SubhashChand,Seema,RekhaRani,Vijayata
CHAPTER – V
SubhashChand,Seema,RekhaRani,Vijayata
CONCLUSIONS &
SUGGESTIONS
The Present work is basically of applied nature. The whole work
is related to the development of new inorganic materials and their
characterization on the basis of certain parameters which ultimately
become helpful in deciding the application of the synthesized materials
SubhashChand,Seema,RekhaRani,Vijayata
for separation purposes. These separations show their significance in
water pollution control by ion exchange. These developed materials
are of specific type of ion-exchangers known as inorganic cation
exchangers. These exchangers are solid materials which are
responsible for a phenomenon known as ion exchange. In least words
almost work is based on a separation technique known as ion-
exchange.
It has been known for a long time that certain minerals can
exchange one ion for another :
R-A+B+ R-B+A+
These developed materials are of specific type of ion
exchangers known as inorganic action exchangers. Though a number
of inorganic cation exchangers have been reported yet there is the
need of more and more and better and better inorganic cation
exchangers. From type of ion-exchangers point of view I would say
that my focus is on inorganic cation exchangers only. In this
connection it isimportant to mention that my exchangers are based on
antimony(IV) and bismuth(III) metal ions. If I state the class of my ion
exchangers on the basis of number of components present in them I can say
that my cation exchangers are three component inorganic cation ion
exchangers. My aim was to develop better exchangers at least from some of
reported ion-exchangers in different ways. On comparing with the reported
exchangers, I am happy to state that my exchangers were found to be better
SubhashChand,Seema,RekhaRani,Vijayata
in one way or the other from some of the reported cation exchangers.
Initially at the time of the submission of my synopsis to C.C.S. University for
the approval of my proposed research plan, infrastructure available at the
place of work, economic aspect and availability of the chemicals and other
required materials in the market were kept in view. After my research work
now I can conclude that all the considerations taken at the beginning proved
to be fruitful in making available the different things required in doing the
different experiments etc. Even after unavailability of any financial support
research work went on smoothly. Time was very important factor as the lab
was available to us from 9.00 am to 5.00 pm only. It was not possible to avail
the lab before and after the stated time. Therefore sometime it was
inconvenient to perform the lengthy experimental procedures. Anyway i
succeeded in synthesizing three new inorganic cation exchange
materials which may be called inorganic cation exchangers. These
exchangers were characterized on the basis of ion exchange capacity,
thermal stability, chemical stability distribution studies and instrumental
studies which included IR, TGA and XRD. Characterization of the
exchangers were done keeping in view the application. The
exchangers were applied for binary separation of metal ion pairs and
removal of metal ions from aqueous media.
First synthesized inorganic cation exchanger is antimony(III)
iodovanadate which was prepared by the mixing of the solutions of
antimony trichloride, potassium iodotate and sodium metavanadate in
3:2:2 ratio respectively. Ion exchange capacity was determined by
SubhashChand,Seema,RekhaRani,Vijayata
column method and I.E.C. was found to be 2.46 meq/g for Na+ ions.
The ion exchange capacity was also determined by PH titration
method. I.E.C. was found to be nearly same. In addition to sodium
ions I.E.C. for K+, Mg2+, Ca2+, and Ba2+ were also determined. The
results are recorded in table 2.4 of chapter II. Thermal stability of the
exchanger was studied in the laboratory using muffle furnace. Different
samples of the exchanger of the same amount were exposed
todifferent temperatures for same time. Loss in weight of each sample
was recorded. It was concluded that there is no loss in weight of the
exchanger up to 500C. At 1000C only 2% loss in the weight of the
exchanger was recorded. Even at 3500C only12% loss in weight was
determined. Heating effect on IEC of the exchanger was also seen. At
500C the exchanger is not found to loose its I.E.C. while at 1000C loss
in IEC was seen to be 0.12 meq/g. Chemical stability was studied against six solutions of different strengths. 2M H2SO4, 4M H2SO4, 4M
HNO3, 4M HCl, 2M NaOH and 2M NH4Cl were found to have effect on
the ion exchanger. Ion-exchanger was completely dissolved in 4M
HCl. Distribution studies were carried out for Mg2+, Zn2+, Cd2+, Pb2+,
Ni2+, Co2+, and Mn2+ using batch method. Kd values were calculated
using the following expression :
Kd =
Where
I = Initial amount of the ion in the solution phase.
SubhashChand,Seema,RekhaRani,Vijayata
F = Final amount of the ion in the solution phase.
V = Volume of the solution (ml).
W = Weight of the ion exchanger (g).
High Kd value was found for Ni2+ that is 111.25 ml/g
while Kd values for Mg2+, Zn2+, Cd2+, Pb2+ were found 90.5, 4.13,
18.4, and 16.44 respectively. Metal ion pairs Ni2+-Zn2+, Ni2+-Pb2+,
Pb2+-Zn2+ and Ni2+-Cd2+ were selected for Binary separation using
the exchanger on the basis of large difference in Kd values of the
metal ion pairs. In Pb2+-Zn2+ metal ion pair 100% elution was achieved
for Pb2+ ions. Toxic metal ions such Pb2+, Cd2+ and Ni2+were
successfully removed using different eluents and exchanger. Different
components of the exchanger were confirmed on the basis of IR.
Thermal stability was also interpreted with the help of TGA curve.
Crystalline nature of the exchanger was ascertained on the basis of
XRD of the exchanger.
Second synthesized inorganic cation exchanger is bismuth(III)
iodotungstate which was prepared by the mixing of the solutions of
bismuth nitrate, potassium iodate and sodium tungstate in 1:2:2 ratio
respectively. Ion exchange capacity was determined by column
method and was found to be 1.00 meq/g for Na+ ions. The ion
exchange capacity was also determined by PH titration method. IEC
was found to be nearly same. In addition to sodium ions I.E.C. for K+,
Mg2+, Ca2+, and Ba2+ were also determined. The results are recorded
in table 3.4 of chapter III. Thermal stabilityof the exchanger was
SubhashChand,Seema,RekhaRani,Vijayata
studied in the laboratory using muffle furnace. Different samples of the
exchanger of the same amount were exposed to different
temperatures for same time. Loss in weight of each sample was
recorded. It was concluded that there is no loss in weight of the
exchanger up to 500C. At 1000C only 2% loss in the weight of the
exchanger was recorded. Even at 3500C only 8% loss in weight was
determined. Heating effect on IEC of the exchanger was also seen. At
500 C the exchanger is found to loose its IEC by 1% while at 1000C
loss in IEC was seen to be 19%. Chemical stability was studied against twenty five solutions of different strengths. 0.05 M H2SO4, 0.05
M HNO3 and 0.05 M HCl were found to have no effect on the ion
exchanger. 0.1M H2SO4, M H2SO4, 0.2 H2SO4, 2M H2SO4, 0.1M
HNO3, M HNO3 0.2M HNO3, 2M HNO3, 0.1M HCI, M HCI 0.2M HCI,
2M HCI, M KOH, 0.2M KOH, 0.1M NaOH, M NaOH, 0.2M NaOH, M NaNO3, 0.2M NaNO3 & 2M NaNO3 solutions on treating with ion-
exchanger dissolved the exchanger partially while the exchanger was
found to be completely dissolved in 2M KOH and 2M NaOH.
Distribution studies were carried out for Mg2+, Zn2+, Cd2+, Pb2+, Ni2+,
Co2+, and Mn2+ using batch method. Kd values were calculated
using the expression as stated earlier.
High Kd value was found for Ni2+ that is 111.25 ml/g
while Kd values for Mg2+, Zn2+, Cd2+, Pd2+ were found 5.85, 12.73,
3.39, and 4.74 respectively. Metal ion pairs Ni2+-Zn2+, Ni2+-Pb2+, Ni2+-
Mg2+ and Ni2+-Cd2+ were selected for binary separation using the
SubhashChand,Seema,RekhaRani,Vijayata
exchanger on the basis of large difference in Kd values of the metal
ion pairs. In Ni2+-Pb2+ and Ni2+-Cd2+ metal ion pairs 100% elution was
achieved for Ni2+ ions. Toxic metal ions such ions Pb2+, Cd2+ and
Ni2+were successfully removed using different eluents and exchanger.
Different components of the exchanger were confirmed on the basis of
IR. Thermal stability was also Interpreted with the help of TGA curve.
Amorphous nature of the exchanger was ascertained on the basis of
XRD of the exchanger.
Third synthesized inorganic cation exchanger is antimony(III)
tungstosilicate which was prepared by the mixing of the solutions of
antimony trichloride, potassium iodotate and sodium metavanadate in
3:2:2 ratio respectively. Ion exchange capacity was determined by
column method and I.E.C. was found to be 0.76 meq/g for Na+ ions.
The ion exchange capacity was also determined by PH titration
method. I.E.C. was found to be nearly same. In addition to sodium
ions I.E.C. for K+, mg2+, Ca2+, and Ba2+ werealso determined. The
results are recorded in table 4.4 of chapter IV. Thermal stability of the
exchanger was studied in the laboratory using muffle furnace. Different
samples of the exchanger of the same amount were exposed to
different temperatures for the same time. Loss in weight was recorded
of each sample. It was concluded that their is no loss in weight of the
exchanger up to 500C. At 1000C only 2% loss in the weight of the
exchanger was recorded. Even at 3500C only 10% loss in weight was
determined. Heating effect on IEC of the exchanger was also seen. At
SubhashChand,Seema,RekhaRani,Vijayata
500 C the exchanger is found to loose its IEC by 8% while at 1000C
loss in I.E.C was seen to be 22%. Chemical stability was studied against six solutions of different strengths. 2M H2SO4, 4M H2SO4, 4M
HNO3, 4M HCl, 2M NaOH and 2M NH4Cl were found to have effect on
the ion exchanger. Ion-exchanger completely dissolved in 4M HCl.
Distribution studies were carried out for Mg2+, Zn2+, Cd2+, Pb2+, Ni2+,
Co2+, and Mn2+ using batch method. Kd values were calculated using
the earlier stated expression.
High Kd value was found for Ni2+ that is 120 ml/g while Kd
values for Mg2+, Zn2+, Pb2+ were found 85, 5 and 16.85 respectively.
Metal ion pairs Ni2+-Zn2+, Ni2+-Pb2+, Pb2+-Zn2+ and Pb2+-Mg2+ were
selected for Binary separationusing the exchanger on the basis of
large difference in Kd values of the metal ion pairs. In Ni2+-Pb2+ and
Ni2+-Cd2+ metal ion pairs 100% elution was ensured for Ni2+ ions. The
results are recorded in table 4.10 of Chapter IV.
Toxic metal ions such ions Pb2+, Cd2+ and Ni2+were
successfully removed using different eluents and exchanger. Different
components of the exchanger were confirmed on the basis of IR.
Thermal stability was also interpreted with the help of TGA curve.
Amorphous nature of the exchanger was ascertained on the basis of
XRD. Aforesaid ion exchangers were compared with some of the
reported ion exchangers such as zirconium(IV) tungstoiodophosphate,
zirconium(IV) tungstate, zirconium(IV) iodophosphate, zirconium(IV)
SubhashChand,Seema,RekhaRani,Vijayata
iodomolybdate, zirconium(IV) iodovanadate, tin(IV) tungstate, tin(IV)
tungstovanado-phosphate, titanium tungstate, thorium tungstate,
iron(III) tungstate, chromium tungstate, bismuth tungstate, antimony
tungstate. I have also compared my two other ion-exchangers
(Bismuth(III) iodotungstate and Antimony(III) tungstosilicate) with
seven other ion exchangers on the basis of IEC, selectivity and nature.
It can be seen from the table 5.2 that my exchangers show higher ion
exchanger capacity. Similar comparison of my ion-exchanger
antimony(III) iodovanadate with five otherexchangers. Ion-exchange
capacity of my exchanger is highest (Table 5.1).
On comparing my ion-exchanger (Bismuth(III) iodotungstate)
with four other reported ion-exchangers on the basis of loss in I.E.C
from a temperature of 1000C to 2000C I found that my exchanger
exhibited very small loss in I.E.C in comparison to others (refer table
5.3).
Effect of temperature on IEC of different ion exchangers
including my exchanger (AIV) was studied. The studies revealed that
my exchanger exhibit better resistance to heat than others (Table 5.4
and Fig. 5.1).
On the basis of the above analysis it can easily be concluded
that my ion-exchangers are far superior to some of the reported ion
exchangers. The conclusion itself proves the worth of the work.
SubhashChand,Seema,RekhaRani,Vijayata
The present work includes synthesis, characterization and
application of three new inorganic cation exchangers. The work can be
expanded by either modifying or introducing the techniques. Some of
the suggestions are given as under:
1. In the present work simple mode of synthesis is adopted the
synthesis can be tried by refluxing the reactants.Refluxing may
produce the material with improved properties.
2. In the present work PH of the resulant solutions obtained by
intermixing of the reactants was maintained one. The variation in
PH of the resultant solutions may be tried to find better materials.
3. I have synthesized inorganic cation exchangers. Synthesis of
hybrid cation exchangers can be done by taking some
organic compounds.
4. Ion-exchanger bed of one ion-exchanger is tried at one time in
the present work. Mixed bed of the cation exchangers can be
used for different applications.
5. Chemical stability against many more chemicals of different
concentrations can be studied. The loss of components of the
exchanger can be determined and therefore the loss of the
structure of the exchanger can be studied.
SubhashChand,Seema,RekhaRani,Vijayata
6. Distribution studies for many moremetal ions can be done and
Kd values for them can be calculated. Their values will help in
finding the selectivity of for metal ions.
7. In the distribution studies more metal ion pairs can be seen and
binary separations can be performed.
8. Though the removal of some metal ions is done with the help of
the three new ion-exchangers, yet removal of some more other
metal ions can be performed.
9. Water softening can be achieved with the help of the
synthesized ion exchangers.
10. Different antacid tablets can be analysed to see the percentage
of Mg2+ (magnesium ions).
11. The exchanger can be analysed quantitatively and then the
empirical formula can be established.
12. Exhausted exchangers can be regenerated to reuse.
Regeneration capacity can also be studied.
13. Potentiometric titration can be performed.
14. Kinetic study may be the part of the work.
SubhashChand,Seema,RekhaRani,Vijayata
TABLE 5.1
SubhashChand,Seema,RekhaRani,Vijayata
COMPARATAIVE STUDY O
FANTIMONY(III)IODOVANADATEWITHFIVEOTHEREXCHANGERS
Sl.
No.
Inorganicionexchanger I.E.C
at 100
I.E.C. LossinLEC
% loss
2. Zirconium(IV)tungstoiodophosp 1.82 1.60 0.22 12.08
3. Tin(IV)tungstovanadophosphate 1.80 1.50 0.30 16.66
4. Zirconium(IV)iodophosphate 1.60 1.40 0.20 12.6
5. Zirconium(IV)iodomolybdate 1.30 1.00 0.30 23.07
TABLE 5.2
SubhashChand,Seema,RekhaRani,Vijayata
COMPARATAIVE STUDY OF BISMUTH(III)DOTUNGSTATE
Sl.
No.
Material/IonExchanger Typeof IEC Selectivity
2. Antimony(III)tungstosilicate Amorphous 0.78 Ni(II), Pb(II)
3. Zirconiumtungstate Semi-transparant - Cs(I),R.K.(I),Na(I)
4. Tin(IV)tungstate Amorphous 0.58 Ba(II),Sr(II),Pb(II),Cu(II)
5. Titaniumtungstate Amorphous 0.4-0.76 Cs(I),Mg(I),Ca(II)
6. Thoriumtungstate Amorphous 0.46 Cs(I),K(I),Na(I)
7. Iron(III)tungstate Amorphous 0.86 Ce(IV)
8. Chromiumtungstate Amorphous 0.02 Th(IV), Hf(IV)
9. Bismuthtungstate - 0.75 Pb(II)
SubhashChand,Seema,RekhaRani,Vijayata
TABLE 5.3
COMPARATAIVE STUDY OF ISMUTH(III)
Sl.
No.
Inorganicionexchanger I.E.C
at 100
I.E.C. LossinLEC
% loss
2. Zirconium(IV)tungstoiodophosphate
1.82 1.60
0.22 12.08
3. Tin(IV)tungstovanadophosphate
1.80 1.50
0.30 16.66
4. Zirconium(IV)iodophosphate
1.60 1.40
0.20 12.6
5. Zirconium(IV)iodomolybdate
1.30 1.00
0.30 23.07
SubhashChand,Seema,RekhaRani,Vijayata
TABLE 5.4
COMPARATAIVE STUDY OFANTIMONY(III)
IODOVANADATEWITH FOUROTHEREXCHANGERS
Sl.
No.
Inorganicionexchanger IEC
at 40°C
IEC
at 50°C
IEC
at 100°C
IEC
at 200°C
IEC
at 300°C
IEC
at 400°C
IEC
at 5 00
IEC
at
°C
1
2.
Antimony(III)iodovanadateZirconium(IV)tu
ngstoidophosphateTin(IV)tungstovanadopho
sphateZirconium(IV)iodophosphateZirconiu
m(IV)iodomolybdate
-
2.20
1.83
2.64
-
2.5
1.82
2.40
1.60
1.89
1.35
1.77
1.00
0.80
0.90
-
0.7
8
-
0.6
SubhashChand,Seema,RekhaRani,Vijayata
TABLE 5.5
COMPARATAIVE STUDY
OFAIVWITH FOUOTHEREXCHANGERS
SubhashChand,Seema,RekhaRani,Vijayata
REFERENCES 1. Singh Premvir, Rawat J.P. and Rahman N.; Talanta (2002) 1-10.
(ZIV) 2. Mishra N.K.; J. Indian Chem. Soc. Vol. 80, July 2003, PP. 714-
716. 3. Nabi S.A., Usmani S. and Rehman N.; 1996. Ann. Chim 2/521
(ZIP). 4. Nabi S.A. and Siddiqui W.A.; 1986 Bull. Chem. Soc. JPh 59,
2003. 5. Siddiqui Weqar Ahmad and Khan Shakil Ahmad; Bull. Maer.
Sci., Vol. 30, No. 1 February 2007, PP. 2007 (TTVP) 6. Qureshi S.Z. and Rehman N.; 1987a Bull. Chem. Soc. Fr. 6 959.
SubhashChand,Seema,RekhaRani,Vijayata
LIST OF PUBLISHED RESEARCH PAPERS
1. Ion exchange capacity determination of Antimony(III) molybdate
a synthesized inorganic material and its characterization
Published in International Transactions in Applied
Sciences.April-June 2010, Volume2, No-2, PP.331-341.
2. Synthesis, Characterization and Analytical Application of
Antimony (III) tungstosilicate an inorganic ion exchanger.
Published in International Transactions in Applied
Sciences.April-June 2011, Volume 3, No-2, P.P. 191-198.
LIST OF PRESENTED RESEARCH PAPERS
1. ‘Synthesis and Characterization of Bismuth(III) iodotungstate, An
Exchanger’. Presented in ‘International Conference on Green
Technologies for Greener Environment’ on January 27th-30th,
2010, C.C.S. University, Meerut.
SubhashChand,Seema,RekhaRani,Vijayata
2. ‘Synthesis and Characterization of Antimony(III) iodovanadate’.
Presented in ‘National Conference on Recent Aspects of
Biological and Medicinal Chemistry’ on 20th & 21st February,
2010, Lajpat Rai Post-Graduate College, Sahibabad
(Ghaziabad) U.P.
3. ‘Synthesis and Characterization of Antimony(III) tungstosilicate
an Inorganic ion exchanger’. Presented in ‘2nd National Seminar
on Recent Trends in Advancement of Mathematical and Physical
Sciences’ on 30-31 January, 2010 at D.N. College, Meerut.
4. ‘Analytical Separation of Toxic Metal from Polluted water using
ion exchanges’. Presented in National Conference Environment
Problems & their Remedial Measure on 24-26 March, 2012 at
Ch. Charan Singh University, Meerut.
5. ‘Water Quality Situation of Some Indian Rivers’. Presented in
National Symposium on Green Technology for sustainable Development on 18 April, 2012 at Radha Govind group of Institutions, Institute of Informatics & Management Sciences.
SubhashChand,Seema,RekhaRani,Vijayata
LIST OF SEMINARS/CONFERENCES/ SYMPOSIUMS ATTENDED
1. National Seminar on Recent Trends in Advancement of
Mathematical & Physical Sciences on 6th November, 2006 at D.N. (P.G.) College, Meerut.
2. National Seminar on “Environment & Human Concern” on
February 17, 2008 at Deva Nagri College, Meerut. 3. National Symposium on Environment and Sustainable
Development on November 14, 2008 at Meerut College, Meerut. 4. National Conference on Recent Aspects of Biological and
Medicinal Chemistry on 20th & 21st February 2010, Lajpat Rai Post-Graduate College, Sahibabad, Ghaziabad.
5. International Year of Chemistry 2011 (Unesco& IUPAC) on
02.12.2011, at Meerut College, Meerut (Co-operation in Quiz Contest held on 2.12.2011). 6. National Seminar on Recent Trends in Advancement of
Mathematical and Physical Sciences on 17-18 March 2012 at Deva Nagari College, Meerut.
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