BAKU HIGHER OIL SCHOOL CHEMICAL ENGINEERING DEPARTMENT SEPARATION PROCESSES A LABORATORY REPORT 1 NAME Aysu Zamanova EXPERIMENT TITLE Batch Distillation GROUP NUMBER 19.1 DATE OF EXPERIMENT 07/10/2022 DATE OF SUBMISSION 23/10/2022 SUPERVISOR Hajar Nabiyeva Table of Contents Synopsys: .............................................................................................................................. 2 Introduction: ......................................................................................................................... 3 Theory:.................................................................................................................................. 7 Experimental Framework: ................................................................................................... 12 Safety Precautions: ...................................................................................................................... 12 Experimental equipment: ............................................................................................................. 13 Procedure .................................................................................................................................... 16 Results: ............................................................................................................................... 17 Discussion: .......................................................................................................................... 23 Conclusion: .......................................................................................................................... 28 Bibliography ........................................................................................................................ 29 Appendix A: ......................................................................................................................... 31 1 Synopsys: Definite, elaborate, alongside with succinct apprehension besides precise phenomena in terms of the demonstration of speculative and academic peculiarities, paramount figures, as well as the preponderant objective of the introductory laboratory report that is indicated as comprehension of main aspects and working principle of batch distillation column where especially rectification process of ethanol-water compound was carried out, will be conscientiously addressed amidst the laboratory report. Throughout the scrutiny, certain goals should have been attained including monitoring, determination, and controlling of several features of mixture such as temperature alongside the distillation column device, analysis of the generated materials as the bottom and the top product, furthermore, carrying out material balance of the products of rectification column. Foregoing distillation column utilized for observing rectification process of ethanol and water mixture was produced by company named GUNT company and was specified as CE600. In the context of measurement of profile segment of temperature, specifically 10 individual points of temperature ranging from evaporator to the top part of the packed distillation column were noted down, with the most pivotal one being 3rd magnitude since it is the signifying temperature value within the evaporator also with the leading number amongst the others. At the starting point of experiment reboiler temperature was around 72.2β, and temperatures of each section was repeatedly measured with the ranging timespan around 8-15 minutes until evaporator tank temperature reaching 92β. Subsequently, once distillate formed within the tank after passing through condenser analysis of product sample was initiated so as to figure out certain qualities bearing density through volume and mass computations that is for apprising ethanol quality by dint of table prepared by GUNT company. Through calculations it was deduced that at the end of the process an amount of 1.282 kg distillate could be collected with the ethanol mass balance being 86.67%, meanwhile initial feed to rectification column was 6kg with the mass percentage of ethanol standing at 25%, meaning that higher quality ethanol mixture was obtained. Nevertheless, error values for ethanol and total mass balance were acceptable as roughly 5.4 and 14%, respectively. Following results section of the report, within discussion part all possible causes which have led to such errors were described. 2 Introduction: The preeminent aim for conducting such laboratory scrutiny was denoted as to apprehend most predominant understandings of rectification column alongside with the phenomena of separation processes by means of utilizing aforementioned CE600 column which moreover provides noteworthy opportunity of comprehending main structure and basis of separation columns. Taking into consideration that designing and understanding chemical/process engineering applied devices such as pumps, reactor columns, heat exchangers, compressors and distillation columns are of significant importance, since design characteristics and features as quality of materials, construction method, and distillation mechanism refers to a pivotal role within the industrial processes. Regarding to the worldwide application of industrial processes through production approach, certain factors incorporating refining, enrichment, purification, and concentration are important for producing and generating products with required standards; as a consequence, various distillation and separation techniques have been developed for meeting the preferable concentration and purification of components such as analytical separation as chromatography which is highly utilized for discernment of complex compounds; meanwhile, preparative separation techniques are utilized for purification and refinery of the products that is remarked to possess almost comparable structures with analytical separation. (Seader, n.d.) Nevertheless, methods utilized within laboratory scale production and purification of materials may differ from that of industry scale processes since whilst within laboratory chemists are focused on separating mixtures with light-hydrocarbons through chromatography with gas-liquid, chemical engineers mostly relies on distillation columns for separating exactly same compounds. Generally, within chemical industrial processes whenever refinement of substances are required considering that certain raw materials must be processes prior to the introduction to the reaction section, extract gases which are incondensable as well as the undesirable by products, cleansing the stream products, and recycling the needed compounds back to the process, distillation columns are highly demanded so as to increase the value and purity of the produced material. With the highly applications of separation devices, quite a few methods within the industrial scale has been developed such as distillation, stripping, 3 extraction, and absorption; therefore, the fundamental science behind the separation processes is noted to be phases which are banded together and are in equilibrium. (Wankat, n.d.) The separation processes most commonly rely on either the physical or the chemical properties of the materials especially the discrepancies between those aspects where the main ideology behind such phenomena on all occasions depends on the formation, dimension, and structure of material molecules, charges of the components, solubilities within exact solvents, densities, and boiling points. Although being highly-utilized process within high-tech era of our planet, distillation processes are studied and discovered to date even back to 3500 before the common era within Mesopotamia, Syria, China, and Egypt, with the predominant purpose of carrying out operation for perfumery. So as to remove pivotal oil components from the herb materials through application of evaporation and condensation of liquids which were architecturally discovered with the pots and stills found in excavations within the areas of Baghdad in Iraq. Figure 1. Extraction pot and its structure discovered in Baghdad. (Kockmann, n.d.) The liquid mixture poured inside the pot is vaporized through heat transfer around the below part of the pot while some part of the vaporized substances condenses to the colder cap as described in the figure 1. Furthermore, created droplets run through the ring and collected there, in the exact part the organic materials such as the herbs and needed leaves have been separated by the liquid mixture. Meanwhile, for the fermented mixtures separation process may be carried out in order to separate alcohol substances through vaporizing and condensing to the rings that are carried out for fragrances and perfumery 4 oils, in the meantime the exact process is applied within industry with further reflux and extraction with the device named as Soxhlet extractor. Several types of distillation processes are quite utilized within the industrial applications each of them possessing certain features and structures with the predominant objective of reaching maximum efficiency, with the types including simple, steam, short path, fractional, vacuum, zone, and air-sensitive distillation processes. (V.R. Dhole, 1992) While simple distillation technique introduces the method of heating the liquid compounds until they reach the boiling point which ends up an instant condensation process of produced vapors, fractional distillation requires a fractioning column where consequent vaporizationcondensation steps are carried out, that is called as rectification method. The other leading dispersity between rectification and simple distillation is the differences between boiling points of substances need to be separated since although fractional distillation was developed to separate liquids with quite close boiling points, for the sake of purification of separated materials boiling points for simple distillation should not be close. Moreover, steam distillation as the other separation method is utilized for separating heat-sensitive materials, not needing high temperature values for the whole system, slightly heated steam line passes through the liquid mixture in order to vaporize certain part of the compound. (McCabe, 2004)Whenever the requirement is to vaporize mixtures with high boiling temperature points, vacuum distillation is referred since increasing temperature till higher numbers would eventually cause undesirable energy and efficiency repercussions and rather than foregoing process, decreasing pressure for the decrease in boiling points is denoted to be much more effective; nevertheless, other application area is separating components which decompose at relatively high temperatures. Once the vapor pressure reaches the pressure surrounding the system, vaporization process is initiated, following with the condensation and collection of the top product as a distillate. With the solely distinction from the vacuum column being the addition of inert gas when the process is fully completed, air sensitive vacuum columns are highly utilized for compounds that will react with the air components. Throughout industrial chemical productions of materials, certain substances may indeed reveal as well as display characteristics which may lead to unstable features within surrounding at high temperature, hereinafter short path distillation is specified for 5 purification of compounds which is named as a short path since distance moves through a compact distance prior to collection of condensate. Consequently, the zone distillation introduces a method where melting the substance partially is necessitated preceding the vaporization and condensation process where a zone heater is applied within a long container. (Ouljic, 2014) In case of complementary application of distillation and rectification processes, certain sectors must be prenoted for comprehending the momentousness of distillation columns. Considering that water scarcity is considered as the world-wide problem, distillation refers to a huge solution for desalination plants which incorporates with the rectification methods so as to further decontaminate insalubrious water sources, which moreover are applied for fields such as lead-acid batteries, and humidifiers especially with low volume. (Bode, 1977)With the prevailing intention of reducing the vapor pressure of crude oil obtained from the underground wells for supplemental secure stowage and conveyance, one of the techniques of distillation so-called as oil stabilization is of utmost importance. The preliminary objective of conducting the initial experiment was to apprehend the essential aspects of separation process throughout inspecting distillation of water-ethanol mixture: with scrutinizing temperature, volume, mass, and density values for further obtaining quality of ethanol compound. The report then undertakes theory section amidst of which theoretical hypothesizes, arithmetical equivalences in the context of mass, density, and volume, as well as the equations relating mass balances referring to the most volatile components with the equilibrium conditions. Furthermore, distillation column unit also known as CE600 will be elucidated in a thorough fashion. Consequently, initiated with the explanation of main parts of column, progressive methodology of experimentation will be beheld. Figures obtained throughout laboratory scrutiny will thereupon be referred for algebraic calculations, regarding to the results of computations remarked in the tables of temperature profiles of distillate formations, meanwhile for later visual representations of mass fraction of most volatile component which in this case is ethanol will be plotted. Subsequently, probable culprits for noticeable variances between practical and hypothetical values, expectancies for carried out investigations, analysis of plotted graphics will be extensively explained, pursued with a summary of scrutiny with recapitulating experimentation. 6 Theory: Overall, distillation processes have been applied to quite a few sectors throughout centuries ranging from household applications to industries with the preliminary intention of separating components from a mixture with the predominant principle lying within the boiling points, also known as the volatility differences of the substances contributing to the mixture. Since started from the ancient times around the first century A.D., in the modernworld efficiency of the separation processes can be increased through consuming appropriate energy sources with the increment on the equilibrium stage numbers. The whole idea behind distillation process mostly is engaged with equilibrium stage concept with a theoretical presence, within each stage in the distillation column the assumptions of vapor-liquid equilibrium and movement of vapor liquid as the distillate alongside with the liquid product to the bottom part is considered as real case concepts. Although real-case physics features may totally accept foregoing phenomena for trayed columns, for the packed columns this idea will probably bear certain misconceptions and deviations. (Berry, 1972) With the stages of distillation column being adjusted with appropriate structure, algebraic calculations based on theoretical p resumptions will fit the figures for real distillation Figure 2. Equilibrium stage concept. (Skogestad, 2000) columns even the ones with packed columns. Vapor-liquid equilibrium for the ideal mixtures is figured out through the Raoult’s law stating the fact of interrelationship between partial vapor pressure of the component with its mole fraction in liquid phase and saturated pressure of the exact component, which is denoted as, where the saturated pressure is given as the temperature function only: ππ = π₯π ∗ ππ π ππ‘π’πππ‘ππ (1) Furthermore, with Dalton’s law, which assumes partial pressure of a component is the function between mole fraction within vapor phase and total vapor pressure of the system, 7 taken into consideration, mole fractions, as well as vapor-liquid equilibrium is figured out: (University, 2016) ππ = π¦π ∗ ππ‘ (2) π¦= π π₯ππππ ππ‘π’πππ‘ππ (3) ∑ π₯ ∗ ππ ππ‘π’πππ‘ππ π π π Meanwhile the relative volatility conception indicates the deviations between the boiling points within 2 phase mixtures, that is directly connected with the equilibrium constant K value, where K value indicates the ratio between mole fraction in vapor phase and liquid phase, in this expression πππ describes relative volatility of the components: π¦π (π₯ ) πΎπ πππ = π¦ππ = (4) πΎ π (π₯ ) π In order to formulate the sufficient accuracy within the system for later computations an expression has been developed as: πππ = √πππ,π‘ππ ∗ πππ,πππ‘π‘ππ (5) Moreover, VLE (vapor-liquid equilibrium) relationship will then become an expression as, where further expression ππ describes common component: π π π₯π π¦π = (6) ∑ π π ππ₯ π Throughout batch distillation process, the mixture entering as a feed in liquid feed contains both MVC and LVC, abbreviations standing for most volatile components and least volatile components, with the components being ethanol and water for this experiment, furthermore once the vaporization process is initiated within the column process of condensation and evaporation creates a connection between liquid and vapor phases. However, the energy required for boiling the most volatile component is acquired through the fixed reboiler under the still pot, while the vaporized substance then passes through a total condenser resulting in the condensed stream within the distillate section. (Tham, 2006) Within distillation columns the reflux is forwarded to the top part of the column since some part of condensed substance is collected; however, while reflux provides desirable consequences for separation of substances, it also authorizes a 8 circumstance for controlling the temperature at the bottom part of the column. Notwithstanding the fact that increment in the reflux ratio generates contact between downflowing liquid alongside with the up-flowing vapor so as to acquire an equilibrium heat, material transfer and balance, so further purification of product, it calls for higher rate for vaporization as well as more energy. Reflux ratio expression has been developed as the ratio of the liquid that is removed back to the column and removed product as condensate: πΏπ π = (7) π· Figure 3. Distillation column. (Porter, 2011) Furthermore, several points should be taken into consideration in order to control the reflux ratio since this can be regarded as one of the key points of bath distillation process. Initially, the reflux ratio setpoint is persistent within the separation process, once decrement occurs in the percentage of most volatile component within the still, the composition of the overhead product seems to experience relative changes. As a consequence of which, a pre-determined number for reflux ratio should be kept constant as a means to provide an unchanging mole percentage of most volatile component. Nonetheless, reflux ratio control may involve several complicated procedures such as cyclic procedure pattern, efficiency based on thermodynamic laws, and optimization of residence time. Furthermore, side stream within the whole system may also influence the reflux ratio such as further appendage of feed can be involved to the system. (Qingli Qian, 2011) 9 Referring to the initial approach, within the laboratory experimentation reflux ratio was set with the percentage standing at 50%. Another predominate part for the calculations of distillation column is mass balance throughout the system. Figure 4. Distillation column with connected equilibrium stages. The initial assumption here is perfect mixing inside the stages between both of the phases, while the material balance for the whole system can be expressed with the algebraic equation as: πππ,π = (πΏπ+1 ∗ π₯π,π+1 − ππ ∗ π¦ ) − (πΏ ππ‘ π,π ∗π₯ π π,π −π π−1 ∗π¦ π,π−1 ) (7) Where, πΏπ πππ ππ πππ π‘βπ π‘ππ‘ππ ππππ’ππ‘π ππ ππππ€ πππ‘ππ πππ ππππ’ππ πππ π£ππππ, πππ ππππ‘ππ£πππ¦, ππ₯πππ‘ππ¦ πππ π‘βπ π π‘πππ ππππππ ππ π, π€βππβ ππ π‘βππ πππ π π£ππππ ππππ£ππ π π‘πππ π πππ πππ‘πππ π π‘πππ π + 1, πππππ€βπππ π‘βππ π ππππ πππ ππππ’ππ ππ π − 1. Whenever the steady state is considered for the operation conditions, remark indicating altering of component moles within each stage relative to the time should be considered as 0: πππ,π ππ‘ =0 However, to simplify the process of material balance around the system, streams in and out of the distillation column are given as liquid feed stream (F), distillate condensed and 10 collected (D), and bottom product of column (B); in the meantime, mole fractions within liquid phases for F, D, and B are expressed as π₯πΉ, π₯π·, πππ π₯π΅. Hence after, mass balance equation will be provided as: πΉ = π· + π΅ (8) πΉπ₯πΉ = π·π₯π· + π΅π₯π΅ (8.1) With the flowrates expressed in kmoles. Reflux ratio being kept constant throughout the process, expressions are deduced and denoted for the short time span of the process as: ππ· = −ππ π₯πππ· = −π(ππ₯π΅) (8.2) (8.3) πππ₯π΅ = ππ(π₯π· − π₯π΅) (8.4) Once these balanced equations are considered an expression named Rayleigh equation being based on differential equations and is used to study the hydrodynamic stability of the shear flows. In this case, the equation with the integrated formula where the boundaries are formulated as starting point from π₯πΉ until it reaches the number in π₯π΅ meaning from the feed values to the bottom figures: π₯π΅ π΅ ππ₯π΅ ln = ∫ πΉ π₯πΉ π₯π· − π₯π΅ (8.5) Although all the values and further calculated figures were of pivotal importance, figuring out the value for distillate most volatile component fraction was denoted as the preliminary objective. With the density being revealed, mass fraction could be deduced from the table provided; henceforward, density values for ethanol must be calculated with the expression provided below: π= ππππ₯ ππ π¦π π‘ππ − ππ£ππ π ππ = ππππ₯ ππππ₯ (9) Where, π ππ π‘βπ ππππ ππ‘π¦ ππ π‘βπ πππ₯π‘π’ππ, ππππ π’πππ ππ ππ πππ πππ‘ππ ππ’ππ. ππππ₯ ππ π‘βπ πππ π ππ π‘βπ πππ₯π‘π’ππ , ππ₯ππππ π ππ π€ππ‘βππ ππ. ππππ₯ ππ π‘βπ π£πππ’ππ ππ πππ₯π‘π’ππ, ππππ π’πππ ππ πππ‘ππ ππ’ππ. ππ π¦π π‘ππ ππ π‘βπ πππ π ππ π π¦π π‘ππ, πππ π π‘βπ π£ππ π ππ π€ππ‘β π‘βπ π πππ’π‘πππ ππ‘π πππ, ππππ π’πππ ππ ππ. 11 ππ£ππ π ππ ππ π‘βπ πππ π ππ π‘βπ ππππ‘π¦ π£ππ π ππ, ππππ π’πππ ππ ππ. With the temperature changing from the reboiler as the bottom part of distillation column to the top, measuring and noting down the values in each part was the main procedure of experiment. The temperature in which distillation process should stop was around 92β, which was pre-determined value which was chosen with the concentration of the initial mixture boiling point as well as that of pure water within the operating pressure so as to avoid any kind of evaporator temperature surpassing that of boiling point of least volatile component, moreover, whenever temperature passes this limit value the efficiency of the distillation column will drop and a permissible limit is exceeded by the amount of LVC amount In the evaporator, with the quality of separated material being decreased. So, the end temperature will be obtained through the equation: ππππππ = ππ΅,πππ₯π‘π’ππ + ππ΅,π€ππ‘ππ 2 (10) Experimental Framework: Within the experimental procedure part of this laboratory experimentation, preliminary, concise, as well as precise aspects and data in the context of the regarded unit gadgets, devices, and apparatus for measuring needed sections will be assiduously taken into account; in the meantime, step-by-step, and consecutive procedure for carrying out laboratory scrutiny with predominant objective of figuring out main factors for distillation processes will be remarked. Safety Precautions: Taking into account that certain safety issues may occur within the laboratory experimentations, precautions in order to prevent any harm to human beings as well as to the devices within the laboratories. While certain standard rules have been referred to, additional safety preventives must indeed be contemplated. Therefore, being aware of the dangers and hazards is of predominant significance. Initially, notwithstanding the fact that isolation material has been utilized for covering reboiler parts in order to both avoid any additional heat loss to the system to keep increasing the efficiency of the system and avoiding skin contact with extremely hot parts of 12 device, some parts of the reboiler was open and any contact would cause skin burns. Furthermore, in case of any contact of electricity grid with undistilled water would bear undesirable repercussions such as any kind of shock with the non-designated parts. In addition to the electricity sockets, electricity problems may as well occur within cabin of the distillation equipment, on the grounds of this touching electrical parts of laboratory column and confronting occurred problems are not authorized by the personnel and supervisors; however, cabin should be kept opened whenever the device is unplugged from the electricity socket. Consequently, since ethanol as the main substance of the experimentation possesses features of being highly flammable, ignition within the system would be a disastrous condition, thus presence of flame should be not allowed. One of the most must-be-prevented occurrence within laboratory systems is explosions of the materials once passing the temperature of ignition detonation may be initiated, so prohibition of introducing substances with ignition temperatures being exceeded should be taken into consideration. (Syed A. Taqvi, 2018) Meanwhile, extreme conditions of pressure within the sealed system may lead to the implosion considering that scorches of the red surfaces inside the burned areas results in leaking of hot stream including water and ethanol with the concentration of former being relatively higher. Alongside with the pressure conditions, any acquaintance with excessive heat and the humidity resulting from the excessive usage of steam exhaustion and thermal weariness. Therefore, limit conditions of both pressure and temperature should not be surpassed. Experimental equipment: Addition to the standard equipment required within the laboratory experimentations such as beakers, thermometers, electronic scales for measuring the mass of empty beakers as well as with the mixture within so as to calculate sole mass of the required component, a preliminary device for initiative scrutiny of separation processes was unit called as CE 600 fabricated by company named G.U.N.T that is the device as an exact identity of distillation column within industrial processes with the single difference being the size of gadget. The tools of the forgoing rectification column allowed a batch distillation process for this experiment. Even though the whole unit consisted of 3 various classifications of distillation columns, with the types being columns with sieve and bubble trays, and packed one, the ultimate kind was selected which indeed allows rate of mass exchange with higher scale. 13 The feed to the system can be introduced within various heights with 3 different sections; for the moment, preheating of the product is desirable and carried out with heat exchanger. Furthermore, presence of additional heat exchangers authorizes temperature control for both distillate and the bottom product considering that while the total condenser is utilized for changing the phase of the top product from distillation column, the heat exchanger exists with the fluid being water in order to cool down the bottom product coming from the reboiler at the end of the procedure. In the meantime, energy transmitted to the mixture is obtained from an evaporator with electrical powering adjusted under the distillation column. While technical devices have already been constructed as a part of rectification column, further electrical gadgets such as PLC touch screens for adjusting the trainer, and integrated router for indeed operating the trainer within an alternative route through the end device. Moreover, the whole structure of the distillation column named as CE 600 is indicated with the picture described below: 14 Figure 5. Structure and parts of distillation column. 1. Feed pump was constructed in order to forward the introductory feed to the system. 2. Feed tanks are used for conserving the feed whose volumes are 2x5 L. 3. Control board was mostly utilized so as to measure the temperature as well as reflux ratio within the system. 4. Tank used to collect the distillate of the top product. 5. To create a vacuum experimentation within the system, glass filters are used. 6. Pressure gauge. 7. Valve to forward the reflux. 8. Phase separation tank which could be used in the system if more than 3 components existed in the system. 9. Total condenser. 10. Valve to forward the reflux. 11. Diaphragm-based differential pressure sensor for measuring pressure loss. 12. Solvent tank for cleaning purposes. 15 13. Column for forwarding the material. 14. Flowmeter used to measure the amount of cooling water. 15. Evaporator with electrically powered with the volume being 10 liters. 16. Heat exchanger for cooling down the temperature of the bottom product. 17. Tank for collecting the bottom product. 18. Mostly used indicator for temperature measurement within the ranges of 1 to 12. 19. Temperature measurement with the ranges being from 13 to 16. 20. Control panel for reflux ratio. 21. Pressure loss indicator panel. 22. Switch. 23. Controller. 24. USB port. 25. Preliminary switch. 26. Emergency button. 27. Measurement and indicator for level since warning occurs whenever the level is measured to be lower than the critical moment. 28. Controlling of feed pump. 29. Controlling of heater. Procedure: As the initial step of the laboratory experimentation was introduction of ethanol water mixture with the concentrations being 25% and 75%, respectively; in the meantime, rectification column is plugged into sockets with the water network being started. Once the ethanol water mixture was introduced into the feed tanks of the distillation column, feed pump was activated with the valves for the pioneering flow of water inside the evaporator. Subsequently, the power of the evaporator was adjusted with 4000W, while that of reflux stayed at its 100% value which was initiated succeeding transferring all the water inside the evaporator tank, with the flowrate of water standing at 150 liters per hour that is measured through the flowmeter. Furthermore, temperatures throughout the system should be noted down through the usage of control panel with the numbers for temperatures ranging from T3 to T12. Whenever the temperature of the evaporator that is temperature denoted as T3 reaches 70 degree Celsius, heating power from the evaporator decreases. While the operation conditions for the heating power is given as the 30% of the maximum power, reflux ratio was adjusted with 50%. Consequently, distillate start forming within the 16 tank of collection, reflux ratio within the rectification column changes with the value staying at 50% of its figure, meanwhile the interval for measuring the temperature of each of the section reaches 10 to 15 minutes. After waiting for a certain period of time, the valve connected to the distillate collector tank is then opened in order to obtain certain amount of top product, prior to the step of measuring empty beaker after which the total weight of beaker with the substance inside was measured by means of an electric scale. However, for calculation of the required aspects not only the weight of the substance but also the temperature had to be measured with the thermometer. The process of sample taking from the top section of rectification column kept occurring until the stages reached around 18 with the last sample being taken, after each stage the sample taken from the tank is then poured inside the flask for not losing any kind of product. Once the temperature of the evaporator, as mentioned above T3, reached 92 degrees Celsius, evaporator should be on the off position meanwhile after waiting for around 5 minutes, reflux ratio within the system was then surged to 100%. Nevertheless, since the bottom product coming from the reboiler was extremely hot, cooling water was utilized within the heat exchanger in order to decrease the temperature of the remnant bottom product with it then poured inside the tank collecting for bottom product. Furthermore, the remnant was then discharged into the flask for calculation of total volume and mass of substance. Afterwards, the experiment is totally concluded with finally shutting down the system through removing it from the electricity. Results: In order to comprehend the carried-out experimentation with deeper understanding, graphs should be plotted with the calculations specifically on the mass percentage numbers should be done. As an initial step for results section of this report, temperature profiles should be plotted. Although temperature values were readily available through a hardware installed within the distillation column with the values being transferred to the user interface of device, figures 17 were noted down manually so as to meet the requirements of scrutiny in terms of temperature distributions. As a consequence, two individual profiles of temperature are plotted differentiated from the start point of distillate formation. Temperature profile before distillate formation 100 T3 90 T4 T5 T6 T7 T8 T9 10:19 tIME a.m. 10:26 T10 T11 T12 Temperature in celcius 80 70 60 50 40 30 20 10 0 9:50 9:57 10:04 10:12 10:33 10:40 10:48 Graph 1. Temperature values prior to distillation process 95 Temperature profile after distillate formation T3 T4 T5 T6 T7 T8 T9 T10 T11 T12 tEMPERATURE IN CELCIUS 90 85 80 75 70 65 60 10:48 11:02 11:16 11:31 11:45 12:00 12:14 TIME a.m. Graph 2. Temperature values after distillation process 18 12:28 Product analysis: With mainly focusing on the produced product form the distillation column, overall mass balance as well as material mass percentage fractions will be figured out throughout algebraic calculations. Three individual predominant analysis of the product, mass, volume, and as well as density, namely, will be highly regarded. Initially for mathematical computations of mass percentage of ethanol in the system, tables provided in the manual indicating mass percentage of ethanol referring to both temperature and density, reference densities as well as reference mass fractions were chosen for carrying out interpolation. Although all the calculations are denoted in Appendix A, as an example, mass fraction of ethanol within the first sample is introduced as: Table 1. First sample analysis. First Sample Time, a.m. Total mass, g Net mass, g 10:27 Beaker mass, g 128.7 40.2 Temperature, Density, β kg/m^3 50 Ethanol mass % 88.5 25 93.507% 804 Volume, ml Reference density 1, kg/m^3 802.63 Reference density 2, kg/m^3 805.41 Reference MVC mass fraction 1 94 Reference MVC mass fraction 2 93 Distillate formation started around 10:22 a.m., approximately 5 minutes prior to taking first sample from the distillate. With a reference to formulae 9, density was calculated as: π= ππ‘ππ‘ππ − πππππππ π = 128.7 − 88.5 50 = 0.804 π ππ = πππ ππ ππ With the temperature value standing at 25 degrees Celsius, and the reference densities alongside with mass fractions, ethanol fraction is algebraically computed by dint of interpolation: πΈπ‘% = πΈπ‘%(πππππππππ 1) + πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 93 − 94 ∗ (π − π(πππππππππ 1)) = 94 + ∗ (804 − 802.63) = ππ. πππ 805.41 − 802.63 While all calculations are introduced in the Appendix, overall values are then introduced as a table: 19 Table 2. Sample analysis of whole process. Time 10:53 10:58 11:03 11:08 11:13 11:18 11:23 11:28 11:33 11:38 11:43 11:48 11:53 11:58 12:03 12:08 12:13 12:23 Net mass, g Volume, ml Temperature, Density kg/m^3 β 40.2 53.8 70.2 65.4 65 71.6 41.6 68.1 82.6 71 84.4 58.7 72.1 87.3 95.5 67.5 79.3 108.3 50 67.5 84 80.5 79.8 87 52 83.5 99.5 86.1 102.1 71 86.5 107 112.5 82 95 131 25 23 23.5 23 24.7 24 22.5 26 25.1 24.6 24 23.8 24.5 25 24.5 25 25 23.5 804 797.03 811.9 812.42 814.54 822.99 803.8 815.57 830.151 824.623 826.641 826.641 833.526 815.888 848 823.171 834.737 826.718 Ethanol mass percentage 93.507 95.729 91.098 91.934 89.717 86.717 93.621 88.897 82.563 85.878 85.706 85.323 82.393 89.107 76.527 86.309 81.732 85.434 Once mass fractions of ethanol in the top product have been calculated, a diagram indicating the trend of mass percentage of ethanol in distillate product is plotted: 20 Mass percentage of most volatile component (ethanol) versus time 100 Ethanol Mass Percentage % 95 90 85 80 75 10:48 11:02 11:16 11:31 11:45 12:00 12:14 12:28 Time Graph 3. MVC mass fraction altering during distillation process Following aforementioned phenomena, calculations on overall material balance should be computed with the predominant intention of figuring out the deviations from the theoretical aspects which is mainly based on as the feed is equal to the sum of bottom and top product. Nevertheless, initially information on the each section as top, bottom, and feed flowrates must be introduced. Table 3. Mass balance. Feed Total Ethanol/water Net Mass, g Temperature Density Ethanol Volume ml % mass mass, g 25% kg/m^3 6000 23 Top Product 21 1500 Total Ethanol/water Net Mass, g Temperature Density Ethanol Volume ml % mass kg/m^3 mass, g 1557 86,67 823,764 1111,629 1282,6 24,26 Bottom Prdocut Total Ethanol/water Net Mass, g Temperature Density Ethanol Volume ml % mass kg/m^3 mass, g 4449,76 4.033 987.356 177,1899 4393,5 28 Sum Total mass, g Ethanol mass, g Initial 6000 1500 Final 5676,1 1288,819 Deviation 5.39% 14,07% For the material balance of the experimentation, initially conditions for feed such as total mass, mass percentage of ethanol within the mixture, and temperature should be figured out. Considering that temperature measurement of the substance initially was not carried out prior to the scrutiny, overall room temperature value was taken into consideration, in the meantime mass of the feed was deduced as 6kg, while mass fraction of most volatile component was 25%. For the top product, while total volume was figured out through summing all the individual volumes, net mass was an empirical value and as a consequence density value through which mass fraction of ethanol was possible to be figured out by dint of interpolation of density values with mass percentage at 24,26β that is found as average temperature value for top product. Following that, once the experimentation was almost finalized, further bottom product was taken out of the bottom product tank in order to measure conditions of the wastage with the water percentage corresponding to almost 96% of the whole product; meanwhile, temperature was measured to stay at 28β. Furthermore, deviations from the initial feed product must be deduced through calculations indicated below, while overall mass balance equations lead to about 5.4% error, that of ethanol was higher by roughly 8,7%. 22 πΌπ‘ππ‘ππ = πΌπΈπ‘ = |6000 − 5676,1| 6000 |1500 − 1288,819| 1500 ∗ 100 = 5.39% ∗ 100 = 14,07% Discussion: Processes being related to and relied on rectification processes similar to the carried-out experiment are considered to be of preliminary significance which indicates and provides paramount insights into distillation processes utilized in a quite a few complexes ranging from oil and gas industries, pharmaceuticals, analysis of complex materials, separation pathways for mixtures, which in this laboratory experimentation was given as ethanol and water mixture. Overall, process was conducted through separation of water and ethanol mixture through referring to the batch distillation column with the most volatile component being vaporized as the distillate product of the process, which indeed included controlling, monitoring, and noting down the changes of the temperature values starting from the temperature of evaporator and ending with the top column temperature given as the T-12, meanwhile amongst those values total temperature values throughout the system was as well taken into account, followed by calculations of ethanol quality within each taken sample on a regular basis so as to figure out mass fraction of the substance. Therefore, for further immersed understanding of the process additionally graphical methods have been utilized such as plotting the graphs mostly dealing with temperature profiles, and material balance over the whole process with the error being deduced. The utilized batch system distillation column was adjusted with several gadgets and sensors enabling monitoring system conditions. In the meantime, feed as a mixture of water and ethanol substances with the net mass of liquid mixture being 6kg, where mass concentration of ethanol stood at 25%, was introduced to the system at the beginning of the whole process. Alongside to the aforementioned technological gadgets, apparatus as thermometer was also used for deducing temperature of each sample, both distillate and bottom product. Another preliminary factor to be considered within the discussion section is the expectations from the experimentation even prior to beginning the process itself which could be contemplated and discerned throughout the scrutiny. Initially, one of the 23 anticipations about the process was distillate formation temperature of evaporator since as expected whenever temperature of evaporator reached 86.5-87 degree Celsius first condensate distillate product started forming with the top column temperature soaring immediately to 79,1 degree Celsius, in which first bubbles generated within the distillation column went to the top part prior to escaping from the rectifying section and entering total condenser to be condensed to turn into distillate product. Although in the initial conditions’ concentration of MVC was higher within the first bubbles formed, as the time goes by and distillation process continues further quality of ethanol on both the distillate and bottom product should decrease considering that while some part of the ethanol is transferred to the top product, as the time goes and temperature increases, LVC also gets to the top part. With the electric power of distillation column changing, temperature profiles should follow an upward trend since the power kept increasing for better distillation process within the system. Following this case, for the mass balance of the rectification column, theoretically without a doubt the values should be the same since no amount of mass lost is taken into consideration, meanwhile for the real case indeed some deviations from the ideal case was deduced which was ineluctable. One of the predominant parts for distillation columns is the fact that as temperature profiles increases quality of the most volatile component at the end of the process will be lower in comparison with the initial conditions. Since the process literally stopped at 92 degree Celsius, the main anticipation and reason for such an act can be explained through as foregoing phenomena, MVC will be less as time passes thus increasing mass percentage of LVC, which in this case was water, which would lead to inefficient distillation process. Before starting the discussion of empirical values obtained form results section, it should be mentioned that plotted graphs as well as obtained values from algebraic calculations as well as equations indicated in theory section commensurate with the expected phenomena. Looking at the graph plotted initially in the results section, it is obvious that temperature values indicate time-period beginning with heating process being initiated through the evaporator and ending up with the first moment of distillation process; in the meantime, latter sketched graph describe trend followed by temperature values until the end of the process. Once evaporator was initiated, small increases of temperature within the evaporator was witnessed due to heat production in the system, while other temperature 24 values except from T4 stayed almost the same, which could be caused due to T4 temperature being close enough to the evaporator section with heat being transferred. One of the noteworthy points here is that as just mentioned within the theory part, once evaporator is ignited so as to generate heat, all the temperatures within the system experienced upward inclination; nonetheless, a decrease of temperature value for T6 is discernible in the 2nd graphics with the temperature witnessing a decrease by 18β. This phenomenon could be exemplified through understanding that several glitches within the sensors could occur and create undesirable consequences. Whenever time reached 10:26 a.m., temperature of distillation column sections except for T3 and T4, surged until values reached values around 70 degree Celsius. An immediate increase in the values of other temperatures can be related to the increasing rate of sensors picking heat from the vaporization process. Whenever temperature of the top column reaches around 79.1β which commensurate with T3 temperature being 86.5β, evaporation process commences with the initial bubbles surging through the condenser by generation individual inaugural liquid phases within the top tank. Furthermore, fluctuations within the system temperatures can also be accredited to reflux ratio since temperature of the forwarded substance will be lower compared to the top part of the system which actually is considered as one of the preliminary purposes of refluxing products. Taken into consideration that power arranged to the evaporator is mainly intercorrelated with temperature increase within the system, whenever an increase in power was reviewed, from the graphs a steep growth of temperature profile was observed leading to the apprehension that initial slope of increment was rather lower compared to the latter one. Moreover, approximately constant lines within the graphs are acknowledged as well cannot be ignored; nevertheless, stabilized lines in the system do not particularly create or is mainly responsible to abnormalities since certain amount of loss of temperature within the system is possible through vapor temperature loss to surrounding alongside with temperature and heat transfer with the forwarded top distillate to column itself. One of the reliable grounds for stopping distillation process whenever temperature of evaporator reaches 92β is to prevent additional pressure losses in the system through avoiding harms and damages to distillation column. 25 In terms of the mass analysis of distillation process with mainly focusing on material balance regarding 2nd table and 3rd graph, initial mass concentration of ethanol within the system was calculated to be 93,5%, meanwhile following the same procedure second mass concentration was deduced as 95,73%; nevertheless, the phenomena of azeotrope should be taken into account as once an azeotrope is generated within the system as water/ethanol mixture is prone to create such factor, the recovery of ethanol within the system cannot be higher than 95,635%, as a consequence of which calculated values for 2nd mixture is theoretically unachievable. Nonetheless, although measurement issues may have occurred during experiment, conditions of the system may have affected azeotrope formation values, thus maximum quality which could be obtained through distillation must be altered. Following, ethanol mass fractions stayed amongst the values of 85%-90%, with the lowest value being 76,5% whenever time reached a time of 12:03, although certain deviations within the system from a downward trend occurred, overall decreasing quality of most volatile components indicated a similarity towards the anticipated phenomena. Studying the graph of mass fraction of ethanol over the distillation process, although an overall downward trend was expected and witnesses, certain time-frames such as 11:23 a.m., 11:58 a.m., and 12:23 p.m. were deduced to experience higher values for ethanol mass fraction with the values standing at roughly 93.62, 89.11, and 85.43, namely, which could for the last example might be exemplified through accumulation phenomena of distillate sample within the distillate tank since with involving as well as the initial distillate product sample with higher mass percentage of most volatile component. Following the discussion of material balance of the products, the volume of the top product was deduced throughout the summation of all individual values of the ethanol/water mixture with the mass percentage of former being dominant; nevertheless, final volume of the distillate should not have been figured out as summation since depending on the mass fraction alongside with the temperature of the system, arrangements of ethanol and water molecules are altered which in its turn prevents consideration of this mixture as an ideal condition. Another predominant section of discussion part is considering potential concepts which could have led to errors and discernible deviations between theoretical and empirical values. When dealing with technological devices such as gadgets and user interface 26 indicating temperature profiles of system, errors are chiefly regulated and attributed to malfunctions of devices rather than human-based oddities since nearly no human interaction is required for temperature measurement. Through being used for a long period of time, some malfunctions, extremely used parts of device may require for restoration of tech-based parts for even more precise measurements. Furthermore, as temperature values were taken through observing appeared numbers on the interface, oscillations of those values especially for evaporator and top column led to worrisome calculations and measurements. However, all predominant potential culprits which could have provoked undesirable divergences as a main source of errors, are principally generated through calculations of material balance considering that abundant computations, as have described within appendix A, might have caused inaccuracy. Initially, although could be considered as frivolous, temperature measurements within the system was nearly problematic as initial conditions for feed to the distillation column was not measured which have ended up with the impression and assumption that this value was roughly 23β; meanwhile, ethanol concentration figures was indeed calculated by a reference to the temperature of sections. As addition to the causses of faulty figures obtained, since ethanol mass percentages have been calculated with references to both temperatures and densities within the substances, any kind of miscalculations of aforementioned thermodynamical properties would certainly instigated subsequent blunders and inaccuracies of ethanol mass percentage values; for the time being, farther algebraic computations relied on ensuing two interpolations, even three whenever temperature value was not measured as an integer, have profoundly affected veracity of experimentation. In terms of preventing faulty calculations and misreading on the thermometer which can be accounted as human-being fault causes, referring to an electronic, technologically manufactured thermometer would avoid imprecise temperature values. Even for the density values being accurate as much as possible, utilizing a device so-called as densitometer would avoid the necessity of measuring both volume and mass of the samples through beaker scales and mass scale, which might carry certain error percentages within itself, for further calculation density values. Meanwhile ethanol mass in both distillate and wastage was deduced through acquired mass percentage values, and thus those accumulated oversights have ended up with relative high error for ethanol mass, 27 with the number standing at 14.07%. Although aforementioned culprits are indeed also included for overall mas balance errors within distillation column, another huge phenomenon in this case can be indicate as losses of substance particles. Those droplets of ethanol-water mixture which are captured as well apprehended within rectification section with the parts mostly being heat exchangers, container tanks for both bottom and top products, phase separation containers, and other parts, creating an accumulation even though for an ideal case this property is taken as negligible. As the end of the experimentation was reached, once bottom product was drained as the wastage, all attempts and efforts were made in order to totally leak all substance in the bottom tank. Considering that calculations were carried out based on the purity levels of both reactants as ethanol and water being pure substances and even though distilled water was utilized in the system, some parts of the liquid mixture alongside with the dissociated solid parts of substances within water and ethanol solution which eventually prevented accurate calculation of density values in the system leading to probable miscalculations and errors in the result values. Furthermore, one of the aspects which could have affected accuracy of the result section is the quality of ethanol since throughout the calculations solely 100% ethanol quality was taken into account. Conclusion: Preliminary laboratory experimentation carried out was predominantly dedicated for measuring quality of most volatile component within ethanol water mixture by dint of batch distillation column which was possible to figure out with computation of substantial values, plotted graphs indicating trend followed by ethanol mass fraction, and preponderant essence behind distillation process. The main objective was to obtain higher ethanol concentration substance from water ethanol mixture with 25% quality, dealing with CE600 rectification column which eventually lead to a distillate product with 86.67% ethanol mass fraction substance with its total mass being 1282.6 grams, whereas ethanol contributed 4.033% to the bottom product. Although values had been calculated for mass balance computations, certain deviations from the initial mixture were discernible when compared with the initial conditions regarding both the total liquid mixture and the ethanol constituent. 28 Whereas physical properties and external conditions played a paramount role causing error within the system, generally speaking the total downward trend for the quality, also known as mass fraction, of ethanol with lower vaporization temperature was expected from the system as distillation process continued occurring, with that of water increasing. Through evaluation of temperature profiles by dint of plotting the graphs have generated almost anticipated consequences as anticipated with the total trend for these values following an upward style. Another factor worth noting is the time and conditions of first distillate formation which roughly corresponded to 10:27 a.m. with temperature value standing at 84,6 degree Celsius, with the T-12 value standing at 24,1 degree Celsius. Distillation process continued for overall roughly 3 hours starting with the arrangement of feed preparation and ending up with taking the sample from the bottom product. Ultimately, though errors for ethanol mass balance was 14.07%, that of total material balance was 5.39% which was relatively low, potential culprits for those problems have been denoted on the discussion section. Since distillation processes are omnipresent within industrial processes, studying and examining rectification column is of utmost importance. Bibliography 1. Wankat, P. C., n.d. Separation Process Engineering. s.l.:Pearson. 2. Skogestad, I. J. H. a. S., 2000. Distillation Theory. Trondheim, Norway: Norwegian University of Science and Technology Department of Chemical Engineering. 29 3. Ouljic, Z., 2014. Types of Distillation Column Internals. Netherlands: Delft University of Technology. 4. Bode, H., 1977. Lead-acid batteries. New york, NY : John Wiley and Son, Inc. . 5.Porter, E., 2011. Thermopedia. [Online] Available at: https://www.thermopedia.com/content/703/ [Accessed 11 10 2022]. 6. Berry, R. W. a. M. W., 1972. Terminal composition control of a binary distillation column. Edmonton, Alberta, Canada: University of Alberta. 7. University, H.-W., 2016. Separation Processes A. Edinburgh, United Kingdom: Heriot-Watt University. 8. Syed A. Taqvi, L. D. T., 2018. Fault detection in distillation column using NARX neural network. s.l.:The Natural Computing Applications forum. 9. Qingli Qian, H. W. P. B. G. Y., 2011. Effects of water on steam rectification in a packed column. Tianjin, China: Tianjin University. 10. Seader, J., n.d. Separation Process Principles. Utah: University of Utah. 11.Kockmann, N., n.d. History of Distillation. Dortmund, Germany: s.n. 12.V.R. Dhole, B. L., 1992. Distillation Colum Targets. Manchester M60 IQD, U.K.: UMIST. 13. Tham, M., 2006. An introduction to Distillation Columns. Costello and Associates. 14. McCabe, W. s. J. a. H. P., 2004. Unit Operations of Chemical Engineering. 5th ed. Hoboken, New Jersey: Wiley-Interscience. 30 Appendix A: 2nd sample: ππ‘ππ‘ππ − πππππππ 142.3 − 88.5 π = πππ. ππ ππ = = 0.79703 π 67.5 ππ ππ π= πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 97 − 96 ∗ (π − π(πππππππππ 1)) = 96 + ∗ (797.03 − 797.82) 797.82 − 794.90 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 3rd sample: Since temperature was 23.5 degree Celsius, initially density values at 91% and 92% ethanol mass fractions must be figured out through interpolation: 809.89 − 809.02 π(πππππππππ 1) = 809.02 + ∗ (23.5 − 24) = πππ. πππ (ππ% ππππππππ) 23 − 24 π(πππππππππ 2) = 811.73 + π= 812.60 − 811.73 ∗ (23.5 − 24) = πππ. πππ (ππ% ππππππππ) 23 − 24 ππ‘ππ‘ππ − πππππππ 156.70 − 88.5 π = πππ. π ππ = = 0.8119 π 84 ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 91 − 92 ∗ (π − π(πππππππππ 1)) = 92 + ∗ (811.9 − 809.455) 812.165 − 809.455 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 4th sample: π= ππ‘ππ‘ππ − πππππππ 153.9 − 88.5 π = πππ. ππ ππ = = 0.81242 π 80.5 ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 92 − 91 ∗ (π − π(πππππππππ 1)) = 91 + ∗ (812.42 − 809.89) 812.60 − 809.89 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 5th sample: ππ‘ππ‘ππ − πππππππ 153.5 − 88.5 π = πππ. ππ ππ = = 0.81454 π 79.8 ππ ππ Since temperature was 24.7 degree Celsius, initially density values at 89% and 90% ethanol mass fractions must be figured out through interpolation: 813.53 − 814.40 π(πππππππππ 1) = 814.40 + ∗ (24.7 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 π= 31 π(πππππππππ 2) = 817.05 + 816.17 − 817.05 ∗ (24.7 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 89 − 90 ∗ (π − π(πππππππππ 1)) = 90 + ∗ (814.54 − 813.791) 816.434 − 813.791 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 6th sample: π= ππ‘ππ‘ππ − πππππππ 160.1 − 88.5 π = πππ. ππ ππ = = 0.82299 π 87 ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 87 − 86 ∗ (π − π(πππππππππ 1)) = 86 + ∗ (822.99 − 824.84) 822.26 − 824.84 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 7th sample: ππ‘ππ‘ππ − πππππππ 240.6 − 198.8 π = πππ. π ππ = = 0.8038 π 52 ππ ππ Since temperature was 22.5 degree Celsius, initially density values at 94% and 95% ethanol mass fractions must be figured out through interpolation: 801.55 − 802.41 π(πππππππππ 1) = 802.41 + ∗ (22.5 − 22) = πππ. ππ (ππ% ππππππππ) 23 − 22 π= π(πππππππππ 2) = 805.23 + 804.37 − 805.23 ∗ (22.5 − 22) = πππ. π (ππ% ππππππππ) 23 − 22 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 94 − 95 ∗ (π − π(πππππππππ 1)) = 95 + ∗ (803.8 − 801.98) = ππ. πππ% 803.3 − 801.98 πΈπ‘% = πΈπ‘%(πππππππππ 1) + 8th sample: π= ππ‘ππ‘ππ − πππππππ 156.6 − 88.5 π = πππ. ππ ππ = = 0.81557 π 83.5 ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 89 − 88 ∗ (π − π(πππππππππ 1)) = 88 + ∗ (815.57 − 817.92) 815.30 − 817.92 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 9th sample: 32 π= ππ‘ππ‘ππ − πππππππ = 82.6 = 0.830151 π = πππ. πππ ππ π 99.5 ππ ππ Since temperature was 25.1 degree Celsius, density values for this sample can be taken approximated as 25 degrees Celsius, thus calculations are introduced as: πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 84 − 83 ∗ (π − π(πππππππππ 1)) = 83 + ∗ (830.151 − 829.05) 829.05 − 831.57 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 10th sample: ππ‘ππ‘ππ − πππππππ 71 = 0.824623 π = πππ. πππ ππ = π 86.1 ππ ππ Since temperature was 22.5 degree Celsius, initially density values at 85% and 86% ethanol mass fractions must be figured out through interpolation: 823.96 − 824.84 π(πππππππππ 1) = 824.84 + ∗ (24.6 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 π= π(πππππππππ 2) = 827.39 + 826.51 − 827.39 ∗ (24.6 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 85 − 86 ∗ (π − π(πππππππππ 1)) = 86 + ∗ (824.623 − 824.312) 826.862 − 824.312 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 11th sample: π= ππ‘ππ‘ππ − πππππππ 84.4 = 0.826641 π = πππ. πππ ππ = π 102.1 ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 86 − 85 ∗ (π − π(πππππππππ 1)) = 85 + ∗ (826.641 − 824.84) 827.39 − 824.84 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 12th sample: π= ππ‘ππ‘ππ − πππππππ = 58.7 = 0.826761 π =. πππ. πππ ππ π 71 ππ ππ Since temperature was 23.8 degree Celsius, initially density values at 85% and 86% ethanol mass fractions must be figured out through interpolation: 824.84 − 825.71 π(πππππππππ 1) = 825.71 + ∗ (23.8 − 23) = πππ. πππ (ππ% ππππππππ) 24 − 23 33 π(πππππππππ 2) = 828.26 + 827.39 − 828.26 ∗ (23.8 − 23) = πππ. πππ (ππ% ππππππππ) 24 − 23 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 85 − 86 ∗ (π − π(πππππππππ 1)) = 86 + ∗ (826.761 − 825.014) 827.594 − 825.014 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 13th sample: ππ‘ππ‘ππ − πππππππ 161 − 88.9 π =. πππ. πππ ππ = = 0.833526 π 86.5 ππ ππ Since temperature was 24.5 degree Celsius, initially density values at 82% and 83% ethanol mass fractions must be figured out through interpolation: 834.07 − 834.95 π(πππππππππ 1) = 834.95 + ∗ (24.5 − 24) = πππ. ππ(ππ% ππππππππ) 25 − 24 π= π(πππππππππ 2) = 832.44 + 831.57 − 832.44 ∗ (24.5 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 83 − 82 ∗ (π − π(πππππππππ 1)) = 82 + ∗ (833.526 − 834.51) 832.005 − 834.51 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 14th sample: π= ππ‘ππ‘ππ − πππππππ π = 87.3 = 0.815888 107 π ππ = πππ. πππ ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 90 − 89 ∗ (π − π(πππππππππ 1)) = 89 + ∗ (815.888 − 816.17) 813.53 − 816.17 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 15th sample: ππ‘ππ‘ππ − πππππππ 95.5 = 0.848 π = πππ ππ = π 112.5 ππ ππ Since temperature was 24.5 degree Celsius, initially density values at 76% and 77% ethanol mass fractions must be figured out through interpolation: 848.85 − 849.72 π(πππππππππ 1) = 849.72 + ∗ (24.5 − 24) = πππ. πππ(ππ% ππππππππ) 25 − 24 π= π(πππππππππ 2) = 847.28 + 846.41 − 847.28 ∗ (24.5 − 24) = πππ. πππ (ππ% ππππππππ) 25 − 24 34 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 77 − 76 ∗ (π − π(πππππππππ 1)) = 76 + ∗ (848 − 849.285) 846.845 − 849.285 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 16th sample: π= ππ‘ππ‘ππ − πππππππ = π 67.5 = 0.823171 82 π ππ ππ = πππ. πππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 86 − 85 ∗ (π − π(πππππππππ 1)) = 85 + ∗ (823.171 − 826.51) 823.96 − 826.51 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 17th sample: π= ππ‘ππ‘ππ − πππππππ = π 79.3 = 0.834737 95 π ππ ππ = πππ. πππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 82 − 81 ∗ (π − π(πππππππππ 1)) = 81 + ∗ (834.737 − 836.56) 834.07 − 836.56 = ππ. πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 18th sample: π= ππ‘ππ‘ππ − πππππππ = 108.3 = 0.826718 π = πππ. πππ ππ π 131 ππ ππ Since temperature was 23.5 degree Celsius, initially density values at 85% and 86% ethanol mass fractions must be figured out through interpolation: 824.84 − 825.71 π(πππππππππ 1) = 825.71 + ∗ (23.5 − 23) = πππ. πππ (ππ% ππππππππ) 24 − 23 π(πππππππππ 2) = 828.26 + 827.39 − 828.26 ∗ (23.5 − 23) = πππ. πππ (ππ% ππππππππ) 24 − 23 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 85 − 86 ∗ (π − π(πππππππππ 1)) = 86 + ∗ (826.718 − 825.275) 827.825 − 825.275 = ππ. πππ% Bottom Product Sample: πΈπ‘% = πΈπ‘%(πππππππππ 1) + π= ππ‘ππ‘ππ − πππππππ π = 171.8 = 0.987356 174 π ππ 35 = πππ. πππ ππ ππ πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 5−4 ∗ (π − π(πππππππππ 1)) = 4 + ∗ (987,356 − 987,30) 988,99 − 987.30 = π, πππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + Top Product Total Sample: π= ππ‘ππ‘ππ − πππππππ = 1282,6 = 0.823764 π = πππ. πππ ππ π 1557 ππ ππ Since temperature was 24.26 degree Celsius, initially density values at 85% and 86% ethanol mass fractions must be figured out through interpolation: 821.39 − 822.26 π(πππππππππ 1) = 822.26 + ∗ (24,26 − 24) = πππ, πππ (ππ% ππππππππ) 25 − 24 π(πππππππππ 2) = 824.84 + 823.96 − 824.84 ∗ (24,26 − 24) = πππ, πππ (ππ% ππππππππ) 25 − 24 πΈπ‘%(πππππππππ 2) − πΈπ‘%9πππππππππ 1) π(πππππππππ 2) − π(πππππππππ 1) 87 − 86 ∗ (π − π(πππππππππ 1)) = 86 + ∗ (823,764 − 822.034) 824,611 − 822,034 = ππ, ππ% πΈπ‘% = πΈπ‘%(πππππππππ 1) + 36