6.2: Melting point determination of Succinic Acid:
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1 6.1: Results: In the present study, an embedded system for determining the melting point of chemicals is developed. The measuring system has temperature sensitivity up to 0.07 C with good accuracy. The heating block required for determination of melting point is custom made. The temperature controller which provides a programmable heating rate to the heating block is also designed. The visual imaging device which is used to recorded the process. It can be saved and replayed many times to confirm the change of material under study. The real time melting point graph for temperature versus % of transmittance (photo detector data) is plotted in MATLAB. The entire data is stored in a specific file for ready reference. Melting point test is done for various chemicals and the data is presented in the next section. 6.2: Melting point determination of Succinic Acid: The sample Succinic acid [56] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 197 C. The sample has shown a near flat response up to 186.2ºC and a sudden transition took place and stayed high at C prior to this at 120ºC the particle realignment at micro level took place. This has been observed through first order derivative graph. After crossing 186.2ºC the optical transition started a steep rise in the optical data is observed and recorded. The transition is noted to 188.6ºC which falling standard values. Figure 6. 1 shows the melting point graph of Succinic acid. 224
2 Figure 6.2 shows the first order derivative graph of Succinic Acid. In the derivative curve noise like disturbance is observed from 120 C to 130ºC. Later remain flat and produced a transition at 187.9ºC. This value is the actual melting point of Succinic acid. The transitions that have been observed from 120ºC to 130ºC might be realignment of particles in the capillary tube. Table 6.1 gives the information of Succinic acid. 225
3 Table 6.1: Melting point data of chemical compound Succinic Acid S. No. Parameter Value 1 Name of the chemical compound Succinic Acid 2 Chemical formulae C 4 H 6 O 4 3 Status of the chemical compound Dry powder 4 Melting point range Image of the capillary after the Melting process 226
4 Figure 6.1: Melting point graph of Succinic acid. 227
5 D D=187.9 Figure 6.2: First order derivative graph of Succinic Acid. 228
6 6.3: Melting point determination of Benzamide The sample Benzamide [57] is filled into the capillary tube and inserted into melting point apparatus subjected for heating from room temperature to 135 C. The sample has shown a flat response up to 128.6ºC and sudden transition took place and stayed high at C prior to this at 90 to 100ºC the particle realignment at micro level took place. This has been observed through derivative curve. The transition is noted to C which falling standard values. Figure 6.3 shows the melting point graph of Benzamide. Figure 6.4 shows the first order derivative graph of benzamide. In the derivative curve noise like disturbance is observed from 90 C to 100ºC. Later remain flat and produced a transition at 130ºC. This value is the actual melting point of benzamide. The transitions that have been observed from 90ºC to 100ºC might be evaporation of water particles associated with the sample. In the normal graph this was not found very clearly, where as in the derivative curve it is clearly observed that water might have evaporated from the sample. Table 6.2 gives the information of benzamide. 229
7 Table 6.2: Melting point data of chemical compound Benzamide S. No. Parameter Value 1 Name of the chemical compound Benzamide 2 Chemical formulae C 7 H 7 NO 3 Status of the chemical compound White Powder 4 Melting point range Image of the capillary after the Melting process 230
8 Figure 6.3: Melting point graph of Benzamide 231
9 Figure 6.4: First order derivative graph of benzamide. 232
10 6.4: Melting point determination of Benzoic Acid The sample Benzoic Acid [58] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 130 C. The sample has shown a flat response up to 121.3ºC and sudden transition took place and stayed high at C prior to this at 98.9ºC the particle realignment at micro level took place. This has been observed through derivative curve. The transition is noted to C which falling standard values. Figure 6.5 shows the melting point graph of Benzoic Acid. Figure 6.6 shows the first order derivative graph of Benzoic acid. In the derivative curve noise like disturbance is observed from 90 C to 100ºC. Later remain flat and produced a transition at This value is the actual melting point of benzoic acid. The transitions that have been observed from 90ºC to 100ºC might be evaporation of water particles associated with the sample. In the derivative curve at the point marked as C is the value there evaporated water escaped from the capillary tube leaving a space, and then at the point D the melting of the compound is identified. In the normal graph this was not found very clearly where as in the derivative curve it is clearly observed that water might have evaporated from the sample. Table 6.3 gives the information of benzoic acid. 233
11 Table 6.3: Melting point data of chemical compound Benzoic Acid S. No. Parameter Value 1 Name of the chemical compound Benzoic Acid 2 Chemical formulae C 7 H 6 O 2 3 Status of the chemical compound White powder 4 Melting point range Image of the capillary after the Melting process 234
12 Figure 6.5: Melting point graph of Benzoic Acid 235
13 Figure 6.6: First order derivative graph of Benzoic acid. 236
14 6.5: Melting point determination of Cinnamic Acid The sample Cinnamic Acid [59] is filled into capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 140 C. The sample has shown a flat response up to 132.3ºC and sudden transition took place and stayed high at C prior to this at 90 to 100ºC the particle realignment at micro level took place. This has been observed through derivative curve. The transition is noted to 133.9ºC which falling standard values. Figure 6.7 shows the melting point graph of Cinnamic Acid. Figure 6.8 shows the first order derivative graph of cinnamic acid. In the derivative curve noise like disturbance is observed from 90 C to 100ºC. Later remain flat and produced a transition at 133.4ºC. This value is the actual melting point of cinnamic acid. The transitions that have been observed from 90ºC to 100ºC might be evaporation of water particles associated with the sample. In the normal graph this was not found very clearly, where as in the derivative curve it is clearly observed that water might have evaporated from the sample. In the derivative curve at the point marked as C is the value there evaporated water escaped from the capillary tube leaving a space, and then at the point D the melting of the compound is identified. Table 6.4 gives the information of cinnamic acid. 237
15 Table 6.4: Melting point data of chemical compound Cinnamic Acid S. No. Parameter Value 1 Name of the chemical compound Cinnamic Acid 2 Chemical formulae C 9 H 8 O 2 3 Melting point range Status of the chemical compound White crystalline compound 4 Image of the capillary after the Melting process 238
16 Figure 6.7: Melting point graph of Cinnamic Acid 239
17 Figure 6.8: First order derivative graph of Cinnamic acid 240
18 6.6: Melting point determination of Urea The sample Urea [60] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 140ºC. During this process it is observed that the compound is very stable up to 131.6ºC. The visual images also show no change in the solid state condition. After crossing C there is a steep rise is observed in the optical data at the material is entirely in the form of liquid state. Figure 6.9 shows the melting point graph of Urea. The transition is noted from to which are agreeable with standard values. Figure 6.10 shows the first order derivative graph of Urea. In the derivative curve a transition is observed at 132ºC. This value is the actual melting point of Urea. Table 6.5 gives the information of Urea. 241
19 Table 6.5: Melting point data of chemical compound Urea S. No. Parameter Value 1 Name of the chemical compound Urea 2 Chemical formulae CH 4 N 2 O 3 Status of the chemical compound White Crystals 4 Melting point range Image of the capillary after the Melting process 242
20 Figure 6.9: Melting point graph of Urea 243
21 D D=132 Figure 6.10: First order derivative graph of Urea 244
22 6.7: Melting point determination of Resorcinol The sample Resorcinol [61] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 116ºC. During this process it is observed that the compound is very stable up to 103.2ºC. At the particle realignment at micro level took place. This has been observed through derivative curve. The visual images also show no change in the solid state condition. After crossing C it is observed that the optical transition started at exactly 110.8ºC the entire compound turned into liquid giving steep rise in intensity is detected and recorded with the optical detector. From 110 to 116 the there is a disturbance in the signal due to change of colour in the liquid. The transition is noted to C which falling standard values. Figure 6.11 shows the melting point graph of resorcinol. Figure 6.12 shows the first order derivative curve of Resorcinol. In the derivative curve noise like disturbance is observed from 103 C to 108ºC. Later produced a transition at 109.4ºC. This value is the actual melting point of resorcinol. The transitions that have been observed from 103ºC to 108ºC might be realignment of particles. Table 6.6 gives the information of resorcinol. 245
23 Table 6.6: Melting point data of chemical compound Resorcinol S. No. Parameter Value 1 Name of the chemical compound Resorcinol 2 Chemical formulae C 6 H 6 O 2 3 Status of the chemical compound White Crystals 4 Melting point range Image of the capillary after the Melting process 246
24 Figure 6.11: Melting point graph of Resorcinol. 247
25 Figure 6.12: First order derivative graph of Resorcinol. 248
26 6.8: Melting point determination of Salicylic Acid The sample Salicylic acid [62] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 185ºC. During this process it is observed that the compound is very stable up to 158.6ºC. The visual images also show no change in the solid state condition. After crossing C it is observed that the optical transition started at exactly 161.2ºC the entire compound turned into liquid giving steep rise in intensity is detected and recorded with optical detector. From 162 C to 185ºC a slight depression of the optical signal is noticed. The transition is noted to 161.2ºC which falling standard values. Figure 6.13 shows the melting point graph of Salicylic acid. The first order derivative taken on the present data has produced a sharp transition line at C. This may be considered as a mean value of the melting point transition. This value is the actual melting point of Salicylic acid. Figure 6.14 shows the first order derivative graph of Salicylic acid. Table 6.8 gives the information of Salicylic acid. 249
27 Table 6.7: Melting point data of chemical compound Salicylic Acid S. No. Parameter Value 1 Name of the chemical compound Salicylic Acid 2 Chemical formulae C 7 H 6 O 3 3 Status of the chemical compound Dry Powder 4 Melting point range Image of the capillary after the Melting process 250
28 Figure 6.13: Melting point graph of Salicylic acid 251
29 D D=160.9 Figure 6.14: First order derivative graph of Salicylic acid 252
30 6.9: Melting point determination of 8-Hydroxyquinoline: The sample 8-Hydroxyquinoline [63] is filled into the capillary tube and inserted into the melting point apparatus subjected for heating from room temperature to 85ºC. During this process it is observed that the compound is very stable up to 74.8ºC. The visual images also show no change in the solid state condition. After crossing 74.8 C it is observed that the optical transition started at exactly 76.1ºC the entire compound turned into liquid giving steep rise in intensity is detected and recorded with optical detector. From 76.1 C to 90ºC the signal remained in flat response. The transition is noted 74.8 to 76.1 C which falling standard values. Figure 6.15 shows the melting point graph of 8-Hydroxyquinoline. The first order derivative taken on the present data has produced a sharp transition line at 74.9 C. This may be considered as a mean value of the melting point transition. This value is the actual melting point of 8- Hydroxyquinoline. Figure 6.16 shows the first order derivative graph of 8- Hydroxyquinoline. In the derivative curve a transition is observed at 74.9ºC. Table 6.8 gives the information of 8-Hydroxyquinoline. 253
31 Table 6.8: Melting point data of chemical compound 8-Hydroxyquinoline S. No. Parameter Value 1 Name of the chemical 8-Hydroxyquinoline compound 2 Chemical formulae C 7 H 6 O 3 3 Status of the chemical Dry Powder compound 4 Melting point range Image of the capillary after the Melting process 254
32 Figure 6.15: Melting point graph of 8-Hydroxyquinoline 255
33 D=74.97 Figure 6.16: First order derivative graph of 8-Hydroxyquinoline. 256
34 Table 6.9: Sample Melting point data from the experimental unit S. No Chemical Name Melting Point Range Measured Value 1 Succinic Acid Benzamide Benzoic Acid Cinnamic acid Urea Resorcinol Salicylic acid Hydroxyquinoline
35 6.10: Conclusion: In the present study, an embedded based instrumentation system for determining the melting point. The instrument if designed for the precision control of the temperature to the heating block. The photo detector OPT101 is used to trace the transmission of the light through sample. Due to the heat, the sample undergoes different transitions that are identified with photo detector. Instead of manual observation, the camera records the process and stored on the memory. The movie part can be replayed to observe the phenomenon. To perform the measurement all the sensors are interfaced with microcontroller ADuC 7061MKZ, which is the heart of the system. This device is more economical, reliable, and portable. With the present system, a pharmacist can analyze the purity of the chemical substance. 6.11: Future scope of the study: However, the same system can be extended to determine the melting point of chemicals, by incorporating a versatile scientific camera and connecting it to micro USB of the smart phone and using the MATLAB cloud for the same GUI or by using Java for android. This in turn eliminates the usage of a Personal Computer or Laptop. By using the present microcontroller reduces the production costs. There is no need of additional circuitry. 258
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