Spectroscopic, Optical,Thermal and Microhardness Studies Of 4-Formylnitrobenzene

IJSRD - International Journal for Scientific Research & Development| Vol. 3, Issue 08, 2015 | ISSN (online): 2321-0613

Spectroscopic, Optical, Thermal and Microhardness Studies of 4Formylnitrobenzene S.Sozhaveni1 S.Kanimozhi2 G.V.pandian3 P.C.Jobe Prabhakar4 1,3 Assistant Professor 4Associate Professor 1,2,4 Department of Physics 3Department of Chemistry 1 A.D.M. College, Nagapattinam 2,3,4T.B.M.L. College, Porayar Abstract— An interesting optical organic crystal of 4Formylnitrobenzene crystals has been grown by slow evaporation solution growth technique using CCl4 as growth medium. The solubility of 4-Formylnitrobenzene in carbon tetra chloride at various temperature ranges from 30 0C to 500C was determined. After solubility determination, the metastable zone width of 4-Formylnitrobenzene in CCl4 was determined. The resulting crystals were subjected to FT-IR, UVand-H1 NMR spectral studies. The purity and high thermal stability of the grown crystals were determined using Thermal analysis. Vickers microhardness studies provide information about the hardness of the grown crystal.

Key words: Solution Growth, Spectral Characterization, Microhardness Studies

solubility of 4-Formylnitrobenzene in carbon tetra chloride at various temperature ranges from 300 to 500 was determined [2].

After solubility determination, the metastable zone width of 4-Formylnitrobenzene in CCl4 was determined.

Saturated solutions of 4-Formylnitrobenzene in CCl4 at different temperatures were allowed for systematic slow cooling. The temperature at which the first nucleation was observed which corresponds to their width of metastable zone. The solubility of 4-Formylnitrobenzene and the metastable zone width of 4-Formylnitrobenzene in CCl4 is shown figure 1

I. INTRODUCTION For the past three decades, the field of opto electronics, optic communication has experienced tremendous advancements. Recently the Organic material are gain more attention due to their enormous application in opto electronic and optic communication technologies [1-5].

Organic compounds are often formed by very weak Vander walls and hydrogen bonds and possess high degree of delocalization. Hence they are optically more nonlinear than inorganic crystals. Recent researches have mentioned that organic crystals are bulk in size, hard, stable, and large Nonlinear optical susceptibilities compared to the inorganic crystals but they have poor mechanical properties 4Formylnitrobenzene has wide application in the very essential field of telecommunication and optical information storage devices. Slow evaporation solution growth technique has been widely used to grow organic nonlinear optical and several other types of crystals [6-11]. These crystals are used in the area of optical communication, optical information process and optical computing. Organic molecular non-linear crystals possess shorter wavelength, optical quality, sufficiently larger non-linear co-efficient spectral, structural and optical studies are important tools in the characterization of various materials. The harvested crystals were characterized by FT-IR spectral analysis, UV, X-ray diffraction (XRD), and Microhardness studies.

Fig. 1: The solubility and metastability of 4 Formylnitrobenzene III. RESULTS AND DISCUSSION A. FTIR Spectral Analysis The Infrared spectral analysis has been carried out to understand the chemical bonding and it provides useful information regarding the molecular structure of the compound [12-15]. The Fourier transform infrared (FT-IR) spectrum of 4-Formylnitrobenzene was recorded using KBr pellet technique between 400cm-1 and 4000cm-1 The FT-IR spectrum is shown in figure-2.The peaks at 1344cm-1 and 1517.50cm-1 are assigned to nitro group in aromatic ring.

The peaks at 1603.52cm-1 and 1576.48cm-1. Further confirms the presence of aromatic ring. The peak at 2750 cm-1 shows aldehyde functional group. The peaks at 529.83cm-1 and 460.81cm-1.Further confirms the presence of NO2 group in aromatic ring.

II. EXPERIMENTAL TECHNIQUE The analar sample of 4-Formylnitrobenzene was further purified by repeated recrystallization. The extent of solubility of 4-Formylnitrobenzene in various solvents viz CH3Cl3, CCl4 were determined.

Finally 4Formylnitrobenzene was grown by solution technique using CCl4 as growth medium.

The saturated solution of 4-Formylnitrobenzene was prepared in a beaker at room temperature. Then it was allowed for systematic slow evaporation. Well needle shaped crystals were obtained in one to two days. The

Fig. 4: FT-IR spectrum of 4-Formylnitrobenzene

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Spectroscopic, Optical, Thermal and Microhardness Studies Of 4-Formylnitrobenzene (IJSRD/Vol. 3/Issue 08/2015/168)

B. UV – Visible spectral studies UV-Visible Spectral study is very useful technique to determine the optical properties and transparency of a substance [16-21].The UV-Visible spectrum of 4Formylnitrobenzene crystal was recorded using Lambda 25 spectrometer is shown in figure-3.To determine the transmission range and hence to know the suitability of solution grown 4-Formylnitrobenzene crystals for optical applications, the UV – visible spectrum was recorded. The UV- visible spectrum of solution grown 4Formylnitrobenzene is shown in figure. The spectrum further shows about 85 percent transparency of solution grown 4-Formylnitrobenzene for a wide range between 500 and 2500nm.

Formylnitrobenzene .There is an intense single weight loss at 160oC with a total weight loss at 430oC of about 98 %.The thermogram further shows the thermal stability and crystalline nature of the grown crystal [25-30].Because of the sharp endothermic peaks shows the good degree of crystallinitys of the 4-Formylnitrobenzene.

Fig. 5: Thermoramme of 4-Formylnitrobenzene

Fig. 3: UV-Visible spectrum of 4-Formylnitrobenzene C. NMR Spectral Studies NMR – spectroscopy is used to determine the molecular structure based on the chemical environment of the magnetic nuclei like H1, C13, P31 etc even at low concentrations. In the spectrum there are two characteristic peaks. In 4-Formylnitrobenzene there 2 sets of protons 2ortho protons and 2-meta protons.

The doublet at 7.43 δ and 7.57 δ is assigned to two m-protons. The doublet at 8.12 δ and 8.24 δ is assigned to two o-protons [22-24].

Fig. 4: NMR spectrum of 4-Formylnitrobenzene D. Thermal Analysis Thermal properties of harvested crystal of 4Formylnitrobenzene were studied in powder form by recording TGA and DTA response curve in the temperature range between 00C to 5000C. Thermal studies have been carried out using on SDTQ 600R 20.9 BUILD 20Instrument at a heating rate of 10 0C/min under nitrogen atmosphere.

The thermograme of 4-Formylnitrobenzene shows in figure 9. The DTA analysis shows a sharp peak at 103oC which corresponds to the melting pointing of 4-

E. Microhardness Analysis Measurement of hardness is a useful nondestructive testing method to determine the hardness of the materials. The microhardness value correlates with other mechanical properties such as elastic constants and yield strength. The hardness of a material depends on different parameters such as lattice energy, Debye temperature, heat of formation and interatomic spacing[30].

Fig. 6: Microhardness values vs load for 4Formylnitrobenzene Vickers microhardness test was carried out on 4Formylnitrobenzene crystal using microhardness tester fitted with a diamond indenter. The indentations were made using a Vickers pyramidal indenter for various loads. The diagonals of the impressions were measured using Shimadzu, Model HMV-2 hardness instrument.

The average diagonal length of the indented impression was calculated and the Vickers microhardness number (Hv) was found from the relation Hv=2Psin (θ/2)/d2.If p is the applied load (kg) and d is the average diagonal length of the indentation impressions (mm) and the angle between the opposite faces of the diamond pyramid is θ=136o then Hv in Kg/mm is given by Hv=1.8544(P/d2) kg/mm2 Where, 1.8544 is a constant of a geometrical factor for the diamond pyramid The variation of microhardness values with applied load is shown in figure 7. From the Vickers microhardness studies it observed that the hardness values increases up to load of 50g. For load above 50g crack started developing around the indentation mark which may be due to the

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Spectroscopic, Optical, Thermal and Microhardness Studies Of 4-Formylnitrobenzene (IJSRD/Vol. 3/Issue 08/2015/168)

release of internal stresses. The presence of cracks confirms the decrease in microhardness.

Fig. 8: The plot of log p vs log d Work hardening coefficient n, a measure of the strength of the crystal is computed from the log p-log d plot and it is found to be 3.5.Onitsch [31] inferred that the values of n lies between 1 and 1.6 for hard materials and for soft materials it is above 1.6.

IV. CONCLUSION An Intresting organic 4-Formylnitrobenzene crystal were successfully grown using slow evaporation solution growth technique, using CCl4 as a growth medium. The solubility of 4-Formylnitrobenzene in CCl4 at different temperature was determined which shows that the percentage solubility increases with temperature.

The FT-IR spectral report confirms the purity and functional group of the crystal. The UV-Visible spectrum proves the transparent nature of the crystal between 500 and 2500nm. Nuclear magnetic resonance spectrum of solution grown 4-Formylnitrobenzene also confirms purity by the presence of the peaks, which are characteristic, and in accordance with the molecular structure of 4Formylnitrobenzene. The TGA and DTA traces confirm that the crystal is thermally stable at 1030C. Vickers Microhardness studies shows that the hardness values increases up to load of 50g.The optical transparency, thermal stability, and crystalline nature of 4Formylnitrobenzene may be useful in deciding the application oriented properties.

ACKNOWLEDGEMENT One of the authors G.V.P. thank University Grant Commission, New Delhi for the award of UGC: minor project [File No. 4- 1/2008 (BSR)]. The authors thank the management and principal of T.B.M.L.College for their support. As the author thank C.Anusha,Department of BioChemistry,Bharathidasan University,Trichirappalli. Authors are grateful to Dr. Brindha Department of Center for Advanced Research in Indian System of Medicine (CARISM).

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