Instrumentation at Ugelstad Laboratory

 

NANO ITC 2G (Isothermal Calorimeter)

Isothermal Calorimeter (TA Instruments, USA) is a thermodynamic technique that directly measures the heat released or absorbed during a molecular binding event.  The ITC is used to determine thermodynamic parameters such as enthalpy (∆H) and equilibrium constant. More particularly the application include the study of interaction between components and the determination of self-association properties of different molecules. 

 

Quartz Crystal Microbalance, QCM-Z500

The KSV QCM-Z500 microbalance (KSV Instruments Ltd., Finland)   is a computer controlled quartz crystal microbalance based on impedance analysis for determining the frequency (f) and the quality of resonance (Q) of quartz crystals in a gaseous or liquid environment. In other words, it is a mass sensing device with the ability to measure very small changes in mass on a quartz crystal resonator in real-time. The technique also determines viscoelastic properties of surface bound layers. The QCM is used to study molecular interactions and molecular adsorption to solid surfaces in our lab. 

 

Brewster Angle Microscope

The KSV Optrel BAM300 (KSV Instruments Ltd., Finland) BAM – Brewster Angle Microscopy, is a special technique for investigation of organic thin films – Langmuir films. KSV Optrel BAM 300 is a laser powered, CCD video camera imaging microscope for real-time observation of Langmuir films on air/water interfaces or on dielectric substrates. Live video recording to the lateral resolution of 1 microns at speed of up to 25 images/sec can be seen on PC screen while data is recorded to the hard disk.  Compared to other characterization methods KSV's BAM technique provides more powerful and economical means for non-invasive (non-contact) study of your thin films. 

 

Quartz Crystal Microbalance (QCM)

The Q-sense D300 QCM (Q-Sense AB, Sweden) is used to study molecular interactions and molecular adsorption to solid surfaces. The technique determines masses and viscoelastic properties of surface bound layers. 

 

Langmuir-Blodgett Minitrough

The Langmuir-Blodgett Minitrough (KSV Instruments Ltd., Finland) is used to determine film properties of monolayer films at a liquid surface or interface (Langmuir films) and for deposition of mono- or multilayer onto solid substrates (Langmuir-Blodgett films).

The surface pressure is determined through the Wilhelmy-plate method and the surface area is controlled by two symmetrically moving surface barriers. Applications are studies of asphaltene-resin films, their film structure and strength, and mixed films composed of proteins and lipids related to biochemistry.

 

The Fluorescence Microscope (Nikon LV 100D)

The Fluorescence Microscope (Nikon LV 100D) acts as a normal microscope, but in addition has the ability to display only fluorescent species in the sample. The technique can be used to directly determine the partitioning and local concentration in an emulsion of fluorescent molecules, for example asphaltenes or resins, and particle - polymer interactions by use of energy transfer (FRET).

The microscope is equipped with a MicroPublisher 5 MP color camera with Firewire connection for image capturing."

 

Digital Video Microscope (DVM)

The Digital Video Microscope (Scan Imaging) consists of a Nikon Eclipse ME600 microscope fitted with a CoolSNAP-Pro camera by Media Cybernetics. It is used to study properties of emulsions. Parameters of special interest are droplet size distributions, droplet concentration, droplet geometry and droplet interactions (flocculation and coalescence). It can also be used to study wax precipitation and micellar and liquid crystal behavior.

 

Atomic Force Microscope (AFM)

The Veeco diCaliber Atomic Force Microscope is used to map the surface topography of substrates and deposited layers (Å - mm scale). Ugelstad Laboratory has an atomic force microscope (AFM) for imaging surface morphology and measuring surface physical properties. Imaging is available in TappingMode (PhaseImaging with integrated I/O modulation plus board) for soft samples and contact mode for hard samples. Precise adhesion measurements can also be performed with the AFM.

 

Plasma Chamber

The Plasma Chamber (MKS Instruments) is used for chemical modification of surfaces by means of a glow-discharge. Functional groups can be implanted or thin films deposited onto the substrate.

 

KF Coulometer 831

The KF Coulometer 831 (Metrohm) is used for accurately determining of very small amounts of water in petrochemicals.

 

Malvern Zetasizer 3000HS

Malvern Zetasizer Nano ZS (Malvern Instruments, UK) is used to study the particle size and zeta potential, and molecular weight of dispersions, emulsions, gas hydrates and so on. The connection of a titrator allows automated determination of the iso-electric point, pH and conductivity. The software also allows you to program Standard Operating Procedures and precise temperature control for accurate measurements.

 

Malvern Zetasizer Nano ZS


The Zetasizer Nano ZS is a high performance two angle particle and molecular size analyzer for the enhanced detection of aggregates and measurement of small or dilute samples, and samples at very low or high concentration using dynamic light scattering with ‘NIBS' optics. The connection of a titrator allows automated determination of the iso-electric point, pH and conductivity.

The instrument applies a known electrical field and measures how fast the particles move in a liquid-i.e. the velocity; using this as well as viscosity and dielectric constant the software calculates the zeta potential. 

 

CAM 200 - Optical Surface Tension/Contact Angle Meter equipped with high-speed camera

CAM 200 (KSV Instruments Ltd., Finland) is a video camera-based contact angle meter for measurements of static or dynamic contact angles. Furthermore, surface & interfacial tension measurements can be performed using the pendant drop or raising drop technique. This unit is equipped with a FireWire camera module for measuring 100 images/second.

 

Critical Electric Field Emulsion Stability Cell

This is a method for testing emulsion stability for "stable" water-in-oil emulsions. An electrical field is applied to an emulsion and the electrical field is steadily increased while the current that passes through the sample is continuously measured. The critical electric field is defined as the electric field necessary to achieve a sudden increase in the current. E-crit has been developed at NTNU.

 

Millipore Simplicity® Personal Ultrapure Water System

The Simplicity® system (Millipore) produces water virtually free of organic and inorganic contaminants; the produced water is then suitable for applications such as buffer preparation for liquid chromatography instruments, preparation of solutions for spectrophotometry, spectroscopy, or other analytical techniques and biochemical experiments. 

 

Analytical HPLC

The high performance liquid chromatograph system is mainly used to determine the concentrations of naphthenic acids with methodology developed at Ugelstad Laboratory. The system is built from the following modules (Shimadzu): two pumps, a degasser, a gradient mixer, an auto-injector, a column chiller/heater, an UV/vis detector and a fluorescence detector. The separation is based on affinity chromatography.

 

TriStar 3000 Gas Adsorption Analyzer

The TriStar 3000 (Micromeritics Instrument Corporation, USA) provides high-quality surface area and porosimetry measurements on solid materials by using the technique of gas adsorption.

The instrument is used for measuring surface area, pore size, pore volume and the hysteresis loops of mesoporous catalytic materials, and for adsorbents in general. 

 

Carbolite - High Temperature Furnace

The Carbolite BWF 11/13 high temperature furnace (Carbolite) is used for calcination and sintering.

 

Fourier-Transform (Mid) Infrared Spectrophotometer

The Tensor 27 (Bruker Optics) has a spectral range from 7,500 to 370 cm-1 with a standard KBr beamsplitter. In order to allow for collection of mid-IR spectra of non-diluted crude oils as well as solid samples, the instrument is equipped with a Bruker Golden Gate diamond ATR (Attenuated Total Reflection) cell. The instrument has an interface with the HPLC for analysis of crude oil fractions. In addition, the instrument can be operated separately with an ATR or flow cell.

 

Fourier-Transform (Near) Infrared Spectrophotometer

The Multi Purpose Analyzer (MPA) (Bruker Optics) has a spectral range from 12,800 to 4,000 cm-1, which allows for spectral characterization in the near-infrared regime. The instrument is used for analysis of crude oil components and studies of particle growth. 

 

UV-vis Spectrophotometer

The UV-2401PC (Shimadzu) has a single monochromator system with a spectral range from 190-1100 nm, and is equipped with a TCC-240 temperature control unit (7-600C), and an ISR-240A Integrating sphere attachment for diffuse and total reflectance measurements from liquids and solids in the range from 240-800 nm. The low stray light/wide dynamic range/small beam size combination makes this instrument well suited to handle a variety of practical situations.

 

Maran 23 MHz PFG NMR

The Oxford Instruments Maran Ultra is used to study self-diffusion, droplet size distributions and emulsion stability of w/o emulsions (o/w inversion phenomenon). 

 

Horiba Jobin Yvon LabRam High Resolution Raman Microscope

The LabRAM HR800 system provides ultra-high spectroscopic resolution and a unique wavelength range capability that provides both great flexibility and high performance. It is an integrated, simple to use, and high stability bench-top instrument designed to undertake reproducible Raman measurements at various spectral resolutions. The high resolution mode is uniquely ideal for the precise characterization of position and shape of bands of spectra of crystalline and amorphous materials e. g. oxide catalysts and carbon nanomaterials. The instrument can be used also for samples mapping (using confocal microscope and motorized stage) and for liquids analyzing (with remote fiber optic head).

(UV, VIS, NIR operation)   T

 

Density/Concentration Meter - DMA 5000 M

The DMA 5000 (Anton Paar Ltd.) density meter is used for measuring the density of solutions.

Features:

  1. Density range - 0 to 3 g/cm3
  2. Permanently stored specific gravity/concentration conversions:
    - Alcohol tables

    - Extract/sugar tables
    - API functions
    -Acid/base tables
  3. 20 tables/equations for your own concentration conversions.

 

Vertical Gravity Separator

Vertical gravity separator is an approach to investigate the differences between the emulsion stability found in batch tests and the stability found with the same fluids in a continuous system under steady state.

The advantage of the vertical setup is its low volume, approximately 12 litres for this system. Two progressive cavity pumps, one for oil and one for water are used to pump liquid from the feed separator (the bigger column). The streams are mixed before they enter the control valve in front of the test separator. The valve will create an emulsion if the differential pressure (DP) is large enough. Choking the valve gives higher DP and smaller droplets. The test separator can then be used to study the emulsion layer at different water cuts, droplet sizes, concentrations and other relevant parameters and compare with conventional batch tests.

 

Rheometer Physica MCR 301

The Anton Paar Physica MCR 301 rheometer in our lab is used to analyze structural properties (i.e.viscosity, storage and loss modulus) of liquids, dispersions, emulsions and so on.

 

Horiba Jobin Yvon Fluorolog-3 fluorometer with TCSPC attachment
 

Features:

  •  World's most sensitive spectrofluorometer
  •  Can detect 50-femtomolar fluorescein
  •  Unique, modular system
  •  Interchange wide range of computer-controlled accessories: spectrometers, detectors, sources, and more!
  •  Totally computer-controlled
  •  All-reflective optics

Applications are aggregation state of high-molecular weight components related to crude oil precipitation, concentration determination at below ppm levels and protein-lipid-nanoparticle interactions in aqueous environments.

 

Turbiscan Lab Expert

The Turbiscan Lab Expert (Formulaction) measures transmission and backscattering from dispersions (concentrated and dilute) as a function of time and relative vertical (y-axis) sample coor-dinates. This allows for determination of mean size, stability and shelf-life in real (unmodified) systems.

 

KSV Interfacial Shear Rheometer ISR 400

(KSV Instruments Ltd., Finland) Quantitative measurement of shear stress at fluid interfaces has long eluded researchers employing standard rotational rheometers, particularly at very low viscosity or elasticity.

With the introduction of the Interfacial Shear Rheometer (ISR 400), KSV removes the guesswork. A teflon-coated magnetic needle is floated in a half-cylinder at the gas/liquid or liquid/liquid interface, and moved with an applied magnetic field. The movement of the needle is observed microscopically, and the difference between applied force and measured position provides phase shift, viscosity, elastic and loss moduli, creep and relaxation times. Since the KSV Interfacial Shear Rheometer (KSV ISR 400) can be integrated with a standard KSV Langmuir trough, these measurements can be applied to both soluble and insoluble films.

 

Metrohm 809 Titrando titration device(TAN)

The Titrando unit from Metrohm consists of a magnetic stirrer, a dosing device and a suitable electrode. It is used to determine the total concentration of acids (TAN) or bases (TBN) present in a sample, by titration.

 

pH Meter

The pH meter (Mettler Toledo) is used to measure pH in solutions. The measurement is based on the activity of hydrogen ions.

 

Laborota 4003 Rotavapor

The Laborota 4003 Rotavapor (Heidolph Instruments) is used to separate liquids by adding vacuum and heat.

 

Inolab Cond Level 2, Conduct Meter

The Inolab Cond Level 2, Conduct Meter (WTW Wissenschaftlich-Technische Werkstätten GmbH) is used to measure conductivity. The analysis based on the ability a solution has to conduct electricity.

 

Coldfinger

The coldfinger (developed at NTNU) is used to obtain paraffin deposits on various surfaces from waxy crude oils. The device consists of a temperature controlled cylindrical vessel with rotational flow provided by an overhead rotating motor.  Laminar and turbulent mixing conditions are provided by a rotating cylinder or impellar, espectively.  Deposits are formed on a coupon mounted on the side wall, in thermal communication with a coolant fluid.  Currently, the coldfinger is limited to shearing rates less than or equal to 602 inverse seconds.

Applications include:

1.         The effect of Heat, Mass, and Momentum      Transfer Conditions on Deposition Rates
2.         Micro-crystalline Wax Deposition
3.         Macro-crystalline Wax Deposition
4.         Polymeric Inhibitor Evaluation

 

Sinterface PAT-1 tensiometer

The Drop and Bubble Shape Tensiometer PAT-1 from Sinterface (Germany) allows to measure the surface and interfacial tension of liquids by the analysis of the shape of pendant and sessile drops or buoyant and captive bubbles. By measuring the surface and interfacial tension as a function of time, the kinetic of adsorption of surfactants at the liquid/air or liquid/liquid interfaces can be studied.

The rheological properties of the interface (elasticity and viscosity) can also be determined by subjecting the drop to periodic oscillation of their volume and measuring the induced variations of surface/interface tensions.

 

Thermal Gradient Quartz Crystal Microbalance

The Thermal Gradient Quartz Crystal Microbalance (TG-QCM) was developed jointly by NTNU and KSV Instruments (Helsinki, Finland).  The TG-QCM is used to determine the mechanism of incipient wax deposition on various surface materials. 

The apparatus consists of a quartz crystal which is mounted in direct fluid contact with a flow chamber.  The quartz crystal is in thermal communication with a cold mass, and warm waxy oil is pumped through the chamber.  Thereby, the TG-QCM is able to emulate the heat, mass, and momentum transfer conditions associated with wax deposition in oil transportation pipelines. 

The apparatus consists of a quartz crystal which is mounted in direct fluid contact with a flow chamber.  The quartz crystal is in thermal communication with a cold mass, and warm waxy oil is pumped through the chamber.  Thereby, the TG-QCM is able to emulate the heat, mass, and momentum transfer conditions associated with wax deposition in oil transportation pipelines.  Measured electromechanical oscillation parameters provide information regarding the deposition mechanism.  Surface crystallization is evidence by uniform reductions in normalized resonance frequencies associated with the 3rd-11th harmonic overtones.  Gel adherence is evidenced by increases in energy dissipation factors associated with the 3rd-11th harmonic overtones.

Applications include:
1.    Investigating the mechanism of wax deposition from macro-crystalline and micro-crystalline wax.
2.    Investigating the effect of heat transfer on    the wax deposition mechanism.
3.    Polymeric inhibitor evaluation
4.    Investigating incipient wax by deposition from o/w and w/o emulsions.

 

SARA HPLC

The high performance liquid chromatograph system (Shimadzu) is used for fractionation of deasphaltenated crude oil into saturates, aromatics and resins. The automated procedure can be done either analytically or preparative. The instruments setup offers logging of UV-(dual mode) and RI-signals as well as fraction collection from these signals.

 

Bubble Pressure Tensiometer BP100

Bubble Pressure Tensiometer BP100 from Krüss (Germany) allows to measure the dynamic surface tension at constant or variable surface age (from 5 ms (high dynamic) up to 100 s (almost static)).

The instrument provides fully automatic measuring process by software controlled immersion of the capillary. Thanks to its built-in compressor the instrument does not need an external compressed air connection. A high-precision pressure sensor  determines the maximum pressure during bubble formation, from which the surface tension is calculated.

In addition to the time-dependent surface tension, the measurement also supplies the equilibrium value according to Hua & Rosen. Diffusion and adsorption coefficients can be calculated from surfactant concentration series – these are important parameters where the mobility of surfactants is concerned. 

 

Tensiometer

The Sigma 70 tensiometer (KSV Instruments Ltd., Finland) is used for determination of:

• Surface tensions

• Interfacial tensions

• Contact angles

• Wettability of powders

• Critical micelle concentrations

The principle of this instrument is force measurements by an electrobalance as a probe (Du Nouy ring, Wilhelmy plate, sample holder, etc.) is immersed and withdrawn from liquids. 

 

Spin Drop Video tensiometer (SVT 20)

The SVT 20 (DataPhysics Instruments GmbH, Germany) enables us measuring fluid/fluid interfacial tensions down to ultralow values. The method is based on the longitudinal deformation of a fluid bubble inside a heavier liquid in a capillary tube rotated at high velocities. By observation of the drop shape with a high resolution CCD camera the interfacial tension between the two fluids is calculated with high accuracy from mathematical models taking rotation speed, the fluids densities and temperature into account. At our laboratory this method is currently used for characterizing oil/brine/surfactant systems within a project on enhanced oil recovery. The lowest values measured with the SVT 20 at Ugelstad were in the area below 10-5 mN/m, quiet close to the limit of 10-6 mN/m which is given by the producer.

 

Q2000 Differential Scanning Calorimeter 

Name: TA Instruments Q2000 Differential Scanning Calorimeter

Purpose:  Materials and Fluid Characterization, Heat Flow Measurements, Crystallization, Precipitation, Protein Folding, Enthalpy Measurements, Asphaltene Precipitation Kinetics, Model Hydrate Formation Kinetics, Paraffin Wax Analysis, Amorphous/crystallinity determination
General Usage Areas: Polymers, Colloids, and Petroleum

 

Q600 Thermogravimetric Analyzer with DSC

TA Instruments Q600 SDT Thermogravimetric Analyzer with DSC

Purpose: Materials and Fluids Characterization, Thermal Stability, Film Stability, Oxidation Processes,  PPD/YPD Stability Qualification, Surfactant Stability Assessment, Asphaltene Pyrolysis, Demulsifier Stability Analysis, KHI/AA stability analysis, PolymerGeneral Usage Areas: Polymers, Colloids, and Petroleum

 

VASCOTM partical size analyser


VASCOTM particle size analyser (Cordouan Technologies, French) is a unique laboratory instrument for nano to micro particle size measurements in liquid with particle size range from 1 nm to 6000 nm. It can be used for the investigation of Ink, polymers, metallic oxide nanoparticles, micellar dispersions, etc. The instrument principle relies on Photon Correlation Spectroscopy (PCS) also called dynamic light scattering (DLS). Compared to conventional particle size analysers, the VASCO original optical design allows quasi-instantaneous measurements in dark and concentrated solutions without sample dilution or filtration. Powerful data collection and analysis is provided by the proprietary software nanoQ™.