Synthesis of deuterium

Preparation of deuterium

Synthesois of deuterium

Synthesis of deuterium

Flask E of the glass apparatus shown in figure contains an Al crucible with excess metallic sodium.

Preparation of deuterium from heavy water and sodium

Preparation of deuterium from heavy water and sodium

Vessel V contains the heavy water reagent. The latter is introduced in the absence of atmospheric moisture. After cooling V with liquid nitrogen, the apparatus is carefully evacuated, with stopcocks 1 and 2 open. Stopcock 2 is then closed and the heavy water is distilled slowly onto the sodium by cooling E with liquid nitrogen. To complete the reaction, E is then heated for several hours to 350°C. After opening stopcock 2, the deuterium produced is transferred for purification into a receptacle filled with degassed charcoal and left there for some time at —196°C. If fresh sodium is used, the deuterium product will still contain some few percent of hydrogen after the purification (hydrogen was dissolved in the metal and existed as sodium hydroxide). Pure deuterium, containing less than 0.2% hydrogen and other foreign gases, is only obtained in the second run with the same piece of sodium. The yield of deuterium is quantitative.

Reference: G. Brauer, Handbook of Preparative Inorganic Chemistry, Vol 1, 122-123p, Academic Press, New York, 1965.

Preparation of deuterium from heavy water and magnesium

Preparation of deuterium from heavy water and magnesium

Preparation of deuterium from heavy water and magnesium

In an elongated flask of a Pyrex apparatus, pre-evacuated to 10-4 mm., 20 g. of heavy water is slowly evaporated. The vapor passes through the reaction tube, set vertically on top of the flask. The tube (I.D. 2.4 cm. and 55 cm. long) contains 130 g. of metallic magnesium shavings of various sizes, with coarse particles on the bottom and loose powder on top. The column filling is supported by a perforated platinum disk which rests on glass lugs inside the tube. The metallic magnesium is heated to 480°C by a tubular furnace. After an extended period of time, some magnesium silicide will form on the walls of the heated glass tube. To avoid this, it is suggested that the metallic magnesium be placed in a tube of unglazed hard porcelain which is then inserted into a Pyrex or Vycor tube and melt-sealed to the latter at one end. With such an arrangement the metallic magnesium may even be heated to a somewhat higher temperature and its reactivity thus enhanced. For purification, the deuterium product passes through a trap filled with glass wool and kept at —196 C. It is taken out from the generator as quickly as possible, either by condensation with liquid hydrogen or by forcing it into an attached storage container. An in-line flowmeter and a manometer allow constant checking of pressure. The rate of evolution can be controlled by varying the supply of heat to the heavy water flask. A maximum flow of 0.5 mole of deuterium/hour may be obtained. Since the first Ds fraction may be contaminated with some Hs from the Mg and from the apparatus walls, it is advisable to collect some of the first D3 fraction in a separate vessel. The deuterium formed later is very pure. The yield is quantitative.

Reference: G. Brauer, Handbook of Preparative Inorganic Chemistry, Vol 1, 122-123p, Academic Press, New York, 1965.

Preparation of deuterium by electrolysis

Preparation of deuterium by electrolysis of heavy water

Preparation of deuterium by electrolysis of heavy water

An electrolytic cell, holding 60 ml. of liquid and made from a standard ground glass joint, as shown in figure.

Electrolysis of heavy water

Electrolysis of heavy water

The male part of the ground joint continues into a cylindrical water jacket (only partly shown in the diagram) which surrounds the cathode. The Pt electrodes are also cylindrical and are prepared by fusing together a Pt wire with a Pt foil. The heavy water electrolyte is acidified with 25% D2SO4. (If no D2SO4 is available, carefully dehydrated K2SO4 or Na2CO3 can also be used.) After evacuation of the cell at A and B, electrolysis is begun at a low current to prevent foaming at low pressures. After a short time, however, the current can be increased to 5 amp. The temperature of the electrolyte must not be allowed to rise. If the deuterium product gas is to overcome the pressure drop due to narrow tubes and a liquid head in the attached purification apparatus or reactor, the pressure in the cell must be maintained at a higher level by means of a throttling  valve in the O2 outlet. The deuterium product still contains small amounts of O2 and D2O vapor. Very pure gas may be obtained by heating the electrolysis product over platinized asbestos, followed by drying with liquid nitrogen. At 5 amp., two liters of deuterium per hour is obtained. Small quantities of deuterium are stored in sealed glass flasks or over mercury.

Reference: G. Brauer, Handbook of Preparative Inorganic Chemistry, Vol 1, 124-125 p, Academic Press, New York, 1965.

InChI

InChI=1S/H2/h1H/i1+1D

InChI Key

UFHFLCQGNIYNRP-VVKOMZTBSA-N

Canonical SMILES

[HH]

Isomeric SMILES

[2H][2H]

MeSH Synonyms

Deuterium, Deuterons

Depositor-Supplied Synonyms

DEUTERIUM, Dideuterium, 7782-39-0, Heavy hydrogen, Hydrogen-2, D2, Diplogen, Hydrogen-d2, Deuterium molecule, UNII-AR09D82C7G, Hydrogen, isotope of mass 2, HSDB 294, Deuterium (gas), EINECS 231-952-7, UN1957, Deuterium, compressed, AC1L2NHT, 361860_ALDRICH, 368407_ALDRICH, 617474_ALDRICH, AR09D82C7G, DTXSID2064810, CHEBI:29294, UFHFLCQGNIYNRP-VVKOMZTBSA-N, MFCD00064812, UN 1957, IN001911, IN018820, (2)H2, Deuterium, compressed [UN1957] [Flammable gas], I01-19865

Removed Synonyms

deuterio, tritio, Deuterons, CID24523, NA1957, D003903

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