Characterization

IR – Near, Far and Mid IR

Infrared spectroscopy can be used to identify and study chemicals. The energy in the infrared region corresponds to the vibration between atoms in chemical compounds. Hence, the absorbed energies in the infrared spectrum may reveal the presence of chemical bonds between the atoms.

• Near IR (10000-4000 cm−1)
• Mid IR (4000-400 cm−1)
• Far IR (400-40 cm−1)

• 6 spectrophotometers
• Transmission, diffuse reflectance (DRIFT) and attenuated total reflection (ATR) modes
• Detectors: DTGS (5400-265 cm−1), MCT (5000-600 cm−1)
• Separators: KBr (mid-IR), (near-IR)
• Specific cell to record the IR spectrum under controlled atmosphere
• Possibility to couple with TGA and GCMS

UV

The ultraviolet-visible spectroscopy is a method routinely used for the quantitative analysis.

Range: 190-3500 nm

Temperature control (up to 100°C) for liquid sample

Solid sample with integration sphere

Perkin Elmer Lambda1050 &

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Measurement of thermal behavior of polymer.

DSC (modulated DSC)

Differential Scanning Calorimetry (DSC) is a thermoanalytical technique that measures enthalpy changes in polymers due to changes in their physical and chemical properties as a function of temperature or time.

Mettler DSC 1

Temperature: from -140 to 700 °C

Examples of investigations: melting temperature, glass transition, crystallization temperature, Cp, cristallinity

TGA/DSC

Thermal Gradient Analysis is a technique that measures the change in weight of a sample as it is heated, cooled or held at constant temperature.

Mettler TGA/DSC 1

Temperature: from ambient to 1200°C

Examples of investigations: absorption and desorption of gases, quantitative content, identification of decomposition products

Can be coupled to FTIR

DMA

Dynamic Mechanical Analyzer is used to measure mechanical and viscoelastic properties of materials.

Mettler DMA 1

Temperature: from -190°C to 600°C

Deformation modes: bending, tension, shear and compression

Examples of investigations: glass transition, Young module

Flash DSC

Mettler Flash DSC 1

Temperature:

Examples of investigations: melting temperature, glass transition, crystallization temperature

Gas chromatography (GC) is a common technique to separate chemical compounds. The sample is brought to gas phase, and then to a desired column to separate the compounds.

GC can be used either as an individual equipment or connected online to a reactor. There are mainly two type of GC :

• classic

Very common equipment for separation, qualification and quantification of chemical compounds. Possible to analyze a separate sample, as well as online measurement.

• 18 GC systems
• 4 equipped with auto-sampler
• Variety of available columns to separate hydrogen, nitrogen, oxygen, CO, CO2, light hydrocarbons, heavy hydrocarbons, functionalized hydrocarbons (aldehyde, ketone, amine, ether, ester, silane), chiral compounds

• micro - GC

Frequently used as online analytic tool, allowing fast product determination (typical in few minutes), due to integration of separate modules specifically designed to separate the defined gaseous products.

• 6 microGC systems
• all online connected to reactors
• Variety of available modules to fastly separate hydrogen, nitrogen, oxygen, CO, CO2, light hydrocarbons.

All GC systems are equipped with suitable detectors such as :

• FID (Flame-ionization detector)

Most suitable for hydrocarbon determination with high sensitivity. The output signal is virtually proportional with the carbon number, allowing estimation of the conversion and selectivity for pure hydrocarbon conversion without standard curves.

• TCD (Thermal conductivity detector)

Most suitable for the determination of inorganic gaseous substances. Also applicable for hydrocarbons and functionalized hydrocarbons.

• MS (Mass spectrometry)

Suitable for all chemical compounds with fairly high sensitivity. Also allows direct qualitative determination of the chemical substance based on mass fragments.

Size exclusion chromatography (SEC) is a separative method in which polymers in solution are fractionated by their size or their molecular weight.

As the sample is separated and eluted from the column, it can be characterized by :

• Conventional Calibration
• Universal Calibration
• Light scattering

Investigations: Mn, Mw, Đ, Rg, Rh, LCB

Three chromatography systems are available :

SEC in THF or toluene solvent

Viscotek TDAmax :

Temperature: up to 80°C

Solvent : Tetrahydrofuran, Toluene

Detectors : RI, Light Scattering (RALS, LALS), Viscometer, UV Sample type: Synthetic polymers, Copolymers

SEC in TCB solvent at 150°C for Polyolefin

High temperature Viscotek system

Temperature : up to 160°C

Solvent : 1, 2, 4-Trichlorobenzene

Detectors : RI, Light Scattering (RALS, LALS), Viscometer, UV Sample type: Polyolefins (HDPE, LDPE, LLDPE, PP)

SEC in DMSO or DMF solvent

Agilent Infinity 1260

Temperature : 70°C

Solvent : dimethyl sulfoxide, dimethylformamide

Detectors : RI, UV, MALS Sample type: synthetic polar polymers

Adsorption measurements can inform about porosity (micropores and mesopores) or metallic nanoparticles sizes with chemisorption analysis.

N2 physisorption at 77K can measure adsorption isotherm for surface area and pore size analysis.

H2 and CO chemisorption measurement is used to determined active site of metals (Pt, Pd, Ni…).

The lab is equipped with one BELSORP-max and three Micromeritics ASAP2020.

• Rheometer

We are equipped with a rotational, stress-controlled HAAKE MARS 60 rheometer from Thermo Scientific to measure time- and temperature-dependent viscoelastic properties of elastomers, foams, gels, liquids or latexes.

Two Peltier cells (Plane and Cylinder), combined with a variety of measuring geometries and appropriate active or passive hoods, enable us to test most samples under nitrogen atmosphere, over a range of temperature from -40 to 200°C.

• Brookfield Vicosimeter

The DV2T Viscometer measures fluid viscosity at given shear rates. The principle of operation is to drive a spindle immersed in the sample through a calibrated spring. The viscous drag of the fluid against the spindle is measured by the spring deflection with a rotary transducer. The measurement range (in centipoise or milliPascal.seconds) is determined by the rotational speed of the spindle, the size and shape of the spindle, the container the spindle is rotating in, and the full scale torque of the calibrated spring. The higher the torque calibration, the higher the measurement range.

• Tensile testing machine

• Intrinsic Viscosity Analyzer (IVA)

The IVA instrument is a dual-capillary relative viscometer that can analyze polymers intrinsic viscosity and viscosity average molar mass (Mv). Used for polyolefins, PET, PVC…

• Melt Index

The Mflow is a modular, expandable instrument with which the melt mass and melt volume flow rate can be determined. Depending on the polymer being tested, the Mflow can be fitted with different test weights

These techniques are used for the measurement of the Chemical Composition Distribution (CCD) of Polyolefins.

Sample type : LLDPE, iPP, aPP

Temperature : up to 160°C

Solvent : 1,2,4-trichlorobenzene

Application : short chain branching, CCD

Calibrated for : ethylene propene, ethylene hexene, ethylene butene, ethylene octene, ethylene octadecene

• TREF/CRYSTAF

Temperature rising elution fractionation (TREF) and crystallization analysis fractionation (CRYSTAF) are separation techniques for the characterization of semicrystalline polymers. They are proposed to measure the Chemical Composition Distribution (CCD) in Polyolefins.

CRYSTAF analyzes CCD of polyolefins during a crystallization cycle and TREF during a dissolution cycle.

In CRYSTAF the process is done in a single temperature ramp (crystallization step), while the polymer solution concentration is monitored by using an infrared detector.

In TREF the sample is first dissolved and then introduced into a column. The polymer fractionation occurs by deposition of layers of decreasing crystallinity, or increasing branch content, as temperature goes down.

TREF technique still requires a second temperature cycle to quantify each fractions and generate the CCD curve.

• CEF/TGIC

In a same instrument we can perform CEF or TGIC method.

CEF mode, Crystallization Elution Fractionation, is based on a new crystallization concept combining the power of CRYSTAF and TREF to get the separation of the different components of the polyolefin in significantly lower time.

High Temperature HPLC, also known as Thermal Gradient Interaction Chromatography (TGIC), has become recently an innovative technique for the analysis of polyolefins.

The TGIC technique uses a carbon based column to measure the composition distribution in polyethylene copolymers. This technique requires an adsorption step during the cooling and a desorption step with a heating.

• DLS - Dynamic Light Scattering and Zetasizer

DLS is used to determine the size distribution profile of small particles in suspension. The lab is equipped of a Malvern NanoZS and a Malvern NanoS90. The particle size range available is from 0,3nm to 10µm.

Zeta potential measurements are available with the NanoZS.

• Laser diffraction paricle size analyzer

Laser diffraction analysis use diffraction patterns of a laser beam to measure the size of particles from nanometers to millimeters. The lab is equipped of a Malvern Mastersizer 3000.

The particle size range available is from 40nm to 3,5mm.

Dispersions in water or dry powders can be both analyzed.

• Turbidimetry

Turbidimetry is the process of measuring the loss of intensity of transmitted light due to the scattering effect of particles suspended in it. The lab is equipped of a Formulaction Turbiscan Lab.

Different kind of destabilization mechanisms (creaming, sedimentation, flocculation, coalescence…) can be determined.

Particle size range available : from 10nm to 1mm. Concentrated latexes can be directly analyzed.

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• pH meters

The lab is equipped of several pH meters, classically from Mettler company. We can analyze aqueous solutions and latexes.

• Conductometer

The lab is equipped of a Metrohm conductivity module. Conductometric titration and conductimetry measurements are possible.

• Force Tensiometer

It’s used to measure the surface tension and interfacial tension of liquids. The lab is equipped of a Krüss Easy Dyne.

• Karl Fisher

Karl Fischer titration is the classical method for the determination of water content in liquid samples.