 Å) in transmission geometry. XRD can be used to analyze both crystalline and amorphous samples by measuring either conventional diffraction patterns or high Q-range total scattering patterns for pair distribution function (PDF) analysis. Measurements can be performed in room or elevated temperature up to 800⁰C.
The IR spectrometer is used for fast routine IR spectra acquisition in the 4000-400 cm⁻¹ range with a maximum resolution of 0.9 cm⁻¹, although in practice higher resolution than 4 cm⁻¹ is seldom necessary. IR spectra can be measured on both liquid and solid samples.
The UV-Visible (UV/VIS) spectrophotometer measures absorption of light in 190-1100 nm range. Measurements are possible in either ex situ mode in cuvettes or in situ using an external probe. The instrument is mostly used for the determination of elemental concentrations (e.g., Fe²⁺, As, Si, P) using well-established colorimetric methods. In addition, the spectrophotometer can also be used for the in situ and real-time monitoring of the nucleation, crystallization and growth of minerals, and is equipped with Single Cell Peltier System for temperature control and sample stirring.

Instruments

Surface Area Analyzer
Zeta-Potential Analyzer
Particle Analyzer
Optical Microscope
Light Microscope
UV-VIS Spectrophotometer
FTIR SPECTROMETER - Fourier Transform Infrared Spectrometer Traditional (dispersive) infrared techniques experience difficulties due to the '1 wavenumber at a time' nature of data acquisition. This leads to either a poor signal to noise ratio in a spectrum or a very long time needed to obtain a high quality spectrum. Both these situations cause problems with kinetic work. The first gives inherent large errors, the second prohibits in-situ work. These problems can be overcome using Fourier transform infrared spectroscopy (FT-IR) that is based on the interferometer originally designed by Michelson and a mathematical procedure developed by Fourier that converts response from the 'time' to the 'frequency' domain. In the Michelson interferometer a parallel, polychromatic beam of radiation from a source (A) is directed to a beam splitter (B), made from an infrared transparent material, such as KBr. The beam splitter reflects approximately half of the light to a mirror, known as the fixed mirror (C), which in turn reflects the light back to the beam splitter. The rest of the light passes through to a mirror, moving continuously, at a known velocity, back and forth along the direction of the incoming light and this is known as the moving mirror (D). Upon reflection from the moving mirror, radiation is then directed back to the beam splitter. At the beam splitter some of the light that has been reflected from the fixed mirror combines with light reflected from the moving mirror and is directed towards the sample. After passing through the sample (E) the radiation is focused onto the detector (F). The detectors are sufficiently fast to cope with time domain signal changes from the modulatio n in the interferometer. Additional information available at http://physics.nist.gov/Divisions/Div842/Gp1/fts_intro.html (Source: Global Change Master Directory (GCMD). 2023. GCMD Keywords, Version 16.3 [...] )
FTIR Spectrometer - Fourier Transform Infrared Spectrometer
Thermal Analysis Platform
An x-ray powder diffractometer is primarily used for the identification of phases in powder form. An x-ray beam of known wavelength is focused on a powdered sample and x-ray diffraction peaks are measured using a germanium detector; the d-spacing of the observed diffraction peaks is calculated using Bragg's Law [n*lamda = 2dsin(theta)]. The Scintag Pad V automated powder diffractometer uses a Cu x-ray tube with variable filters, a four-sample changer, and a low-noise, high efficiency, liquid-nitrogen cooled germanium detector. The goniometer is automated and software packages are run from a PC running Windows NT 4. A number of Scintag software packages are available for routine powder diffraction data acquisition, background correction and peak identification. Unknowns can be matched to JCPDS cards in an on-line database. Other software is available for quantitative analysis of powder mixtures, unit cell refinement, Rietveld analysis, and GSAS structural analysis. Samples sho uld be prepared as powders with a grain size of 10 um (approximately), and typically about 100 milligrams of sample is required. Additional information available at "http://www.gps.caltech.edu/facilities/analytical/xrd.html" [Summary provided by Caltech]
An x-ray powder diffractometer is primarily used for the identification of phases in powder form. An x-ray beam of known wavelength is focused on a powdered sample and x-ray diffraction peaks are measured using a germanium detector; the d-spacing of the observed diffraction peaks is calculated using Bragg's Law [n*lamda = 2dsin(theta)]. (Source: excerpt from NASA; UUID: f54aafd2-925e-4653-b897-c6ae4e094c69) (Source: Global Change Master Directory (GCMD). 2023. GCMD Keywords, Version 16.3 [...] )
XRPD - X-Ray Powder Diffractometer
PXRD, Powder X-Ray Diffractometer, XRD

Analytical Methods

Surface Area Analysis
BET Methods, Gas Sorption, Pore Volume Analysis
Zeta-Potential Measurement
Particle Analysis
Grain Size Distribution, Imaging Particle Analysis, Particle Shape, Particle Size Distribution
MICROSCOPES are instruments that magnify the image of small objects.
Laboratory methods using instruments that employ optical lenses or radiation to study objects too small to be seen by the naked eye. (Source: USGS; https://apps.usgs.gov/thesaurus/term-simple.php?thcode=2&code=740) (Source: Global Change Master Directory (GCMD). 2023. GCMD Keywords, Version 16.3 [...] )
Microscopy
Scientific techniques using a microscope with one or more lenses illuminated with visible light to view small objects. (Source: USGS; https://apps.usgs.gov/thesaurus/term-simple.php?thcode=2&code=835)
Optical Microscopy
Light Microscopy
UV-VIS Spectrophotometry
UV-VIS Spectroscopy
FTIR SPECTROMETER - Fourier Transform Infrared Spectrometer Traditional (dispersive) infrared techniques experience difficulties due to the '1 wavenumber at a time' nature of data acquisition. This leads to either a poor signal to noise ratio in a spectrum or a very long time needed to obtain a high quality spectrum. Both these situations cause problems with kinetic work. The first gives inherent large errors, the second prohibits in-situ work. These problems can be overcome using Fourier transform infrared spectroscopy (FT-IR) that is based on the interferometer originally designed by Michelson and a mathematical procedure developed by Fourier that converts response from the 'time' to the 'frequency' domain. In the Michelson interferometer a parallel, polychromatic beam of radiation from a source (A) is directed to a beam splitter (B), made from an infrared transparent material, such as KBr. The beam splitter reflects approximately half of the light to a mirror, known as the fixed mirror (C), which in turn reflects the light back to the beam splitter. The rest of the light passes through to a mirror, moving continuously, at a known velocity, back and forth along the direction of the incoming light and this is known as the moving mirror (D). Upon reflection from the moving mirror, radiation is then directed back to the beam splitter. At the beam splitter some of the light that has been reflected from the fixed mirror combines with light reflected from the moving mirror and is directed towards the sample. After passing through the sample (E) the radiation is focused onto the detector (F). The detectors are sufficiently fast to cope with time domain signal changes from the modulatio n in the interferometer. Additional information available at http://physics.nist.gov/Divisions/Div842/Gp1/fts_intro.html
Infrared spectroscopy in which a Fourier-transform spectrometer is used to separate the transmitted radiation into its component wavenumbers. (Source: IUPAC; https://iupac.org/wp-content/uploads/2019/10/PAC-REC-19-02-03.R2_PR191002MC.pdf (Source: Global Change Master Directory (GCMD). 2023. GCMD Keywords, Version 16.3 [...] )
FTIR Spectroscopy - Fourier Transform Infrared Spectroscopy
Technique where the difference between heat flow rates into a sample and a reference material is measured (heat-flow DSC). Technique where the difference between the electrical powers into a sample and a reference material is measured (power compensation DSC). (Source: IUPAC; https://doi.org/10.1515/pac-2012-0609)
DSC - Differential Scanning Calorimetry
Heat-flow DSC, Power Compensation DSC
A technique where the temperature difference between a sample and a reference material is measured. (Source: IUPAC; https://doi.org/10.1515/pac-2012-0609)
DTA - Differential Thermal Analysis
In any work where a confusion may arise between TG and Tg (the glass transition temperature), the abbreviation TGA or the full term “thermogravimetry” should be used. (Source: IUPAC; https://doi.org/10.1515/pac-2012-0609)
TGA - Thermogravimetric Analysis
Thermogravimetry (TG)
An x-ray powder diffractometer is primarily used for the identification of phases in powder form. An x-ray beam of known wavelength is focused on a powdered sample and x-ray diffraction peaks are measured using a germanium detector; the d-spacing of the observed diffraction peaks is calculated using Bragg's Law [n*lamda = 2dsin(theta)]. The Scintag Pad V automated powder diffractometer uses a Cu x-ray tube with variable filters, a four-sample changer, and a low-noise, high efficiency, liquid-nitrogen cooled germanium detector. The goniometer is automated and software packages are run from a PC running Windows NT 4. A number of Scintag software packages are available for routine powder diffraction data acquisition, background correction and peak identification. Unknowns can be matched to JCPDS cards in an on-line database. Other software is available for quantitative analysis of powder mixtures, unit cell refinement, Rietveld analysis, and GSAS structural analysis. Samples sho uld be prepared as powders with a grain size of 10 um (approximately), and typically about 100 milligrams of sample is required. Additional information available at "http://www.gps.caltech.edu/facilities/analytical/xrd.html" [Summary provided by Caltech] (Source: Global Change Master Directory (GCMD). 2023. GCMD Keywords, Version 16.3 [...] )
XRPD - X-Ray Powder Diffraction
PXRD, Powder X-Ray Diffraction, X-Ray Diffraction, X-Ray Diffraction Analysis, XRD

Laboratory Keywords

In addition to the instruments and analytical methods listed above, these keywords help to describe the work done in the laboratory. This may include the type of samples, standard materials, specific preparative or analytical methods and specific instrument characteristics.

ζ Potential

Disciplines

Geoscience > Geochemistry > Geochemistry
Geochemistry
Geoscience > Geochemistry > Mineralogy
Mineralogy

The Research Network for Geosciences in Berlin and Potsdam

Characterization Tools - Mineral Synthesis

GFZ Helmholtz Centre for Geosciences

About the Laboratory

Characterization Tools - Mineral Synthesis

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Description

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Analytical Methods

Laboratory Keywords

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