W.

Scott Rader
Ljiljana Solujic
E. B. Milosavljevic
J. L. Hendrix
Department of Chemical
and Metallurgical Engineering,
Mackay School of Mines,
University of Nevada,
Reno, NV 89557
J. H. Nelson
Department of Chemistry,
University of Nevada
Reno, NV 89557
Photochemistry of Aqueous
Solutions of Dicyanomercury(II)
and Potassium Tetracyano-
mercurate(Il)
Photochemically induced reactions of dicyanomercury(II) and potassium tetracy-
anomercurate{H) in alkaline aqueous solutions were investigated in detail. The
studies were conducted in the presence or absence of a titanium (IV) oxide semi-
conductor photocatalyst utilizing sunlight as the irradiation source. It was established
that the cyanide ion liberated from the thermodynamically stable mercury-cyano
species can be photocatalytically oxidized via cyanate and nitrite to nitrate. In
addition, the process removes over 99 mol% of mercury from the solution. In the
absence of the photocatalyst, no photoproducts were detected and mercury remained
in solution. The results obtained may have ramifications for the use of solar power
for the efficient treatment of large quantities of precious metals mill tailings wastes
containing various cyanide species. In addition, in order to follow the fate of cyanide
in these experiments, a novel gas-diffusion flow injection analysis system for the
determination of cyanide from the thermodynamically stable mercury-cyano com-
plexes was utilized.

Introduction
Most of the cyanide species in the environment result from
industrial sources such as electroplating, blast furnaces, coke
producing plants, gas works, etc., with the largest volume
generator being precious metals mining operations. Despite
the toxicity of the cyanide species, the mining industry foresees
no satisfactory replacement of cyanidation in gold metallurgy.
Naturally occurring mercury is found in the earth's crust at
concentrations of -0.08 /xg/g (ppm), mostly in the form of
cinnabar (HgS) (Greenwood and Earnshaw, 1984). Elemental
mercury is obtained as a by and/or waste product in precious
metals cyanidation. In the presence of cyanide, mercury can
form various cyanide compounds with Hg(CN)2 being the prev-
alent species. However, in the presence of excess cyanide,
[Hg(CN)4]2~ may be present in appreciable amounts (Sharpe,
1976).
A great deal of research has been done on the photocatalytic
conversion of organic and inorganic compounds utilizing Ti0 2
as a photocatalyst. Frank and Bard (1977a, 1977b) established
that the cyanide ion is photocatalytically oxidized at the surface
of Ti0 2 to cyanate. Our recent investigations (Milosavljevic et
al., 1992; Pollema et al., 1992) verified that cyanide is first
oxidized to cyanate. However, contrary to earlier studies, we
Contributed by the Solar Energy Division of THE AMERICAN SOCIETY OF
MECHANICAL ENGINEERS for publication in the ASME JOURNAL OF SOLAR ENERGY
ENGINEERING. Manuscript received by the ASME Solar Energy Division, Dec.
1993; final revision, Apr. 7, 1994. Associate Technical Editor: C. E. Wyman.
have established that cyanate is subsequently further oxidized
via nitrite to nitrate. In addition, our research group has re-
cently demonstrated that even very stable hexacyanoferrate(II)
and -(III) ions undergo photochemical degradation in the
presence of titanium(IV) oxide producing ultimately nitrate
ion and iron(III) oxide or hydroxide (Rader et al., 1993). It
should be noted that none of the commercially available meth-
ods for removing and/or destroying cyanide (alkaline chlori-
nation, hydrogen peroxide treatment, INCO's S02-air process,
and FeS04 addition) are able to detoxify cyanide from ther-
modynamically stable iron-cyano species (Scott, 1984; Knorre
and Griffiths, 1984; Devuyrst et al., 1984). In addition, there
is no information in the literature concerning whether these
commercial methods are able to completely oxidize cyanide
from mercury-cyano species.
Of all the studies focusing on the photocatalytic conversion
of various species, few have dealt directly with mercury. Ten-
nakone and coworkers (1993) reported that mercury ions are
not photoreduced and deposited as metal on Ti0 2 in an ox-
ygenated solution. Tennakone (1984) also reported that in the
absence of oxygen, there is partial deposition of elemental
mercury, and complete deposition becomes possible only in
the presence of a reducing agent. Serpone (1987), on the other
hand, found that photoreduction of Hg(II) from its chloride
salt occurs even in the presence of oxygen. As expected, this
process is more efficient in the absence of oxygen. Once re-
duction of mercury occurs, either in the presence or absence

Journal of Solar Energy Engineering AUGUST 1994, Vol. 116/125

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of oxygen, the prevalent species reported to be formed is el- RE
emental mercury (Tennakoneetal., 1993;Serponeetal., 1987).
The fact that, to the best of our knowledge, there are no
papers dealing with the photocatalytic conversion of mercury- •pa
P
cyano species, has been the impetus behind the present re- D
search. This paper is a continuation of the feasibility studies A 2.0

-. w
designed to discern whether solar power can be used for the H 1.0
-" v
»w
efficient treatment of wastes containing various cyanide spe- C 1.0
cies.
1
Fig. 1 Flow injection manifold used for quantification of cyanide in the
pretreated sample. C: carrier (0.2 M HCI); R: reagent (0.2 M HCI), A:
Experimental Section acceptor solution (0.01 M NaOH), P: peristaltic pump, I: injection valve
(100 nL sample loop), MC: mixing coil, D: diffusion cell, FC: amperometric
Materials. Titanium(IV) oxide in the mostly anatase form flow-through cell, PO: potentiostat, RE: recorder, W: waste. Flow rates
(70 percent) was obtained from Degussa as material P25, which are given in mL/min.
was shown earlier to have a high efficiency for cyanide oxi-
dation (Rose and Nanjundiah, 1985). This photocatalyst has
a surface area of 50 ± 15 m2/g with an average particle size of
only 30 nm and compacted density of 150 g/L (Degussa Corp., Model 3100 atomic absorption spectrometer coupled to a MHS-
1990). Dicyanomercury(II) was obtained from Aldrich and 10 hydride generation system using NaBH4 as the reductant
used as received. Potassium tetracyanomercurate(II) was pre- (Perkin-Elmer, 1986). In order to compensate the suppression
pared from dicyanomercury(II) and potassium cyanide by the of mercury signals that were observed previously for some
literature method (Brauer, 1963). All other chemicals were of other stable mercury complexes (Sakamoto et al., 1991), all
reagent grade and were used as received. All solutions were the calibrations were performed with Hg(CN)2 standards.
perpared using distilled water. Cyanide was analyzed by a novel analytical method con-
Experimental Procedure. The photocatalyzed conversion sisting of two steps: (1) sample pretreatment, and (2) cyanide
experiments of Hg(CN)2 and [Hg(CN)4]2~ at Ti0 2 particles in quantification finish. In the pretreatment step a sequestering
the sunlight were performed in Reno, NV (39°N) from Apr. agent is added at room temperature to a sample containing
11 to July 27, 1993. In the first experiment (Apr. 11 to Apr. mercury-cyano species. The sequestering agent forms a very
25) 1L of 0.040 mM solutions of K2[Hg(CN)4] or Hg(CN)2 (pH thermodynamically stable complex with the mercury(II) ion.
was adjusted and maintained at 10.5 with a 1.0 M NaOH The resulting ligand-exchange completely releases CN~ from
solution) were placed in four separate large PVC dishes (two the coordination sphere of the corresponding mercury-cyano
dishes containing Hg(CN)2 and two containing [Hg(CN)4]2") complex. The treated samples are then subjected to an assaying
so that the solution depth was about 3 cm and the surface area step in order to determine the cyanide concentrations. In our
approximately 350 cm . To one PVC dish of each type 10.0 g tests we have employed flow injection gas-diffusion with am-
of titanium(IV) oxide powder was added and all four were perometric detection for the quantification of cyanide. The
covered and placed in the sunlight. Two additional covered manifold utilized is shown in Fig. 1.
PVC dishes were placed in the dark, both containing 0.040 The flow injection analysis system depicted operates in the
mM Hg(CN)2 solution. To one of these controls Ti0 2 was following manner: A 100 /xL aliquot of the pretreated sample
added. All solutions were sampled daily around 12:00 noon, is injected by the rotary valve (I). Line (C) is a hydrochloric
and analyzed for cyanide, cyanate, nitrite, nitrate, and soluble acid carrier which takes the injected solution to a merging
mercury. The samples containing Ti0 2 were centrifuged for at point with another hydrochloric acid line (R). A mixing coil
least an hour prior to analyses. positioned downstream ensures thorough acidification of the
To corroborate the results and determine the fate of mercury, sample. The HCN formed on-line diffuses from the donor
the experiments with 0.40 mM mercury-cyano solutions were stream through the PTFE microporous hydrophobic mem-
performed from June 19 to July 11. Two additional controls brane into the high pH acceptor solution (A), which converts
were placed in the dark (both contained 0.40 mM [Hg(CN)4]2~, HCN to NaCN. The acceptor solution flows through an am-
one having 10.0 g of Ti0 2 added). Samples were taken and perometric cell equipped with a silver working electrode, a
analyzed for the species described above. The final experiment platinum counter electrode and an Ag/AgCl reference elec-
was done on July 27, 1993 in which solutions of Hg(CN)2 and trode. Cyanide is quantified at the silver working electrode
[Hg(CN)4]2~ (0.40 mM) in the presence of Ti0 2 were irradiated. which is kept at a potential of 0.10 V versus the reference
Samples were taken each hour and analyzed. electrode. The precision of the method is better than a relative
standard deviation of two percent (at sub /ig/mL levels) with
To understand the fate of mercury, several qualitative and a throughput of 30 sample per hour. The limit of detection is
semi-quantitative experiments were done on the second set of approximately 2 /xg/L.
samples (June 19-July 11). At the end of the experiment, all
solutions which contained Ti0 2 were centrifuged and the fil-
trates were discarded. The Ti0 2 containing the deposited mer- Results and Discussion
cury species was washed with distilled water thoroughly, and
then placed into several centrifuge tubes. The following re- Solar Irradiation of Hg(CN)2. The results of the speciation
agents were then added separately: distilled water, dilute HN0 3 studies for the photocatalyzed conversion of Hg(CN)2 in the
(0.1 M), dilute HCI (0.1 M), and concentrated HN0 3 . The presence of Ti0 2 particles are shown in Fig. 2((a) 0.040 mM
solutions were analyzed for mercury using the atomic absorp- and (b) 0.40 mM). As may be seen from this figure, solar
tion method described below. An additional experiment was irradiation in the presence of Ti0 2 very effectively decomposes
performed in which no reductant was used in the CVAAS (cold Hg(CN)2. In the experiment with an initial Hg(CN)2 concen-
vapor atomic absorption spectroscopy) system. tration of 0.040 mM (similar concentrations of mercury were
observed in actual tailing impoundments), the CN" values
5
Analytical Procedures. Concentrations of cyanate, nitrite decrease below the detection limit (2 /ug/L; 7.7xl0~ mM)
and nitrate were determined by a previously described ion within seven days. A similar CN~ concentration profile was
chromatography method (Pollema et al., 1992). observed for the experiment illustrated in Fig. 2(b) (initial
Soluble mercury was monitored utilizing a Perkin-Elmer Hg(CN)2 concentration of 0.40 mM). In the same experiment,

1 2 6 / V o l . 116, AUGUST 1994 Transactions of the ASME

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 DATE
Fig. 2(a)
T I I i I I I I I I i i i i i i i i
& & & & & J? & * * *
DATE
Fig. 2(b)
Fig. 2 Concentration profiles for 14-day sunlight irradiation of a 0.040
mM Hg(CN)2 solution (a) and 22-day irradiation of a 0.40 mM Hg(CN)2
solution (b) in the presence of a Ti0 2 phtocatalyst: ( v ) C N ~, ( • ) O C N ~,
(a)Hg(ll), a n d ( i ) N O - 3
the concentration of cyanate rises rapidly to —0.60 mM (75
mol%) in one day and levels off at -0.14 mM (17.5 mol°7o)
after 19 days. The concentration of OCN~ in the 0.040 mM
experiment reaches the maximum value of 0.057 mM (71 mol%)
after two days. The concentration of the same species at the
end of the irradiation is -0.027 mM (33 mol°7o). As may also
be seen from Figs. 2(a) and 2(b) the final N03" concentrations
are 0.058 and 0.660 mM, respectively. This corresponds to 71
and 83 mol% conversion of initially present cyanide. Finally,
as can be seen from this figure, mercury is almost completely
removed from the irradiated solutions to the levels of ap-
proximately 60 /tg/L (a value that corresponds to the solubility
of elemental mercury).
Solar Irradiation of [Hg(CN)4]2~. The results of the spe-
ciation studies for the photocatalyzed conversion of
[Hg(CN)4]2~ in the presence of Ti0 2 particles at two different
concentration levels are shown in Fig. 3. As may be seen from
this figure, solar irradiation in the presence of a photocatalyst
also effectively decomposes [Hg(CN)4]2". In the experiments
Journal of Solar Energy Engineering
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Fig. 3(a)
i — i — r T — i — i — i — i — i — i — i — i — i — i — i — i — i — i — i — i — i — i — i — r
* ^ $ & & & & ^ * * * * * &
DATE
Fig. 3(b)
Fig. 3 Concentration profiles for 14-day sunlight irradiation of a 0.040
mM [Hg(CN)4]2_ solution (a) and 22-day irradiation of a 0.40 mM [Hg(CN)4]2-
solution (b) in the presence of a Ti0 2 photocatalyst ( T ) CN ~, ( • ) OCN~,
(a)Hg(ll), and ( A ) NO-3
with initial [Hg(CN)4]2" concentrations of 0.040 and 0.40 mM,
the CN~ values decrease below the detection limit within six
and ten days, respectively. In the 0.40 mM experiment, the
concentration of cyanate rises rapidly to reach the maximum
after three days at 1.13 mM (71 mol%) level. At the end of
this experiment the cyanate concentration is found to be 0.35
mM (22 mol%). As may be seen from Fig. 3(a) the corre-
sponding OCN" values for the 0.040 mM experiment are found
to be 0.122 mM (76 mol%) and 0.064 mM (40 moI%). The
N03~ concentrations at the end of the experiments are 0.108
and 1.29 mM, which corresponds to 68 and 81 mol% con-
version of initially present cyanide, respectively. Finally, as
may be seen from this figure, mercury is almost completely
removed from the irradiated solutions decreasing to a level of
~60/xg/L.
Small amounts of NO2" are also detected by ion chroma-
tography in all the sunlight irradiation experiments with the
photocatalyst present (maximum levels of — 13 and — 20 mol%
for the 0.40 and 0.040 mM experiments, respectively). Similar
AUGUST 1994, Vol. 116/127

TIME
Fig. 4 Concentration profiles for one day sunlight irradiation experi-
ments for a 0.40 mM Hg(CN)2 solution [ ( i ) CN~ and ( • ) Hg(ll)] and for
a 0.40 mM [Hg(CN)J2_ solution [(v) CN" and ( a ) Hg(ll)]
phenomena were reported in our previous paper (Pollema et
al., 1992) where it was unequivocally established that nitrite
is an intermediary product in the photocatalytic oxidation of
cyanate to nitrate. In addition, it should be noted that mass
balance calculations indicate that the analyzed species (CN~,
OCN~, N02~ and N0 3 ") account for about 90-100 mol% of
the initial cyanide concentrations in all of the photocatalytic
experiments.
In all experiments without Ti0 2 and in the control experi-
ments performed in the dark (with and without the photoca-
talyst) the decrease in cyanide and soluble mercury
concentrations are less than 5 mol% and no formation of
cyanate, nitrite and nitrate is observed.
From all the data presented it may be concluded that oxi-
dation of CN" from Hg(II) species in the presence of Ti0 2
follows the same path as that previously established for free
cyanide (Pollema et al., 1992) and for cyanide from thermo-
dynamically stable Fe(II) and Fe(III) complexes (Rader et al.,
1993). In each case cyanide is oxidized to nitrate through the
intermediate formation of cyanate and nitrite according to the
mechanism that has been described and debated (Frank and
Bard, 1977a, 1977b; Pollema et al., 1992; Milosavljevic et al.,
1992; Peral et al., 1990):
Ti0 2 + # i ; - ~ T i 0 2 + e ~ + h +
+ +
CN~+H20 + 2h ->OCN"+2H
+ +
O C N - + 3 H 2 0 + 6 h - N 0 2 : + C 0 2 + 6H
N0 2 " + H 2 0 + 2h + - N03~ + 2H + (4)
The reactions (2)-(4) are overall reaction schemes (without
implying mechanistic detail). It is quite possible that other
oxidizing agents produced at the valence band of the semi-
conductor, such as hydroxyl and/or perhydroxyl radicals, are
responsible for oxidation of the CN" ion.
Fate of Mercury. Figure 4 illustrates the concentration pro-
files for the one day irradiation experiment of the Hg(CN) 2
and [Hg(CN)4]2~~ solutions in the presence of Ti0 2 . As may
be seen, cyanide levels decrease substantially as a function of
the irradiation time. For example, after 12 hours, less than 1
mol^o of CN~ remains in the solution that initially contained
0.40 mM Hg(CN) 2 . On the other hand.when [Hg(CN) 4 ] 2 " is
irradiated, only about 50 mol% of CN~ is photocatalytically
oxidized to OCN". In addition, almost all of the soluble mer-
cury is precipitated from the irradiated Hg(CN) 2 solution, how-
1 2 8 / V o l . 116, AUGUST 1994
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ever no substantial change in Hg-concentration is found even
after 12 hours of irradiating the [Hg(CN) 4 ] 2 " solution. These
observations, in conjunction with the relatively high K{ and
K2 values found for the dissociation of C N - from [Hg(CN)4]2~
(K1 = 2.2x 10" 3 ; K2 = 2.8x 10" 4 ) (Sharpe, 1976), indicate that
the first step in the photocatalytic conversion of tetracyanom-
ercurate(II) is the dissociation of the weakly coordinated CN"
ions:
[Hg(CN)4]2 " # Hg(CN) 2 + 2CN " (5)
Hence, it is safe to assume that the decrease in soluble mercury
concentration occurs by the photo-reduction of Hg(CN) 2 spe-
cies.
Several qualitative and semi-quantitative experiments were
performed in order to elucidate the nature of the mercury
species present in the ash colored precipitate found at the
surface of Ti0 2 after the irradiation experiments. When filtered
Ti0 2 is treated with dilute HCI or H N 0 3 for two hours, only
a part of the gray precipitate dissolves and the CVAAS analyses
of the filtrate show soluble mercury present. When concen-
trated nitric acid is added, no gray precipitate on Ti0 2 is visible
after 30 minutes and, as expected, the concentration of mercury
in the solution is higher than in the previous experiments. In
addition, it should be noted that a yellowish-orange precipitate
of HgO is observed on the walls of the PVC dishes in which
the irradiation experiments are carried out. These observations
indicate that Hg(I) and/or Hg(II) oxides, as well as elemental
mercury are precipitated onto the photocatalyst. The presence
of Hg(0) is further supported by a noticeable signal obtained
by the CVAAS experiment in which no reductant is utilized.
A plausible reaction mechanism for the conversion of
Hg(CN)2 to the different mercury species experimentally ob-
served can be summarized by the following equations:
2Hg2++2e--Hg2+ (6)
Hg|^+2e-~2Hg(0) (7)
2Hg(0) + H 2 0 ** Hg 2 0 + H 2 (8)
H g 2 O ^ H g O + Hg(0). (9)
Equations (6) and (7) represent the photocatalytic processes in
which Hg(II) species are reduced to Hg(I) and/or Hg(0) by the
reaction with photogenerated electrons in the conduction band
of Ti0 2 . Equation (8) is based on the research of Tennakone
and Wickramanayake (1986) which established that in the pres-
ence of Ti0 2 in an alkaline aqueous mixture water is photo-
reduced, oxidizing Hg(0) to Hg 2 0. It is well known that Hg(I)
compounds disproportionate to Hg(0) and Hg(II) Eq. (9))
(Greenwood and Earnshaw, 1984). The complexity of the con-
duction band reduction processes is further increased by the
(1) fact that in the air-equilibrated suspensions oxygen is com-
peting with mercury(II) for the photogenerated electrons.
(2)
(3)
Conclusion
The present study has demonstrated that by using sunlight
as the irradiation source it is possible to completely oxidize
cyanide from the thermodynamically stable dicyanomer-
cury(II) and tetracyanomercurate(II) species in the presence of
titanium(IV) oxide. In addition, the process removes over 99
mol% of mercury from the solution. Since the photochemical
products are significantly less hazardous contaminants than
cyanide, photocatalytic oxidation may be a viable method for
decontamination of wastes containing various mercury-cyano
species.
Acknowledgments
The authors wish to acknowledge the financial support of
the United States Bureau of Mines under the Mining and Min-
eral Resources Institute Generic Center Program (Grant
Transactions of the ASME
Gl 125232-3226, Mineral Industry Waste Treatment and Re-
covery Generic Center).
References
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