Lab Facilities

Differential Scanning Calorimeter

In our lab, we employ the sophisticated Setaram μDSC7 Evo Differential Scanning Calorimeter to unravel the complexities of wax precipitation in oils under varying pressures. This state-of-the-art instrument is central to our determination of critical parameters such as the Wax Appearance Temperature (WAT), Wax Dissolution Temperature (WDT), and the characteristics of wax samples extracted under different conditions. Our DSC apparatus boasts a highly precise two-stage temperature control system, with a broad range extending from -45 °C to 120 °C. This range enables us to execute both cooling and heating cycles at rates from 0.001 °C/min to 2 °C/min, thanks to the integration with a high-performance Julabo chiller. To accommodate our high-pressure studies, the DSC is equipped with robust cells. These cells are versatile, capable of withstanding pressures up to 400 bar for low-pressure applications, and scaling to the demands of high-pressure scenarios of up to 1000 bar.

Schematics of the μDSC apparatus.

Rheometer

At our lab, we are equipped with the advanced Anton Paar Modular Compact Rheometer Series MCR 302, a critical instrument that allows us to meticulously characterize the rheological properties of oils. This sophisticated piece of equipment is vital in our determination of oil viscosity, gelation temperature, and yield stress, which are essential parameters in understanding and predicting the behavior of oil under various thermal and stress conditions.

Our MCR 302 rheometer enables precise measurements across a wide range of conditions. It has the capability to cool samples down to -50°C and heat them up to 200°C, which is instrumental in simulating and studying the thermal effects on oil properties. The equipment’s torque capacity spans from a delicate 0.5 Nm to a robust 230 Nm, catering to a broad spectrum of fluid viscosities and characteristics.

Schematics of the Rheometer.

Cross polarized microscope (CPM)

In our lab, the intricate crystallographic properties of oil including crystal size, shape, and number density are meticulously examined using the BH200-MR series cross-polarized microscope from AmScope. This high-caliber microscope is outfitted with magnification lenses ranging from 4x to 50x, enabling us to conduct a detailed and precise analysis at multiple scales.

To complement and enhance the capabilities of our microscope, we have integrated the Instec TS102S Peltier thermal stage. This thermal stage boasts a versatile temperature range from -25°C to 90°C and accommodates microscope slides in its 24mm x 75mm sample area. Further extending our analytical precision, this thermal stage is connected to a C100W benchtop chiller, providing the additional cooling power needed for the thermal plate. It operates by cycling water through an internal reservoir with a volume of 860 ml, thereby maintaining a consistent and optimal cooling environment.

Schematics of CPM.

Cold Finger

Our lab utilizes a specialized cold finger setup to conduct in-depth investigations on paraffin deposition. This crucial study aids us in identifying key characteristics of paraffin such as wax content, critical carbon number. The core of our setup is a jacketed vessel with a capacity of 1000 ml and an internal diameter of 101.6 mm, perfect for accommodating substantial sample sizes. The cold finger probe, integral to our setup, has an outer diameter of 171 mm and a length of 90 mm. Both the jacketed vessel and the cold finger probe are connected to two independent water baths. These water baths offer a wide operating temperature range from -20°C to 120°C, providing us with the flexibility to explore paraffin deposition under various thermal scenarios. To ensure thorough mixing and interaction within the vessel, we have positioned it atop a 2mag luMIX magnetic stirrer. This stirrer boasts a broad speed range from 100 to 2000 RPM and has a maximum stirring capacity of 2000 ml, allowing us to simulate dynamic fluid movements akin to those found in pipeline systems.

Cold Finger Apparatus.

Flow loop

In our lab, we utilize a flow loop system to conduct paraffin deposition experiments. The flow loop, stretching over 11 meters in length and featuring a 1-inch diameter, comprises multiple sections including an acrylic part for visual monitoring, a copper segment for the return flow, and a stainless-steel section specifically designed for testing. Central to the system is a 25-liter stainless steel tank, equipped with a heating jacket that ensures the temperature within the tank is precisely maintained. The Chromalox microTHERM CMX temperature controller, which doubles as a heater and pump, propels the model oil through the system at rates up to 20 kg/min, roughly equivalent to 25 L/min. The accuracy of our flow rate measurements is guaranteed by a Coriolis mass flow meter from Emerson, which also records temperature and density. Temperatures are recorded before and after the test section, with the aid of three thermocouples strategically placed to measure the top, side, and bottom of the section. Furthermore, any pressure differences from the inlet to the outlet of the testing section are captured by a Rosemount pressure drop transmitter, ensuring we have a complete understanding of the flow conditions. Our testing section mimics the actual conditions of a pipeline environment, with a 1-inch diameter steel pipe, one meter in length. This section employs a pipe-in-pipe design where the external coolant flow replicates the seabed temperature, controlled by a PolyScience chiller. This chiller is pivotal in regulating the coolant’s flow rate, temperature, and the rate of cooling or heating. All of these vital measurements are fed into a DAQ system, which interfaces with a custom LabView program, enabling us to record and analyze experimental data.

Schematics of the Flow loop.

Batch Crystallizer

Our lab has an in-house designed 150 ml batch crystallizer made up of 316 SS with a pressure rating of 100 bar. The crystallizer has acrylic viewing windows on two faces, each with a diameter of 30 mm. A Polyscience refrigerated chiller with a temperature range of -10 °C to 40 °C is employed to cool the crystallizer. The set up is equipped with pressure transmitter and an analog pressure gauge to measure pressure and thermocouple for temperature measurement. A DAQ system with Labview interface on a computer is used to record the data.

This system can be used to measure thermodynamic phase equilibrium, morphology of hydrate crystals and kinetics of hydrate formation.

Batch Crystallizer Setup.

Semi Batch Crystallizer

Our lab has an in-house designed 1000 ml crystallizer made up of 316 SS with a pressure rating of 100 bar. A 1000 ml gas reservoir or supply vessel is connected to the crystallizer via a control valve. A Polyscience refrigerated chiller with a temperature range of -10 °C to 40 °C is employed to cool the crystallizer and the supply vessel. The set up is equipped with pressure transmitter and an analog pressure gauge to measure pressure and thermocouple for temperature measurement. A motor-powered stirrer is attached to the top flange of the crystallizer. The control valve is operated using a PID controller. A DAQ system with Labview interface on a computer is used to record the data. This facility has state of the art capabilities to perform batch and semi-batch experiments.

This system can be used to measure kinetics of hydrate formation and dissociation and can be operated as fixed bed reactor or stirred tank reactor.

High-pressure prototype reactor

Our lab has a custom-built high-pressure prototype reactor to demonstrate hydrate-based desalination. The setup consists of a gas reservoir, reactor, data acquisition system, and temperature control system. The crystallizer is designed explicitly with inbuilt cooling channels and glass windowpanes on the sides to observe hydrates growth. The crystallizer has a stirrer with two impellers to mix the liquid and gas phase at desired rpm. Two omega thermocouples with a temperature range of 0 to 1500 °C are used to measure the liquid and gas phase temperatures. A stainless-steel pipe (diameter of 2 inches) is fitted with mesh and a 2” ball valve below the discharge section. A mesh of sizing 20 at the bottom of the reactor separates hydrates formed in the reactor from the water. A pneumatic valve (CV) connected to a PID controller maintains the reactor pressure constant by supplying gas from the gas reservoir during experiment. A Polyscience refrigerated chiller with a temperature range of -10 °C to 40 °C is employed to cool the crystallizer and the gas reservoir. A DAQ system with Labview interface on a computer is used to record the data.

Schematics of the High-pressure prototype reactor.