A review of experimental methods for solid solubility determination in cryogenic systems

Over the past years, there have been a number of serious explosions in air industry, which have resulted in workers injuries and fatalities. At the same time, there has been an increase in the use of air separation products for industrial activities.The quality of air entering an air separation plant is of crucial importance for its safe and reliable operation and the interest in the solubility data of solids in cryogenic liquid solvents is closely connected to the problem of impurities accumulation in the process plant and storage tanks. Such accumulations, especially in liquid oxygen, may cause fouling and blockage in heat exchangers and pipelines and they may eventually cause serious explosions. For this reason the air contaminants composition in liquid oxygen must be determined with great precision.This paper aims at reviewing experimental methods for determining the solubility of solid compounds that may be present in the cryogenic liquefaction processing of air distillation. A review of the literature data on solubility of solids in liquid oxygen and nitrogen is included as well.Emphasis is given to the difficulties in setting-up measuring apparatuses working at extreme conditions, i.e. low compositions and low temperatures.     

Equipment using a “static-analytic” method for solubility measurements in potentially hazardous binary mixtures under cryogenic temperatures

A new apparatus designed to study, at cryogenic temperatures, thermodynamic equilibria of potentially explosive binary systems such as hydrocarbon-oxygen mixtures is described herein. This equipment has an equilibrium cell which was especially designed to minimize hazards while allowing accurate phase equilibrium measurements. Reliability of results, obtained with this equipment has been verified by working on the nitrogen-propane system, for which data are already available in literature, over a large range of compositions and at various temperatures. Four isothermal curves describing liquid phase compositions at 109.98, 113.77, 119.75 and 125.63 K have been determined. Our experimental data are represented within 2% in compositions and in pressures through the Peng-Robinson equation of state implying Mathias-Copeman alpha function and Huron-Vidal mixing rule. Comparisons to literature allow pointing out: good agreement is observed with Kremer and Knapp data (1983) while the three sets of Poon and Lu data (1974) presenting systematic positive deviation are consequently judged as suspicious.     

Hardness and toughness investigations of deep cryogenic treated cold work die steel

In consideration of good results about the application of deep cryogenic treatment (DCT) on materials, the effect on the microstructure and properties (hardness, toughness and the content of retained austenite) of a new developed cold work die steel (Cr8Mo2SiV) was examined. The execution of the deep cryogenic treatment in different processes showed a varying effect on materials. It was shown that the hardness of the DCT specimens was higher (+0.5HRC to +2HRC) whereas the toughness was lower when compared with the conventionally treated specimens (quenching and tempering). Following the DCT process retained austenite transformed into martensite, however, not completely.     

Accidental release of hydrogen from a cryogenic tank

Liquid hydrogen at 20 K was harmlessly released at Turin’s Porta Susa station over a period of seven hours on 9 July 1991 through the safety valve of a dewar-type tank on a railway wagon following the loss of the vacuum between its two walls. Commercially available programs were unable to model this type of release in the unusual conditions in which this hydrogen had been stored. A model illustrating the course of the accident was therefore worked out. A start was made by examining the changes in the physical and thermodynamic properties of the hydrogen progress in the dewar to find out how long it had taken to build up the pressure needed to open the safety valve.Owing to the complex geometry of the insulating layer in the interspace of the dewar on which the liquefaction of the air took place, the heat exchange coefficient could not be determined a priori. It was therefore assumed and subsequently quantified by means of an iterative process. The thermodynamic data were then used to examine the outflow of the hydrogen from the venting line. Flow dynamic calculations showed that the hydrogen was entirely lost through the safety valve and that pressure losses along the approx. 3-m line were negligible. The model also showed that the speed of the outflow was subsonic. The speed evaluated will enable the dispersion of the hydrogen and hence the areas at risk to be evaluated in the subsequent stages of the study.     

Performance measurements of a 7 mm-diameter hydrogen heat pipe

A gravity assisted heat pipe with 7-mm diameter has been developed and tested to cool a liquid hydrogen target for extracted beam experiments at COSY. The liquid flowing down from the condenser surface is separated from the vapor flowing up by a thin wall 3 mm diameter plastic tube located concentrically inside the heat pipe. The heat pipe was tested at different inclination angles with respect to the horizontal plane. The heat pipe showed good operating characteristics because of the low radiation heat load from the surroundings, low heat capacity due to the small mass, higher sensitivity to heat loads (to overcome the heat load before the complete vaporization of the liquid in the target cell) due to the higher vapor speed inside the heat pipe which transfers the heat load to the condenser.     

Transient thermodynamic behavior of cryogenic mixed fluid thermosiphon and its cool-down time estimation

Thermosiphon is an efficient heat transfer device by utilizing latent heat of fluid at liquid-vapor phase change. One of the disadvantages of thermosiphon, however, is that the operational temperature range is fundamentally limited from the critical point to the triple point of the working fluid to maintain two phase state. Nitrogen (N₂) and tetrafluoromethane (CF₄) were selected as the mixed working fluid to widen their original operational temperature range. Thermodynamic behavior of mixture and its effect on the cool-down time were investigated. A simple calculation model was proposed to estimate the cool-down time of the thermosiphon evaporator prior to experiments. The calculated results agreed well with the experimental results within 5% error. The cool-down time reduction was not achieved by mixing two components at once due to the separation of mixture. One idea to avoid this problem was suggested in this paper where the estimated cool-down time was reduced 17.8% compared to pure N₂.     

A capacitance based axial position sensor for cryocoolers

The recent development of a Stirling cryocooler designed to operate with a body temperature of less than 220 K required an axial motor position sensor which could operate over this temperature range. Although linear variable differential transformers (LVDTs), have traditionally been used, these are temperature dependent and would have required development due to integrated electronics, which could not be used at these low temperatures. A sensor was therefore developed based on the principle of measuring the capacitance between static and moving concentric rings. The design is presented along with the signal conditioning circuit. Experimental results show that the sensor had suitable bandwidth with a temperature independent gain between room temperature and 220 K. Future developments are described including a similar sensor to measure the radial motion of a motor during operation.     

Mechanical tests of ATLAS Barrel Toroid tie rods

An installation has been designed and manufactured to test the tie rods of superconducting magnets of Atlas Barrel Toroid at tension load 2.5 MN (about 520 MPa maximum tensile stress) and with temperature gradient along the tie rod from 10 K to 270 K. All the 64 tie-rods have withstood the loading and remained in an elastic mode without any traces of plastic behavior.     

Development of a miniature cryogenic fluid circuit and a cryogenic micropump

This article presents the development of a miniaturized cryogenic fluid circuit for distributed cooling of low-temperature tracking detectors in high-energy physics (HEP). The heart of the circuit is a prototype cryogenic micropump. This volumetric pump is compatible with cooling powers of about 10-100 W, and capable of producing pressure heads of up to around 0.3 MPa. Besides detector and electronics cooling in HEP, potential applications are found in the field of superconductor technology.     

Dielectric coefficient and density of subcooled liquid oxygen

The results of high precision dielectric coefficient measurements of subcooled liquid oxygen in the temperature range from 56 to 91 K and under pressures up to 1 MPa are reported. The measurements are performed using a three-terminal flat plate capacitor and a single-frequency, ultra-precision capacitance bridge. Measurement results are combined with the previously published data in different pressure and/or temperature ranges to express the dielectric coefficient and the Clausius-Mossotti relation in an equation form. This new expression covers both the liquid and the gaseous state, and predicts the density of oxygen to better than 0.1% over the entire range of interest. The results reported in this paper are expected to be especially useful for capacitance-based measurements involving fluid oxygen such as liquid level and void fraction measurements of two phase flow.     

Capacitive level meter for liquid hydrogen

A capacitive level meter working at low temperatures was made to use in magnetic refrigerator for hydrogen liquefaction. The liquid level was measured from the capacitance between parallel electrodes immersed in the liquid. The meter was tested for liquid nitrogen, hydrogen, and helium. The operation was successful using an AC capacitance bridge. The estimated sensitivity of the meter is better than 0.2 mm for liquid hydrogen. The meter also worked with pressurized hydrogen.     

Absolute dynamic viscosity measurements of subcooled liquid oxygen from 0.15 MPa to 1.0 MPa

New absolute dynamic viscosity measurements of subcooled liquid oxygen are presented which were acquired in the pressure and temperature domains from 0.15 MPa to 1.0 MPa and from 55.20 K to 90.19 K, respectively. The measurements were acquired with an uncertainty of 1% at a 95% confidence level using a pressurized gravitational capillary (PGC) viscometer specifically designed for subcooled liquefied gases. The measurements are summarized by Arrhenius–Eyring plot parameters (μ = Ae^E/RT), and interpreted with respect to the chemical reaction rate theory of viscosity by Eyring. The Arrhenius–Eyring plot parameters reproduce the dynamic viscosity measurements with only a 2% RMS error, which is remarkable considering just two parameters are involved, A, the factor which includes the weak pressure dependence of the dynamic viscosity, and E/R, the barrier energy of the flow, where R is the universal gas constant. Although the Arrhenius–Eyring plot parameters do not have a discernible pressure dependence in the present work, the pressure coefficient versus temperature for the dynamic viscosity was determined from line plots of the dynamic viscosity versus pressure. The pressure coefficients suggest that the pressure dependence is very weak, yet positive, and increases with decreasing temperature. Measurements at pressures an order-of-magnitude higher are required to confirm this suggestion.     

Real gas choked flow conditions at low reduced-temperatures

Real gas choked mass flux is calculated for a frictionless stream expanding isentropically until it reaches the speed of sound and without phase changes. The other parameters associated with the choked state are the pressure, density, temperature ratios, and the speed of sound. Departure of the choked mass flux from the ideal gas model is discussed first in absolute terms and then in relative terms, using the Principle of Corresponding States, for gases with boiling points in the low temperature range. Reduced-stagnation pressures are examined up to values of 30 for hydrogen, neon, nitrogen, argon, methane, krypton, xenon, and R-14 and up to 100 for ⁴He. The corresponding reduced-stagnation temperatures go down to 1.4 and in some cases down to 1.2 for nitrogen and argon. Also discussed are the limiting values of stagnation parameters for which no phase change occurs in the choked state. Compared to the ideal gas, the mass flux may almost double and the critical pressure ratio may decrease by an order of magnitude. The relevance of results is discussed qualitatively and quantitatively for Joule-Thomson cryocooling.     

High-pin density feedthrough for superfluid helium applications

A vacuum tight high-pin density feedthrough for use in superfluid helium has been developed. The design and construction based on commercially available Framatome connectors is described.     

Thermal conductivity of subcooled liquid oxygen

The thermal conductivity of liquid oxygen below 80 K and pressures up to 1 MPa has been measured using a horizontal, guarded, flat-plate calorimeter. The working equation of the calorimeter is based on the one-dimensional Fourier’s law. The gap between the calorimeter plates was measured in situ from a capacitance measurement. The cooling power to the calorimeter is provided by a two-stage Gifford-McMahan cryocooler. The absolute temperatures are measured using platinum resistance thermometers. The results are compared to existing data and analytical models.     

Visualization for heat and mass transport phenomena in supercritical artificial air

A laser holography interferometer is applied to investigate heat and mass transport phenomena around the pseudo-critical line of supercritical artificial air with a composition of 79% nitrogen and 21% oxygen. In a previous study, we successfully observed the heat transport phenomenon, the piston effect, around the pseudo-critical line of nitrogen. The same experimental set-up is applied to the supercritical artificial air, which is a compressible binary mixture fluid. We attempt to suppress the generation of natural convection, and successfully observe the heat and mass transport phenomena, which are the soret effect and the piston effect, respectively. Here, we discuss these effects observed in the supercritical artificial air.     

A very light and thin liquid hydrogen/deuterium heat pipe target for COSY experiments

A liquid hydrogen/deuterium heat pipe (HP) target is used at the COSY external experiments TOF, GEM and MOMO. The target liquid is produced at a cooled condenser and guided through a central tube assisted by gravitation into the target cell. An aluminum condenser is used instead of copper, which requires less material, improves conductivities and provides shorter cooling down time. Residual condenser temperature fluctuations in the order of ≈0.4 K are reduced by using thermal resistances between the cooling machine and the condenser of the heat pipe combined with a controlled heating power. A new design with only a 7-mm-diameter HP has been developed. The diameter of the condenser part remains at 16 mm to provide enough condensation area. The small amount of material ensures short cooling down times. A cold gas deuterium HP target has been designed and developed which allows protons with energy ?1 MeV to be measured. A 7-mm-diameter HP is used to fill a cooling jacket around the D₂ gas cell with LH₂. The D₂ gas is stabilized at 200 mbar to allow for thin windows. Its density is increased by factor 15 compared to room temperature.     

Visualization techniques applied to thermo-fluid phenomena in cryogenic fluids

A variation of visualization techniques such as Shadowgraph, Schlieren and holographic interferometry, has been so far applied to visualize thermo-fluid phenomena in cryogenic fluids, superfluid helium (He II) and supercritical nitrogen, by some researchers. This paper is a review of these visualization techniques used in cryogenic fluids as well as an introduction of visualization techniques.     

A new apparatus for mechanical Q-factor measurements between 5 and 300 K

Today’s laser interferometric gravitational wave detectors are sensitivity limited by thermal noise of the optical components within the detection band of about 0.1-1 kHz. Cooling down these parts to cryogenic temperatures is a promising technique to increase the sensitivity of the gravitational wave detectors by at least one to two orders of magnitudes. Cooling substantially increases the material Q-factor contributing to reduced thermal noise. This article describes a new cryogenic apparatus which allows the measurement of the mechanical Q-factor - as a measure of internal losses - in a temperature range from 5 K up to 300 K. The requirements for cryogenic Q-factor measurements and their realization are shown. The measuring technique as well as the key parameters are discussed. Exemplary, measurements on crystalline quartz and silicon (1 0 0) are given to characterize the setup.     

Fracture and deformation properties of Ni-Fe superalloy in cryogenic high magnetic field environments

The present paper includes experimental and analytical data on the fracture properties of a nickel-iron superalloy, a ferromagnetic austenite, at 4 K in magnetic fields of 0 and 6 T. The tensile, notch tensile and small punch tests are employed. A finite element analysis is also performed to convert the experimentally measured load-displacement data into useful engineering information. To interpret the results we review the available theory of the influence of magnetic field on the stress intensity factor for a crack in ferromagnetic materials.