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Test methods and equipment – part 1

This site presents test methods and equipment used in, among other things, identification of products’ materials and contamination, chemical composition, material emissions, technical cleanliness inspection, tests of petroleum products and working fluids

On this site:

Elemental analysers

Oxygen, nitrogen and hydrogen analyser

Leco ONH836 elemental analyser

  • an instrument equipped with thermoconductive and infrared detectors
  • for determining the content of light elements (oxygen, nitrogen, hydrogen) in metal alloys
  • used, among others, to indicate hydrogen embrittlement
  • complements techniques such as ICP-OES and WD-XRF in the analysis of metals and their alloys

Marking range

  • H: 1 – 100 ppm
  • O: 0.001 – 0.050%
  • N: 0.002 – 1.50%

Carbon and sulphur analyser

CS-125 Carbon and sulphur analyser

  • for the determination of carbon and sulphur content in metal alloys
  • complements techniques such as ICP-OES and WD-XRF in the analysis of metals and their alloys

Marking range

  • C: 0.003 – 4.5%
  • S: 0.002 – 0.60%

Chromatography

Chromatography is a physico-chemical method of separating mixtures of substances, in which the components to be separated are divided between two phases: a stationary phase stationary phase and a mobile phase, moving through the chromatographic column. The mobile phase is a gas, usually helium or hydrogen in gas chromatography. The mobile phase is a liquid or a mixture of liquids in gas chromatography.

Chromatography is based on the phenomenon of intermolecular interactions between the components of the mixture being analysed and the filling of the column. The different partitioning of the components of the mixture between the mobile and stationary phases results in differences in the migration velocity and separation of the components.

The chromatographic separation results in a chromatogram, i.e. a plot of the indication of the signal obtained in the detector as a function of time. The part of the chromatogram illustrating the detector signal for a single substance is the peak.

Liquid chromatography

Agilent 1260 infinity high performance liquid chromatograph (HPLC) with UV-VIS detection (diode array detector, DAD)

  • Used in the qualitative and quantitative analysis of soluble compounds in the mobile phase 
  • It enables the analysis of compounds with different molecular weights, volatility and high temperature unstable compounds
  • It is used in the analysis of carbonyl compounds (including formaldehyde and acetaldehyde) and phthalates emitted from materials

Gas chromatography

Agilent 7820A gas chromatograph equipped with Agilent 7693A liquid sample loader

The chromatograph is dedicated to the research of petroleum products, allowing for

  • their identification and determination of the presence of impurities
  • analysis of engine oils and fuels – incl. enables comparative testing of the composition of mixtures
  • quantifying the presence of fuel in engine oil.
Agilent 7820A gas chromatograph

Agilent 7890A gas chromatograph with flame ionisation and mass detector (GC-FID/MS)

This chromatograph is equipped with

  • MSD Agilent 5975C Inert mass spectrometer and FID flame ionization detector
  • Agilent 7683B liquid sample loader
  • Headspace Sampler Agilent G1888
  • Termodesorber Markes UNITY2 with ULTRA2 sample changer
  • Microcell for emission tests

The chromatograph is intended for qualitative analyzes (identification of compounds)
and quantitative organic substances from liquid and gaseous samples by the following methods:

  • Headspace – e.g. testing of Volatile Organic Compounds (VOC) emissions under static conditions
  • Temperature desorption – e.g. testing of VOC emissions based on air samples collected on appropriate adsorbent beds
  • VOC emission tests from materials under dynamic conditions (e.g. according to VDA 278)
  • Direct feeding of liquid samples

Agilent 7890B gas chromatograph with a nitrogen-phosphor and mass detector (GC-NPD/MS) and olfactometric port

This chromatograph is equipped with:

  • MSD Agilent 5977A mass spectrometer and NPD nitrogen phosphor detector
  • Gertsel olfactometric port
  • Agilent 7683B liquid sample loader
  • termodesorber Markes UNITY2

The chromatograph, by separating the analyzed samples into individual organic compounds, allows for:

  • Identification of compounds
  • Analysis of the quantitative composition of the samples
  • Odor analysis of individual compounds separated during chromatographic analysis, with simultaneous identification using mass spectrometry

The Agilent 7890B gas chromatograph is dedicated to the analysis of amines, nitrosamines and other organic compounds containing nitrogen and phosphorus.

Chromatograf gazowy z detektorami NPD i MSD oraz portem olfaktometrycznym

Ion chromatography

Chromatographic analysis of the test, extract, allows the separation of individual ions to be obtained in chromatograms.

Metrohm – 930 Compact IC Flex Ion chromatographies

Using this set of ion chromatographs and the corresponding standard solutions, in the BOSMAL laboratory, we carry out, among other things, a detailed evaluation of the ionic purity of the surface of the test pieces. On the basis of the tests, qualitative and quantitative analysis is possible, as well as the determination of the main anions, such as chlorides and bromides, and the main cations, such as sodium, ammonium ion and potassium. The test methodology introduced allows measurement of ions at low concentration levels (of the order of 1 mg/L). In addition, it is possible to determine fluoride, chloride, nitrite, nitrate, bromide, phosphate and sulphate anions. Of the cations, it is additionally possible to determine: lithium, calcium and magnesium. The test is carried out on aqueous solutions, solutions from surface washing or from solvent extraction carried out at room temperature or elevated temperature, e.g. in closed containers or bags of appropriate purity (e.g. according to IPC-TM-650 method no. 2.3.28.2).

Spectrometry

Inductively Coupled Plasma Optical Emission spectroscopy (ICP-OES)

Inductively coupled plasma optical emission spectrometry (ICP-OES) is an analytical method for determining the elemental composition of a test substance. The method analyses the electromagnetic radiation produced by excitation of atoms in a plasma flame. The advantage of the method is its very high sensitivity (it is possible to analyse samples weighing from about 1 mg), while the disadvantage is the necessity of running the sample into solution (microwave-assisted high-pressure dissolution in acids), and thus the destruction of the sample analysed during the test.

PerkinElmer Optima 4300 DV Inductively Coupled Plasma Optical Emission spectroscopy (ICP-OES)

  • allows analysis of the elemental composition of samples of metals and alloys, sludge, dust, ash and the content of elements in aqueous solutions, composites, plastics, rubbers and automotive catalysts
  • solid samples are mineralised in acids (under increased pressure in a microwave mineraliser or in an open system) or fused before analysis
  • the spectrometer has a wide analytical range

The instrument can determine the following chemical elements:

Li, Be, B, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Pb, Sr, Y, Zr, Nb, Mo, Rh, Pd, Rb, Ag, Cd, In, Sn, Te, Cs, Ba, Hf, W, Pt, Au, Hg, Pb, Bi, Ta

PerkinElmer Optima 8300 DV Inductively Coupled Plasma Optical Emission spectroscopy (ICP-OES)

  • allows analysis of the elemental composition of samples of metals and alloys, sludge, dust, ash and the content of elements in aqueous solutions, composites, plastics, rubbers and petroleum products and automotive catalysts
  • solid samples are mineralised in acids (under increased pressure in a microwave mineraliser or in an open system) or fused before analysis
  • analysing the elemental content of fuels, including gasoline via a cooled mist chamber
  • for the analysis of the elemental content of engine oils, transmission oils, coolants, lubricants, etc.
  • the spectrometer has a wide analytical range

The instrument can determine the following chemical elements:

Li, Be, B, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Pb, Sr, Y, Zr, Nb, Mo, Rh, Pd, Rb, Ag, Cd, In, Sn, Sb, Te, Cs, Ba, Hf, W, Pt, Au, Hg, Pb, Bi, Ta

X-ray fluorescence spectrometry (XRF)

X-ray fluorescence spectrometry (XRF) is an analytical method for determining the elemental composition of the substance under investigation. It is based on the analysis of photons arising from electron jumps between orbitals, which are caused by bombarding the sample under examination with X-rays. The main advantage of this method is that it is non-destructive and samples can be analysed repeatedly. The disadvantages are the need for quite large sample volumes and the relatively high radiation energy, which often also penetrates the material.

Rigaku ZSX Primus II wavelength-dispersive X-ray fluorescence spectrometer (WD-XRF)

  • allows analysis of the elemental composition of samples of metals and alloys, sludge, dust, ash and the content of elements in composites, plastics, rubbers, petroleum products and automotive catalytic converters
  • the 4kW X-ray tube allows very precise analytical measurements
  • allows examination of surfaces with heterogeneous composition
  • allows the distribution of elements present on the surface of samples and filters to be mapped
  • allows examination of the content of elements in engine oils, gearboxes, coolants, lubricants, etc.
  • wide analytical range

Range of elements to be determined:

Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Pb, Sr, Y, Zr, Nb, Mo, Rh, Pd, Ag, Cd, In, Sn, Sb, Te, Cs, Ba, Hf, W, Pt, Au, Hg, Pb, Bi, C, S, O, Cl, Br

Selected instruments for sample preparation for spectrometric studies

Berghof SpeedWave4 – Microwave Digestion System

  • Auxiliary device for the preparation of samples in the analysis of elemental composition
  • Reproducible digestion processes thanks to homogeneous microwave distribution
  • Microwave digestion with active reaction monitoring

Katanax X-300 fluxer 

  • Auxiliary device for the preparation of samples in the analysis of elemental composition
  • Allows 2 samples to be melted at the same time
  • Melting the comminuted solids in the presence of fluxes allows pearls of homogeneous composition to be obtained for elemental composition studies

VIS spectrophotometers

Hach Lange DR 3800 VIS spectrophotometer

It is a VIS spectrophotometer with a wavelength range of 320 to 1100 nm.
Among other things, the instrument is equipped with multiple wavelength mode, wavelength scan and time waveform. It takes digital readings, given directly in units of concentration, as absorbance or percentage of transmittance.

Spectrophotometric colour measurements

BYK-mac i spectrophotometer

The BYK-mac i spectrophotometer is a unique, portable instrument for simultaneous multi-angle colour measurement and analysis of metallic pastes.

It enables:

  • classic 5-angle colour measurement at angles of 15º/25º/45º/75º/110º
  • additional -15° colour measurement for interference pigments
  • sparkle’ and “graininess” measurement for the investigation of sparkle and grain effects of metallic pigments
  • fluorescence detection and measurement

CF57/CA X-Rite spectrophotometer

Color i5 X-Rite spectrophotometer

Fourier Transform Infrared Spectroscopy (FTIR)

FTIR infrared spectroscopy uses radiation in the infrared range which, as it passes through a sample of the test substance, is selectively absorbed by vibrating bonds between atoms. The frequency of these vibrations is characteristic of the functional group in question. The spectrogram (spectrum) of the substance obtained as a result of the test makes it possible to indicate the characteristic functional groups present in the test sample and, as a result, to identify, for example, a plastic or a type of organic liquid.

ThermoFisher Scientific Nicolet is50 Fourier transform infrared (FTIR) spectrometer

The spectrometer is equipped with test adapters: transmission and reflection (ATR and HATR), which enable testing of both solutions and solids.
NICOLET is50 spectrometer:

  • It is used to identify the base material of plastics, foams, adhesives, rubbers, solvents, petroleum products
  • Allows for the identification of small sizes of solid impurities (very often in a non-destructive way)
  • Enables the performance of comparative analyzes to determine the differences between the sample base materials
  • Allows for the analysis of surface contamination in the form of stains, discoloration, tarnish by direct collection or extraction with a properly selected solvent
  • In specific cases, it also allows the identification of inorganic substances, e.g. fillers

Thermo Scientific Nicolet 6700 Fourier Transform Infrared (FTIR) spectrometer

The spectrometer is equipped with test adapters: transmission and reflection (ATR and HATR), which enable testing of both solutions and solids.
NICOLET 6700 spectrometer:

  • It is used to identify the base material of plastics, foams, adhesives, rubbers, solvents, petroleum products
  • Allows for the identification of small sizes of solid impurities (very often in a non-destructive way)
  • Enables the performance of comparative analyzes to determine the differences between the sample base materials
  • Allows for the analysis of surface contamination in the form of stains, discoloration, tarnish by direct collection or extraction with a properly selected solvent
  • Enables quantitative measurements – benzene content, FAME content, glycol content, soot content, degree of oxidation and nitration
  • In specific cases, it also allows the identification of inorganic substances, e.g. fillers

Thermo Nicolet iN10 IR Microscope FTIR spectrophotometer

Spectroradiometric measurements

Stellar Net Inc. SILVER NOVA TEC X2 spectrometer

This equipment is used together with SpectraWiz software and the following accessories:

  • 2” integrating sphere,
  • wolfram-halogen lamp, deuterium lamp,
  • heads for reflection and transmission measurements.

Thermal analysis

Differential Scanning Calorimetry (DSC)

Differential scanning calorimetry (DSC) is a thermoanalytical technique.
Measurement carried out by the differential scanning calorimetry method consists in determining the amount of heat transferred to or taken from the tested sample, per unit of time, necessary to maintain the same temperature of the sample and a neutral thermal reference (empty crucible) during their heating or cooling at a constant speed. The proportionality of the measurement signal to the heat flux in the DSC enables the direct measurement of the heat capacity and the determination of the cp (T) relationship, and thus the quantitative “observation” of the course of changes in the sample material on the basis of the shape of the DSC curve. The value of the heat flux (dH / dt) depends first of all on the type of transformation or thermal reaction taking place in the sample, and also on the instrumental factors of the measurement.

TA Instruments Q2000 Differential Scanning Calorimetry (DSC)

Device operating temperature range: -90 ° C – 550 ° C
Cooling module (intracooler) RCS (no use of liquid nitrogen)

Thermogravimetry (TGA)

Thermogravimetry (TGA) is a technique belonging to the group of thermal analysis methods in which the mass changes of a sample under a specific temperature regime are determined. Losses or increases in mass depend most strongly on the stoichiometry of the reactions occurring during analysis. The technique allows the determination of the individual components of a substance, the determination of the magnitude of the thermal transformation and the temperature at which this transformation takes place. Thermogravimetry also makes it possible to study phase transitions and reactions (e.g. oxidation).

TA Instruments Q500 thermogravimetric analyzer (TGA) coupled with a Nicolet iS50 FTIR spectrometer

Device operating temperature range: from RT to 1000° C
Controlled heating rate from 0.1 to 100° C / min

Concurrent coupled techniques involve examining a sample using two (or more) instrumental techniques. Techniques of this type include thermogravimetry coupled with infrared spectrometry (TGA-FTIR), which enable the study of waste gases during thermal degradation. The test sample is heated at a constant rate according to a controlled temperature program, and the change in mass as a function of temperature is measured, and the gases generated during the thermogravimetric analysis are analyzed simultaneously. Alternatively, the sample is held at a specific, constant temperature and the change in weight over time is measured over a specified period of time while analyzing evolved gaseous products. The stage ending the measurement is the interpretation of the IR spectrum, from which information is obtained about the functional groups and types of bonds that were in the tested portion of the gas released from the degraded material at a given temperature or time interval.

Microscopy techniques

Electron microscopy SEM

SEM EVO MA25 Zeiss scanning electron microscope, with EDS Oxford Instruments analyser and EBSD Bruker analyser

Scanning electron microscope with the ability to work in high and low vacuum mode, which allows you to analyze both conductive and non-conductive samples. It has SE (secondary electron) and BSE (backscattered electron) imaging, it is also equipped with EDS (energy dispersive X-ray spectroscopy) and EBSD (electron backscatter diffraction) analyzers by Bruker.

Research opportunities:

  • work in high and low vacuum mode Praca w trybie wysokiej próżni (conductive samples analyze) i w trybie niskiej próżni (non-conductive samples analyze)
  • Qualitative and quantitative analysis and mapping the elemental composition of samples
  • Evaluation of the fracture surface fractography enabling the determination of the fracture nature, material discontinuities and e.g. hydrogen embrittlement, identification of undesirable inclusions on the fracture surface
  • Analysis of the size and type of non-metallic inclusions
  • Linear microanalysis of diffusion coatings and layers
  • Classification of pollutants on filters – technical cleanliness tests
  • Possibility of testing relatively large samples (300x200x200 mm)

Light (optical) microscopy

Light (optical) microscopy – in addition to standard light microscopes, you can find digital microscopes, metallographic microscopes and several other types.

Zeiss M1m optical, metallographic microscope

  • Magnification 12.5 – 2500x
  • AxioVision image analysis software
  • Reflected light observation techniques
    • Bright field
    • Dark field
    • Polarization
    • Differential interference contrast.
    • Differential interference contrast in circular polarization.
  • The possibility of observation in transmitted light.
  • Built-in automated table that allows you to scan the surface.
  • Module for folding surfaces – Mosaix (up to 4 cm).
  • 3D module.
  • Particle Analysis module for filter contamination analysis
  • NMI module for the analysis of non-metallic inclusions
  • Module for graphite analysis in cast irons
  • Grain size analysis module
  • Microstructure analysis
  • Thickness measurements of oxide, metallic and paint coatings
  • Identification of the type of corrosion (pitting, surface, intercrystalline)
  • Corrosion depth measurements
  • Porosity analysis

Keyence VHX-6000 digital microscope

  • Magnification 20 – 1000x
  • Advanced image sharpening
  • High quality and resolution images
  • Observation in reflected and transmitted light
  • Observation at varying angles
  • Removing reflections
  • A high-speed automated table that allows you to scan the surface
  • Quick folding of the surface (up to 4 cm)
  • 3D surface visualization
  • Surface roughness measurement
  • Automatic particle counting
  • Automatic edge detection
  • Real-time measurements

Keyence VHX-7000 digital microscope

  • Magnification 5 – 1000x
  • Advanced image sharpening
  • High quality and resolution images
  • Observation in reflected and transmitted light
  • Observation at varying angles
  • Removing reflections
  • A high-speed automated table that allows you to scan the surface
  • Quick folding of the surface (up to 4 cm)
  • 3D surface visualization
  • Surface roughness measurement
  • Automatic particle counting
  • Automatic edge detection
  • Real-time measurements

dhs-Cleanalyzer Professional 5 µm optical microscope

  • with motorised table
  • particles are measured in size classes according to ISO 16232, VDA 19.1 and other customer requirements

Keyence VHX-7000 digital microscope with head for laser elemental analysis EA-300 series

  • Magnification 5 – 1000x
  • Advanced image sharpening
  • High quality and resolution images
  • Observation in reflected and transmitted light
  • Observation at varying angles
  • Removing reflections
  • A high-speed automated table that allows you to scan the surface
  • Quick folding of the surface (up to 4 cm)
  • 3D surface visualization
  • Surface roughness measurement
  • Automatic particle counting
  • Automatic edge detection
  • Real-time measurements
  • head for laser elemental analysis EA-300 series

Metallographic specimen preparation line (Struers) – cross cut

  • Citopress-20 Inlay press
  • Grinding and polishing machine RotoPol-22
  • Grinding and polishing machine LaboPol-21
  • Grinding and polishing machine Tegramin 25
  • Electropolishing machine LektroPol-5

Equipment for testing emissions and odours from materials

Micro-Chamber/Thermal Extractor (µ-CTE) Markes

µ-chamber thermal extraction method consists of placing and heating up of a plastic or rubber sample or finished product in a microchamber of 44 cm3 capacity. Substances emitted are then sampled dynamically onto an appropriate deposit, depending on the type of the compound being analysed; then, qualitative and quantitative analyses are conducted using the gas and liquid chromatography methods.

WKE1000 Weiss / Vötsch oraz EK1000 Olfasense Environmental chambers 1 m3 for VOC emission testing

  • A 1 m3 environmental chamber for testing VOC emissions from materials, semi-finished and finished components.
  • It allows tests to be carried out at constant or variable temperature, with controlled relative humidity and air flow.
  • The chamber is equipped with an FID detector, measuring the total concentration of hydrocarbons in the chamber in real time.
  • It allows air samples to be taken (for odour testing) or concentrated for analysis of VOCs, carbonyl compounds, amines, nitrosamines and phthalates.

Testing using the environmental chamber makes it possible to obtain information about the amount and type of compounds emitted from components made of different materials and of different dimensions, such as dashboards, car seats, carpets, etc. Tests are carried out in the chamber in accordance with international standards such as ISO 12219-4 and ISO 12219-6, as well as in accordance with the internal standards of major automotive companies.

HAAKE PHOENIX II+K20 with DC30 Fogging Tester

These tests rely on the condensation of evaporated, volatile components from the interior fittings on the vehicle windscreen, particularly the windscreen. The fogging characteristics can be determined by:

  • fogging value – quotient of reflectometer 60° value of glass plate with fogging precipitate and reflectometer 60° value of the same glass plate without fogging precipitate
  • fogging value – quotient of transmittance of glass plate with fogging precipitate and transmittance of the same glass plate without fogging precipitate
  • components condensation (G) – difference of the weight of aluminium foil with and without fogging precipitate

Laboratory for odour testing

A room with constant, controlled temperature and humidity, free of odour-emitting materials and substances. In this room, qualified personnel test the odours (in terms of their intensity and type) emitted from a variety of materials and components in a comfortable environment. It is also a training ground for current and potential members of the odour assessment panel.
The very subjective, at first glance, testing method makes it possible, in many cases, to point out errors that have been made in the processing of plastics and the production of components.
A long and intensive training process, participation in international proficiency tests, participation in training organised by OEMs and in-house research work make it possible to ensure the impartiality and competence of the personnel in the odour tests.

Laboratory and equipment for testing technical cleanliness

Clean room – cleanliness test room and equipment

  • ISO Class 6 cleanroom
  • is equipped with an automated PALL Cleanliness Cabinet for spray washing of the components to be tested, with interchangeable nozzles and adjustable flow rate, enabling cleanliness tests of complex-shaped objects
  • depending on the size and shape of the objects to be tested, contaminants can also be extracted from their surfaces in the ultrasonic bath
  • various techniques can be used to wash contaminants from objects: spray washing, ultrasonic extraction, rinsing or shaking
  • room equipment allows gravimetric analysis of contaminants
  • the separated contamination of objects can also be subjected to quantitative analysis (size, amount and type of contamination: metallic particles, non-metallic particles and fibres) based on dedicated optical microscopes
  • by means of a scanning electron microscope (SEM-EDX), it is possible to analyse the elementary composition, based on this also on hardness, of the contamination particles

PALL cleanliness cabinet automatic pressure washing station (with the possibility of cleaning large parts)

Automated component spray wash cabinet, with interchangeable nozzles and adjustable flow rate. Allows cleanliness testing of complex-shaped objects of considerable size.

Particle extraction system

Equipment for testing petroleum products and operating fluids


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