Monitoring and control system design for a 13C isotope separation 3-

column cascade

Cristina I. Muresan, Clara M. Ionescu, Eva H. Dulf, Roxana Both

Technical University of Cluj-Napoca, Dep. Of Automation, Gh. Baritiu Street, no.26-28,
400027 Cluj-Napoca, Romania; tel. +40 264 401821, e-mail: cristina.pop@aut.utcluj.ro;

The 13C isotope enriching process has experienced an increased interest due to its use in
the diagnosis of several diseases or as tracers in various research domains. A common
solution for 13C separation is the cryogenic distillation process of high-purity carbon
monoxide (CO) in a dedicated column, with a condenser at the top for producing the liquid
downstream, a boiler at the bottom to produce the vapour upstream and an efficient thermal
insulation since the distillation occurs at about -194°C. In Romania, at the National Institute
for Research and Development for Isotopic and Molecular Technologies Cluj-Napoca, such a
column was designed and built, initially with pure scientific aims, which further allowed for
an industrial use, in which the 13C concentration was raised up to 9.5%. Such research results
prove to be highly useful since no European centre “produces” this isotope and current
literature studies do not present any scientific/ technological data about the industrial structure
and/or operation of the separation equipment for 13C. However, since the demand for 13C is
especially directed towards a compound that has a much greater concentration, up to 90%, a
3-column cascade is build, with the schematic representation given in Figure 1.
For a proper operation of the cascade a
dedicated monitoring and control system is
designed using LabVIEW, in which the
monitored parameters are: the top and
bottom pressures in each column, the liquid
nitrogen level in the unique condenser, the
feed flow into the first column, the
intermediary flows between the 3 columns,
the waste flow from the first column, the
product flow from the third column, the
electrical powers supplied at each of the
three columns’ boilers and the three liquid
CO levels in the columns’. In order for the
Figure 1. Schematic representation of the cascade to operate efficiently, the top and
3-column 13C cryogenic isotope separation bottom pressures and the liquid CO levels at
cascade with the monitored parameters the boilers need to be kept at their
prescribed setpoints.
This is achieved by manipulating the control inputs: the flows between the columns, the
feed, waste and product flow, as well as the liquid nitrogen level and the electrical powers.
The experimental results show that using the proposed monitoring and control system the 3-
column cascade may be kept at an optimal operation point.
References (Partial list):
1. Pop, C.-I., Ionescu, C. M., De Keyser, R. (2012), Time delay compensation for the
secondary processes in a multivariable carbon isotope separation unit, Chemical
Engineering Science, vol. 80, pp. 205-218
2. W. L. Luyben, Control of a Train of Distillation Columns for the Separation of Natural Gas
Liquid, Ind. Eng. Chem. Res., vol. 52 (31), pp. 10741–10753, 2013