SECTION 26

Rhenium
O . GLEMSER

Rhenium Metal

Prepared by reduction of NH 4 ReO 4 or KReO4 with H s .

I. Fine NH4ReO4 powder is slowly heated to 200-250°C in very
pure H s and held at that temperature for three hours. The tem-
perature is then raised to 500°C and the reduction completed at
1050°C (six hours). The boats and reactor tubes should be por-
celain.
If heating rates are too high, part of the product evaporates
as the oxide and deposits to form a mirror on the cooler parts of
the tube.
II. KReO-n in a silver boat, is reduced in very pure H 3 at 500°C.
The product is extracted with H3O containing a small amount of
HC1, dried and again reduced with H 3 ina porcelain boat at 1000°C.
PROPERTIES:
Atomic weight 186.22. Gray metal powder; the solid has a
platinum-like luster. M.p. 3170°C; d 20.35; Brinell hardness 250.
Readily soluble in nitric acid and slowly in sulfuric acid. Crystal
structure: A 3 type.
REFERENCES:
I. W. Biltz and G. A. Lehrer. Nachr. Gb'tt. Ges. 1931, 193.
II. W. Biltz. Z. Elektrochem. 37, 498 (1931); W.Geilmann. Private
communication.

Rhenium (III) Chloride

ReCl3

186.2 33.01. 292.6

Rhenium metal is placed in a reactor consisting of a hard
glass tube joined to a receiver manifold with seven bulbs
1476
 RHENIUM 1477

sealed on. The air is displaced with oxygen-free H 3 and the Re

then heated in a stream of Cl a . The raw sublimate is collected
in the first bulb; it is resublimed into the second bulb under
oxygen-free, dry N 2 (the less volatile ReCl 3 remains in the first
bulb). The operation is repeated using the next set of bulbs, etc.
The ReCl3 fractions are then collected from all the bulbs and
resublimed at 2-3 mm. and 500-550°C.

ANALYSIS:

Oxidation to ReO-i" with sodium hydroxide + H 3 O 3 ; the ReC>4~

ion is precipitated as nitron hydrogen perrhenate.

PROPERTIES:

Dark purple-red crystals. Bimolecular under normal condi-

tions (Re 3 Cl s ). Converted in moist air to ReCl* 2H 3 O (2-3 hours);
the water of hydration is readily removed by heating to 100°C in
vacuum over P 3 O 5 . Soluble in water with a deep dark-red color;
the solution turns cloudy after several hours because of hydrolysis,
and black Re 2 O 3 • H3O is precipitated. Complete hydrolysis on
boiling. Soluble in glacial acetic acid and dioxane (reddish-purple
color), alcohol and liquid ammonia; slightly soluble in ether. A
AgNO3 solution produces a precipitate only after lengthy heating
with nitric acid. Forms well-crystallized compounds with RbCl,
CsCl and organic bases. Hexagonal crystal structure.

REFERENCES:

W. Geilmann, F. W. Wrigge and W. Biltz. Nachr. Gott. Ges. 1932,

582; W. Geilmann and F. W. Wrigge. Z.anorg. allg. Chem. 214,
249 (1933); O. W. Kolling. Trans. Kansas Acad. Sci. 56, 378
(1953).

Rhenium (V) Chloride

ReCl5
5
Re + /2Cl2 = ReCl 5
186.2 55.0/. 363.5

Rhenium metal is placed in a boat which is inserted into the

hard glass apparatus of Fig. 328. The air is displaced by O 2 -free
nitrogen and the Re chlorinated at 500°C in a stream of Cl 3 . The
evolving black-brown vapors are condensed at a as a black solid.
The apparatus is sealed off at 1, connected at 5 to a high vacuum,
1478

Re

Fig. 328. Preparation of rhenium (V) chloride

evacuated and heated from 20 to 50°C; small fractions of the very
volatile ReOCl4 (b.p. 223°C) are then condensed i n d a n d e . The
bulk of the ReCl 5 is driven into b at 150 to 250°C, the tube melt-
sealed at 2, and the substance sublimed at 200°C from b to c,
leaving only a slight residue in b. Finally, the tube is melt-sealed
at 3 and 4 and the preparation distributed (by shaking) into the
small tubes attached at c; the latter are then melt-sealed.

PROPERTIES:

A deep, black-brown powder; dark brown vapor. Sensitive to

air, sublimation at atmospheric pressure results in decomposition.
Hydrolyzed by water, forming various products. Soluble in hydro-
chloric acid (green solution) with liberation of Cl 2 .
REFERENCES:

W. Geilmann, F. W. Wrigge and W. Blitz. Angew. Chem. 46, 223

(1933); Z. anorg. allg. Chem. 212, 244 (1933).

Potassium Rhenium (IV) Chloride

K2ReCl,

Re + 2C1 2 + 2 KCl = K2ReCl8

186.2 44.01. 149.1 477.1

Fine Re powder is intimately ground with KCl (10% excess) and

slowly heated to about 300°C in a porcelain boat, first under N 3 and
then in a slow Cl 3 stream. The K 2 ReCl s is formed immediately
and only a slight quantity of rhenium chlorides is volatilized.
Following cooling in a stream of N s , the substance is dissolved in
some hot 5% HC1 and recrystallized; the remainder is obtained
by concentration and crystallization during cooling.
Alternate method: Reaction of KReCUwith KI and hydrochloric
acid. The procedure is involved and it is difficult to obtain a
pure product [H. Schmidt, Z. anorg. allg. Chem. 21J, 188(1933);
O. W. Rolling, Trans. Kansas Acad. Sci. 56, 379 (1953)].
 RHENIUM 1479

PROPERTIES:

Yellowish-green powder or regular green crystals. Melts

with decomposition. Addition of cone. HSSO4 at moderate tem-
peratures produces HC1. Fair solubility in water. Solubility in
12% HC1: 21.4 (0°C); 30.3 (18°C) g./liter; in 37% HC1: 3.3 (0°C);
3.7 (18°C) g./liter. d j 5 3.34. Crystal structure: type J l x .

REFERENCE:

W. Geilmann. Private communication.

Rhenium (VI) Oxychloride

ReOCI4
Prepared via reaction of He 2 O 7 with ReCl 5 .
Rhenium metal is chlorinated at 500°C in a stream of Cl 2 in
the apparatus described for the preparation of ReO 3 Cl. Following
cooling, the Cl 3 is displaced with O 2 and the sections of the tube
in which brown-black crystals of R e d s have appeared are heated
with a small flame to50-70°C. TheReCls melts (often with appear-
ance of a flame) and the crystals turn into a brown liquid, which is
then distilled in a stream of N 3 into a well-cooled U tube receiver.
The excess C l a is evaporated, the apparatus filled with O s , and the
liquid brought to a gentle boil. Heating at 200°C in an N 3 stream
is continued for an hour in order to completely remove all traces
of ReO 3 Cl. Then about one third of the remaining liquid is dis-
tilled off. The receiver is now replaced by a fresh one and, except
for a small residue, the remaining liquid is distilled over.
Alternate method: From ReCl 3 and dry O a at 110 to 130°C
[O. W. Rolling, Trans. Kansas Acad. Sci. 56, 378 (1953)].

PROPERTIES:

Formula weight 344.05. Fibrous needles; dark orange in thin,

brownish-red in thick layers. M.p. 29.3°C, b . p . 223°C (slight
decomposition). Decomposes at 300°C. Immediately forms ReO3Cl
on heating in a stream of Oa . Hydrolyzed by water to rhenium (IV)
hydroxide and HReO4.

REFERENCE:

A. Brukl and K. Ziegler. Ber. dtsch. chem. Ges. 65, 916 (1932).
1480 26. G. GLEMSER

Rhenium (VII) Oxychloride

ReO3CI

Prepared by reaction of Re 3 O 7 (excess) with ReCl 5 .

Two boats, one containing five and the other two parts of Re,
are placed in a high-melting glass reactor tube in a manner such
that heating of one will not raise the temperature of the other.
A U-shaped tube and two condensation traps are connected to
the reactor by means of ground-glass joints (the traps are cooled
to — 65°C with alcohol-Dry Ice). The air in the apparatus is dis-
placed with O 3 and the first boat (the one containing five parts
of Re) is heated in a slow stream of O 3 in such a way that the
Re3O? formed is deposited in the tube (the U tube must be cooled
to a low temperature during this operation). The oxygen is then
displaced with Cl 3 and the second boat heated in a stream of Cl s .
The rhenium chlorides formed in this manner react with the Re s O 7
and the products of this reaction are condensed in the U tube. Any
cocondensed Cl 3 is evaporated; then, the ReO3Cl is distilled
over as the first fraction boiling above 100°C (it is usually very
light blue or green). On repeated fractionation in a stream of
N 3 the product becomes colorless.
Alternate method: From ReO 3 and dry Cl 3 at 160-190°C.
Yields exceed 70% [C. J. Wolf, A. F. Clifford and W. H. Johnston,
J. Amer. Chem. Soc. 79, 4257 (1957)].
PROPERTIES:

Formula weight 269.68. Colorless liquid: strongly light refract-

ing. M.p. 4.5°C, b.p. 131 °C (corr.). Reacts instantaneously with
Hg, Ag, stopcock grease and numerous other organic compounds.
Soluble in CC1 4 . Hydrolyzes to HReO4 and HC1.
REFERENCE:

A. Brukl and K. Ziegler. Ber. dtsch. chem. Ges. 65, 916 (1932).

Rhenium (IV) Oxide

ReO2

I. 2Re2O7 + 3 Re = 7 ReO2
'/,„: 96.9 55.9 152.8

A stoichiometric mixture of Re and Re3C>7 is heated to 300°C

for one day in a small, evacuated, thick-wall quartz tube, which is
 RHENIUM 1481

sealed by melting; the reactants are then heated to 600-650°C for

an additional day. The product is orthorhombic ReO s .
II. Heating of NH^ReO^ in vacuum at 500°C yields monoclinic
ReO 3 of the MoO3 type; above 500°C, orthorhombic oxides are
formed.
PROPERTIES:

Formula weight 218.22. Gray-black powder; dissociates in a

high vacuum at 1000cC to Re and Re a O 7 . Readily oxidized by O 3 .
Insoluble in weak acids, but dissolved by cone, halogen acids.
Converted to HReO 4 by H 3 O 3 and HNO3. d%s 11.4. Heat of forma-
tion: —70 kcal.
REFERENCES:

I. W. Biltz. Z. anorg. allg. Chem. 214, 227 (1933).

II. W. H. Zachariasen. Amer. Crystallographic Assoc. Program
and Abstracts of Winter Meeting, F 4 (1951); A. Magneli. Acta
Crystallogr. (Copenhagen) 9, 1038 (1956).

Rhenium (VI) Oxide

ReO3

I. REDUCTION OF Re 2 O 7 BY CARBON MONOXIDE

Re 2 O 7 + CO = 2ReO 3 + CO 2
484.4 22.41. 468.4 22.41.

The apparatus is a glass tube sealed at one end; about 1 g. of

Re 2 O 7 is sublimed into it in a stream of O 3 . When the reaction
is completed, the apparatus is evacuated and filled with CO to a
pressure of 760 mm. The glass tube is then slowly heated to
175°C in a glycerol bath and held at that temperature until the
preparation turns blue. The temperature is then slowly raised
to 225°C and later, when red ReO3 is formed, to 280°C. The run
requires two to three hours. The yield is quantitative.
II. Reaction of Re 3 O 7 with dioxane to form a complex compound,
which dissociates at 125-145 °C to ReO3 and some volatile pro-
ducts.
The apparatus consists of a reaction flask protected against
moisture; 4 ml. of dioxane is rapidly added to 1 g. of Re3O7
under anhydrous conditions (the dioxane should be predistilled
1482 26. G. GLEMSER

over Na metal). The mixture is gently heated on a water bath until

a clear, colorless solution is obtained. Local overheating must be
avoided, since it produces cloudy solutions and, ultimately, con-
taminated products. The flask is then placed in an ice bath to
freeze the solution. After the freezing, the frozen substance
is allowed to melt. The Re3C>7-dioxane complex crystallizes
in the form of a dense, pearly-gray precipitate; the excess
dioxane becomes liquid. The freezing-melting operation is then
repeated, the excess of dioxane decanted, and the compound
dried in a vacuum desiccator at room temperature over cone.
H a SO 4 . The dry complex is rapidly placed in a crucible and
carefully heated on a hot plate (125 to 145°C). The substance is
melted, forming a colorless to bluish-green liquid, which later
dissociates to red ReO 3 and some volatile, Re-free products. The
ReO3 thus formed is pure. The yield is about 95%.
PROPERTIES:

Formula weight 234.22. Red powder. During reduction of

Re s O?, the preparation passes through intermediate stages with
hues ranging from green to dark blue (rhenium blue) until the
final red color is obtained. Decomposed in high vacuum at 400°C
to Re s O 7 and ReO 2 . Not attacked by hot hydrochloric acid, but
converted to HReO^ by strong HNO3. Disproportionates in warm
NaOH to ReO 3 and NaReO 4 ; NaOH + H s O a instantaneously produce
NaReO 4 . d | 5 6 . 9 ; heat of formation: —146.0kcal. Crystal structure:
DO 9 type.

REFERENCES:

I. A. D. Melaven, J. N. Fowle, W. Brickel and C. F. Hiskey in:

L. F. Audrieth, Inorg. Syntheses, Vol. Ill, New York-Toronto-
London, 1950, p. 187.
II. H. Nechamkin and C. F. Hiskey. Ibid., p. 186; H. Nechamkin,
A. N. Kurtz, and C. F. Hiskey. J. Amer. Chem. Soc. 73, 2828
(1951).

Rhenium (VII) Oxide

Re2O7

2 Re + V2O2 = Re 2 O 7
372.4 78.41. 484.4

The compound is prepared in a combustion tube to which a

U tube is sealed on; the latter is attached to a condensation trap.
 RHENIUM 1483

Both ends of the tube are protected against humidity by vessels

containing CaCl 2 and cone. H2SO4, The rhenium metal is placed
in a porcelain boat situated in the front section of the tube, which
is heated to 150°C while a very fast stream of oxygen is passed
over the metal. Crystals of Re 3 O 7 deposit in the front section of
the tube and in the condenser tube (there is virtually no vapor
mist); if the starting Re is not entirely alkali-free, some KReC>4
will remain in the boat. The Re 3 O 7 should be resublimed in a
stream of O 2 .
The compound is used in the preparation of HReO 4, of the lower
oxides and of very pure Re (reduction with H a ).
PROPERTIES:
Bright-yellow crystalline powder. M.p. 301.5°C, b.p. 362.4°C;
d|, s 6.103; heat of formation:—295.9 kcal. Extremely hygroscopic.
Readily soluble in H 8 O, forming HReO4; soluble in alcohol; spar-
ingly soluble in ether. Stored in melt-sealed glass tubes. Rhombic
crystals.
REFERENCES:
W. Geilmann. Private communication; W. A. Roth and C. Becker.
Z. phys. Chem. 159, 29 (1932); K. Wilhelmi. Acta Chem. Scand.
8, 693 (1954).

Sodium Rhenate (IV)

Na2ReO3
ReO2 + 2NaOH = Na2ReO3 H2O
218.2 80.0 280.2

The apparatus is shown in Fig. 329. A gold crucible c is intro-

duced into the quartz apparatus through opening e and placed in

a e

electric furnace
Fig. 329. Preparation of sodium rhenate (IV). a quartz tube; b
crucible-shaped attachment; c gold crucible; d thermocouple; I
movable gold shield (splash shield).
1484 26. G. GLEMSER

the attachment b; a stream of oxygen-free N 3 is passed from h to

g. After thorough flushing with N 2 , 10 g. of very pure and dry
NaOH is introduced (through /) into c. The apparatus is then
heated to 500 °C and 4 g. of dry ReO 3 added by shaking to the melt.
The ReO a dissolves, the melt turns reddish-brown, and water
vapor escapes through f. After the reaction is completed, the
heater is removed and attachment b cooled with ice water; this
spalls the solidified melt off the crucible walls. The fused mate-
rial contains (clearly separated) an upper layer of NaOH and a
lower stratum of the brown rhenate. The fused cake is gently
crushed, leached with deaerated ice water, decanted, filtered in
the absence of air, washed with alcohol and dried, again in the
absence of air. The filtering and drying device shown in Fig. 52,
p. 74, is handy in this operation.
Alternate method: Fusion of ReO 3 with NaOH [W. Geilmann,
F. W. Wrigge and W. Biltz, Z. anorg. allg. Chem. 214, 233 (1933)].

SYNONYM:

Sodium rhenite.

PROPERTIES:

Brown powder. On heating in air, converts to the yellow per-

rhenate. Insoluble in H3O and in bases; soluble in cone, hydro-
chloric acid, converting to the green H s ReCl 6 .
REFERENCE:

I. and W. Noddack. Z. anorg. allg. Chem. 215, 134 (1933).

Ammonium Perrhenate

NH4ReO4

Re2O7 + 2 NH3 + Hj,O = 2 NH4ReO4

484.4 536.6

A solution of Re 3 O 7 in some water is prepared, excess am-

monia is added and the solution evaporated in a platinum crucible
placed on a water bath.
Alternate method: Rhenium sulfides, oxides or rhenium metal
are dissolved in HNO3. The solution is evaporated and diluted
with ammonia. Recrystallization is required ! May be used to
prepare pure rhenium (see p. 1476).
 RHENIUM 1485

PROPERTIES:

Thick, white, hexagonal crystals. Dissociates in air above

200°C to form NH3) H3O and Re 3 O 7 . Solubility: 2.9 (0°C); 6.2
(20°C); 32 (80°C) g. of salt/100 g. H3O; d 3.63. Crystal structure:
HO4 type.
REFERENCE:

I. and W. Noddack. Z. anorg. allg. Chem. 181, 23 (1929).

Barium Perrhenate

Ba(ReO4)2

An aqueous solution of Re 2 O 7 (= HReO4) is neutralized exactly

with baryta water, using neutral red as the indicator. The residue
is dried, and the water-containing salt is converted to anhydrous
Ba(ReO 4)3 in vacuum or by heating to 120°C.
PROPERTIES:

Formula weight 637.80. Colorless columns or rhomboids. Solu-

bility: 1.8 (0°C); 5.3 (20°C); 47 (70°C) g. of salt/100 g. H 3 O.
Solubility in alcohol: 2.4 g/liter of solution at 18.5°C.
REFERENCES:

I. and W. Noddack. Z. anorg. allg. Chem. 181, 25 (1929); W. Lewino.

Thesis, Univ. of Hamburg, 1932.

Barium Rhenate (VI)

BaReO4

Prepared by reducing Ba(ReC>4)2 with ReO 3 andNaOHin a melt.

The apparatus is the same as that used in the preparation of
Na 3 ReO 3 (Fig. 329). Sodium hydroxide (20 g.) is fused in crucible
c under a stream of N 3 ; then, 8.00 g. of Ba(ReO4)3 is added, fol-
lowed by 2.00 g. of ReO s . The melt is heated to 500°C and held at
that temperature for one hour. It is then cooled to 300°C and held
at that temperature for one hour. The heater is then removed and
attachment b cooled with ice water. The melt cake is broken up
and treated with 96% alcohol at 0°C; this loosens the NaOH and
NaReCU in the melt: the former reacts with any unconverted
Ba(ReO4)3 to form NaReO4 and Ba(OH)3; the latter remains in the
I486 26. G. GLEMSER

residue. The product is filtered, using the device shown in Fig. 52,
p. 74, and washed with some alcohol. It contains some NaOH and
Ba(OH) s .
ANALYSIS:

The compound is disproportionated in acetic acid. Theleached-

out Re (VII) fraction is filtered off and precipitated with nitron; the
Re (IV) fraction is oxidized to Re (VII) and also precipitated with
nitron.
PROPERTIES:
Formula weight 387.58. Foliage-green powder; readily dissoci-
ated. Slowly turns black in vacuum and white in air (formation of
ReO4~). Instantaneously dissociated by water, acids and bases.
The presence of a slight amount of free NaOH is required for
stability.
REFERENCE:
I. and W. Noddack. Z. anorg. allg. Chem. 215, 143 (1933).

Rhenium (IV) Sulfide

ReS2

I. Re + 2S = ReS2
186.2 64.1 250.3

Rhenium and sulfur are mixed in stoichiometric proportions

and heated for 18 hours in an evacuated, sealed small quartz
tube at 980-1000°C.
II. Hydrogen sulfide is used to precipitate Re2S7 from a hydro-
chloric acid solution; the precipitate is filtered off with suction
and washed with water and briefly with acetone. It is dried in a
quartz or hard glass tube sealed at one end. It is then heated in
high vacuum to 600°C until no further S sublimes out. The result
is ReS 3 only slightly contaminated with sulfur.
Alternate method: Heating of Re in a stream of H3S to red
heat [H. V. A. Briscoe, P . C. Robinson and E. M. Stoddart, J.
Chem. Soc. (London) 1931, 1441],
PROPERTIES:
Black solid (platelets are seldom recognizable); somewhat
volatile at 1000°C. Strongly attacks quartz at 1000°C. No appreci-
able solubility in bases, alkaline sulfides, hydrochloric andsulfuric
 RHENIUM 1487

acids. Converted by oxidizing agents to HReC>4. d|° 7.506; heat of

formation: —70.5 kcal. Crystal structure: C7 type.

REFERENCES:

I. R. Juza and W. Biltz. Z. Elektrochem. 37, 499 (1931).

II. W. Geilmann and G. Lange. Z. analyt. Chem. 126, 321(1953).

Rhenium (VII) Sulfide

Re2S7

2KReO4 + 7H2S + 2 HC1 = Re2S7 + 2 KC1 + 8 H2O

578.6 155.01. 72.9 596.9 149.1

A solution of KReO 4, containing 30 ml. of hydrochloric acid

per 100 ml. of solution, is saturated for four hours with H 2 S. The
precipitated sulfide is washed with H 3 S-saturated, 3% HC1 water.
The product is filtered in the absence of air, washed and then
dried, first in a high vacuum for two hours at 140°C and then in
high vacuum over freshly prepared P 3 O 5 (60 hours at 165-170°C).
Alternate method: Precipitation with compressed H3S from a
solution of KReO 4 in hydrochloric acid; there is no need for the
high HC1 concentration in this case. The workup is similar to
that described above [W. Geilmann, Z. analyt. Chem. 126, 321
(1943)].

PROPERTIES:

Black, readily oxidized powder. Dissociation to ReS 3 and S

begins at 250°C. Insoluble in hydrochloric and sulfuric acids in
the absence of air; oxidized by nitric acid or H 3 O 3 plus a b a s e
to HReO 4. d | 5 4.866.

REFERENCE:

W. Biltz and F. Weibke. Z. anorg. allg. Chem. 203, 4(1931).

Barium Mesoperrhenate

Ba3(ReO5)2

Prepared by fusion of Ba(ReC>4)3 with NaOH. The apparatus

is the same as used in the preparation of Na 2 ReO 3 (Fig. 329).
1488 26. G. GLEMSER

Crucible c is used to fuse 3 g. of Ba(ReO 4 ) 3 with 5 g. of car-

bonate-free NaOH under a stream of CO 3 -free air. The hot melt
is red and cloudy. After cooling, it is crushed, leached with 90%
alcohol to remove the excess NaOH and the NaReO 4 formed in
the process, then filtered, again washed with alcohol and dried
with suction.

ANALYSIS:

The salt is decomposed with CO 3 -free water; the Ba is pre-

cipitated as BaSO 4 and the ReO4" as nitron hydrogen perrhenate.

PROPERTIES:

Formula weight 944.52. Small, lemon-yellow hexagonal tablets

and columns. Turns red upon heating to 800°C, returns to yellow
on cooling. Stable in dry air. The wet salt is decomposed by CO 2
into BaCO3 and Ba(ReO4)3.

REFERENCE:

I. and W. Noddack. Z. anorg. Chem. 215, 146 (1933).

Workup of Rhenium Residues

Precipitates of nitron hydrogen perrhenate from analyses of

rhenium are collected and stored separately from rhenium solu-
tions .
Workup of nitron precipitates: The material is carefully d e -
composed in a stream of H s , the products washed and oxidized to
Re a O 7 , and the latter dissolved in H a O and concentrated in the
presence of KOH or ammonia. The KReO4 or NH4ReO4 obtained in
this manner can be used without further purification.
Workup of various solutions: To avoid unnecessary contamina-
tion of the air with Re, the solution is neutralized and concentrated
(if necessary, by boiling). It is then cooled and acidified with hydro-
chloric acid and the Re precipitated under pressure as RegS?. The
RegSy is washed and dissolved in KOH + H 3 O S , and the KReO4 is
allowed to crystallize out. If the KReO4 is still not sufficiently
pure, it is reduced with H 3 and oxidized with O a to Re 3 O 7 , and the
latter is used to obtain Re or the perrhenate.
If traces of Mo must be removed, the procedure is as fol-
lows: the Re is precipitated with H3S (under pressure) as Re 3 S 7 ,
the precipitate is dissolved in KOH + H S O 3 , and the traces of Mo
 RHENIUM 1489

are removed by extraction of the neutral solution with 8-hydroxy-

quinoline or chloroform. Following repeated precipitation under
pressure as Re 2 S 7 , the product is dissolved in KOH + H 3 O 2 and
crystallized as KReO4. The KReO4 is recrystallized from hot
water.