Analysis Laboratory

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Analysis Laboratory

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Departments

The Analysis Laboratory consists of two departments:

  1. The Chemical Analysis Department
  2. The Physical and Structural Characterization Department

The Analysis Laboratory within INCDMNR-IMNR, is accredited RENAR (LI Nr.1056 / 16.04.2015) for:

  • Determination of Cu, Fe, Mg, Mn, Ni, Zn content within aluminum, aluminum alloys and technology solutions, by inductively coupled plasma optical emission spectrometry ICP-OES;
  • Determination of Cd, Ca, Pb, Au and Ag content by flame atomic absorption spectroscopy, in ores, concentrates and technological solutions;
  • Qualitative phase analysis by X-ray powder diffraction of polycrystalline inorganic materials.

The Analysis Laboratory of INCDMNR-IMNR is RENAR offers a wide range of services, such as:

  • Analysis regarding the chemical composition and the structure of materials and products resulted from metallurgy, inorganic chemistry, technology of ceramic materials and composites;
  • Determination of major elements and impurities in metals, alloys, metallic powders, inorganic chemicals, minerals, ores, ceramics, refractories, composites, slags, minerals;
  • Determination of rare earth content in various matrices; în diferite matrici;
  • Evaluation of environmental pollution: water, air, soil;
  • Powders analysis by X-ray diffraction: identification and quantification of crystalline phases, determination of crystallinity, crystallite size determination and microdeformations, as well as the characterization of crystalline structure: indexing, crystallization system, lattice parameters.
  • Quantitative and semi-quantitative determinations using the following methods: volumetry by neutralization reactions – acidimetry, alkalimetry; volumetry by redox reactions – permanganometry, iodometry, bicromatometry, bromatometry; gravimetry – gravimetric dosing of Sn, Si, Ba, SO42-, CO2, moisture content, calcination loss, carbon content, volatile substances, ashes.
  • Qualitative microscope analysis for construction materials, natural stone, metals and welds.

Endowment

Bragg-Brentano method, X ray powder diffraction with radiation source CuKα an SOL X detector in θ–θ vertical geometry. Software: SLEVE + and PDF-4+ database, allows crystalline phase identification and quantification, crystallinity, crystallite size and microdeformations, as well as crystalline structure characterization: Indexing, crystallization system, lattice parameters.

Having the following modules: flame module to determine the following elements Cu, Co, Cd, Pb, Sb, Zn, Ni, Fe, Cr, Mg, Ca, Na, K, Rb, Li, Sr, Ga, In, Au, Ag, Pt, Pd, Rh, graphite furnace, vapor generator in order to determine the following elements As, Bi, Sb, Se, Sn, Te. Quantitative determination of metals in a wide range of concentrations: from ppb up to tens of %, using several measurement techniques.

for DSC-TG analysis. Temperature range: 20°C – 1600°C. Heat flow between 1°/min and 40°/min. Used gases: argon, helium or air. The amount required for an analysis is approximately 20 mg. Alumina crucibles are used.

With high resolution, fully digitized, produced by FEI Company, incorporated with Energy Dispersive X-Ray Spectrometer, produced by EDAX, consisting of ELEMENT Silicon Drift Detector Fixed, Element EDS Analysis Software Suite. The Quanta 250 system, purchased in 2017, is designed to study conductive, non-conductive and/or hydrated samples in their natural state, without additional preparation (metallization).

With polarized light, reflected and transmitted – Axio Imager A1m, produced by Carl Zeiss Microimaging Gmbh, purchased in 2007, equipped with a digital camera for image acquisition and AxioVision Release 4.8.1 dedicated software for image processing.

Produced by Anton Paar, with Vickers indenter, purchased in 2007.

Produced by Buehler, purchased in 2007, for powders and delicate samples.

Services

The Analysis Laboratory can offer a wide range of services, such as:

  • establishing the materials and products chemical composition and structure.
  • determination of major elements and impurities in metals, alloys, metal powders, inorganic chemicals, ores, ceramic, refractory, composite, slag, minerals;
  • determination of rare earth contents in different matrices in metallic and non-metallic products;
  • determination of environmental pollution: water, soil;
  • thermal analysis for different types of materials.

Laboratory analysis can provide a wide range of services such as:

X-RAY DIFFRACTION

RENAR accredited laboratory (certificate LI No.1056/16.04.2015) for qualitative phase analysis by X-ray powder diffraction of inorganic polycrystalline materials.

Equipment name: Bruker-AXS D8 ADVANCE Diffractometer, Bragg-Brentano method for X-ray diffraction on powders having a CuKα radiation source and a SOL X detector, in vertical geometry θ – θ. The software SLEVE + and PDF-4+ database.

Applications:

  • Crystalline phase identification and quantification;
  • Crystallinity determination;
  • Average crystallites size determination;
  • Micro deformation determination;
  • Crystalline structure characterization: indexing, crystallization system, cell parameters.

Interest fields:

  • Chemistry;
  • Metals and alloys;
  • Geology – Mineralogical analyzes: asbestos, rocks, clays, zeolites, ores;
  • Environmental protection: industrial waste, by-products;
  • Construction materials;
  • Pigments;
  • Inorganic fertilizers.

ATOMIC ABSORPTION SPECTROMETRY

RENAR accredited laboratory (certificate LI No.1056/16.04.2015) for content determination of Cd, Ca, Pb, Au and Ag, by flame atomic absorption spectrometry from ores, concentrates and technological solutions.

Other elements in the non-accredited system can be determined.

Atomic absorption spectrometry ensures the quantitative determination of metal contents in a wide range of concentrations.

Equipment name: Atomic absorption spectrometer – AAS ZEEnit 700, Analytic Jena AG, with:

  • flame;
  • graphite furnace for liquid samples;
  • hydride and cold vapor generator.

Quantitative determination of metal content in a wide range of concentrations: from ppb to tens of %, using several measurement techniques.

Flame module equipped with double beam optics and background correction, for achieving determinations in both the absorption and atomic emission for alkaline metals. With this module, the following elements can be determine: Cu, Co, Cd, Pb, Sb, Zn, Ni, Fe, Cr, Mg, Ca, Na, K, Rb, Li, Sr, Ga, In, such as Au, Ag, Pt, Pd, Rh.

Graphite furnace module determine traces ad ultra- traces of metals.

Hydride and cold vapor generator have low detection limits for elements hydrides As, Bi, Sb, Se, Sn, Te.

THERMAL ANALYSIS SetSys Evolution

SETSYS Evolution, Setaram, France, can perform DSC/TG thermal analysis. Specification: temperature range between 20°C – 1600°C; heat flow 1°/min – 40°/min; gases: argon, helium or air. The amount required for an analysis is approximately 20 mg. Alumina crucibles are used.

Applications:

  • determination of thermal behaviour of metals, alloys or oxides;
  • determination of heat flow;
  • kinetic studies.

MINERAL ANALYSIS BY OPTICAL MICROSCOPY in polarized, reflected and transmitted light, on the following types of samples: minerals; sedimentary rocks, metamorphic rocks, magma rocks, ore deposits, mining concentrates; slags and volatile dusts in the metallurgical industry; etc.

METALLOGRAPHY BY OPTICAL MICROSCOPY on the following types of samples: metals, special alloys, metallic composites, hybrid composites, ceramic and metal coatings, semiconductors.

VICKERS MICROHARDNESS tests

SCANNING ELECTRON MICROSCOPY SEM-EDAX

CHEMICAL ANALYSIS Volumetry and gravimetry

Laboratory perform quantitative and semi-quantitative determinations using the following methods:

VOLUMETRY:

 

Volumetry by neutralization reactions

 

Acidimetry

• dosage of strong acids with strong bases,

Alkalimetry

• dosage of strong bases with strong acids

• dosage of free ammonia;

• dosage of free ammonia from ammonia salts;

 

Volumetry by redox reactions

 

Permanganometry

• Ca dosing

• Ca activ dosing

• Mn (metoda Volhard) dosing

 

Iodometry

• Sn dosing

• sulphides dosing

• Sb dosing

 

Bicromatometrie

• Fe dosing

 

Bromatometrie

• Sb dosing

 

GRAVIMETRY:

 

Gravimetric dosing

Sn, Si, Ba, SO42-, CO2,

Moisture content

 

Calcination loss, carbon content, volatile substances, ashes.

 

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