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ISSN: 2278 – 1323
                          International Journal of Advanced Research in Computer Engineering & Technology
                                                                              Volume 1, Issue 4, June 2012



    Behavior of mixture of Sulfamic Acid and
                Sodium Chloride
                                 Dr. Rita A. Gharde1*, Divakar T. Chunarkar 1,

              Department of Physics, Mumbai University, Kalina (Santacruz), Mumbai – 400 008. (India)

                            E-mail ID: gharde.rita@gmail.com, divakar.chunarkar@rediffmail.com

Abstract:-                                                 analyses a revealed the diffraction pattern for
                                                           sulfamic acid and sodium chloride crystal have
         A mono crystal known as single crystal            almost the same set of peaks [2]. Our study also
of sulfamic acid (H2NSO3H) and sodium chloride             found that good quality crystal growth material
(NaCl) is an inorganic non-linear optical material         can only be obtained into doping range this were
was grown by slow evaporation solution growth              suggest a new approach for using material for
technique. In this work, we are interested in              the crystal growth material. It is found that the
growing single crystal for non-linear optical              dielectric constant of the material is enhanced
application. Beside this, we are trying to develop         due to doping of Sodium Chloride so Sulfamic
new material that, have specific thermo                    Acid. This can be used in many application. For
mechanical properties to be used as a                      example. Azo dyes Industries, Influent water
suspension for the mirror in advanced                      Treatment Plant, Swimming pool and material
gravitational waves detector in order to decrease          strength     increasing   in   dyes    etc    [3].
low thermal noise. Crystallization may be carried          Crystallization is important as an industrial
out from a vapor, from a melt or from a solution.          process because of the material that are and
                                                           can be marketed in the form of crystals.
         Nucleation and crystal growth are two
important steps involved in the synthesis of any           Key Words :–Growth from solution, X-ray
material. The present study discuss how the                diffraction, FTIR, nonlinear optical material,
nucleation and crystal growth rates can be                 Melting Point, pH scale and Dielectric studies
modified by the changing experimental                      etc.
parameter like starting regent, solvent,
temperature, pressure etc. Mainly focus on the             Introduction :-
recent progress in the synthesis, properties,
modification and application of crystal growth             Crystallization is an important and industrial
material as whole with special emphasis. A                 process because of the number of martial can
variety of material in the big size dimension has          be marketed in the form of crystals. Its wide use
been synthesis and are characterized [1].                  is probably due to the highly purified and
                                                           attractive form of a chemical solid, which can be
         Crystal growth technology can be used             obtained from relatively impure solution in a
gainfully     to      enhance        biotechnology         single processing step .The shape of the particle
development, has been fabricated and tested                involve the stacking of atom in cretin sequence
with a variety of optical, electrical, magnetic or         direction [4]. The atomic arrangements are
dielectric properties, present study doping of             govern by the inter atomic course and chemical
sulfamic acid and sodium chloride were                     bonds. With growth in size, the crystalline order
prepared by unidirectional crystal and the                 starts appearing and ultimately result in chunks
influence of the compound on structure, quality            of In a particle, the ratio of number of atom, on
and optical properties were investigated. FTIR             the surface to the total number of atom is matter
and X-Ray diffraction and dielectric study                 exhibiting solid like properties inversely


                                                                                                         230
                                      All Rights Reserved © 2012 IJARCET
ISSN: 2278 – 1323
                          International Journal of Advanced Research in Computer Engineering & Technology
                                                                              Volume 1, Issue 4, June 2012


proportional to the particle size. Crystalline             Preparing single crystal is a solid throughout
material exhibits grain structure feature, which           which the atoms or molecule are arranged in a
differ from those shown by bulk solid. The                 regularly repairing pattern [8].
stability of the crystals and the value of the
equilibrium lattice parameter are controlled by            Experimental Set up :
balance between short range repulsive forces
                                                            As shown in fig.1 the schematic diagram of the
and long range coulomb forces. The later forces
                                                           experimental set up is shown in fig. It consist of
are comparatively more affected by the crystal
                                                           a growth ampoule made out of glass with seed
size changes depending on the size the particle.
                                                           mounting pad. An outer glass shield tube
As a result the physical properties such as
                                                           protect and holds the inner growth ampoule. A
magnetic,      Ferro   electricity  and    super
                                                           ring heater positioned at the top of the growth
conductivity of materials are expected to be
                                                           ampoule was connected to the temperature
effected [5].     In conventional slow solvent
                                                           controller and it provides the necessary
evaporation growth, all crystal bounded by
                                                           temperature for solvent evaporation.         The
planner habit faces contain separate region
                                                           temperature around the growth ampoule was
common to each fact having their own sharply
                                                           selected based on the solvent used and was
defined growth direction known as growth
                                                           controlled with the aid of the temperature
sector.
                                                           controller. Depending on the growth rate of the
          The boundaries between these growth              crystal, the ring heater was the moved down
sector are more strain than the extended growth            using a translation mechanism [7].
sector due to mismatch of the lattice on either
                                                           Fig.1 Experiment set up mixture sample
side of the boundary are result of preferential
incorporation impurities into the lateral section.
Further, in solution growth method many of the
commonly observed, characteristic growth
induced defect structure comprising growth the
sector and boundaries, growth bounding, solvent
inclusion, dislocation and staking faults can be
attributed to impurities. Single crystal are free
form internal boundaries. They give rise to
characteristic x-ray diffraction pattern. A single
crystal can be as big as few centimeter or it may
be as small as fraction as a centimeter such
that its feature can not be seen by necked eye.
Such crystal is called mono crystal. It is known
                                                           Charechtarisation:-
that the demotion of the typical unit cell is high
into 5X 10-8cm. Hence even if mono crystal has             X-ray Diffraction Analysis :-
104 unit cell, it size will be 5 x 10-4 cm which
can be seen the necked eye), Following factor to            Powder x ray diffraction spectrum of a grown
grow crystal form solution [6].                            crystal has been recovered on SIEFERT X-ray
                                                           diffracto meter. The sample was scanned for 30
    1) A good solubility for the given solute.             range 20 to 800C and at a scan rate 3mm per
    2) A good temperature coalition of solute
                                                           min. The X-ray diffraction spectrum shown in
       solubility
    3) Less viscosity                                      fig.1. The powder XRD was taken and compared
    4) Less volatility.                                    SADA data [8]. The cut and polish wafer,
    5) Less corrosion and non toxicity.                    fabricated out of the grown doping single crystal
    6) Small vapor pressure.                               was subjected to x-ray diffraction spectrum were
    7) Cost advantage.                                     analyzed and indexed using the XRD



                                                                                                         231
                                      All Rights Reserved © 2012 IJARCET
ISSN: 2278 – 1323
                          International Journal of Advanced Research in Computer Engineering & Technology
                                                                              Volume 1, Issue 4, June 2012


instrument, software package and the data                  Fig.3. FTIR Spectrum of mixture sample
obtained by the powder XRD analysis are in
accordance with the single crystal XRD data.
The calculated plans satisfy the general
reflection condition of space group observed
form the structure determination of the crystal.
In previous study the single crystal XRD reveals
that the Sulfamic Acid crystal belongs to
orthorhombic structure. From this spectrum
proved to be highly useful in determining
structure and dimension of crystal as well as in
the study of number of properties of x-ray is
same as like a previous sulfamic acid sample
the value of 0 for the first order reflection form
the three faces of doping crystal are found [7].           The range of slpfamic acid sample and doping
We conclude that there is not much change in               sample is nearly same. The FTIR spectra of the
the molecular structure of sulfamic acid due to            crystal were recorded in the sulfamic acid and
doping of sodium chloride. As shown in fig.2.              doping sample in the frequency range 400 to
Powder X-ray diffraction pattern of mixture                6000 cm-1 using Jusco spectro meter model 610
sample                                                     FTIR at the resolution of 490 arb. It is an
                                                           important material for possible application the
                                                           single crystal FTIR show that, the doping crystal
                                                           belongs to Centro symmetric space group [9].

                                                           Melting Point :-

                                                           We studied the melting point of grown doping
                                                           crystal by capillary melting method. Crush
                                                           doped crystal sample and filled in the capillary
                                                           tube and measure the melting point with the help
                                                           of the help of the melting point instrument. We
                                                           found that it gives higher heat energy as
                                                           compared to sulfamic acid single crystal. Such
                                                           type of material are used in the photo electric
FTIR :-                                                    effect.

 The recorded FTIR spectra of doped sample as              PH Scale :-
shown in fig.3 were compared with the previous
                                                            The solution are acidic or alkaline depend upon
spectra of sulfamic acid of the functional group.
                                                           the two ions is present grater concentration than
The pick around 5200 cm-1 is due to N-H
                                                           the other [10]. The doping crystal is an acidic
stretching and the bond observe at 3900 cm-1
                                                           medium and its pH value of preparing 1%
arises symmetric abrasion of NH3 group of both.
                                                           solution is 1.82 by using model CL – 46 SR. No.
                                                           4944, power 230 V ac pH meter about 310C
                                                           normal temperature. In this doping crystal we
                                                           found that, Na being highly electro positive
                                                           removes H2 atom from sulfamic acid and form
                                                           Na salt of Sulfamic acid. Hence no effect on the
                                                           crystal. Due to Na+ is more electropositive then
                                                           H+ and hence doping sample formed is more



                                                                                                        232
                                      All Rights Reserved © 2012 IJARCET
ISSN: 2278 – 1323
                          International Journal of Advanced Research in Computer Engineering & Technology
                                                                              Volume 1, Issue 4, June 2012


hard and with high melting than previous crystal.
It is found that doped single crystal are more
clear than the single crystal of sulfamic acid form        Reference:-
that we can predicted that due to doping. The
Impurity inside the crystal is less reduce without             1) Arun Sethi,Reader of Chemestry, University
change.                                                            of Lakhnow.
                                                               2) W.L.      Wang,M.Wang,W.D.         Huang,OPT
Dielectric Studies :-                                              MATTER 27 (2007)609.
                                                               3) K.Shankarnarayanan,P.Ramasamy, Crystal
The mixture single crystal crushed in the powder
                                                                   growth method .
form, there are no any shape and size. Such
                                                               4) K.Shankarnarayanan,P.Ramasamy,Journal
type of crushed material filled in the assemble of
                                                                   of Crystal Growth 280(2005).467-473.
dielectric instrument and found the capacitance
with help of multi meter. The precaution must                  5) Msuhiko Hara, WOlfgana Kloll, Riken review
be taken that the air do not pass through the                      No . 45(2002).
copper plate therefore to used the rubber ban                  6) K.Shankarnarayanan,P.Ramasamy,Journal
packed with fevi quick. The doping material with                   of Crystal Growth 292 (2006) 445-448.
high dielectric constant vales are quite good can              7) R.Ramesh                                Babu,
be used in tunneling devices, insulator,                           K.Se3thuraman,R.Gopalkrishan,P.Ramasam
fabricated capacitance and in other electric field                 y,Journal of Crystal Growth xxx(2006)xxx.
                                                               8) S.A.Martin Brito Das,S.Natrajan,Material
Result at a glance:-                                               letters xx(2007)xxx-xxx.
 Sulfamic acid and sodium chloride doped                       9) Jolanta Prawer,Institute of Physics,Technical
unidirectional seeded single crystal was                           University of Lodz,wolczalska-219,93005
successfully grown by slow evaporation solution                    Lodz Poland.
grown technique.         From the study x-ray                  10) S.S.Gupte,A.Marcalrno,D.Pradhan,C.F.Desai
diffraction, FTIR it is confirm that vibration                     N.J.Melipohi,Allied Physics 89 (2001) 4939.
frequency of doped sample. The crystal is                      11) L.A.Guzman,N.Kubota,M.Yokota,A.Soro,K.A
extremely good of orthorhombic structure and                       ndo,Department of Chemical Engg.IWATE
properties also same as compare to the                             University 435- Ueda.
previous crystal [10]. But hardness are more as                12) Yoshim, Kawahata, Yasunori Tominga
compared to sulfamic acid single crystal and                       Department of Physics and Chemestry
clarity is also very high as like as a diamond                     Ochamomiu University Otsnka,Bunkio-Ku,
crystal than this single crystal [11]. The melting                 Tokyo 112-8610 Japan.
point of the doped crystal is found to be 2110C to
2180 and dielectric constant to be 31088. This
type of material used in the azo dyes industries
                                                                    Divakar T. Chunarkar [M.Sc.-Physics]
strength increase the strength of materials.
                                                                    Department. Of Physics Kalina (Santacruz)
Acknoledgement :-                                                   Mumbai University Mumbai india-4000098.

I am thankful to Dr. D. C. Kothari Head of the                      Dr. Rita A. Gharde [M.Sc. PH.D.]
Department of Physics, University of Mumbai. I                      Assi. Pro. Of Physics
am grateful to thanks Archana and Vrushali
                                                                    Depart. Of Physics
mam and I am also extreamly greatful to Mam.
                                                                    Mumbai University Mumbai (Santacruz)
Ranjana B. Patil Principal, Pravin patil Engg.
                                                                    India-4000098.
and Tech.College, and thankful to all Staff
member of Formokem India Corporation
Kashigaon Branch.



                                                                                                           233
                                      All Rights Reserved © 2012 IJARCET

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230 233

  • 1. ISSN: 2278 – 1323 International Journal of Advanced Research in Computer Engineering & Technology Volume 1, Issue 4, June 2012 Behavior of mixture of Sulfamic Acid and Sodium Chloride Dr. Rita A. Gharde1*, Divakar T. Chunarkar 1, Department of Physics, Mumbai University, Kalina (Santacruz), Mumbai – 400 008. (India) E-mail ID: gharde.rita@gmail.com, divakar.chunarkar@rediffmail.com Abstract:- analyses a revealed the diffraction pattern for sulfamic acid and sodium chloride crystal have A mono crystal known as single crystal almost the same set of peaks [2]. Our study also of sulfamic acid (H2NSO3H) and sodium chloride found that good quality crystal growth material (NaCl) is an inorganic non-linear optical material can only be obtained into doping range this were was grown by slow evaporation solution growth suggest a new approach for using material for technique. In this work, we are interested in the crystal growth material. It is found that the growing single crystal for non-linear optical dielectric constant of the material is enhanced application. Beside this, we are trying to develop due to doping of Sodium Chloride so Sulfamic new material that, have specific thermo Acid. This can be used in many application. For mechanical properties to be used as a example. Azo dyes Industries, Influent water suspension for the mirror in advanced Treatment Plant, Swimming pool and material gravitational waves detector in order to decrease strength increasing in dyes etc [3]. low thermal noise. Crystallization may be carried Crystallization is important as an industrial out from a vapor, from a melt or from a solution. process because of the material that are and can be marketed in the form of crystals. Nucleation and crystal growth are two important steps involved in the synthesis of any Key Words :–Growth from solution, X-ray material. The present study discuss how the diffraction, FTIR, nonlinear optical material, nucleation and crystal growth rates can be Melting Point, pH scale and Dielectric studies modified by the changing experimental etc. parameter like starting regent, solvent, temperature, pressure etc. Mainly focus on the Introduction :- recent progress in the synthesis, properties, modification and application of crystal growth Crystallization is an important and industrial material as whole with special emphasis. A process because of the number of martial can variety of material in the big size dimension has be marketed in the form of crystals. Its wide use been synthesis and are characterized [1]. is probably due to the highly purified and attractive form of a chemical solid, which can be Crystal growth technology can be used obtained from relatively impure solution in a gainfully to enhance biotechnology single processing step .The shape of the particle development, has been fabricated and tested involve the stacking of atom in cretin sequence with a variety of optical, electrical, magnetic or direction [4]. The atomic arrangements are dielectric properties, present study doping of govern by the inter atomic course and chemical sulfamic acid and sodium chloride were bonds. With growth in size, the crystalline order prepared by unidirectional crystal and the starts appearing and ultimately result in chunks influence of the compound on structure, quality of In a particle, the ratio of number of atom, on and optical properties were investigated. FTIR the surface to the total number of atom is matter and X-Ray diffraction and dielectric study exhibiting solid like properties inversely 230 All Rights Reserved © 2012 IJARCET
  • 2. ISSN: 2278 – 1323 International Journal of Advanced Research in Computer Engineering & Technology Volume 1, Issue 4, June 2012 proportional to the particle size. Crystalline Preparing single crystal is a solid throughout material exhibits grain structure feature, which which the atoms or molecule are arranged in a differ from those shown by bulk solid. The regularly repairing pattern [8]. stability of the crystals and the value of the equilibrium lattice parameter are controlled by Experimental Set up : balance between short range repulsive forces As shown in fig.1 the schematic diagram of the and long range coulomb forces. The later forces experimental set up is shown in fig. It consist of are comparatively more affected by the crystal a growth ampoule made out of glass with seed size changes depending on the size the particle. mounting pad. An outer glass shield tube As a result the physical properties such as protect and holds the inner growth ampoule. A magnetic, Ferro electricity and super ring heater positioned at the top of the growth conductivity of materials are expected to be ampoule was connected to the temperature effected [5]. In conventional slow solvent controller and it provides the necessary evaporation growth, all crystal bounded by temperature for solvent evaporation. The planner habit faces contain separate region temperature around the growth ampoule was common to each fact having their own sharply selected based on the solvent used and was defined growth direction known as growth controlled with the aid of the temperature sector. controller. Depending on the growth rate of the The boundaries between these growth crystal, the ring heater was the moved down sector are more strain than the extended growth using a translation mechanism [7]. sector due to mismatch of the lattice on either Fig.1 Experiment set up mixture sample side of the boundary are result of preferential incorporation impurities into the lateral section. Further, in solution growth method many of the commonly observed, characteristic growth induced defect structure comprising growth the sector and boundaries, growth bounding, solvent inclusion, dislocation and staking faults can be attributed to impurities. Single crystal are free form internal boundaries. They give rise to characteristic x-ray diffraction pattern. A single crystal can be as big as few centimeter or it may be as small as fraction as a centimeter such that its feature can not be seen by necked eye. Such crystal is called mono crystal. It is known Charechtarisation:- that the demotion of the typical unit cell is high into 5X 10-8cm. Hence even if mono crystal has X-ray Diffraction Analysis :- 104 unit cell, it size will be 5 x 10-4 cm which can be seen the necked eye), Following factor to Powder x ray diffraction spectrum of a grown grow crystal form solution [6]. crystal has been recovered on SIEFERT X-ray diffracto meter. The sample was scanned for 30 1) A good solubility for the given solute. range 20 to 800C and at a scan rate 3mm per 2) A good temperature coalition of solute min. The X-ray diffraction spectrum shown in solubility 3) Less viscosity fig.1. The powder XRD was taken and compared 4) Less volatility. SADA data [8]. The cut and polish wafer, 5) Less corrosion and non toxicity. fabricated out of the grown doping single crystal 6) Small vapor pressure. was subjected to x-ray diffraction spectrum were 7) Cost advantage. analyzed and indexed using the XRD 231 All Rights Reserved © 2012 IJARCET
  • 3. ISSN: 2278 – 1323 International Journal of Advanced Research in Computer Engineering & Technology Volume 1, Issue 4, June 2012 instrument, software package and the data Fig.3. FTIR Spectrum of mixture sample obtained by the powder XRD analysis are in accordance with the single crystal XRD data. The calculated plans satisfy the general reflection condition of space group observed form the structure determination of the crystal. In previous study the single crystal XRD reveals that the Sulfamic Acid crystal belongs to orthorhombic structure. From this spectrum proved to be highly useful in determining structure and dimension of crystal as well as in the study of number of properties of x-ray is same as like a previous sulfamic acid sample the value of 0 for the first order reflection form the three faces of doping crystal are found [7]. The range of slpfamic acid sample and doping We conclude that there is not much change in sample is nearly same. The FTIR spectra of the the molecular structure of sulfamic acid due to crystal were recorded in the sulfamic acid and doping of sodium chloride. As shown in fig.2. doping sample in the frequency range 400 to Powder X-ray diffraction pattern of mixture 6000 cm-1 using Jusco spectro meter model 610 sample FTIR at the resolution of 490 arb. It is an important material for possible application the single crystal FTIR show that, the doping crystal belongs to Centro symmetric space group [9]. Melting Point :- We studied the melting point of grown doping crystal by capillary melting method. Crush doped crystal sample and filled in the capillary tube and measure the melting point with the help of the help of the melting point instrument. We found that it gives higher heat energy as compared to sulfamic acid single crystal. Such type of material are used in the photo electric FTIR :- effect. The recorded FTIR spectra of doped sample as PH Scale :- shown in fig.3 were compared with the previous The solution are acidic or alkaline depend upon spectra of sulfamic acid of the functional group. the two ions is present grater concentration than The pick around 5200 cm-1 is due to N-H the other [10]. The doping crystal is an acidic stretching and the bond observe at 3900 cm-1 medium and its pH value of preparing 1% arises symmetric abrasion of NH3 group of both. solution is 1.82 by using model CL – 46 SR. No. 4944, power 230 V ac pH meter about 310C normal temperature. In this doping crystal we found that, Na being highly electro positive removes H2 atom from sulfamic acid and form Na salt of Sulfamic acid. Hence no effect on the crystal. Due to Na+ is more electropositive then H+ and hence doping sample formed is more 232 All Rights Reserved © 2012 IJARCET
  • 4. ISSN: 2278 – 1323 International Journal of Advanced Research in Computer Engineering & Technology Volume 1, Issue 4, June 2012 hard and with high melting than previous crystal. It is found that doped single crystal are more clear than the single crystal of sulfamic acid form Reference:- that we can predicted that due to doping. The Impurity inside the crystal is less reduce without 1) Arun Sethi,Reader of Chemestry, University change. of Lakhnow. 2) W.L. Wang,M.Wang,W.D. Huang,OPT Dielectric Studies :- MATTER 27 (2007)609. 3) K.Shankarnarayanan,P.Ramasamy, Crystal The mixture single crystal crushed in the powder growth method . form, there are no any shape and size. Such 4) K.Shankarnarayanan,P.Ramasamy,Journal type of crushed material filled in the assemble of of Crystal Growth 280(2005).467-473. dielectric instrument and found the capacitance with help of multi meter. The precaution must 5) Msuhiko Hara, WOlfgana Kloll, Riken review be taken that the air do not pass through the No . 45(2002). copper plate therefore to used the rubber ban 6) K.Shankarnarayanan,P.Ramasamy,Journal packed with fevi quick. The doping material with of Crystal Growth 292 (2006) 445-448. high dielectric constant vales are quite good can 7) R.Ramesh Babu, be used in tunneling devices, insulator, K.Se3thuraman,R.Gopalkrishan,P.Ramasam fabricated capacitance and in other electric field y,Journal of Crystal Growth xxx(2006)xxx. 8) S.A.Martin Brito Das,S.Natrajan,Material Result at a glance:- letters xx(2007)xxx-xxx. Sulfamic acid and sodium chloride doped 9) Jolanta Prawer,Institute of Physics,Technical unidirectional seeded single crystal was University of Lodz,wolczalska-219,93005 successfully grown by slow evaporation solution Lodz Poland. grown technique. From the study x-ray 10) S.S.Gupte,A.Marcalrno,D.Pradhan,C.F.Desai diffraction, FTIR it is confirm that vibration N.J.Melipohi,Allied Physics 89 (2001) 4939. frequency of doped sample. The crystal is 11) L.A.Guzman,N.Kubota,M.Yokota,A.Soro,K.A extremely good of orthorhombic structure and ndo,Department of Chemical Engg.IWATE properties also same as compare to the University 435- Ueda. previous crystal [10]. But hardness are more as 12) Yoshim, Kawahata, Yasunori Tominga compared to sulfamic acid single crystal and Department of Physics and Chemestry clarity is also very high as like as a diamond Ochamomiu University Otsnka,Bunkio-Ku, crystal than this single crystal [11]. The melting Tokyo 112-8610 Japan. point of the doped crystal is found to be 2110C to 2180 and dielectric constant to be 31088. This type of material used in the azo dyes industries Divakar T. Chunarkar [M.Sc.-Physics] strength increase the strength of materials. Department. Of Physics Kalina (Santacruz) Acknoledgement :- Mumbai University Mumbai india-4000098. I am thankful to Dr. D. C. Kothari Head of the Dr. Rita A. Gharde [M.Sc. PH.D.] Department of Physics, University of Mumbai. I Assi. Pro. Of Physics am grateful to thanks Archana and Vrushali Depart. Of Physics mam and I am also extreamly greatful to Mam. Mumbai University Mumbai (Santacruz) Ranjana B. Patil Principal, Pravin patil Engg. India-4000098. and Tech.College, and thankful to all Staff member of Formokem India Corporation Kashigaon Branch. 233 All Rights Reserved © 2012 IJARCET