LABORATORY FOR SIZE, SHAPE AND CHEMICAL IDENTITY
The physical geographical researches mostly require the determination of the particle size distribution, therefore historically the capacity of the Laboratory for Sediment and Soil Analysis has been formed in this area. Recently in we have capacity for size distribution measurement in the scale from 10 cm to 3Å. To this the conventional (riddling) and the currently obtainable most advanced instrumentation is available.
In the micron and submicron size range the chemical/mineralological properties affect the size, therefore the particle analysis section also performs measurements with the most advanced instrumentation in this area.
Sieving
Retsch Sieve Shaker 200 (2005)For the mesurement of the coarse textured materials and for the separation of the farctions conventional sieving method is available. The analog-contorlled sieve shaker has wet clamping devices, too.
Dry sieving: 5.6 mm, 4 mm, 2 mm, 1 mm, 0.63 mm, 0.5 mm, 0.25 mm
Wet sieving: 0.63 mm, 0.5 mm, 0.25 mm, 0.063 mm, 0.02mm, 0.01 mm, 0.005 mm.
Laser diffraction particle size distribution analysis
The most frequent measurable sample types in the laboratory are soil and soil-like loose-textured sedimentary rocks, but less often drug samples, metal powders and other homogeneous materials are also measured. If necessary, the laboratory is also capable of analyzing the size of biological samples (cells and vesicles).
Fritsch Analysette 22 Microtech Plus (2009, 2012)
Measuring principle: laser diffraction and dynamic light scattering
Calculation theory: Fraunhoffer approximation (and Mie scattering)
Measuring range: 80 nm – 2 mm
Sample addition method:
liquid dispersion: water and alcohols
Results: volume percentage,
Light sources: 940 nm red laser (10 mW), 531 nm green laser (10 mW)
Detectors: 57 pieces of high resolution photodiode
Fritsch Analysette 22 Microtech (2004)
Measuring principle: laser diffraction
Calculation theory: Fraunhoffer approximation
Measuring range: 100 nm – 0.7 mm
Sample addition method: liquid dispersion
Light sources: 940 nm red laser (10 mW)
Horiba Partica LA 950 V2 (2013)
Measuring principle: laser diffraction and dynamic light scattering
Calculation theory: Mie theory (Fraunhoffer approximation)
Measuring range: 10 nm – 3 mm
Sample addition method:
liquid dispersion: water and alcohols
air dispersion;
small volume cuvette: water, alcohols, organic solvents
Results: volume percentage,
Light sources: 5 mW 650 nm red laser (He-Ne); 3mW 405 nm blue LED
Detectors: 87 pieces of high resolution photodiode; (75 pieces for forward and low-angle scattering and 12 pieces for high-angle and backward scattering)
Measurment reliability:
based on ISO 13320:2009 compliant an accuracy of ± 0.6%, verified on every unit with NIST-traceable mono- and polydisperse size standards: 100 nm, 500 nm, 1.020 µm, 12.01 µm, 102 µm & 1004 µm
Measurement precision:
+/- 0.1% verified on COV NIST-traceable polystyrene latex standards: 100 nm, 500 nm, 1.020 µm, 12.01 µm, 102 µm & 1004 µm
Particle Shape Analysis and Raman spectroscopy
Image Analyser – Raman spectromicroscope (Malvern Morphologi G3SE ID, 2015)Malvern Morphologi G3 ID based on the principle of static automated imaging. It is equipped with a Nikon optical microscope and a Kaiser RamanRxn11 Raman spectroscope. Unlike the laser diffraction, this measurement results the real size of the particles. The measuring range of this instrument covers nearly the same measurement range as the laser diffraction devices’.
Similar to the laser diffraction instruments it is possible to use air and liquid dispersion. In addition to the above mentioned options, the instrument is capable the analysing of materials absorbed on filter papers, thin-sections and hard rocks.
The measurement results generated in a stock contains information from the samples one-by-one, so the morphological analysis of the material after the measurements are possible, the particles can be tested separately.
Size and shape analysis
Measuring principle: static optical imaging
Measuring range: 0.5 µm m – 1 mm
Sample addition method: air dispersion, liquid dispersion, thin-section, filter paper
Measured morphological parameters: circular equivalent diameter, length, width, perimeter, area, circularity, aspect ratio, longevity, convexity
Parameters related to transparency: average intensity, standard deviation of the intensity
Optical system: Nikon CFI 60 brightfield/darkfield system
Sample illumination: episcopic, diascopic
Manual microscope mode: filters and polarization microscope mode
Detector: 5M pixel 2592 x 1944 CCD
Camera pixel size: 2,78 x 2,78 µm
Automatic Episcopic dark area measurement
„Fibre coupled dispersive” Raman spectrometer
Spatial resolution: 3µm;
Spectral analysis of manually selected particles;
Automatic mode: automatic mesurements of samples selected by size and shape parameters
Laser source: 785 nm red laser (500 mW)
Raman shift range: 150cm-1 to 1850 cm-1 by 1 cm-1 steps
Spektral resolutions: 6 cm-1
Partilcle sizing in nano size range
For the analysis of the nano size range, a photon correlation DLS / SLS spectroscopy equipped with an autotitrator and a preparative size exclusion liquid chromatograph (HPLC SEC) with tree different detectors are available. With the help of the autotitrator not just the size, the molecular mass and the zeta potential can be analysed but the isoelectric point of the colloidal systems is also measurable. HPLC not only measures nano scale materials but it can separate size fractions. These fractions can be measured by other instruments.
Photon correlation spectroscope (Malvern nanoZS, 2015)
Light source: He-Ne laser 633 nm (4mW)
Size distribution measurement
Measuring principle: Dynamic Light Scattering,
Calculation theory: Mie scattering,
Measuring range: 0.3 nm - 10.0 µm;
Minimum sample volume: 12µL;
Concentration range: from 0.1ppm to 40%w/v;
Minimum sample concentration: 0.1 mg/ml 15kDa lysozyme
Zeta potential measurement
Simultaneous measurement of the zeta potential and its disrtibution.
Measuring principle: Electrophoretic Light Scattering;
Measuring principle: Phase Analysis Light Scattering (PALS);
Zeta potencial range: +/- 500mV;
Mobility range: +/-20µm.cm/V.s;
Measuring range: 3.8nm - 10.0 µm;
Precision: +/- 10%;
Sensitivity: 0.12µm.cm/V.s in aqueous system, (NIST SRM1980 standard reference material).
Molecular mass measurement
Measuring principle: Static Light Scattering
Absolute molecular weight: between <1000Da - 2x107 Da (determined by the Deby plot method)
Estimated molecural weight: between <1000Da - 2x107 Da (determined by DLS measuremet)
Presicion: +/- 10%
Autotitrator
Size and zeta potential titration
Aquous solution titration
Minimum sample volume: 4ml
Preparative Size Exclusion Liquid Chromatograph (HPLC SEC; Shimadzu LC20 AR, 2017)
SPD-M20A diode ray (n. of diodes: 512 pcs)
Range: 190-800nm
Resolution: 1,2nm
Gap width: 1,2 és 8 nm.
Accuracy: ± 1 nm.
RF-20A FLUORESCENCE DETECTOR
RID-20A REFRACTION DETECTOR
Noise: =< 2,5 nRIU
Drift: =< 0,1 uRIU/h
Range: 0,01 - 500 uRIU
FLOW SELECTION BLOCK ASSY