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61
A Kinetic, Thermodynamic and Stoichiometric Study on the
Reductive Detoxification of Cr(VI) in Aqueous hase !y Sodium
"eta!isu#$hite

I(+,N-./* 0.S.
11
.,/N/* +./.
1
2I/SE* S.-.
2
3(+ 4 /N2IIN* 3./
1

1.Institute of Inorganic 5hemistr6 and !ollution 5ontrol* ,niversit6 of /griculture* !.0.7. 2383 0a9urdi
2.:e"artment of 5hemistr6* 7enue State ,niversit6* !.0.7. 1%211& 0a9urdi 4 Nigeria
1/uthor for corres"ondence; email; saviour.moses<gmail.com

A!stract
In this stud6 Na
2
S
2
(
$
* was assessed as an inorganic reductant of 5r)I# in a=ueous "hase. 3he a>sor>ance of
5r)I# was monitored at 34& nm using a 0ilton +o6 S"ectronic 2%: ,)?)isi>le s"ectro"hotometer at different
tem"eratures 2&' 4 323 @# to stud6 the effect of tem"erature on reduction while* the effect of "A was studied at
"A 3* $* 8* & and 12. 3he effect of concentration was also considered >6 var6ing the concentrations of the
reductants i.e. 4* 6* '* 1% and 12 mg?B# over a "A of $* 2&' @ and $ minutes with concentration of 5r)I# set at
1%mg?B. 3he tem"erature effect showed that the reaction rate increased slightl6 with increase in tem"erature. It
was found that there was a logarithmic increase in time re=uired to reach a certain "ercentage reduction of the
C5r)I#D
initial
* as the "A was increased. 3he 9inetic results showed that the reaction was first 4 order with res"ect
to 5r)I# with the rate e=uation of . 3he activation entro"6 o>tained from "lots of
lnk
obs
?3# vs. 1?3 was -1&8.$3 J.@
-1
.mol
-1
agreeing with the formation of a condensed com"ound. 3he activation
enthal"6 varied from -8.$E1%
-6
- 3.3E1%
-4
9Jmol
-1
# and most cases it was negative showing that the reaction was
rather eEothermic. 3he activation energies o>tained were $'.'8* 6%.'4* 62.'2* 63.'% and 6$.8' 9Jmol
-1
for the
res"ective @elvin tem"eratures of 2&'* 3%'* 31'*323 and 333. 3his increase in activation energ6 with increasing
tem"erature im"lied that >ond >rea9age and "roduct formation was more favoura>le at lower tem"erature.
3he stoichiometr6 suggests that the 5r)I# ; Na
2
S
2
(
$
ratio was 1 5r)I# ; 1.36 Na
2
S
2
(
$
* this value was found to
>e in agreement with the theoreticall6 o>tained result for >oth acidic and al9aline rigimes. 3he findings from the
research show that Na
2
S
2
(
$
could >e used for the reductive detoEification of 5r)I# in "olluted areas.

%& I'TR(D)CTI('
5hromium is one of the a>undant elements in the earthFs crust with an average concentration of 1%% mg B
-1

Emsle6* 2%%1#. 3he concentration range of 5r in rivers and la9es is usuall6 from %.%26 to $.2 Gg B
-1
* in sea
water from %.%%$ to %.' Gg B
-1
* in soil >etween 1 and 3%%% mg g
-1
* in air from %.%%$ to 1% ng m
-3
@otas and
Stasic9a* 2%%%#. 5r is the onl6 elemental solid which shows antiferromagnetic ordering at or >elow room
tem"erature Hawcett* 1&''#. It has also high corrosion resistance and hardness. 0an6 of its com"ounds are
intensel6 coloured. 7ecause of its uni=ue characters* 5r was widel6 used in electro"lating* tanning* "igments*
d6es* industrial water cooling* metal finishing* magnetic ta"es* "a"er "ul" "roducing* "hotogra"hic film*
automotive "arts* chemical manufacturing* wood "rotection* ore and "etroleum refining* metallurgical and
refractor6 "roducing* and other industrial activities 7a>el and ("iso* 2%%8I !ande6 et al.* 2%1%#. :ue to these
industries and other anthro"ogenic activities e.g. dis"osal of "roducts or chemicals containing 5r* or >urning of
fossil fuels#* huge amounts of 5r com"ounds were discharged into the environment* including air* soil* and water
Biu* et al* 2%12#.
/mong the two sta>le forms of 5hromium availa>le in the a=uatic s6stems* 5r )I# and 5r III#*
trivalent chromium is less dangerous. AeEavalent chromium is a "riorit6 metal "ollutant introduced into natural
water from these "rocesses. AeEavalent chromium com"ounds are highl6 toEic when ingested or inhaled.
5arcinogenesis caused >6 heEavalent chromium ma6 result from the formation of mutagenic oEidative :N/
lesions following intracellular reduction to the trivalent form. 5onse=uentl6 an6 heEavalent chromium "resent is
wastewater should >e reduced to 5r III# >efore discharge into the sewer. 3he treatment "rocedure of 5r)I#-
>earing wastewater often com"rise reduction of 5r)I# and an6 of the after treatments such as coagulation-
"reci"itation* active car>on adsor"tion* ion-eEchange or mem>rane se"aration .ang et al., 2%1%I Auang and
Bogan* 2%11 and El 4 ShaJl6* 2%%$#. 3he o>Kectives of our research was to detoEif6 5r)I# >6 reduction using
sodium meta>isul"hite* determine the rate of reduction and also o>tain some thermod6namic "arameters of the
reduction "rocess.
3he two environmentall6 sta>le oEidation states* 5rIII# and 5r)I#* eEhi>it ver6 different toEicities
and mo>ilities. 5rIII# is relativel6 insolu>le in a=ueous s6stems* and eEhi>its little or no toEicit6. In contrast*
5r)I# usuall6 occurs as the highl6 solu>le and toEic chromate anion* and is the sus"ected carcinogen and
mutagen 5osta* 2%%3#.
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62
5hromium)I# is a thermod6namicall6 sta>le form in aero>ic s6stems while chromiumIII# is a sta>le
form in anaero>ic s6stems. 3he fact that >oth 5r forms are often found in aero>ic and anaero>ic environments is
due to the slow 9inetics of 5r)I#?5rIII# redoE reactions Au et al., 2%1%#. 3hus* chromium s"eciation in the
environment ma6 reflect the 9inetics of its redoE transformations and not the e=uili>rium state. :ramatic
differences have >een noted in mo>ilit6* u"ta9e and toEicit6 of >oth chromium oEidation states.
3he ,.S. Environmental !rotection /genc6 ,SE!/# has a""roved several chemical reductants for in
situ treatment of 5r )I# these includeI sodium dithionite* ferrous sul"hate* sodium meta>isul"hite* calcium
"ol6sul"hide* nano - Jero valent Iron. /ll agents o"erate on the same "rinci"le >6 "roviding additional electron
donors to address the high amount of 5r)I# -uertin et al.* 2%%$#.

* "AT+RIA,S A'D "+T-(DS
*&% "ateria#s
/ll solutions were "re"ared using distilled water. /ll glassware and "lastics were washed with distilled water*
rinsed with 1;1# AN(
3
and finall6 with distilled water. 5hromium )I# stoc9 solution was "re"ared from
@
2
5r
2
(
8
7:A# >6 dissolving 2.'2'g of the salt in 1 litre of distilled water. / 2 mgB
-1
5r)I# solution was
"re"ared measuring eEactl6 2mB of the stoc9 solution in 1 B of distilled water. Na
2
S
2
(
$
stoc9 solution was
"re"ared >6 dissolving 1.%g of the salt in a litre of distilled water. Interferences were avoided >6 adding
di"hen6l car>aJide to 5r)I# >efore adKusting the "A of the solution.
*&* +x$erimenta# rocedures.
3he reduction of 5r)I# >6 Na
2
S
2
(
$
was conducted in accordance with the method descri>ed >6 NKo9u and
NweJe 2%%&# with slight modifications. / 1% mB "ortion of 2.% mg?B 5r)I# was measured into a 2$%mB
>ea9er. NeEt* a 2%-mB ali=uot of 2%.% mg?B Na
2
S
2
(
$
was added and the miEture sha9en thoroughl6. 3he "A of
the solution was adKusted using 1.% 0 A
2
S(
4
in the acidic region and 1.% 0 Na(A in the al9aline region >efore
the6 were made to come in contact. 3he ,)?)isi>le s"ectro"hotometer 0ilton +o6 ,S/ S"ectronic 2%:# was
set at 34& nm and the a>sor>ance of 5r)I# was read at that wavelength. 3he a>sor>ance of Na
2
S
2
(
$
was found
to >e wea9 at this wavelength. 3he set u" was done in tri"licate at tem"eratures of 2&'* 3%'* 31'* 323 and 333 @.
In order to stud6 the effect of reaction time on 5r)I# reduction* se"arate set u"s of the a>ove miEture was made
and each monitored for different time intervals of %* 1* 2* 3* 4*$ minutes to minimiJe interference due to
withdrawal of sam"les. 3he reaction was done for the initial "A values of 3* $* 8* & and 12.
3he stoichiometric stud6 was conducted using five concentrations of the reductants; 4* 6* '* 1% and 12
mg?B to assess the concentration 4 de"endence of the reduction. 3he reaction was at 2&' @ and a moderatel6
acidic "A of $. 3he initial concentration of 5r)I# was set at a>out 1%.% mg?B and the reaction time was $
minutes. E=ual volumes of 1%mB each of the reductant and 5r)I# was used for the miEture.

.& Resu#ts and Discussion
.&% +ffect of $-
3a>le 1 "resents the results of the reduction of 5r)I# >6 Na
2
S
2
(
$
at different tem"erature and "A conditions in
a=ueous "hase. / first glance o>servation was that the reaction was fast with more than half of the concentration
reduced at 3%% seconds. 3he rate of reduction was >asicall6 increasing with decrease in "A. 3he rate of reduction
was also slightl6 affected >6 increase in tem"erature with most reaction reaching com"letion at 1'% seconds
when the initial tem"erature was increased to 3%' @. 3he rate in acidic and neutral solutions was faster than in
>asic solution. 3his o>servation agreed with that of 7ill et al.* 1&&'# where an in situ 9inetic reduction of 5r)I#
>6 ferrous iron in solid "hase was studied. 3he findings of the "resent stud6 are also to >e consistent with those
of .itt>rodt and !almer* 1&&6# and ElovitJ and Hish* 1&&4#.
3he rate of reduction de"ends on the s"eciation of chromium in a given "A range as this is shown in
the !our>aiE diagram figure 2#. In order to eE"lain the increase in reaction rate with decreasing "A* one needs to
ta9e into account the s"eciation of >oth 5r)I# and the reductants under these conditions. 3he Eh-"A diagram
shown Hig. 2# "rovides a generaliJed de"iction of the maKor a=ueous chromium s"ecies and redoE sta>ilities
under conditions of chemical e=uili>rium. 3he dominant 5r)I# s"ecies are A5r(
4
-
at "A 1-6 and 5r(
4
2-
at "A L
6. 5r)I# also forms other s"ecies* such as A5r
2
(
8
-
and 5r
2
(
8
2 -
. Aowever* their formation re=uires 5r)I#
concentrations L 1%
-2
molMdm
-3
. 3he increase in reaction rate with decreasing "A can therefore "ro>a>l6 >e
attri>uted to A5r(
4
-
which is reduced more easil6 than 5r(
4
2 4
5otton and .il9inson* 1&''#.
In acidic solution 5r)I# demonstrates a ver6 high "ositive redoE "otential E
o
within 1.33 and 1.3' )*
Higure 1# -reenwood and Earnshaw* 1&'4I Shriver et al. 1&&4* 7all and Nordstrom 1&&'# which denotes that it
is strongl6 oEidiJing and unsta>le in the "resence of electron donors. /s the A5r(
4
-

reduction is accom"anied >6
the A
N
consum"tion as shown in the e=uation >elow;
A5r(
4
-
N 8A
N
N 3e
-
5r
3N
N 4A
2
(
In more >asic solution the reduction of 5r(
4
2-
* generates (A
-
against a gradient as shown in the e=uation >elow
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63
Nie>oer and Jus6s 1&''#. 3he reduction "otential of chromate to 5rIII# h6droEide is -%.13 ) in >asic medium.
5r(
2-
4
N 4A
2
( N 3e
-


5r(A#
3
N $(A
-

.hen a "lot of the logarithm of time ta9en to attain $%O reduction against was made against the "A* it was
found that there was a linear logarithm relationshi" >etween "A and the time ta9en given >6

and the relationshi" showed that the 5r)I# 4 Na
2
S
2
(
$
reaction s6stem rate law has first 4 order de"endence on
CA
N
D. 3his o>servation was o>servation was in agreement with findings o>tained elsewhere 7eu9es et al, 1&&&I
Sweitli9* 2%%2I Nie9er9* et al.* 2%%8 and Iorungwa* 2%14#.


Fig.1. A plot of Concentration of Cr(VI) vs time (secs) for various pH at !" #


Fig.. A plot of Concentration of Cr(VI) vs time (secs) for various pH at $%" #
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64

Fig.$. A plot of Concentration of Cr(VI) vs time (secs) for various pH at $1" #


Fig.&. A plot of Concentration of Cr(VI) vs time (secs) for various pH at $$ #




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6$

Fig. '. A plot of Concentration of Cr(VI) vs time (secs) for various pH at $$$ #



Fig. (. A plot of )ime re*uire+ to reac, '%- re+uction of t,e initial .Cr(VI)/ t
(%.')
at !" an+ $$ # against pH.



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66

Fig. 0 A simplifie+ 1ourbai2 +iagram for c,romium species at 1'% 3C an+ .Cr(a*)/
tot
41%5
"
6
(7ource8 9all an+
:or+strom 1!!", ;ic,ar+ an+ 9ourg 1!!1, :ieboer an+ <us=s 1!"")

.&* Kinetic study
/fter monitoring the reactions at "h6siological tem"erature 2&' @#* the reactions were further considered at
higher initial tem"eratures of 3%'* 31'* 323 and 333 @. 3he reactions were o>served to >e faster as the
tem"erature of the reaction was increased most of the reaction were com"leted at a tem"erature of a>out 3%' @
and at a time of 1'% seconds. / "lot of lnC5r)I#D against time was made figures ' 4 12# and it showed that the
reaction had a first 4 order de"endence on 5r)I#. 3he o>served rate constants k
obs
was o>tained from the slo"es
of the "lots.
Hor each "A and reductant* another "lot of lnk
obs
?3# against 1?3 was made* this was in accordance
with the ElovitJ and Hish* 1&&4#. 3he gra"h was found to >e linear with ver6 nice regression coefficients of
%.&'8 P r
2
Q %.&6%. 3he o>served rate constant was found to >e highest at a "A of 3 and this also increased as the
tem"erature was increased. Hor eEam"le* the k
obs
for the reduction of 5r)I# >6 Na
2
S
2
(
$
was found to 1.228 s
-1

at 2&' @ and when the tem"erature was increased to 3%'@* the k
obs
also increased to 1.26& s
-1
. /nd as the
tem"erature was raised to 31'* 323 and 333 @* the k
obs
* there was a corres"ondent increase of 1.31%* 1.33% and
1.38% s
-1
res"ectivel6. .hen the "A was increased to $* it was o>served that the reaction >ecame slower >ut the
rate still increased as the tem"erature was increased. It was seen that the k
obs
at 2&' @ was %.286 s
-1
and other
tem"eratures such as 3%'* 31'* 323 and 333 @ had %.2'6* %.2&$* %.2&& and %.3%'' s
-1
res"ectivel6. 3his shows
that the reaction is slower at a higher "A and faster at higher tem"erature. 3he higher k
obs
values at lower "A can
>e attri>uted to the fact that there are so man6 "rotons at lower "A that de"lete the electrons there>6 causing
reduction at a higher rate. Increased tem"erature increases the rate of interaction >etween reacting s"eciesI this is
wh6 the k
obs
increased when the tem"erature was increased. 3he trend was also o>served at h6"er al9aline
region regions of "A and 12. /t "A &* the rate of reduction was significantl6 slowI this could >e seen for the
decrease in the k
obs
values. /t a tem"erature of 2&' @* the value was found to >e %.%11 s
-1
>ut rose to %.%11$ s
-1

when the tem"erature was increased to 3%' @ and for 31'* 323 and 333 @* the o>served rate constants >ecame
%.%11'* %.%12 and %.%124 s
-1
res"ectivel6. 3he slow rate o>served at the high "A values can >e attri>uted to the
formation of other s"ecies as seen in figure 3 or the com"lete de"letion of 5r)I# in the solution. 3his
o>servation agrees with the assertions of 7eu9es et. al* 1&&&#.


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Fig. ". A plot of natural logarit,m of .Cr(VI)/ against time (secs) at pH $



Fig. !. A plot of natural logarit,m of .Cr(VI)/ against time (secs) at pH '




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6'

Fig.1% A plot of natural logarit,m of .Cr(VI)/ against time (secs) at pH 0



Fig. 11. A plot of natural logarit,m of .Cr(VI)/ against time (secs) at pH !





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6&

Fig. 18 A plot of natural logarit,m of .Cr(VI)/ against time (secs) at pH 1

3he activation enthal"ies and entro"ies RA
S
and RS
S
# was o>tained from the slo"es and interce"ts of another
"lot of ln@
o>s
?3# against 1?3. 3his is in accordance with the ElovitJ and Hish 1&&4# e=uation

where
) is the tem"erature in @elvin*
k
b
is 7oltJmanFs constant 1.3' T 1%
U23
J?@#*
, is !lanc9Fs constant 6.63 T 1%
U34
Js#* and
+ is the gas constant '.314 J?@?mol#.
3he activation energies was therefore com"uted from the relationshi";
E
a
VRA-3RS


Fig. 1$8 A plot of ln(k
obs
>)) vs 1>) for t,e re+uction of Cr(VI) b= :a

?
'


7ecause of the em"irical manner in which the rate coefficients were derived* the activation "arameters
WHS and W7S must >e ta9en as com"osite values for all reactions "rior to and including the rate-limiting ste".
3he activation entro"6 W7S# is often used as an indicator of the configuration of the activated com"leE. / large
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8%
negative num>er indicates that the reactant molecules are se"arated >6 short >onds* thus the decrease in entro"6
is large and the "re-eE"onential factor Ck
b
)>,# eE"W7S?+#D is small. 3he values of the activation energ6
o>tained when com"ared with that of some organic com"ounds used in chromium reduction was relativel6 lower
at 2&' @. 3he values also revealed that Na
2
S
2
(
$
activation energies that are almost the same at a given
tem"erature and "A. Hor eEam"le* activation energ6 E
a
# of $'.'64$* 6%.'3&$* 62.'1$3* 63.'%2& and 6$.88'3
9Jmol
-1
was o>tained at 2&'* 3%'* 31'* 323 and 333X@ at "A 3 to 12. 3he activation enthal"6 WA# of the
reduction was found to var6 with "A >ut remained constant with change in tem"erature. Hor eEam"le* it
maintained a value of -8.4E1%
-6
9Jmol
-1
at "A 3 >ut for "A $* 8* & and 12* the values >ecame 3.3E1%
-6
* -2.1E1%
-4
-
6.8E1%
-$
and 3.3E1%
-4
9Jmol
-1
res"ectivel6 while the activation entro"6 WS# was -1&8.$323 J.@
-1
mol
-1
for all "A
and tem"erature. 3he action data was com"ared with the values o>tained >6 Yu* 2%%$# at 2&' @ ta>le 1# and it
was clearl6 seen that the WA
Z
o>tained when Na
2
S
2
(
$
was ado"ted as model reductant was lower than the ones
o>tained >6 Yu* 2%%$. 3his is the same when the WS
Z
o>tained was com"ared as it was -1&8.$323 K.@
-1
mol
-1

against the higher values o>tained for the organic reductants.

Ta!#e %& Activation data for Cr(VI) reduction !y or/anic com$ounds at *0 1C
+eductant WH
2
@J?mol# UW7
2
J?@3mol# Ea @J?mol#
)itamin 5 42.4 81.% 63.$
Ethanol 4&.% 12%.2 '4.'
Iso"ro"6l alcohol $3.2 1%8.8 '$.3
7enJ6l alcohol 26.6 1'%.' '%.$
3ri"hen6lcar>inol 4&.4 1%$.% '%.8
7enJh6drol 24.8 1$$.2 8%.&
source8 @u, (%%').

.&. Reaction Stoichiometry
.hile it is 9nown that the reduction of 5r)I# results in the "roduction of 5rIII# s"ecies :eng* 1&&$#* the
reaction with Na
2
S
2
(
$
generates a theoretical stoichiometric e=uation Iorungwa, 2%14#;
2@
2
5r
2
(
8
N 3Na
2
S
2
(
$
N 1%A
2
S(
4
[ 25r
2
S(
4
#
3
N 3Na
2
S(
4
N 2@
2
S(
4
N $A
2
(
3a>le 2 >elow shows the amount mg?B# of 5r)I# consumed when the concentration of Na
2
S
2
(
$
was varied.
Aere* it was o>served that the 4 mg?B of Na
2
S
2
(
$
consumed eEactl6 2.&4 mg?B of 5r)I# giving a stoichiometric
mass >alance 5r)I#? Na
2
S
2
(
$
ratio of 1;1.4. 3his ratio was maintained when the concentration of Na
2
S
2
(
$
was
varied from 4 to 12 mg?B and the result o>tained from the eE"eriment was in agreement with the theoretical ratio
o>tained elsewhere Iorungwa* 2%14#.

TA4,+ *5 Sho6in/ the amount of Cr(VI) consumed as the concentration of 'a
*
S
*
(
0
is varied&
Reductant 'a
*
S
*
(
0
(m/3,) Residua#
(a)
Cr(VI)(m/3,) Consumed Cr(VI)(m/3,)
4 8.%$$6\%.%1 2.&444\%.%1
6 $.$8&4 \%.1% 4.42%6\%.1%
' 4.1$%'\%.11 $.'4&2\%.11
1% 2.6&%$\%.1$ 8.3%&$\%.1$
12 1.23'1 \%.%% '.861&\%.%%
a#0ean value from tri"licate determination \ standard deviation

7& Conc#usion
3his stud6 has demonstrated that whereas Na
2
S
2
(
$
reduced 5r)I# in a=ueous "hase* the reduction rate
decreased with increasing "A and the activation entro"6 WS# of the reduction was largel6 negative with a
relativel6 small value of the activation enthal"6 WA#. 3his gave rise to a -i>>Fs energ6 of activation that has a
smaller value when com"ared with the activation energ6 o>tained from the reduction of 5r)I# >6 some organic
com"ounds under similar eE"erimental conditions. 3hese o>servations are rather advantageous >ecause*
whereas organic com"ounds reduce 5r)I# higher energ6 of activation* Na
2
S
2
(
$
reduced 5r)I# with a lower
energ6 of activation meaning that Na
2
S
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the "rocess in shorter time.

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