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    ME204 Labsheet

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    37 S.M Shahriar Rifat

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    Bangladesh University of Engineering and Technology Department of Mechanical Engineering ME 204 Engineering Thermodynamics Sessional Contact Hour: 1.5, Credit Hour: 0.75 Experiments: (Fuel Testing Lab, 4" Floor, EME Building) 1. (@) Determination of Heating Value of Coal by Bomb Calorimeter (b) Determination of Flash Point and Fire Point of Given Oil 2. (a) Proximate Analysis of Coal (b) Study and Calibration of Thermocouple (©) Calibration of a Bourdon Tube Pressure Gauge by Dead Weight Tester 3. (a) Measurement of Viscosity of an Oil by Saybolt Viscosimeter (b) Study of Sling Psychrometer and Determination of Humidity of Air 4. (a) Determination of Carbon Residue of Given Oil (b) Study of Gas Calorimeter and Determination of Heating Value of Natural Gas by Gas Calorimeter Link to download: http://bit.ly/ME204F TL (Available hardcopy in Fuel Testing Lab) For Inquiry: Dr. Sumon Saha (Room #M413) Mobile: 01926197002 Instructions for Students Necessary points of report writing: Objectives Apparatus (write specification like type, dimensions, range, material, etc.) Schematic Diagram of the Experimental Setup (label properly) Data and Calculation sheets Plotting graphs if any Sample Calculation for a particular observation Results and Discussions (Result and graph analysis, sources of error, means of improvement, question and answers if any) Conclusion Important Instructions: v v Submit the reports in plastic files of color specified for the group You must come to the class before the starting time (for example 2.30 pm). No late attendance. ‘You must submit all the reports of a group together before the end of a lab session, ‘You must come to the class with prior preparation (study the lab sheet supplied, bring necessary graph papers, pages, calculator, reference books, etc.). You must bring this lab instruction sheet during the sessional class. ‘You must prepare the format of the data and the calculation sheets before coming to the class. Viva on the individual experiments will depend on the concerned teacher. Copying another student’s report will be severely dealt with. Bangladesh University of Engineering and Technology Course Number: Group Number: Course Title: Experiment Number: Name of the Experiment(s): Date of Performance: Date of Submission: SUBMITTED BY Name: Student ID: Department: Section: EXPERIMENT NO. I(a) Determination of Heating Value of Coal by Bomb Calorimeter Introduction Heating or calorific value of any fuel is defined as the amount of heat obtained when fuel or some other substance of a specific unit quantity is completely combusted. It is usually expressed in terms of kJ/kg of solid fuel. There are two types of heating value: 1. The lower heating value (net) is the difference between combustion and latent heat of vaporization of the water vapors formed from combustion. 2. The higher heating value (gross) is the heat obtained from complete combustion of a substance. Here, the products of its combustion are cooled down to the temperature of supplied air. Bomb Calorimeter The bomb calorimeter is used to determine the heating value of fuel when burned at constant volume. The fuel, whose heating value is desited, is placed in the fuel pan (crucible). A coil of fine wire dips in the pan. The bomb is charged with oxygen under pressure, When an electric current is passed through the wire, it ignites the fuel. Surrounding the bomb is a bucket containing water to absorb the heat released as the fuel burn, The bomb has an outer jacket, and a dead-air space surrounds the bucket to minimize heat losses to the surroundings. Although the water in the bucket absorbs the major portion of the heat, this heat is not the heating value of the fuel, for the following reasons: The bomb itself absorbs some heat. ‘There is heat exchange with the outer jacket. The ignition wire liberates some energy. ‘The products of combustion are not cooled to the original temperature, Ake ET Because combustion takes place in oxygen, high temperature is attained resulting in the formation of nitric and sulfuric acid, which would not be formed in the normal combustion process, Although the products of combustion are not cooled to the original temperature, the final and. original temperatures are so close that the error is considered small. Furthermore, the error is almost entirely offset when the bomb is standardized. The water equivalent of the bomb is furnished by the manufacturer. This is the amount of water having the same thermal capacity as the bomb and its bucket (empty) The exchange of heat with outer jacket is minimized by maintaining a minimum temperature difference between the two. Corrections are made for small amount of heat transfer, which occurs due to radiation. Corrections are also made for the heat liberated by the ignition wire by determining the amount actually burned. Objective 1, To find the heating value of coal using a bomb calorimeter. Experimental Setup A schematic diagram of the experimental setup is shown in Fig. 1. The setup consists of a Bomb calorimeter (Model: Parr 1341 Plain Oxygen), digital thermometer, stopwatch, analytic balance, fuse wire, water container, ete. The Parr 1341 plain Oxygen Bomb calorimeter consists of an insulated jacket through which the leads for the ignition system run, a metal bucket which will hold the water that serves as the medium through which we will monitor the heat released by the reaction in the bomb, and a cover through which the temperature probe and the stirring shaft run. The stirring shaft has a propeller at the bottom and a wheel at the top, which is attached to the stirring motor mounted on the side of the calorimeter with a rubber belt. Also on the calorimeter’s cover is a metal rod, which can be used to keep the temperature probe in a vertical position not touching the metal bucket. PARTS FOR THE 1341 CALORIMETER Key No. Description 1 Motor Assembly with Pulley, 115V 60 Hz Motor Assembly with Pulley, 230V 50/60 Hz Motor Pulley Stirrer Drive Belt Stier Pulley Stirrer Bearing Assembly Ignition Wire Stirrer Shaft with Impeller ‘Oval Bucket Calorimeter Jacket with Cover 10 ‘Oxygen Combustion Vessel "1 Male Connector Thermistor ©exousen 12) Figure 1. Schematic Diagram of the Experimental Setup. Experimental Procedures All operations required to test a sample or to standardize the plain calorimeter should proceed step-wise in the following manner: 1 2. Prepare the sample and charge the oxygen bomb Fill the calorimeter bucket by first taking the dry bucket on a solution or trip balance; then add 2000(+/-0.5) g of water. Distilled water is preferred, but de-mineralized or tap water containing less than 250 ppm of dissolved solid is satisfactory. The water temperature should be approximately 1.5°C below room temperature, but this can be varied to suit the operator's preference. It is not necessary to use exactly 2000 g, but the amount selected must be duplicated within 4/-0.5 g for each run. Set the bucket in the calorimeter. Attach the lifting handle to the two holes in the side of the screw cap and partially lower the bomb in the water. Handle the bomb carefully during this operation so that the sample will not be disturbed. Push the two ignition lead wires into the terminal sockets on the bomb head, Orient the wires away from the stirrer shaft so they do not become tangled in the stirring mechanism. Lower the bomb ular boss in the bottom of the completely into the water with its feet spanning the ci bucket. Remove the lifting handle and shake any drops of water into the bucket and check for gas bubbles Set the cover on the jacket. Turn the stirrer by hand to be sure that it runs freely; then slip the drive belt onto the pulleys and start the motor. Turn on the Digital Thermometer. Let the stirrer run for § minutes to reach equilibrium before starting a measured run, At the end of this period record the time on the timer of the Digital Thermometer and read the temperature, Read and record temperatures at one-minute intervals for 5 minutes. Then, at the start of the 6" minute, Stand back from the calorimeter and fire the bomb by pressing the ignition button and holding it down until the indicator light goes out. Normally the light will glow for only about ¥4 second but release the button within $ seconds regardless of the light. Caution: Do not have the head, hands or any parts of the body over the calorimeter when firing the bomb; and continue to stand clear for 30 seconds after firing. The bucket temperature will start to rise within 20 seconds after firing. This rise will be rapid during the first few minutes; then it will become slower as the temperature approaches a stable maximum as shown by the typical temperature rise curve, Measure the time required to reach 60 percent of the total rise by estimating the temperature at the 60% point and observing the time when the temperature reading reaches that point. 10, W 12, 14, 16. After the rapid rise period (about 4 or 5 minutes after ignition) record temperatures at one minute intervals until the difference between successive readings has been constant for five minutes. Usually the temperature will reach a maximum; then drop very slowly. However, this is not always true since a low starting temperature may result in a slow continuous rise without reaching a maximum. As stated above, the difference between successive readings must be noted and the readings continued at one-minute intervals until the rate of the temperature change becomes constant over a period of 5 minutes. After the last temperature reading, stop the motor, remove the belt and lift the cover from the calorimeter. Wipe the thermistor shaft and stirrer with a clean cloth and set the cover on the support stand. Lift the bomb out of the bucket; remove the ignition leads and wipe the bomb with a clean towel. Open the knurled knob on the bomb head to release the gas pressure before attempting to remove the cap. This release should proceed slowly over a period of not less than one minute to avoid entrainment losses. After all pressure has been released, unscrew the cap; lift the head out of the cylinder and place it on the support stand. Examine the interior of the bomb for soot or other evidence of incomplete combustion. If such evidence is found, the test will have to be discarded. Wash all interior surfaces of the bomb with a jet of distilled water and collect the washings in a beaker. Remove all unburned pieces of fuse wire from the bomb electrodes; straighten them and measure their combined length in centimeters. Subtract this length from the initial length of 10 centimeters and enter this quantity on the data sheet as the net amount of wire burned. Titrate the bomb washings with a standard sodium carbonate solution using methyl orange or methyl red indicator. A 0.0709N sodium carbonate solution is recommended for this titration to simplify the calculation, This is prepared by dissolving 3.76 grams Na2CO3 in water and diluting to one liter NaOH or KOH solutions of the same normality may be used. Analyze the bomb washings to determine the sulfur content of the sample if it exceeds 0.1%. Correction for Heat Losses Heat loss by radiation from the calorimeter is minimized by starting the determination with the water in the calorimeter enough below room temperature so that the final temperature after combustion will be slightly above room temperature. Thus, the radiation from the room before ignition will tend to compensate that to the room after the temperature rise. Since an appreciable amount of time elapses before the rise in temperature is completed, there will be some heat transfer. The Dickinson method of correction for radiation is prescribed by the ASTM. The rate of temperature change in degree per minute is determined over a 5 minute period just before ignition, and again after ignition when the maximum temperature has been reached. The time of ignition (time a), the temperature at ignition, the thermometer reading taken when the temperature change has become uniform after attaining a maximum and the time at this ‘maximum temperature (time c) are recorded. Time b is defined as the time at which six-tenths of the temperature rise from a to c has taken place. The ignition temperature is then corrected by adding (b — a)n, where r, is the rate in degrees per minute at which the temperature was rising before ignition. The final temperature is corrected by adding (¢ — brs, where rz is the rate of temperature decrease after the maximum was reached. The temperature rise used for calculating the energy liberated is the difference between the corrected ignition and final temperatures. The corrected temperature is to be indicated in Fig. 2. “cal Temperate Fise Cuve ter sau) Pla Calorimeter TEMPERATURE - DEG. C. = ~—Preperiod—-—t i a TIME ~~ MINUTES Figure 2, Typical temperature rise curve for 1341 Plain Bomb Calorimeter. Because a portion of the fuse wire will be found to have bumt to the oxide, a correction for the energy liberated by this reaction must be subtracted from the observed heating value of the sample. This is best accomplished by knowing the heat of combustion of the fuse wire per unit length and the length of the original and unburned portions of the wire. When extreme accuracy is required, the ASTM test procedure should be consulted for the method to be used in correcting the observed heating value for the formation of HNO3 and H,SO4. Since the water vapor resulting from the combustion of hydrogen in the fuel sample is condensed because of the low bomb temperature, the heating value obtained is known as the higher heating value. The lower heating value is determined by subtracting from the higher heating value a quantity equal to the product of the weight of water vapor formed by combustion and the latent heat of vaporization of the water. Relevant Equations Assembly of Data The following data should be available at the completion of a test in a 1341 calorimeter: a= time of firing. +b = time (to nearest 0.1 minute) when the temperature reaches 60 per cent of the total rise. © = time at beginning of period (after the temperature rise) in which the rate of temperature change has become constant. t= temperature at time of firing, {.= temperature at time c. 7 = rate (Semperature units per minute) at which the temperature was rising during the 5- minute period before firing. r= rate (Semperature units per minute) at which the temperature was rising during the 5- minute period after time ¢. If the temperature was falling instead of rising after time ¢, r is negative and the quantity -r2(c — 6) becomes positive and must be added when computing the corrected temperature rise ‘¢1 = milliliters of standard alkali solution used in the acid titration. percentage of sulfur in the sample. cs = centimeters of fuse wire consumed in firing. w m snergy equivalent of the calorimeter, determined under standardization. mass of sample in g. 10 ‘Temperature Rise Compute the net corrected temperature rise (1), by substituting in the following equation: ' =n (b-a)—7,(e-b) w ‘her mo-chemical Corrections Compute the following for each test: 1 =correction in calories for heat of formation of nitric acid (HNOs). = ¢; if 0.0709N alkali was used for the titration. = correction in calories for heat of formation of sulfuric acid (HsS0,). = (13.7) (ca) (mm) = correction in calories for heat of combustion of fuse wite. = (2.3) (cs) when using nickel chromium fuse wire, or = (2.7) (cs) when using iron fuse wire. Gross Heat of Combustion Compute the gross heat of combustion (#,), in calories per gram by substituting in the following equation: oe ‘The following example is presented to clarify the method used in calculating the heating value of a fuel Weight of coal fuel sample 0.9936 g Length of fuse wire 10cm Length of fuse wire not burned 24 em Weight of calorimeter water 2000 gm ‘Water equivalent of calorimeter 432. gm a = 1:44:00 = 1:44.0 = 1:45:24 = 145.2 = 1:52:00 = 1:52.0 f= 24.428 + 0.004 = 24.432°C fe = 27.654 + 0,008 = 27.662°C rn, =+0.010°C /5 min. = +0.002°C /min. nae itt 7m — =-0.004°C /S min, = -0.001°C /min. 1 = 23.9 ml. @ = 1.02% Sulfur C3 = 7.6 cm wire Ww = 2426 cal/°C m — =0,9936g t = 27.662-24.432-(0.002) (1.4)-(-0.001) (6.6) = 3.234°C 1 =23.9.al = (13.7) (1.02) (9936) = 13.9 cal es = (2.3) (7.6) = 17.5 cal Hy = 87342426) 289-139-175 _ gay cally = (1.8) (1841) = 14114 Beulld 0.9936 Discussion 1. Briefly explain the limitations of the experimental setup, if any. 2. Explain the difference between LHV and HHV of the given coal. How do the heat losses affect the reading of heating value obtained from the experiment? Conclusion, ‘Write down the summary of key findings and observations as outlined in the objectives of this experiment Sample Quiz Questions: 1, What are the reasons for the formation of Nitric acid and Sulfuric acid during the test? 2. Why there is an air gap between the calorimeter bucket and the calorimeter jacket? 3. Write down the criteria for complete combustion 12 Data Sheet Determination of Heating Value of Coal by Bomb Calorimeter Calorimeter: Parr 1341 Plain Oxygen Bomb Calorimeter ‘Thermometer: Parr 6775 Digital Thermometer, 0.0001°C Weight of empty pan: Weight of pan + coal: Weight of coal Weight of water Water equivalent of calorimeter be 2 98 09 Total length of fuse wire used ‘Unburned fuse wire Fuse wire actually burnt Calorimeter value of used wire g Room Temperature Table 1: Recording temperature of bomb calorimeter during experiment, cm cm cal/om °C Time Digital Thermometer Reading Time | Digital Thermometer Reading (minute) co) (minute) co) 0 8.30 T 9.00 2 9.30 3 10.00 4 10.30 3 Fire) 11.00 3.15 12 5.30 13 5.45 14 6.00 15 6.15 16 6.30 7 6.45 18 7.00 19 7.15 20 7.30 21 7.45 22, 8.00 23 Please bring one normal mm graph paper for this experiment. Calorific value of coal, HHV = callg = Buu/lb B EXPERIM! IT NO. 1(b) Determination of Flash Point and Fire Point of Given Oil Introduction Flash point is the lowest temperature of the test specimen at which the application of an ignition source causes the vapor of the test specimen to ignite momentarily and the flame to propagate across the surface of the liquid under the specified conditions of test All liquids have a specific vapor pressure, which is a function of that liquid’s temperature and. is subject to Boyle's Law. As temperature increases, vapor pressure increases. As vapor pressure increases, the concentration of vapor of a flammable or combustible liquid in the air increases. Hence, temperature determines the concentration of vapor of the flammable liquid in the air. A certain concentration of a flammable or combustible vapor is necessary to sustain combustion in air, the lower flammable limit, and that concentration is different and is specific to each flammable or combustible liquid. The flash point is the lowest temperature at which there will be enough flammable vapor to induce ignition when an ignition source is applied. It is important to realize that the value of the flash point is not a physical constant but is the result of a flash point test and is dependent on the apparatus design, the condition of the apparatus used, and the operational procedure carried out. Flash point can therefore only be defined in terms of a standard test method, and no general valid correlation can be guaranteed between results obtained by different test methods or with test apparatus different from that specified. Fire point is the lowest temperature at which application of an ignition source causes the vapors of a test specimen of the sample to ignite and sustain burning for a minimum of 5 s under specified conditions of test. A fire point happens when the heat produced is self sustaining, as it supplies enough vapors to combine with air and burn even after the removal of the ignition source. Both flash and fire points are important in order to avoid any fire within the oil. 14 Importance of Flash Point Test ‘The fundamental reason for the requirement of flash point measurements is to assess the safety hazard of a liquid or semi-solid with regard to its flammability and then classify the liquid into a group. If the temperature of the liquid is above its flash point, there is a possibility of getting fire through the liquid. The lower the flash point temperature, the greater the risk. This classification is then used to warn of a risk and to enable the correct precautions to be taken when using, storing or transporting the flammable liquid or oil. Specifications quote flash point values for quality control purposes as well as for controlling the flammability risk. A change in flash point can indicate the presence of potentially dangerous volatile contaminants or the adulteration of one product by another. Test Method There are two basic types of flash point measurement: open cup and closed cup. In open cup devices, the sample is contained in an open cup, which is heated, and, at intervals, a flame brought over the surface. The measured flash point will actually vary with the height of the flame above the liquid surface, and at sufficient height, the measured flash point temperature will coincide with the fire point. The best-known example is the Cleveland open cup. ‘There are two types of closed cup testers: non-equilibrial, such as Pensky-Martens, where the vapors above the liquid are not in temperature equilibrium with the liquid, and equilibrial, such as Small Scale (commonly known as Setaflash), where the vapors are deemed to be in temperature equilibrium with the liquid Objectives 1, To determine the flash point of the supplied oil. 2. To determine the fire point of the supplied oil Experimental Setup A schematic diagram of the experimental setup is shown in Fig. 1, The setup consists of a Pensky-Martens closed cup flash and fire point tester, thermometer, Bunsen burner, ete. In the setup, a brass test cup is filled with a test specimen. The cup is provided with a cover through which a stirrer, provision to insert thermometer and slit to open and close. The thermometer is inserted such that the thermometer bulb should measure oil temperature and should not touch the wall of the cup. The sample is heated and stirred at specified rates. Pensky-Martens closed 15 cup is sealed with a lid through which an ignition source can be introduced periodically with simultaneous interruption of stirring until a flash that spreads throughout the inside of the cup is seen. The comesponding temperature is its flash point. ‘Shuster contol ‘Oi evel penter — steer ‘Ollcup Figure 1. Schematic Diagram of the Experimental Setup. Experimental Procedures L Take an amount of the supplied oil in the crucible and put this in the flash point and fire point apparatus, Place a thermometer within the oil to measure its temperature through the hole in apparatus. Apply heat to the sample of oil using a gas burner, Insert a flame within the oil vapor using the gas nozzle of the apparatus at every 2°C temperature rise of the oil. Keep stirring the oil with the stirring mechanism. Record the temperature at which the oil vapor gives flash of fire and then get away. Keep on applying heat to the oil until it reaches the fire point and gives a continuous flame when the gas nozzle inserted in to the oil vapor. Record the fire point of the oil. 16 Discussion 1, Briefly explain the limitations of the experimental setup, if any. 2. Explain the difference between flash and fire point of the given oil. 3. How does the atmospheric pressure affect the reading of flash and fire points during the experiment? Conclusion Write down the summary of key findings and observations experiment outlined in the objectives of this Sample Quiz Questions: 1. How do you detect flash point during performing the experiment?” 2. Why is it important to know both flash and fire point of any fuel? 3. Is flash point of a particular oil a constant parameter? What are the factors on which the flash point of an oil depends? 7 Data Sheet Determination of Flash Point and Fire Point of Given Oil Barometric Pressure, Pan = ‘Type of Oil Used: mm Hg ‘Table 1: Collection of oil temperature for different observations. No. of Observation Oil Temperature, T ‘Observation: (Yes/No) CO) Flash Point Fire Point 1 2 4 5 6 7 8 9 i0 Flash point of given oil, Task °C Fire point of given oil, Tyre °c 18 EXPERIMENT NO. 2(a) Proximate Analysis of Coal Introduction An analysis of a coal which may be made with the minimum of equipment is the proximate analysis (sometimes referred to as an engineering analysis). The following four constituents are determined by this type of analysis: 1. Moisture 2 Ash 3. Volatile matter 4, Fixed carbon, Moisture Determination Some of the moisture in the coal is known as inherent moisture, ie., it is inherently a part of the structure of the coal and cannot be readily separated from it. The rest of the moisture in the coal is so called free moisture, which will be determined through gradual heating. This process is dependent on the temperature to which it is heated and the length of time, it is held at the elevated temperature. The heating of the coal has a tendency to produce two other effects in addition to driving off the free moisture. It may drive off other volatile constituents of the coal and it may cause some oxidation of the coal. Hence, it should be evident that there is no way of determining exactly the true amount of free moisture in the coal. Ash Determination The ash originally present in the coal is quite difficult to exactly determine. During the heating process, there may be oxidation of some of the material constituents of the coal. The products of oxidation may or may not be driven off from the coal. In addition, there may be some decomposition of mineral constituent, with some of the products being vaporized, Although it is hard to determine the absolute value of the ash in the coal, qualitative results may be obtained when the conditions of the ash determinations are duplicated. 19 Volatile Matter Determination In addition to moisture, coal contains volatile constituents, largely hydrocarbons, which will be driven off by the application of heat. It should be recognize that the amount of volatile matter found by this determination, is a function of the heating time as well as the temperature In order to obtain qualitative results, both of these variables must be controlled as specified. ‘Mechanical losses occur when some coals are heated very rapidly due to too rapid release of volatile matter or steam. These mechanical losses are recognizable by the sparking that occurs when the small fragments of the coals are heated to incandescence as they being expelled. If any sparking occurs, the test results are worthless and the test procedure should be modified ‘A new coal sample should be slowly lowered into the furnace and gradually heated for a period of 5 to 10 minutes. Care should be taken to avoid sparking. The crucible may now be lowered into the regular position and heated at the standard temperature for a period of exactly 6 minutes, Fixed Carbon Determination Some of the carbon content of the coal is in the form of hydrocarbons, which will driven off when the coal is heated. The reminder of the carbon, which cannot be driven off by the application of heat is called fixed carbon, There is no direct way of determining the fixed carbon in a coal, and hence, it must be calculated by subtracting the summation of the moisture, ash and volatile matter weights from the original weight of the coal. Although fixed carbon cannot be vaporized, some of it will burn quite rapidly in the presence of oxygen, particularly at the temperatures used during the determination of volatile matter. Hence, care must be exercised to prevent oxygen from entering the crucible during the determination of volatile matter. This is most readily done by using a close fitting cover on. the crucible. Objectives 1, To determine the moisture content of the supplied coal 2. To determine the ash content of the supplied coal. 3. To determine the volatile matter content of the supplied coal. 4, To determine the fixed carbon content of the supplied coal. 20 Experimental Setup ‘The experimental setup consists of an electric oven, an electric muffle furnace, an electric tube furnace, chemical balance, desiccators, porcelain capsule with flat aluminum cover, platinum crucible with tightly fitting cover, platinum/nichrome wire, etc. The electric oven should have a temperature regulation to 110°C (230°F) and a renewal of air at the rate of 2 to 4 times a minute, which has been dried by passing through sulfuric acid (S.G. 1.84). The electric muffle furnace should have a temperature regulation between 700° and 750°C with good air circulation. The electric tube furnace should have a temperature regulation to 950° + 20°C (1740° + 35°F). The coal sample should pass through a No. 60 sieves. Experimental Procedures 1. Transfer with a spoon or spatula about 1 g. of the coal sample to a porcelain capsule which has been previously heated and dried in a desiccator 2. Cover the capsule and record the weight from the chemical balance. Then dry for 1 hour, uncovered, in the preheated electric oven at about 107° + 3°C. 4, Cool in a dissector over sulfuric acid and record the weight again from the chemical balance. 5. Now the porcelain capsule containing the dried coal should be uncovered and placed in the electric muffle furnace when the furnace is cold. Gradually heat to redness. 7. Finish ignition in between 700 and 750°C, with 0 nichrome wire, until all carbon particles have disappeared, asional stirring with a platinum or 8. Cool in a desiccator and record the weight from the chemical balance. Then continue alternate heating and recording weight until the weight is constant. Record the final weight. 10, Transfer with a spoon or spatula about 1 g. of the coal sample to a platinum crucible 11. Cover the crucible and record the weight from the chemical balance. 12. Now place it in the electric tube furnace chamber, which has been preheated to 950° + 20°C (1740° + 35°F), 13. Heat exactly 7 minutes. 14. Remove and cool without disturbing the cover. Record the weight from the chemical balance. Relevant Equations Determination of Moisture Content in the Coal 21 ‘The moisture content in the given coal is calculated as follows: W, W, eis = Wary — Wy sin where, Whois = Weight of the moisture content in the given coal (g), Wigary = Weight of the capsule with cover containing coal before drying (g), Warary = Weight of the capsule with cover containing coal after drying (g) ‘The percentage of moisture content in the given coal is calculated as follows: f Xu, = Ya 100 = Wee 100% ” Wrot cy Wor where, Xnois = Percentage of the moisture content in the given coal (%), Weeoat = Wigéry ~ Wor = Weight of the first coal sample taken in the porcelain capsule (g), Wpor= Weight of the empty porcelain capsule with aluminum cover (g) Determination of Ash Content in the Coal ‘The ash content in the given coal is calculated as follows: -W, sh 5) Ween = Westy where, Was Warne = Final weight of the capsule with cover containing coal after alternate heating and ‘Weight of the ash content in the given coal (g), cooling (g). The percentage of ash content in the given coal is calculated as follows: an = We 100% o at where, Xwoir = Percentage of the ash content in the given coal (%) Determination of Volatile Matter Content in the Coal The volatile matter content in the given coal is calculated as follows: Woaam = Wig — Wag — Won m where, Wooim = Weight of the volatile matter content in the given coal (g), Wogan = Weight of the crucible with cover containing coal before rapid heating (g), 22 Wojrn = Weight of the crucible with cover containing coal after rapid heating (g). ‘The percentage of volatile matter content in the given coal is calculated as follows: a x100= Wie 100% * Won Wri where, Xvom = Percentage of the volatile matter content in the given coal (%), Wacoat = Wijer ~ Wor = Weight of the second coal sample taken in the platinum crucible (g), Wolar = Weight of the empty platinum crucible with cover (g). Determination of Fixed Carbon Content in the Coal ‘The percentage of fixed carbon content in the given coal is calculated as follows: X = (100 Xeuy — Xe — Xin) % 8) where, Xje = Percentage of the moisture content in the given coal (%) Discussion 1, Briefly explain the limitations of the experimental setup, if any. 2. Explain the importance of proximate analysis of coal. How does the heating condition affect the determination of volatile matter and fixed carbon content in the coal during the experiment? 4, Explain the necessity of cooling of the heated sample before recording the weight. Conclusion Write down the summary of key findings and observations as outlined in the objectives of this experiment. Sample Quiz Questions: ‘What is the difference between inherent moisture and free moisture in the coal? 2. Why is it important to maintain the specified temperature and the time for determination of moisture content in the coal? 3. Is it possible to obtain the absolute value of the ash in the coal by the present experimental procedure? 4, What do you mean by qualitative result? How can one obtain those results? Data Sheet Proximate Analysis of Coal ‘Table 1: Collection of experimental data. ‘Measured Parameters ‘Symbol (unit) | Value ‘Weight of the empty porcelain capsule with aluminum cover Wror (2) Weight of the capsule with cover containing coal before drying [ _ Worar (@) Weight of the capsule with cover containing coal after drying [Waray (@) Final weight of the capsule with cover containing coal after Wane (2) alternate heating and cooling ‘Weight of the empty platinum crucible with cover Wrin @) Weight of the crucible with cover containing coal before rapid | Woia(g) heating ‘Weight of the crucible with cover containing coal after rapid Wan) heating ‘Table 2: Calculation of different constituents in the given coal, Calculated Parameters ‘Symbol (unit) | Value ‘Weight of the first coal sample taken in the porcelain capsule ‘Wecoat (@) Weight of the moisture content in the given coal Wasis (2) Percentage of the moisture content in the given coal Xnois (%) ‘Weight of the ash content in the given coal Wass (@) Percentage of the ash content in the given coal Xen (%) ‘Weight of the second coal sample taken in the platinum Wacoal (@) crucible Weight of the volatile matter content in the given coal Wran @) Percentage of the volatile matter content in the given coal Xvoim (%) Percentage of the fixed carbon content in the given coal Xie, 24 EXPERIMENT NO. 2(b) Study and Calibration of Thermocouple Introduction The thermocouple is the most common type of temperature sensor, primarily because it is inexpensive and easy to use. It is based on the observation that an EMF (Electromotive force) is generated in a circuit of dissimilar materials if the junctions (connecting ends of dissimilar materials) are kept at different temperature. This phenomenon is called the Seebeck Efe and this EMF is known as thermal EMF, which is proportional to the temperature difference between two junctions of a particular thermocouple. Now, if one junction is kept at a fixed temperature, the EMF will depend only on the temperature of the other junction. Usually, one junction known as cold junction is kept at an ice bath (0°C or 32°F), while the other junction called as hot junction is placed at variable temperature (7) which needs to measure. Hence, the thermal EMF developed due to temperature difference between the two junctions becomes a function of hot junction temperature, which can be expressed as, v= F(T) ao where, V= Thermal EMF generated by thermocouple (mV), T = Hot junction (unknown) temperature (°C ot °F). The above relation shows that thermal EMF can be obtained for a particular temperature. Unfortunately, there is no simple functional relationship between V and T for thermocouples in use. Hence, experiments are carried out to establish the relationship between V and T. This relationship can be presented in either tabular or graphical chart form. One example of these relationships is presented in Appendix A for Chromel-Alumel thermocouple. Properties of Thermocouple Materials Although any two dissimilar metals may be used for a thermocouple, certain combinations are unsatisfactory for practical purposes, because of low EMF developed and because of the reversal of the direction of EMF at certain temperature. Some desirable properties of thermocouple materials are as follows: (@ Capability of resisting oxidation and corrosion. (ii) Development of a relatively large EMF 25 (iii) A continuous increase of EMF with temperature over its entire range, (iv) Stability of EMF with respect to temperature. (v)_ Material must be reproducible. ‘Material combinations of some important thermocouples are presented in Table 1 ‘Table 1: List of thermocouple types, materials and working temperature range. jo. | ANSI Type | Material Combinations ‘Temperature Range (*F) T Tron — Constantan®™ 32 to 1400 T Copper — Constantan® 300 to 700 E Chromel” = Constantan™ 32 to 1600 K Chromel” — Alumel® 32 to 2300 Ss Platinum & Rhodium’ — Platinum 32 t0 2700 i “Nominal composition: 55% Cu, 45% *Nominal composition: 10% Cr, 90% Ni ‘Nominal composition: 2% Mn, 95% Ni, 2% Al “Nominal composition: 10% Rh, 90% Pt In order to achieve the traceability and reliability, measuring instruments and sensors should be controlled by verification, validation and calibration. Calibration in measurement technology is the process of comparison of measurement values delivered by a device under lest with a calibration standard of known accuracy. Calibration of the instrument can be defined as finding the dependence between the input and output of the measuring instrument and finding the deviation of measurements. The input for thermocouples is the measure temperature and the output is the thermal EMF generated by thermocouple, The results can be presented as a table, chart or formulas. ‘Objectives To measure temperature of muffle furnace using thermocouple. 2. To plot the actual temperature of muffle furnace versus the observed EMF reading of thermocouple. 3. To plot the actual temperature of muffle furnace versus the observed temperature measured by thermocouple. 4, To plot percentage of error versus the actual temperature of muffle furnace 26 Experimental Setup A schematic diagram of the experimental setup is shown in Fig. 1. The setup consists of a box. type electric muffle furnace (temperature range: 0 to 2000°F or 0 to 1100°C, Power: 1440 W), whose temperature is shown by a dial placed at the top of the furnace. A hand operated lever is attached on the bottom of the furnace to control the heating through variable theostat. Hot junction of the thermocouple will be placed inside the muffle furnace to measure the corresponding EMF change. Instead of putting inside an ice bath, the cold junction is kept at room temperature, and a multimeter/millivoltmeter is used to record the EMF change of thermocouple. Furnace Door Temperature Dial + 5 . Muffle furnace i 3 3 r——) — |ceramic ¥ ai 1 Fiber 3 2 W—] 5 i | METAL B if 7 Cold Junction -- Isothermal Biock Control lever. K-Type Thermocouple Figure 1, Schematic Diagram of the Experimental Setup. Experimental Procedures At first, place the hot junction of the thermocouple inside the muffle furnace. Connect the cold junction with the multimeter terminals. Switch on the muffle furnace to provide heating and start recording the temperature of the furnace from the dial when it shows 200°F. 4 Take the reading of the multimeter at the same time. 5. Continue recording the temperatures of muffle furnace with an interval of 50°F up to 11007 21 Relevant Equations Room Temperature Correction The thermocouple is constructed in such a way that the cold junction should be placed at 0°C or 32°F. Hence, a correction is necessary to get the (corrected) observed ’. However, the cold junction will keep at room temperature during the experiment. EMF reading while measuring the temperature of hot junction of thermocouple. This is called room temperature correction. If the room temperature during the experiment is T.. (°F), the corresponding room temperature correction, Veor (mV) can be determined from the supplied thermocouple chart given in Appendix A. Determination of Corrected Observed EMF Reading If the cold junction is not placed at 0°C or 32°F, the observed EMF reading of thermocouple is calculated using the room temperature correction as follows: Voss = Vinee + Veore? ToT, Vas, Vee Vat T

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