w 2-w 3 (gm) w 3 (gm) (gm) 1 bee wax (nor) bee wax (h &c)

Transcription

1 CHAPTER 4 RESULTS The experimental results are presented in the form of Tables and graphs. The density of different waxes in normal and after giving heat treatment and also for the fat in normal condition is determined. The results obtained from FTIR, XRD and GC-MS are presented in the tabular form. The spectra of each sample are shown in this chapter. So that it will become easy for future discussion to get proper interpretation. Apart from structural study, the electrical property like resistivity is measured. In the present investigation the attention is paid for the measurement of dielectric parameter. The dielectric parameter at microwave frequency region is calculated by using microwave bench at a particular frequency of (8.9 GHz). The dielectric parameters are also computed at microwave frequency region using network analyzer in X and P band (8.2 GHz 18 GHz). The results are presented in different Tables for various samples. In addition to microwave frequency region the dielectric parameters are studied in radio frequency region ( Hz) using Network analyzer and the data is presented in tabular form. The V-I plots are drawn based on experimental data. Activation energy is calculated using jig and LCR meter.

2 The density of different samples is determined and tabulated in Table 4.1. It is noticed that the density of the waxes is less than that of water, but after heat treatment specific gravity of waxes increases slightly, when compared to normal samples. Figures to represent FTIR spectra of different waxes in normal and after heat treatment and fat in normal condition. Tables to present FTIR data of various waxes at the normal and after heat treatment and also for the fat in normal condition. The sample is scanned in the range of 4600 to 400 cm -1 with 4cm -1 resolution. Table shows the data of FTIR spectrum of beeswax in normal condition. It contains wave number of the present investigation and standard chart values. The wave numbers 3390 cm -1, 2966 cm -1, 1732cm -1, 1454cm -1, 1180 cm -1, 958 cm -1, 837cm -1 and 729 cm -1 represent the presence of carbonyl group, fatty acids, esters, CH2 bending, C-C vibration, nucleic acid, =CH2 bending and CH2 rocking respectively. Table gives the data of FTIR spectrum of beeswax after heat treatment. The spectrum gives the presence of wave numbers 2918 cm -1, 2851 cm -1, 1738 cm -1, 1464 cm -1 that indicates stretching vibration, symmetric stretching vibration of lipid acyl CH2 group, lipid absorption from cholesterol esters and CH2 bend respectively. Some of the peaks observed in normal beeswax disappeared but the main constituents remain same even after heat treatment. Table shows the data of FTIR spectrum of microcrystalline wax under normal condition. The spectrum reveals the presence of wave numbers 2920 cm -1,2733 cm -1, 2334 cm -1,1462 cm -1, 1377 cm -1, 889 cm -1 and 717 cm -1 corresponds to CH3-asymmetric stretching of

3 CH3, CO2 (atmospheric absorption), CH2 bend, CH3 symmetric deformation, strong =C-H and =CH2, CH2 rocking respectively. Table reveals the data of FTIR spectrum of microcrystalline wax after heat treatment. The spectrum contains all the compounds with wave numbers 2928 cm -1, 2339 cm -1, 1462cm -1, 1377 cm -1, 889 cm -1 and 721cm -1 that indicate CH3-asymmetric stretching of CH3, CO2 (atmospheric absorption), CH2 bend, CH3 symmetric deformation, strong =C-H and =CH2 and CH2 rocking. Table presents the data of FTIR spectrum of paraffin wax (normal). The spectrum represents CH3-asymmetric stretching of CH3, CO2 (atmospheric absorption), CH2 bend, CH3 symmetric deformation, strong =C-H and =CH2 and CH2 rocking with wave numbers 2918 cm -1, 2336 cm -1, 1462 cm -1, 1379 cm -1, 889 cm -1 and 727 cm -1 respectively. Table gives the data of FTIR spectrum of paraffin wax after heat treatment. The spectrum reveals that compounds in normal samples are not altered even after heat treatment. The functional group present are CH3-asymmetric stretching of CH3, CO2 (atmospheric absorption), CH3 symmetric deformation, strong =C-H and =CH2 and CH2 rocking wave numbers 2916 cm -1,2339 cm -1, 1469 cm -1,1379 cm -1, 889 cm -1 and 721cm -1 respectively. Table shows the data of FTIR spectrum of a fat (normal). The spectrum reveals the presence of compounds such as carbonyl group, stretching vibration CH3, CH2, CH 2 or 3 bands, lipid absorption arising from the C=O group of cholesterol esters, triglycerides, nucleic acid, strong =C-H and =CH2 and CH2 rocking with wave numbers 3466 cm -1, 2918 cm -1, 1730 cm -1, 1161 cm -1, 968 cm -1, 891 cm -1 and 721 cm -1 respectively.

4 Table 4. 1 Measurement of density w 1 w 2 w 3 w 2-w 3 w 0 S.No sample (gm) (gm) (gm) (gm) (gm) ρ 1 bee wax (nor) bee wax (h &c) microcrystalline wax (nor) microcrystalline wax (h&c) Paraffin wax (nor) Paraffin wax (h&c) fat (nor) nor: normal; h&c: heat and cool; w 1: weight of sample in air; w 2 : weight of (applied load + thread ) in water; w 3 : weight of (sample + applied load + thread) in water; w 0: loss of weight; ρ :specific gravity.

5 Wave number (cm -1 ) Figure FTIR Spectra of Beeswax (nor) Wave number (cm -1 ) Figure FTIR Spectra of Beeswax (h&c)

6 Table IR data of Beeswax (normal) analyzed from ISSD S.NO Wave number From present Approximate wave number Compound or functional group assignment from ISSD investigation (cm -1 ) from ISSD (cm -1 ) ~ O-H stretching of hydroxyl group H2O (atmospheric absorption) ~ 3400 carbonyl C=O stretching bond C-H asymmetric stretching of CH3 in fatty acids (strong) O-H (very broad) CO2 ( Atmospheric absorption ) Variable C=C (symmetric reduces intensity) alkenes (strong) C=C asymmetric states Lipid absorption arising from the C=O group of cholesterol esters CH2 bend CH3 symmetric deformation C-C vibration Impurities on KBr disks C=O stretching bands in nucleic acid Strong =C-H and =CH Medium =C-H and =CH2 Out of plane bending CH2 rocking

7 Table IR data of Beeswax (h&c) analyzed from ISSD S.NO Wave number From present Approximate wave number Compound or functional group assignment from ISSD investigation (cm -1 ) from ISSD (cm -1 ) ~ 3400 carbonyl C=O stretching bond C-H asymmetric stretching of CH3 in fatty acids Symmetric stretching vibration of lipid acyl CH2 groups (strong) O-H (very broad) CO2 ( Atmospheric absorption ) Lipid absorption arising from the C=O group of cholesterol esters CH2 bend CH2 rocking

8 Wave number (cm -1 ) Figure FTIR Spectra of Microcrystalline Wax (normal) Wave number (cm -1 ) Figure FTIR Spectra of Microcrystalline Wax (h&c)

9 Table IR data of Microcrystalline wax(nor) analyzed from ISSD S.NO Wave number Approximate wave Compound or functional group From present number from ISSD assignment from ISSD investigation (cm -1 ) (cm -1 ) CH3 asymmetric stretching of CH (med) C-H (Aldehyde C-H) CO2( Atmospheric absorption ) C = C, V(C=C) CH2 bend CH3 symmetric deformation Strong =C-H and =CH CH2 rocking Table IR data of Microcrystalline wax (h&c) analyzed from ISSD S.NO Wave number From present investigation (cm -1 ) Approximate wave number from ISSD (cm -1 ) Compound or functional group assignment from ISSD CH3 asymmetric stretching of CH CO2( Atmospheric absorption ) C = C, V(C=C) CH2 bend CH3 symmetric deformation C-C vibration Strong =C-H and =CH CH2 rocking

10 Wave number (cm -1 ) Figure FTIR Spectra of Paraffin Wax (nor) Wave number (cm -1 ) Figure FTIR Spectra of Parffin Wax (h&c)

11 Table IR data of Paraffin wax (normal) analyzed from ISSD. S.NO Wave number From present investigation (cm -1 ) Approximate wave number from ISSD (cm -1 ) Compound or functional group assignment from ISSD CH3 asymmetric stretching of CH CO2 ( Atmospheric absorption ) alkenes (strong) C=C asymmetric states CH2 bend CH3 symmetric deformation Impurities on KBr disks Strong =C-H and =CH CH2 rocking Table IR data of Paraffin wax (h & c) analyzed from ISSD S.NO Wave number From present investigation (cm -1 ) Approximate wave number from ISSD (cm -1 ) Compound or functional group assignment from ISSD CH3 asymmetric stretching of CH CO2 ( Atmospheric absorption ) alkenes (strong) C=C asymmetric states C-H deformation of CH CH3 symmetric deformation Strong =C-H and =CH CH2 rocking

12 Wave number (cm -1 ) Figure FTIR Spectra of Fat (nor)

13 Table IR data of Fat (normal) analyzed from ISSD S.NO 1 Wave number From present investigation (cm -1 ) Approximate wave number from ISSD (cm -1 ) Compound or functional group assignment from ISSD 3466 ~ 3400 carbonyl C=O stretching bond Stretching vibration, CH3, CH2, CH, 2 or 3 bands CO2 ( Atmospheric absorption ) Lipid absorption arising from the C=O group of cholesterol esters C-H deformation of CH Triglycerides C=O stretching bands in nucleic acid Strong =C-H and =CH CH2 rocking

14 Figures to present 1 H1 (proton) NMR spectra of beeswax, paraffin wax, microcrystalline wax and fat respectively. Proton NMR gives the information about the presence of number of hydrogen atoms and the environment around the proton. NMR of bees wax and fat gives the information like the peak present at 0 to 2 ppm, which tells the presence of aliphatic region. Similarly, the peak at 4ppm gives the possibility of presence of acid group. The peak at 2.4 to 2.2 ppm indicates the presence of CH2 molecule at last but one position. The peak at 7.0 ppm shows the solvent used is CDCL3. The presence of triplet at the end tells the CH3 molecule is present at the end of the aliphatic hydrocarbon chain. The proton NMR of microcrystalline and paraffin wax contains peaks at aliphatic region with triplet at the end and shows that the end molecule contains three protons. As the waxes are dissolved in CDCL3, the peak of CDCL3 is identified in between 7.0 to 8.0 ppm.

15 Figure H1 NMR of Beeswax (normal) Figure H1 NMR of Microcrystalline wax (normal)

16 Figure H1 NMR of paraffin wax (normal) Figure H1 NMR of Fat (normal)

17 Figures to present 13 C NMR spectra of various waxes and fat in normal condition. 13 C NMR gives the information about the number of carbon atoms present and their environment. The 13 C NMR spectra of bees wax and fat confirm the presence of acid group since the peak is present in between 180 to 170 ppm. The solvent CDCL3 signal is found nearer to 80 ppm. The presence of peaks in between 10 to 40 ppm confirms that wax and fat have long chain of hydrocarbons in aliphatic region. The 13 C NMR spectrum of microcrystalline wax and paraffin wax confirms the presence of long chain of hydrocarbons in aliphatic region, since the peak is present in between 10 to 40 ppm. The peak at 80 ppm shows the solvent used is CDCL3.

18 Figure C NMR of Beeswax (normal) Figure C NMR of Microcrystalline wax (normal)

19 Figure C NMR of Paraffin wax (normal) Figure C NMR of Fat (normal)

20 Figures to present Gas chromatography and mass spectrum (GC-MS) of various waxes and fat in normal condition. Tables to give GC-MS experimental data. These Tables are concerned to beeswax, paraffin wax, microcrystalline wax and fat in normal condition. The obtained information data is compared with library NIST or WTLEY and predicted name of the sample. Each Table carries information of retention time, name of the compound eluded, its molecular formulae and molecular weight. This reveals with the increase of retention time, the molecular weight of compound eluded also increasing. The physical properties of compound eluded are obtained and tabulated in Tables to Each Table contains the compounds eluded and its physical properties like melting point, boiling point, density and structure. In the present investigation the more attention is paid on the structure whether the compounds is crystalline or amorphous. The compounds that eluded in GC-MS technique show the density less than 1. It is also found that maximum compounds are crystalline in nature. The GC-MS data of microcrystalline wax is tabulated in Tables and Table present the retention time of the compound emerged, its name, molecular formulae and molecular weight. The data signifies microcrystalline wax, which contains alkanes groups only. The molecular weight of the eluded compound increases with increase of retention time. In Table the data in physical parameter are tabulated. From the table, it is noticed that as the retention time increases the melting point and boiling point also increases. The density of a compound is found to be less than 1 and maximum number of compounds is crystalline in nature.

21 The data obtained from GC-MS data of paraffin wax is shown in Tables and The Table gives retention time of the compound emerged, its name, molecular formulae and molecular weight. The data signifies microcrystalline wax containing alkanes groups. The molecular weight of the eluded compound increases with the increase of retention time. Table presents data on the physical properties of paraffin wax. From this table, it is noticed that as the retention time increases the melting point and boiling point increases. The density of the compound found to be less than 1 and maximum number of compounds are crystalline in nature. Tables and present the GC-MS data of fat. Table shows retention time of the released compound, its name, molecular formulae and molecular weight. From the table it is evident that fat contains alkanes and acid groups. It is noticed that higher molecular weight of compound eluded with the increase in retention time. The Table signifies the compounds released with the increasing melting point, boiling point and time. The density of the compound is found be less than 1 and it is also seen that some of the compounds are crystalline in nature.

22 Figure GC-MS spectra of Beeswax (normal) Figure GC-MS spectra of Microcrystalline wax (normal)

23 Table Details of compounds eluded from Beeswax (normal) through GC-MS technique S.No. Retention Time (min) Name of the compound eluded Molecular formula Molecular Weight (gm/mol) Cyclohexadecane C16H Hexadecanoic acid (palmitic acid) C16H32O octadecane (alpha-") C18H Heneicosane C21H octadecenoic acid (oleic acid) octadecenoic acid (stearic acid) C18H34O C18H36O N-Docosane C22H Tricosane C23 H Tetracosane C24H Pentacosane C25H Hexacosane C26 H Heptacosane C27 H Octacosane C28 H Nanocosne C29 H Triacontane C30 H

24 Table Details of compounds eluded from Microcrystalline wax (normal) through GC-MS technique S.No. Retention Time (min) Name of the compound eluded Hexadecane Octadecane Molecular formula Molecular Weight (gm/mol) C16 H C18 H Nanodecane C19H Eicosane C20H Heneicosane C21H Docosane C22H Tricosane C23H Tetracosane C24H Pentacosane C25H Hexacosane C26H Heptacosane C27H Nonacosane C29H Triacosane C30H Hentriacontane untriacontane C31H Dotriacontane C32H Tritriacontane C33H

25 Figure GC-MS spectra of paraffin wax (normal) Figure GC-MS spectra of Fat (normal)

26 Table Details of compounds eluded from paraffin wax (normal) through GC-MS technique S.No. Retention Time in min Name of the compound eluded Molecular formula Molecular Weight (gm/mol) Heneicosane C21H Docosane C22H Tricosane C23H Tetracosane C24H Pentacosane C25H Hexacosane C26H Octacosane C28H Nanocosane C29H Tricontane C30H Dotricontane C32H Tritricontane C33H decyltetracosane C34H

27 Table Details of compounds eluded from Fat (normal) through GC-MS technique S.No. Retention Time (min) Name of the compound eluded Molecular formula Molecular Weight (gm/mol) n-hexane C6H acetic acid Tetradecanoic acid palmitoleic acid (Hexadecenoic Acid) palmitic acid (Hexadecanoic Acid) Margaric acid (Heptadecanoic acid) Oieic acid (Octadecenoic acid) Stearic acid (Octadecanoic acid) C4H8O2 88 C14H28O2 228 C16H30O2 254 C16H32O2 256 C17H34O2 270 C18H34O C18H36O Tetratetracontane C44H90 619

28 Table Physical properties of eluded compounds of Beeswax (normal) using GC-MS S.No Name of the compound eluded M.P ( C) B.P ( C) Density (gm/cm 3 ) Structure 1 Cyclohexadecane 2 Hexadecanoic acid 3 1-octadecane (alpha-") 4 Heneicosane 5 oleic acid 6 stearic acid (76 mm Hg) (76 mm Hg) (2mm Hg) 39 (3 mm Hg) (2mm Hg) (15 mm Hg) 467 (76 mm Hg) 215 (15 mm Hg) (15 mm Hg) 100 (2 mm Hg) 7 Docosane Tricosane Tetracosane crystalline solid at 62 0 C Saturated fatty acids clear semi liquid White waxy crystalline solid unsaturated fatty acids appearance white solid (3 mm Hg) at 25 0 C Colour less crystalline solid crystals soluble in alcohol combustible crystals Pentacosane Hexacosane Heptacosane Octacosane Nanocosne Triacontane white clistening fluffy flakes white crystalline solid (15 mm Hg) 278 (15 mm Hg) 0.78 water in soluble crystals 0.8 White powder White flakes (3 mmhg) White waxy solid

29 Table physical properties of eluded compounds of Microcrystalline wax (normal) using GC-MS SL.No. Name of the compound eluded M.P ( C) B.P ( C) Density (gm/cm 3 ) Structure of the compound 1 Hexadecane colourless solid 2 Octadecane clear semi liquid 3 Nanodecane White crystalline 4 Eicosane Colour less crystalline solid 5 Heneicosane White waxy crystalline solid 6 Docosane Colour less crystalline solid 7 Tricosane (3 mm Hg) crystals soluble in alcohol 8 Tetracosane combustible crystals 9 Pentacosane white clistening fluffy flakes 10 Hexacosane white crystalline solid 11 Heptacosane (15 mm Hg) 0.78 crystalline solid 12 Nonacosane (3 mm Hg) White flakes 13 Triacontane White waxy solid (3 mm Hg) 14 Hentriacontane crystalline solid 15 Dotriacontane Slightly grey shiny flakes 16 Tritriacontane (3 mmhg) - -

30 Table physical properties of eluded compounds wax (normal) using GC-MS of Paraffin S.No. Name of the compound M.P ( C) B.P ( C) Density (gm/cm 3 ) Structure 1 Heneicosane 39 2 Docosane Tricosane Tetracosane Pentacosane Hexacosane Octacosane Nonacosane Tricontane Dotricontane Tritricontane ( 2 mm Hg) at 25 0 C (3 mm Hg) White waxy crystalline solid colourless crystalline solid crystals soluble in alcohol combustible crystals decyltetracosane (15 mm Hg) (3 mmhg) white clistening fluffy flakes 0.8 white crystalline solid 0.8 White powder or waxy solid White flakes White waxy solid crystalline (3 mm Hg) (3 mm Hg) crystalline

31 Table physical properties of eluded compounds of Fat (normal) using GC-MS S.No. 1 n-hexane 2 Name of the compound M.P B.P Density ( C) ( C) (gm/cm 3 ) Structure Color less liquid acetic acid Color less liquid 3 Tetradecanoic acid White solid palmitoleic acid (Hexadecenoic Acid) palmitic acid (Hexadecanoic Acid) Margaric acid (Heptadecanoic acid) Oieic acid (Octadecenoic acid) Clear liquid White solid Colorless crystalline Pale yellow oily liquid Stearic acid Colorless (Octadecanoic acid) wax like solid Tetratetracontane White solid

32 Figures to present X-ray diffraction (XRD) pattern of various waxes in both the conditions (normal and heat treated) and fat in normal condition. The sharp peaks in the pattern indicate that waxes are crystalline in nature. The peaks in fat are found little bit broad compared to other XRD patterns. It is to be noted a baseline shift in diffractograms of all wax samples of the present investigation. The data obtained from the X-ray diffractograms are tabulated in Tables giving the information of the intensity, angle 2Ѳ and inter planar distance (d) of each wax samples in normal and after giving heat treatment and fat respectively. From tables and it is evident that after heating and cooling beeswax, there is a significant shift in the characteristic peaks. In all the cases there is a decrease in the d-spacing. In both the conditions, the intensity is maximum for the peak at d-spacing A (normal) and A (heat and cool). Tables and presents the XRD data of microcrystalline wax before and after heat treatment. The tables contain information like diffraction angle (2Θ), d-spacing (d) and relative intensity. It is interesting to note that the microcrystalline wax presents 6 peaks before the heat treatment. But once it is heated and cooled, it reveals 4 peaks. The peaks at the d-spacing A, A and A in the case of normal wax are missing when the wax sample is heat treated. In other peaks, small shifts are observed due to the heat treatment. In heated sample, the peak at A is more intense compared to normal sample. An additional peak at A is observed in the heat treated sample. Tables and present X-ray data of normal and heat treated paraffin wax respectively. The x-ray diffractograms reveals no significant variation with respect to position and intensity of peaks. It means heat treatment does not change crystallography of paraffin wax. Table shows X-ray data of animal at. Two peaks at A and A with 100% intensity are evident. The next peak of 66% is found at A.

33 Figure XRD pattern of beeswax in normal condition. Figure XRD pattern of beeswax after heat treatment.

34 Table XRD data of Beeswax (normal) Angle, 2Θ d spacing Relative intensity S.No. (degree) ( 0 A) (%) Table XRD data of Beeswax (heat and cool) Angle, 2Θ d - spacing Relative intensity S.No. (degree) ( 0 A) (%)

35 Figure XRD pattern of microcrystalline wax in normal condition. Figure XRD pattern of microcrystalline wax after heat treatment.

36 Table XRD data of Microcrystalline wax (normal) Angle, 2Θ d - spacing Relative intensity S.No. (degree) ( 0 A) (%) Table XRD data of Microcrystalline wax (h & c) Angle, 2Θ d - spacing Relative intensity S.No. (degree) ( 0 A) (%)

37 Figure XRD pattern of paraffin wax in normal condition. Figure XRD pattern of paraffin wax after heat treatment. Figure XRD pattern of Fat (normal)

38 Table XRD data of Paraffin wax (normal) S.No. Angle, 2Θ (degree) d - spacing ( 0 A) Relative intensity (%)

39 Table XRD data of Paraffin wax (heat and cool) S.No. Angle, 2Θ (degree) d - spacing ( 0 A) Relative intensity (%) Table XRD data of Fat (normal) S.No. Angle, 2Θ (degree) d - spacing ( 0 A) Relative intensity (%)

40 Figure shows the graphs drawn between current along y-axis and voltage along x-axis. The curves represent a linear fit passing through the origin. The electrical properties of different waxes in normal and after heat treated conditions and also fat at normal condition are tabulated in Tables (a) to (d). The different size of circular samples are prepared and the V-I characteristics are drawn. The voltage applied to the sample is gradually increased from 0 to 300 volt and the corresponding current is noted. Depending on the area of cross section and thickness of sample the current varies proportionally with voltage. By knowing the resistance, area of cross section and thickness, the resistivity of the sample is computed. The resistance of a particular sample remains constant throughout the experiment.

41 Table (a) V-I data of Beeswax (normal) S.No Voltage, V Current, I Resistance, R Resistivity, ρ (volt) (na) (GΩ) (GΩ.m) Table (b) V-I data of Beeswax (normal) Mean:-9.3, SD:-0.14 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-9.4, SD:-0.1

42 Table (c ) V-I data of Beeswax (normal) S.No Voltage, V Current, I Resistance, R Resistivity, ρ (volt) (na) (GΩ) (GΩ.m) Mean:-9.3, SD:-0.08 Table (d) V-I data of Beeswax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-9.3, SD:-0.13

43 Table (a) V-I data of Beeswax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (b) V-I data of Beeswax (heat and cool) Mean:-3.27, SD:-0.87 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-3.42, SD:-0.07

44 Table (c )V-I data of Beeswax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (d) V-I data of Beeswax (heat and cool) Mean:-3.53, SD:-0.04 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-3.53, SD:-0.04

45 current(na) current(na) current(na) current(na) 6 5 B C D E B C D E voltage(volt) voltage(volt) Figure V-I Characteristics of Figure V-I Characteristics Beeswax (normal) of Beeswax (h & c) B C D E B C D E voltage(volt) voltage(volt) Figure V-I Characteristics of Figure V-I Characteristics of Microcrystalline wax (normal) Microcrystalline wax (h & c )

46 Table (a) V-I data of Microcrystalline wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-12.6,SD:-0.19 Table (b) V-I data of Microcrystalline wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-12.5, SD:-0.18

47 Table (c) V-I data of Microcrystalline wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-12.76, SD:-0.19 Table (d) V-I data of Microcrystalline wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-12.45, SD:-0.21

48 Table (a) V-I data of Microcrystalline wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.29, SD:-0.04 Table (b) V-I data of Microcrystalline wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.26, SD:-0.04

49 Table4.5.4 (c) V-I data of Microcrystalline wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.27, SD:-0.2 Table4.5.4 (d) V-I data of Microcrystalline wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.24, SD:-0.03

50 Table (a) V-I data of Paraffin wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (b) V-I data of Paraffin wax (normal) Mean:-2.22, SD:-0.07 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.0, SD:-0.08

51 Table (c ) V-I data of Paraffin wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.0, SD:-0.03 Table (d) V-I data of Paraffin wax (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-2.2, SD:-0.02

52 Table (a) V-I data of Paraffin wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (b) V-I data of Paraffin wax (heat and cool) Mean:-0.41, SD:-0.01 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-0.44, SD:-0.01

53 Table (c ) V-I data of Paraffin wax (heat and cool) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (d) V-I data of Paraffin wax (heat and cool) Mean:-0.41, SD:-0.02 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-4.3, SD:-0.01

54 current(na) current(na) current(na) B C D E B C D E voltage(volt) voltage(volt) Figure V-I Characteristics of Figure V-I Characteristics Paraffin wax (normal) of Paraffin wax (h & c) B C D E voltage(volt) Figure V-I Characteristics of Fat (normal)

55 Table (a) V-I data of Fat (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (b) V-I data of Fat (normal) Mean:-4.8, SD:-0.2 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-4.8, SD:-0.2

56 Table (c) V-I data of Fat (normal) S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Table (d) V-I data of Fat (normal) Mean:-4.7, SD:-0.2 S.No Voltage, V (volt) Current, I (na) Resistance, R (GΩ) Resistivity, ρ (GΩ.m) Mean:-4.7, SD:-0.15

57 The dielectric property of the samples is calibrated by using microwave bench at fixed frequency 8.9 GHz. To compute dielectric parameter two point method is implemented. The data are tabulated individually for each sample in tables to Each table provides information of length of sample, maximum voltage without load, minimum voltage with load, tangential equation, the three roots of the equation and dielectric constant corresponds to each solution of the tangential equation. According to two point method when dielectric constant of different size of the sample matches, that particular value is taken to be dielectric constant of the sample. The figure to shows the graphically estimation of dielectric constant of the sample. The curves are drawn by taking different samples along the x-axis and dielectric constant along y-axis. The intersection point of the three curves represented the dielectric constant of the sample.

58 Table Data of dielectric constant of Beeswax (normal) using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out load Dr (cm) With load D (cm) Tan(x)-3.26x= Tan(x)+0.04x= Tan(x)+0.02x= , Tan(x)+0.025x= Tan(x)+0.07x= , Tan(x)+0.16x= Table Data of dielectric constant of Beeswax (heat and cool) using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out load Dr (cm) With load D (cm) Tan(x)-3.02x= Tan(x)-0.67x= Tan(x)+0.35x= Tan(x)+0.29x= Tan(x)-0.3x= Tan(x)+0.07x=

59 Table Data of dielectric constant of Microcrystalline wax (normal) using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out load Dr (cm) With load D (cm) Tan(x)-2.86x= Tan(x)+0.1x= Tan(x)+1.07x= Tan(x)+0.37x= Tan(x)-0.1x= Tan(x)+0.04x= Table Data of dielectric constant of Microcrystalline wax (heat and cool) using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out load Dr (cm) With load D (cm) Tan(x)-2.94x= Tan(x)+0.15x= Tan(x)+0.64x= Tan(x)+0.30x= Tan(x)-0.038x= Tan(x)+0.086x=

60 Table Data of dielectric constant of Paraffin wax (normal)using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out load With load Dr (cm) D (cm) Tan(x)-2.33x= Tan(x)+2.48x= Tan(x)+0.48x= Tan(x)+1.06x= Tan(x)+0.06x= Tan(x)-2.58x= S.No Table Data of dielectric constant of Paraffin wax (heat and cool)using microwave bench Length L (cm) Min Vol With out load Dr (cm) Min Vol With load D (cm) β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r Tan(x)-1.84x= Tan(x)+0.30x= Tan(x)+1.074x= Tan(x)-0.93x= Tan(x)+1.105x= Tan(x)+0.176x=

61 Table Data of dielectric constant of Fat (normal) using microwave bench S.No Length Min Vol Min Vol β=2π/λ g Eqution X 1 X 2 X 3 ε r1 ε r2 ε r3 L (cm) With out With load load Dr D (cm) (cm) Tan(x)-3.73x= Tan(x)-5.76x= Tan(x)+0.51x= Tan(x)+0.52x= Tan(x)-0.44x= Tan(x)-0.025x=

62 Micro wave Bench (a) (b) (c) Figure the graphical method for calculating dielectric constant using Micro wave Bench of sample (a) Beeswax(normal), (b) Beeswax(heat andcool),(c) Microcrystalline wax(normal),(d) Microcrystalline wax(heat and cool). (d)

63 (a) (b) ( c ) Figure the graphical method for calculating dielectric constant using Micro wave Bench of sample (a) Paraffin wax (normal), (b) Paraffin wax (heat andcool),(c) Fat(normal).

64 Also the dielectric parameters are measured in microwave frequency region using transmission line technique in Network analyzer. The data obtained of X-band is reported in tables to for different waxes in both conditions and fat in normal condition. Similarly the dielectric parameters measured in P bands are tabulated in tables to The data reveals as the frequency increases, the dielectric constant decreases at both X and P band. The variation of dielectric loss is inconsistent.the parameter such as penetration depth and conductivity depends on the dielectric loss. Therefore the variation of penetration depth and conductivity is also inconsistent. Figures and present the curves drawn by taking dielectric parameters and frequency. Each figure contains four different graphs. The graph (a) shows variation of dielectric loss (ε ) with respect to frequency (ν). The graph (b) represents dielectric constant (ε') verses frequency (ν) of normal condition of waxes and fat, where as the graph (c) and (d) indicates the relation between the dielectric loss (ε ) verses frequency (ν) and dielectric constant (ε') with respect to frequency (ν) after heat treatment.

65 Table Data of Beeswax (normal) in x-band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

66 (a) (b) ( c ) (d) Figure (a), (b), (c ) and (d) shows variation of ε and ε' with frequency in Beeswax (normal) and Beeswax (heat and cool) respectively.

67 Table Data of Beeswax (heat and cool) in x-band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

68 Table Data of Microcrystalline wax (normal) in x-band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

69 (a) (b) (c) (d) Figure (a), (b), (c ) and (d) shows variation of ε and ε' with frequency in Microcrystalline wax (normal) and Microcrystalline wax (heat and cool) respectively.

70 Table Data of Microcrystalline wax (heat and cool) in x- band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

71 Table Data of Paraffin wax (normal) in x-band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

72 (a) (b) ( c ) (d) Figure (a), (b), (c ) and (d) shows variation of ε and ε' with frequency in Paraffin wax (normal) and Paraffin wax (heat and cool) respectively.

73 Table Data of Paraffin wax (heat and cool) in x-band (8.2 GHz 12.4 GHz) S.NO Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)

74 Table Data of Fat (normal) in x-band (8.2 GHz 12.4 GHz) S.No Frequency, ν GHz Dielectric constant, ε' Dielectric loss, ε Penetration depth, dp (cm) Conductivity, σ (x 10-3 mho/cm)