Combined High Temperature Surface Tension and Density Measurements

Ph.D. Research Project

Explore the posibility of using the Maximum Bubble Pressure method for simultaneous Surface Tension and Density Measurements of molten salts.

Overview

Most density and surface tension measurements have an interdependency between both properties. Even so, typically measurements are made separately, with correction terms to account for other properties. As such, error accumulates when one or the other is not properly accounted for. Due to the difficulties of making these measurements with molten salts, few efforts have been made to measure them congruently. This project aimed to tackle this issue by utilizing the maximum bubble pressure method. This method is easily adapted for measuring both properties, and an experimental system was developed for high-temperature use with molten salts. The components of the system are derived from former experiments at both room and high temperatures, with adaptations to accomidate with the Glove Box Furnace:
Bubbling tube positioning assembly with thermocouple and electrical reference wire for locating the surface of the fluid.

Low flow rate gas line control

Data acquisition and analysis

Room temperature validation experiments
Maximum Bubble Pressure Method Experimental Setup

Bubbling Probe Assembly

The full assembly (After several uses) where the bubbling tube is attached to a micro-screw for precice control when identifying the top surface of the fluid. It is used by with the reference wire to complete an connection between the tube, fluid and wire in order to judge when the tube touches the surface.
Micro-screw adjustable tube

Flange mounting assembly with alumina tube base

Electrical reference wire

Thermocouple that moves with the end of the bubbling tube for precise temperature measurements
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Room Temperature Validation

The method was tested at room temperature using water. This was done to check the bubble forming behavior was appropriately sphereical, and to verify there was no interference from other components.
Average Density Error: 0.66% at 68C

Average Surface Tension Error: 2.52% at 68C

Clean repeatable bubble formation
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High Temperature Density

Density is determined by the slope of the maximum bubble as a funciton of depth. Measurements show agreement between former studies for both salts tested as a funciton of temperature. Specifically with FLiNaK (considered a reference salt) the agreement is highest with studies (Rose, An, Barbork) where density and surface tension are considered together.
Reasonble but higer then desired error of up to 20%.

Strong agreement in trend with respect to temperature.

Strong agreement with magnitude with respect to temprature.
Electronic Circuit
Data Collection

High Temperature Surface Tension

Surface tension measurements however show less agreement compared to density. This is most likely because of interactions that occured at high temperature between the salt, gas and bubbling tube. These interactions cause chemical instubiliites, and most likely effected maximum pressures. Another possiblity is the flow rate may have effected results, as seen in the NaF-ZrF4 surface tension plot.
Similar Magnitude to limited former studies

Similar error to density (20%)

Shows deviation, but this could also be associated with the joint density-surface tension method
Electronic Circuit
Data Collection