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Heavy water in Romania: Scientific and technological research, and plant design

Sfetcu, Nicolae, “Heavy water in Romania: Scientific and technological research, and plant design”, in Telework (January 08. 2023), DOI: 10.13140/RG.2.2.36803.68642, https://www.telework.ro/en/heavy-water-in-romania-scientific-and-technological-research-and-plant-design/

 

Abstract

The National Nuclear Program, the studies of specialized institutes and commercial treaties with other countries, based on the social, economic and political conditions existing in Romania and from a geopolitical point of view, led to the creation of national institutes oriented towards the development of a national nuclear system in which heavy water will play an important role. The pilot laboratory for the experimental research of isotopic separation was built at IFA Cluj-Napoca under the coordination of Marius Peculea, who arrived at the institute in 1959. On March 1, 1970, with the establishment of the State Committee for Nuclear Energy (CSEN) as coordinator of the National Nuclear Program (PNN), the establishment of Plant G in Râmnicu Vâlcea was also approved. IITPIC Bucharest took care of the design part of the heavy water plant, as the general designer, under the aspects of plant feasibility, design and installation schemes, calculation methodology and procedures, how to equip the exchange columns with trays, etc., taking over the technology already existing developed within the Plant G.

Keywords: heavy water, Romania, scientific research, technological research, design

 

Heavy water in Romania: Scientific and technological research, and plant design

Nicolae Sfetcu

 

The National Nuclear Plan, the studies of specialized institutes and trade negotiations with other countries based on the existing social, the economic and political conditions in Romania, and the geopolitical circumstances, led to the creation of national institutes oriented towards the development of a national nuclear system in which heavy water will play an important role. Next comes phase 2 of Kuhn’s theory of scientific structure, of normal science (and technology), within which the solution of the highlighted problems takes shape.

In Romania, there were numerous institutions in the nuclear field with scientific and technological research activity in this field, including educational units with faculties and sections specially dedicated to the nuclear field, such as the Politehnica University of Bucharest (Ghizdeanu et al. 2004) and the Faculty of Physics from the University of Bucharest with the Technological Physics section. (Glodeanu 2007)

In 1968, after the retirement of Professor Horia Hulubei from the management of IFA, the position was taken over by Professor Ioan Ursu, who continued and developed the concepts of his predecessor for the development of nuclear energy, and created the Institute of Nuclear Technologies (ITN) from Pitesti, which it was later transformed into the Institute of Energetic Nuclear Reactors. At Plant G in Râmnicu Vâlcea, Marius Peculea established the pilot station for the development of heavy water production technologies based on the results obtained at IFA in Cluj. (Frangopol 2008)

The Bucharest pump company, in the period 1965-1989, was involved in applied research in the field of deformable solid mechanics to solve specific problems, through static and dynamic strain measurements, and photoelastic research to determine the state of tension in structures or resistance elements . Thus, measurements of vibrations and frequencies, accelerations, speeds and displacements were carried out in soils, constructions and machine foundations, produced by controlled explosions, forge hammers, compressors and pumps, in order to locate the heavy water plant. Many of these studies were carried out by the materials resistance departments in collaboration with laboratories from research institutes, and with the support of departmental research institutes and the Romanian Academy. (Spinei 2019)

In the research activity, the Research Institute for Electronic Components (ICCE) carried out research contracts through the microproduction of some components under special regime (“G”) for the electronic components needed for the heavy water plant, with the support of teaching staff from the Faculty of Automation. (Spinei 2018)

Marius Peculea, in the Interfață între știință și tehnologie – Un exemplu de caz (Interface between science and technology – A case example), (Peculea 2010) highlighted the close connection and complementarity between scientific and technological research in the specific case of heavy water production through H2S-H2O isotopic exchange using GS columns:

  • isotopic exchange space (sieve tray):
    • in scientific research, it is defined as an isotopic balancing element
    • in technological research, it represents a well-defined element with the aim of achieving a contact surface as large as possible between liquid and gas
  • mathematical modeling:
    • in scientific research the intimacy of the phenomenon is pursued
    • in technological research only the flow of the two fluids is of interest
  • behavior of the exchange space:
    • in scientific research, the number of theoretical sieve trays can be determined through iteration
    • in technological research, the performance of the separation column is determined from the characteristic diagram
  • specific loading of the exchange space:
    • in scientific research, the behavior of the process is monitored through pilot laboratory installations
    • in technological research is concerned with obtaining the performance of isotopic separation columns

Peculea completes this research with an equally important stage, the design of the heavy water plant, which deals with the technical documentation of execution and costs, naming the three institutions with a major role in these three stages in the construction and operation of the heavy water plant:

Scientific research Technological research Design
Process study Facility study Industrial plant project
Laboratory pilot Industrial pilot Assistance during construction
IFA – Cluj Uzina G Râmnicu Vâlcea IITPIC București

Table 3. Correlation between scientific research, technological research, and design (Source: (Peculea 2010), modified)

According to (Nică 2016), the main designers involved in the construction of the heavy water plant were:

  • I.T.P.I.C. Bucharest (Institute of Technological Engineering and Design in the Chemical Industry), as a general designer
  • P.A. Bucharest (Design Institute for Automation)
  • S.L.G.C. Bucharest for process water
  • C.S.I.T.E.E. Bucharest (centrifugal compressors for hydrogen sulphide)
  • C.S.I.T. Faur Bucharest (piston compressors for hydrogen sulphide liquefaction)
  • C.I.T.P.V. Bucharest (special hydrogen sulphide water pumps and fans)
  • Designers of the plants supplying machinery, assembly materials, electrical and automation equipment.
  • Designers of the builders and installers.

IFA Cluj

In 1949, the Physics Department of the Romanian Academy was established in Bucharest.

In 1950, the Physics Department of the Romanian Academy Branch was born in Cluj-Napoca.

In 1956, the Institute of Atomic Physics (IFA) is established in Bucharest, Măgurele, and the Cluj Physics Department of the Academy becomes a subsidiary of IFA Bucharest. (INCDTIM 2022)

Research on heavy water began in 1958.

The pilot laboratory for the experimental research of isotopic separation was built here under the coordination of Marius Peculea who arrived at the institute in 1959, it is the first installation for the separation of heavy water made in Romania, in a separation process at two temperatures (bitherm). The original idea was to complete the “bitherm process” with a process at two pressures, a process named by its inventor the “bitherm-bibar” process, with superior performance compared to the “bitherm” system of two temperatures, a world premiere in 1968 (Tãnãsescu 2007)

In 1970, the IFA Section in Cluj became a unit with its own economic management under the name of the Institute of Stable Isotopes, having as its object of activity the carrying out of research and the development of technologies regarding the production of heavy water, stable isotopes, the design and production of scientific equipment for applications of stable isotopes. (INCDTIM 2022)

In the first stage, the research had as its object the prospecting of deuterium sources, the development of deuterium analysis methods, and the development of a deuterium separation method. For the analysis of deuterium, the following were developed: densimetric methods for the total isotopic analysis of water (D/H) using a variant of the droplet method with superior performance to those obtained worldwide, optical methods with a Fabry-Perot spectrometer with magnetostrictive scanning and by pressure variation, and gas chromatography. Research started at IFA Bucharest in 1958 was improved by chromatography. For the isotopic separation, experimented on a laboratory pilot, the isotopic exchange method between water and hydrogen was chosen, developing in parallel research related to the use of hydrogen as an energy source. The institute was the only manufacturer of mass spectrometers in the country, used for measurements of deuterium concentrations in the field of natural concentrations, in dynamic mode, the study of ion-molecule reactions, and isotopic and chemical analyzes in gaseous and liquid samples. (Văsaru 2011)

All these researches from Cluj were classified as strictly secret.

In 1977, the Institute of Stable Isotopes changed its name to the Institute of Isotopic and Molecular Technology ITIM Cluj-Napoca, under the State Committee for Nuclear Energy.

In 1999, through the reorganization of ITIM Cluj-Napoca, the National Research and Development Institute for Isotopic and Molecular Technologies INCDTIM Cluj-Napoca was created (HG 408/1999). (INCDTIM 2022)

The research carried out here in the first years of activity decisively influenced the choice of the natural uranium – heavy water chain in the National Nuclear Program (PNN), (Peculea 2002) materializing in two pilot installations, one monothermal with phase conversion by electrolysis and one free bitherm, operated at two temperatures and two pressures, the achievement being successfully tested also for ammonia-hydrogen isotopic exchange. (Hodor, Peculea, and Străulea 1973) They were completed by patenting the heavy water production technology and capitalizing on it in the design and construction of the heavy water plant, attesting to the importance of oriented fundamental research. (Peculea 2002)

Plant G Râmnicu Vâlcea

Following the research at IFA Cluj regarding the isotopic separation of heavy water on the two pilot installations of the institute, in 1969 a commission was set up to analyze the possibility of industrialization of the heavy water separation technology. The Director of the Design Institute for the Petroleum Industry (IPIP) Ploiești has committed to the realization of the pilot plant at Plant G in Râmnicu Vâlcea. Initially, only the vacuum isotopic distillation of water was adopted, at that time the isotopic exchange method of water – water vapor – hydrogen was considered uncompetitive. In the end, a primary separation stage was adopted through isotopic exchange at two temperatures (bitherm) between water and hydrogen sulphide, and a final stage through isotopic distillation of water under vacuum. (Glodeanu 2007)

On March 1, 1970, with the establishment of the State Committee for Nuclear Energy (CSEN) as the coordinator of the National Nuclear Program (PNN), the establishment of Plant G in Râmnicu Vâlcea was also approved. The pilot plant consisted of four facilities: sodium sulfide production, hydrogen sulfide production, vacuum isotopic distillation of water, and water-hydrogen sulfide isotopic exchange at two temperatures. The facilities were approved on December 3, 1974 and the first heavy water of nuclear quality from Plant G was produced on August 9, 1976. After the first production from Plant G, it was decided to fully use Romanian technology. (Glodeanu 2007)

Research in Plant G developed in four main directions: technology, calculation, laboratory, engineering and verification on the experimental plant, (Ioniţă 2018) with an emphasis on:

  • gas separation processes, advanced purification and recovery technologies;
  • apparatus, methods and equipment for controlling isotopic separation processes;
  • techniques, command and control methods of complex installations with increased risk,

having as its main purpose within the National Nuclear Program the technologies for the production, separation and reconcentration of heavy water, analysis equipment, technical assistance and expertise, monitoring and environmental analyses. (Ștefănescu 2017)

Plant G has provided innovative solutions, new improved materials and the development of specific equipment, mainly through the balance column, the study of hydrodynamic flow on sieve trays, the passivation technology of carbon steel alloy, the passivation technology using pyrite (Patent No. 90 3821 /1986), (Peculea, Beca, and Ștefănescu 1998) the hydrogen sulphide compressor. (Ioniţă 2018)

Marius Peculea appreciates the fact that CSEN, MICh and CNST (National Council of Science and Technology), contrary to a normative act from 1979, maintained the independence in activity of Plant G under the coordination of CSEN. (Glodeanu 2007)

After 1979, through technological research at the Plant G, many solutions were found to the problems posed by the construction and operation of the heavy water plant, such as the passivation by pyritization of the carbon steel G52/28 of the GS columns, the stability in operation of the sieve trays of the isotopic exchange, separation technology by isotopic exchange at two temperatures (bitherm) by introducing an isotopic balancing column (a global innovation), etc. (Glodeanu 2007) And research on the hydrodynamics of the isotopic separation interface increased the performance of the real sieve trays so that the heavy water produced at Drobeta Turnu Severin is considered to be the purest heavy water, both isotopically and chemically. (Peculea 2019)

In 1988, the technological patent for heavy water was issued, based on the application submitted in 1976, and it was used for the design and construction of the heavy water installation at Drobeta-Turnu Severin. (ICSI Râmnicu Vâlcea 2020)

In the book În sfârșit, Adevărul (Finally, the Truth) of gen. Victor Atanasie Stănculescu, he states that “The foundations of the pilot station for obtaining heavy water from Vâlcea were laid in the 60s under the guidance of the Directorate of Foreign Intelligence, as soon as the agent of the Special Brigade TS Polihroniade, code name “Poly”, managed to bring heavy water manufacturing technology from a plant somewhere in the Savannah River — United States. The TS Special Brigade (later SD) was a compartment specialized in economic espionage, within the Foreign Intelligence Directorate.” (Stănculescu 2009) Mircea Turtureanu, the former director of IITPIC Bucharest, states that, although he searched for additional data, he did not find additional confirmations regarding this aspect. (Turtureanu 2016)

The technology resulting from the research at Plant G differs substantially from that used at the Savannah River Plant, among improvements Peculea enumerating: modification of the connections between the floors of the plant increasing the stability in operation and a simple and safe adjustment, perforated trays much simpler than those with bells, humidification and dehumidification of hydrogen sulphide directly at the base of the columns, isotopic distillation columns equipped with B7 packing reducing the volume of the plant without further processing. (Peculea 2019)

The mixed filling from the distillation plant is protected by patent No. 113218.C1(1999). (Peculea 2002) The installation for the production of the heavy water standard developed at Plant G, with an isotopic concentration of 99.995% ±0.002% D/(H + D), is protected by 4 invention patents, allowing the plant to receive authorization for the production and marketing of heavy water standard. (Peculea 2019)

Among the patents obtained in Plant G in research on obtaining heavy water, are(ICSI Râmnicu Vâlcea 2020)

  • 62367 “Process and installation for continuous flow production of high purity hydrogen sulfide”
  • 62368 “Procedure for cleaning a bithermal H2S-H2O isotopic exchange installation”
  • 62370 “Heavy water manufacturing process by H2S-H2O bitherm exchange”
  • 62374 “Quasi-adiabatic isotopic distillation column”
  • 62375 “Method and reflux control device for distillation columns”
  • 62377 “Sodium sulphide manufacturing process”
  • 62378 “Procedure for the production of hydrogen sulphide in a discontinuous system”
  • 62379 “Process and plant for the production of heavy water by H2S-H2O bithermal isotopic exchange”
  • 69866 “Procedure of surface oxidation of metal products”
  • 76953 “Asymmetric control device for anti-pumping protection of a centrifugal compressor”
  • 78668 “Procedure and installation for the purification of waste water from the production of hydrogen sulphide”
  • 83372 “Float for transducer measuring the level of corrosive liquid at high pressure and temperature”
  • 90073 “Device for reducing the whine effect of multi-spill trays”
  • 90131 “Ion analyzer for hydrogen isotopic analysis”
  • 90382 “Process and installation for the formation of a protective deposit with a high pyrite content in bithermal isotopic exchange installations”
  • 90566 “Orderly filling for equipping isotope separation columns”
  • 90567 “Orderly filling for equipping isotope separation columns”
  • 93471 “Procedure for rapid recovery of hydrogen sulphide in industrial installations”
  • 95871 “Method and apparatus for measuring the liquid content in foam”
  • 96678 “Liquid Film Gland and Floating Bushing”
  • 101759 “Procedure for the protection of carbon steel surfaces in heavy water manufacturing plants”
  • 107558 C1 “Catalytic filling for the combustion of stoichiometric mixtures of hydrogen and oxygen”
  • 107842 C1 “Process for the preparation of hydrophobic platinum catalysts”
  • 11 3386 C1 “Mechanical sealing device for hydrogen sulfide-carrying turbofans”
  • 113401 C1 “Device for cooling specimens for resilience tests”
  • 114911 C1 “Process of chemical cleaning of steel pipes”
  • 115129 C “Procedure for obtaining a selective adsorbent”
  • 115367 C “Conservation method of anti-corrosion protections formed by iron sulphides”

“The pilot plant has been operating for more than 10 years. During all this time, it was a source of scientific, technological and thermo-energetic knowledge, which allowed the training of Romanian experts in the field of heavy water.” (Peculea 2007)

Marius Peculea

Marius-Sabin Peculea was born on April 13, 1926, in Cluj. Between 1944 and 1949 he attended the engineering courses of the Faculty of Electromechanics of the Polytechnic School of Timișoara. In 1966 he received his doctorate in thermodynamics, with the doctoral thesis “Thermodynamic study of separation columns, in continuous flow, with three fluids and different reaction temperatures”.

Positions held: (Conphys 2022)

  • Until 1959: Tehnofrig Cluj Plant – Head of the Studies and Designs Service, established by him in 1952
  • 1959 – 1963: ITIM Cluj-Napoca – Principal Researcher II
  • 1963 – 1970: ITIM Cluj-Napoca – Laboratory Head
  • 1970 – 1994: Plant “G” (INC-DTCI-ICSI) Rm. Vâlcea: Director
  • 1994 – 1999: Romanian Academy – General Secretary

Scientific titles, professional degrees:

  • Doctor in thermodynamics (1966)
  • Teaching doctor (1974)
  • Corresponding member of the Romanian Academy (1991)
  • Full member of the Romanian Academy (1993)
  • Doctor Honoris Causa of the Cluj-Napoca Technical University (1995)
  • Doctor Honoris Causa of the Technical University of Construction Bucharest (1996)
  • Doctor Honoris Causa of the University of Craiova (1996)
  • Member of the “Academia Scientiarum at Artium Europaea” Salzburg (1996)
  • Founding member of the Romanian Academy of Technical Sciences (1998)
  • Doctor Honoris Causa of the University of Oradea (1998)
  • Doctor Honoris Causa of the Ovidius University of Constanta (2000)
  • Doctor Honoris Causa of the Polytechnic University of Timișoara (2002)

Professional achievements:

  • Scientific and technical publications: his works mainly address topics related to isotopic separations (heavy water, tritium) and thermodynamics (cryogenics, gas separations), including 6 books, 90 academic papers, 30 invention patents, 88 scientific reports, and 126 scientific conferences.
  • Developed 4 technologies for heavy water separation
  • 12 invention patents awarded at international invention salons (Conphys 2022)

Global priorities: (Ratcu 2017)

  • Deuterium separation process, through successive water-hydrogen isotopic exchange, in the “bitherm-bibar” system (at two temperatures and two pressures) (1966)
  • Heavy water separation process, by water-hydrogen sulphide isotopic exchange, in a bithermic system (at two temperatures), with the isotopic balancing column (1985).

Scientific priorities:

  • Modeling of isotopic separation processes in bitherm system and distillation.
  • Exergetic analysis of isotopic separation processes.
  • Introduction of the technological function to the comparative analysis of isotopic separation processes.
  • Defining actual versus design capacity for an isotope separation facility.
  • Introduction of the t-T diagram (of temperatures) for the calculation of heat exchangers and humidifiers (heat and mass exchange).
  • Definition of the isotopic exchange plate with successive reactions.
  • Introduction of the figure “We” (Weber) in the performance representation of the separation plates. (Ratcu 2017)

Expert of the International Atomic Energy Agency (IAEA), and specialist invited to conferences in the field of heavy water in Germany, India, USA, Canada, USSR, Libya, China, Pakistan

Teaching activity: (Conphys 2022)

  • Polytechnic Institute of Cluj – Department of Thermal Engines: university trainer (1949 – 1950)
  • Babeș Bolyai University in Cluj: university assistant (1950 – 1952; 1954 – 1958)
  • Bucharest Construction Institute: university lecturer (1968 – 1971), university professor at the Department of Thermodynamics, disciplines of Technical Thermodynamics and Heat Transfer (1971- 1989), associate university professor (1989), doctoral supervisor in the discipline of Thermodynamics, specialty separation of isotopes (1969)

Professional awards and distinctions:

  • Award of the Romanian Academy “Dragomir Hurmuzescu” (1981);
  • Order of Scientific Merit Cl. II (1974);
  • Order of Scientific Merit Cl. III (1981);
  • Scientific Merit Medal (1969 and 1979);
  • “Ionel Purica” Award for contributions in Nuclear Energy (1993);
  • Special Award for the contribution to the development of Romanian Thermotechnics (1995);
  • Diploma for special contributions in energy research-development activity (1995);
  • Honorary Citizen of the Municipality of Cluj-Napoca (1996);
  • Order “For Merit” in the rank of Grand Officer (2000)
  • Honorary Citizen of the Municipality of Rm. Vâlcea (2008) (Conphys 2022)

According to (Tãnãsescu 2007),

“What characterizes Marius Peculea in all these searches in a scientific field not accessible to many, was his eternal spirit to ask himself questions, to answer the criticisms brought to a process, most of which, however, were not of “others”, but his own.”

In Marius Peculea’s own words:

“I sought to find the relationship between the separation factor that characterizes a process and the cost price of the product. Specifically for heavy water, we were able to find this relationship by introducing the notion of technological function, which quantitatively represents the quality (intelligence) of the given technological solution for the industrialization of a process”. (Tãnãsescu 2007)

IITPIC Bucharest

In 1977, the chemical and petrochemical industry design institutes were unified into a single institute – the Institute of Technological Engineering and Design for the Chemical Industry (IITPIC)

IITPIC Bucharest took care of the design part of the heavy water plant, as the general designer, under the aspects of plant feasibility, design and installation schemes, calculation methodology and procedures, how to equip the exchange columns with trays, etc., taking over the technology already existing developed within the Plant G.

According to Mircea Turtureanu, the former project director, (Turtureanu 2016) the basic conditions of the project were that the technology should be the one developed at Plant G, and that all materials, machinery and equipment should be made in the country, except for the purchased nitrogen plant from the former DR Germany. Three aspects had to be decided before starting the actual design: the scheme of the isotopic exchange plant (Patent no. 74088/29.03.1980 entitled “Plant for the separation of deuterium by isotopic exchange”), the number of production lines (in finally, four production lines / modules were decided) and the way of coupling the columns, and the problem of the corrosion of the isotopic exchange columns by hydrogen sulphide (the solution of this problem being through pyritization and special characteristics of the steel used). (Turtureanu 2016)

The geotechnical studies were carried out with the help of a specialized institute for land surveys and improvements, ISPIF Bucharest, and for solutions regarding the elimination of organic substances from the process water, the Institute of Hydrotechnical Studies and Designs (ISPH) was consulted. The automation project was carried out by the Automation Design Institute (IPA). In order to prevent incidents of accidents due to uncontrollable releases of hydrogen sulphide into the atmosphere, specific studies were carried out with the help of the Institute of Meteorology and Hydrology (IMH). (Turtureanu 2016)

In 1991, based on Law no. 15/1990 on the reorganization of state economic units as autonomous administrations and commercial companies, by H.G. no. 156/07.03.1991, the commercial company IPROCHIM S.A. Bucharest is established, by fully taking over the assets and liabilities of the Institute of Technological Engineering and Design for the Chemical Industry – IITPIC – Bucharest.

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