Hydrogen Isotope Separation Laboratory

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Hydrogen Isotope Separation Laboratory

• Russian Academy Of Science
• B.P.Konstantinov Petersburg Nuclear Physics
  Institute
• Neutron Research Division

Head of the laboratory Ivan A. Alekseev HISL
total staff 17 employees
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Activity of the Laboratory

• Full scale studies of various hydrogen isotope
  separation methods for the development of heavy
  and light water detritiation technology
• The scientific guidance and design supervision
  for the construction of the reactor PIK heavy
  water Detritiation and Deprotization Plant
• Computer simulation of the studying processes
• Provision and new procedures development of water
  and hydrogen gas isotope analysis
• Production of high quality heavy water and
  gaseous deuterium
• Pilot-scale production deuterium depleted water
  (up to 3 orders of magnitude below natural)

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Semi-industrial Facilities

• Cryogenic distillation (CD)
• The single column of 5.5 m height with the
  interchangeable mass exchange sections of
  diameter up to 300 mm (the vacuum jacket of 1200
  mm diameter)
• Helium supply system (4 kW at 20 K) Reflux flow
  of HD-D2-DT mixtures in the column - up to 10
  kMoles/h
• Provided with the systems of deuterium
  production, gas compression, cleaning and storage
• Water distillation (WD)
• 4 distillation columns of 80 mm diameter and 10 m
  height with very high efficiency (HETP 2.5 cm)
• Combine electrolysis and catalytic exchange
  (EVIO)
• 2 exchange columns of 100 mm inner diameter and
  height of 6.9 m filled with hydrophobic catalyst
  and packing
• Electrolysis cells with capacity of 5 m3 H2 (D2)
  per hour

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Separation Factor Is the Magnitude of an
Elementary Separation Effect
Table. The equilibrium separation factors
hydrogen-water isotope exchanges for tritium ?T
and deuterium ?D at 60 ??

• Separation factor for isotopic exchange between
  water and hydrogen depends on what molecules are
  to be separated
• Relatively high values of separation factor at
  ordinary conditions make the process of
  water-hydrogen isotope exchange attractive for
  the different tasks of hydrogen isotope
  separation. For comparison separation factor for
  water distillation ?H-D1.026 at atmospheric
  pressure

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Demonstration Very High Detritiation Factor With
EVIO Facility

• Repeated contact over catalyst between water
  vapour and gaseous hydrogen and counter current
  between liquid water and vapour-gas mixture
  underlies the CECE process and leads to the
  effect of separation multiplying
• EVIO facility is under operation now. Heavy
  water purification from tritium is successfully
  being carried out with the following
  characteristics
• The achieved separation degree (SD) is more than
  2103
• The top product output capacity is about 8
  litres per day
• Todays results receiving on the column of height
  only 7 m do not have any similar ones in the
  world

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The Task of Pilot-scale Production of Deuterium
Depleted Water at PNPI

• Gaseous hydrogen containing deuterium in an
  amount about 0.1 ppm is needed
• Natural water contains about 150 ppm of
  deuterium. Thus needed separation degree (SD) is
  1.5103. The total required amount of the product
  does not exceed 10 litres.
• This is much less intensive task compared to the
  separation possibilities of our facilities
• EVIO lets to process diluted heavy water waste
  contaminated by tritium and produce high quality
  heavy water. The achieved SD for D-H in a wide
  range of deuterium concentration is about 1105
• The achievable SD for the task of heavy water
  conditioning is about 5103 in any of the
  existing WD column

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Possible Ways and Weak Points of the Task Solution

• Any of the above mentioned methods and existing
  facilities can be used in principle for the
  production of super-light water (0.1 ppm of D)
• But according to the required small scale
  production only two methods were dealt with
• A new laboratory scale installation based on
  Combine Electrolysis and Catalytic Exchange
  (CECE) process and
• One of the existing Water Distillation column
• There are two weak points of this separation task
  solution. They mainly concern earlier used (for
  heavy water production) equipment
• The first is trouble with washing of dead spaces
  and
• The second is lack of operative analysis that
  would allow the tracing of the washing process

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Isotope Analysis of Water by the method of
IR-spectrophotometry

• Threshold sensitivity to content of protium in
  heavy water is 6 ppm. It is due to provided
  standard deviation in measurements of cell
  transmission (T) which is less than 0.1
• Analogous absorption band with maximum at 2500
  cm-1 allow us to analyse small deuterium content
  in light water but with threshold sensitivity of
  only about 15 ppm

Figure. High Concentration Heavy Water Samples
Spectra (d206 micron, fluorite, t33?C)
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Computer Simulation of Non Steady-state Water
Distillation Process Using for Deuterium Depleted
Water Production
Expected reboiler and conden-ser (product)
deuterium con-centration variation with time
N300, P100 kPa, G10 litre/h, Vreb.20 litres,
Vcnd.10 litres, Vpac.5 litres
After 3 runs (with duration gt 300 hours) minimum
measured concentration 3.2 ppm was obtained
(after the last run)
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Laboratory Scale CECE Process for Deuterium
Depleted Water Production or Conditioning

• Electrolysis cells capacity is 0.5 m3 H2 per hour
• Catalytic Burner capacity is the same - 0.5 m3 H2
  per hour
• 1 litre of hydrophobic Catalyst - 0.8 wt. Pt
  deposited on porous styrene-divinylbenzene
  copolymer
• 2.5 litres of Packing - stainless steel
  spiral-prismatic with size 2.22.20.2 mm
• Including such an installation in the structure
  of Gas Circulation System would provide a
  guarantee of low level deuterium admixture

Burner
Product as gas or as water
Condenser
Water dosing pump
Isotope exchange apparatus
Thermostat
Electrolysis Cells
Waste water