SEPARATION PROCESS FUNDAMENTALS LABORATORY EP 316

LABORATORY MANUAL

Lecturer/Instructor:

N!"e Stu#ent ID Course

: : :

FACULTY OF EN$INEERIN$% TEC&NOLO$Y ' BUILT EN(IRONMENT UCSI UNI(ERSITY

)ANUARY * APRIL +,1-

$ENERAL INSTRUCTIONS

The experiments in this manual are designed to give engineering students an introduction to material science including aspects such as atomic structure, material properties and testing. These experiments are also intended to teach students the principles of laboratory protocol and reporting. Students are required to carry out all the experiments following the general methods and procedures presented in this manual. All experiments are to be completed within the allotted time. Students are expected to be prepared prior to coming for the laboratory session. This includes reading the lab procedure thoroughly and understanding the objectives, operations and hazards that may be encountered during the experiment. The laboratory experiments shall be conducted in groups. Thus, students have to learn to organize themselves within the groups and to allocate responsibilities among themselves.

LABORATORY PROCEDURE AND CONTROL

+.1 Lo/0oo1

ou are required to !eep a logboo! for experiments. This must be a bound logboo!. ou are required to translate the procedure of each experiment in the laboratory manual into graphical illustrations or a flowchart in your logboo! before you start. "ecord in your logboo! every action and observation as you carry out the experiment. "ecords should be as brief, but concise, as possible.

#ach experiment in the logboo! should contain the following information$

%i& Title of the experiment %ii& 'ate of the experiment carried out %iii& (bjective of the experiment %iv& )ypothesis of the experiment %v& *rocedure outline or brief description of the method %vi& (bservation %should be recorded throughout the experiment& A logboo! should be neat. +larity of procedure and results are important. Always use a pen to write on your logboo!. ,ista!es made should be crossed out clearly. -se of liquid paper or eraser is not allowed. The lab instructor.lecturer will inspect and sign your logboo! during the lab session and possibly grade them at the end of the semester. +.+ L!0or!tor2 /rou3 ou will be assigned into a group %please refer to the student notice board or outside the lab after the first session of the laboratory meet up&. Students are not allowed to change groups. ou are required to wor! with your group members as much as possible in terms of understanding the experiment and sharing information on the different activities performed by different members. At the end of each of the session, each of the group members is required to carry out peer evaluation. *eer evaluation is private and confidential. The purpose of peer evaluation is to ensure that all group members contribute throughout the laboratory session.

+.3 L!0or!tor2 Re3orts

#ach student will be responsible for preparing an individual report after completing each laboratory experiment. %a& "eport submission "eports must be submitted one 415 6ee1 after the scheduled experiment and within the first ten %/0& minutes of the due lab period. Any unforeseen circumstances must be reported to the lab instructor immediately. 1ate submissions will not be accepted. %b& "eport style.format "eports may be hand2written or typed2written. 3f typed2written, text shall be spaced, using font type 4ew Times "oman and font size /5. 3t is recommended that an equation editor be used, otherwise, equations may be handwritten. Atomic structures and other figures may be drawn by hand. The report shall be$ %i& %ii&
%iii&

6ritten in the passive tense. #xample$ 78ive milligrams of solid was weighed.9 :raphs must be complete with title, axis labels with units and legend where necessary. The scale of the graph should be appropriate for the data obtained.
*lagiarism will not be tolerated.

%c&

"eport contents #ach report should contain the following$ %i& (ii) (iii) Front page %"efer to Appendix A& Table of contents %"efer to Appendix ;& Introduction/background of the experiment +ontains a summary of the experiment that is carried out. This section includes the statement of purpose or objectives of the experiment and an introduction to the technique used. 3t is not necessary to include a discussion of the basic theory relevant to the experiment. The introduction of the report should not be more than 50< of the overall report.

(iv)

Material and Methodology This is a brief description of the experimental approach used. 3t should include a brief description of the test apparatus and instrumentation used, as well as the procedure used to obtain the test results. Summarize the detailed steps used= do not repeat the steps given in your lab experiment.

(v)

Results and discussion Test results obtained from the experiment shall be presented in the applicable format$ 4arrative, tabular, graphical, photographic, or a combination of the above. 4umerical data must be presented realistically with appropriate number of decimal places. 'ata should be tabulated neatly showing raw experimental data, if necessary, and reduced %useful& data. +alculations for reduced data should be briefly described and need not be wor!ed out. 3dentify formulas, charts, tables or handboo!s that were used to obtain the final result. 3f needed, you may refer sample calculations to the appendix. Any questions given in the lab sheet should be answered in the 'iscussion section.

(vi)

onclusion This section summarizes your findings of the experiment. 3f results differ from those expected, provide an explanation based on an analysis of the data. #xamine any assumptions used that could be adversely affecting the results.

(vii)

!imitation of the "xperiment/#ifficulties "ncountered (if any) +onsider any limitations or difficulties encountered during the experiment. 3nclude also any errors that may have occurred. Suggest ways for improvement.

(viii)

Reference A minimum of three %>& references should be cited in your report. "efer to Appendix + for the format of citations.

(ix)

$ppendix (if any)

L!0or!tor2 S!7et2 All safety requirements as specified in this section will be strictly enforced. Students are required to comply with the following rules when in the lab. /. 5. 6ear closed shoes and lab coats at all times while in the laboratory. #ye protection %goggles& should be used when necessary. 6ear suitable attire for lab wor!. 'o not wear loose or bul!y clothes, ties or jewelery when wor!ing around rotating equipment. Students with long hair must tie their hair before entering the lab. (pen2toe shoes and sandals are not permitted. (!ecturer/instructor reserves the right not to allo% students %ho do not follo% this rule to enter the lab)& >. ?. @. A. B. C. D. /0. #ating and drin!ing in the lab are strictly prohibited. All hand phones must be switched off. Always be punctual. Students later than /@ minutes are not allowed to perform the experiment. Students must have a towel %for cleaning purposes&, a logboo! and their lab manual during the lab session. Always follow the instruction of the lab instructor or lecturer before the start of the lab. +lean the bench and return all apparatus to their respective places before you leave the lab. -se only required amounts of reagents to avoid wastage and excess. 'ispose of excess reagents as instructed, never return excess reagents into the bottle. Some used chemicals may be washed down the drain, while others require a different method of disposal. 3f a chemical can go in the sin!, be sure to wash it away thoroughly rather than ris! an unexpected reaction between chemical EleftoversF later. //. /5. />. ,a!e sure you !now the location of the following safety devices$ eyewash station, emergency shower, fire extinguisher, fire alarm station, emergency evacuation route. )andle all equipment with care to avoid damage during experimental operations. +lean up bro!en glass and report to the lab instructor or lecturer immediately.

E8PERIMENT 1: SIE(E TEST ANALYSIS OB)ECTI(E /. To determine the particle size distribution by sieving technique T&EORY Sieving is one of the few principal methods, in which a relatively large quantity of material is physically subdivided in size classes. The separated fractions can be accurately weighed and, thus, the determination of the size distribution functionGbased on massGmay be accurate. The major advantages of the sieving technique are that it allows relatively large samples for analysis or separation, that the principles are easy to understand and that the sieves and sieving equipment are relatively cheap. Also, size fractions are being obtained, which can be used for other purposes %e.g., further analysis or product testing&. APPARATUS Sieve sha!er, electric balance, spanner, brush, soil.sand.

PROCEDURE /. +lean each sieve and the bottom pan using the provided brush. 6eigh the sieve and the bottom pan individually and record the data. 5. 6eigh /!g of sample %soil.sand&. >. Arrange the sieve with biggest aperture size at the top and lowest at the bottom and finally the pan at the most bottom. ?. Sha!e the stac! for a specified length of time at a preset speed. @. 6hen sha!ing is complete, weigh each sieve again individually. A. "ecord the weight of sample retained from each sieve and the pan. B. +omplete the table given. RESULTS AND DISCUSSION H of Aperture sieve size %mm& / 5 > ? @ A B *an Total ,ass of empty sieve : ,ass of sieve I retain sample g Sieve fraction +umulative retained < +umulative undersize <

<

+umulative undersize J /00 K +umulative retained (riginal mass Total of fraction masses 1oss wt J w/ J
%t %/ J % x/00< t

JLLLLLLLLLLLL< %o! if less than 5<& 3n your discussion, you should include the following$ /. *lot the graph of cumulative undersize against average particle size. 5. 'etermine the particle size at < cumulative /A<, @0<, and C?< >. +alculate the particle size distribution using formula$
Size distribution = pC? p/A 5

?. 'iscuss why sieving process is important in chemical engineering. CONCLUSION State the conclusion of the experiment. REFERENCE: /. ,c +abe, 6.1, Smith, M.+. N )arriot, *., 7-nit (peration of +hemical #ngineering9, ?th #dition, ,c :raw2)ill, /DC@.

E8PERIMENT +: BATC& SEDIMENTATION TEST OB)ECTI(E /. 1earning the fundamental principle of separation of solids from suspensions 5. To determine the rate of sedimentation of a sample of particles in a liquid >. To plot a graph between the suspension density at a certain vertical position against time T&EORY Sedimentation uses gravitational forces to separate particulate material from fluid streams. The particles are usually solid, but they can be small liquid droplets, and the fluid can be either a liquid or a gas. 3n sedimentation, particles are falling from rest under the force of gravity. Therefore in sedimentation, ta!es the familiar form of Sto1es9 L!6$ 'T J x5g%Op 2 Of&./CP where Op J Of J g J xJ PJ 'T J density of particle, !g m2> density of fluid, !g m2> gravity, m s25 particle diameter, m molecular viscosity, 4 s m25 terminal settling velocity, m s2/

Sto!eFs 1aw applies only in streamline flow and strictly only to spherical particles. Sto!esF solution is applicable for settling at low "eynolds numbers % ReQQ /&. Sto!esF 1aw applies only to cases in which settling is free, that is where the motion of one particle is unaffected by the motion of other particles. The objective of sedimentation process analysis is to determine the rate at which solid particles accumulate in the lower end of the container. A graph of the interface height versus time is !nown as the sedimentation curve.

MATERIAL AND APPARATUS :raduated cylinder, stop watch, ruler, stirring rod, bea!er, chal! and water. Pre-lab assignment: The force balance for a settling particle %at terminal velocity& is 8drag J , g2 8buoyancy %where g is the gravitational acceleration, 8drag is drag force, , is the particleFs mass and 8buoyancy is buoyancy force, R Of g, R is the particleFs volume & And thus, 8drag J %Op 2 Of & g S '> .A 8drag J > S Pf ' 'T 'erive Sto!esFs 1aw. PROCEDURE /. *repare a @00m1 graduated cylinder with a ruler. 5. 6eigh /0g of sample and put in a bea!er. 8ill in the bea!er with >002?00m1 of tap water. ,ix suspension vigorously to achieve even mixing. Transfer the suspension to the prepared graduated cylinder. >. The start2time for measurement is when the object has reached several centimeters below the surface and stop2time is several centimeters above bottom. ?. 8or every five seconds interval, record the height of the clear area. @. "epeat the same process for > times and the average height was recorded. A. *lot the graph of the interface height versus time. 8rom the graph, calculate the settling velocity of suspension at any point of time. Then, determine the particle diameter, x. B. 'iscuss the graph that you have plotted.

RESULTS AND DISCUSSION Time )eight

:iven Tuestion$ +alculate the settling velocity of dust particles of %a& A0mm and %b& /0mm diameter in air at 5/U+ and /00!*a pressure. Assume that the particles are spherical and of density /5C0 !g m2>, and that the viscosity of air J /.C x /2@ 4 s m25 and density of air J /.5 !g m2>. CONCLUSION State the conclusion of the experiment. REFERENCE State the reference used.

E8PERIMENT 3: CENTRIFU$ATION OB)ECTI(ES /. "ecognize the fundamentals of centrifugation 5. (perate a centrifuge at a pilot scale INTRODUCTION The centrifuge is a widely used instrument for the separation of components. This operation is a separation process that uses centrifugal force to separate two mixed liquids or insoluble solids from liquids %suspension&. The centrifuge wor!s using the sedimentation principle, where the centripetal acceleration causes more dense substances to separate out along the radial direction %the bottom of the tube&. ;y the same to!en, lighter objects will tend to move to the top %of the tube= in the rotating picture, move to the centre&. T&EORY *rotocols for centrifugation typically specify the amount of acceleration to be applied to the sample, rather than specifying a rotational speed such as revolutions per minute. The acceleration is often quoted in multiples of g, the standard acceleration due to gravity at the #arthVs surface. This distinction is important because two rotors with different diameters running at the same rotational speed will subject samples to different accelerations. Since the motion is circular the acceleration can be calculated as the product of the radius and the square of the angular velocity. Traditionally named W"elative centrifugal forceW %"+8&, it is the measurement of the acceleration applied to a sample within a centrifuge and it is measured in units of gravity %times gravity or X WgW&. 3t is given by

where is earthVs gravitational acceleration, is the rotational radius, is the rotating speed, measured in revolutions per unit of time. 6hen the rotational speed is given in revolutions per minute %"*,& and the rotational radius is expressed in centimeters %cm& the above relationship becomes $

is the rotational radius measured in centimeters %cm&, is rotating speed measured in revolutions per minute %"*,&. MATERIAL AND APPARATUS +entrifuge unit, centrifuge tube, ruler, sample %ferrocene I toluene.sugar cane .chocolate drin!& PROCEDURE /. #nsure an authorized member of staff outside the laboratory is made aware that the centrifuge is going to be operated with the information provided on the test procedure sheet. This person should be notified again once the test is complete. 5. Turn on the main power (4 using the switch on left hand side of the centrifuge. >. The 1#' displays will indicate the current status and settings. ?. *ress the 13' !ey to unlatch the lid. @. 3nsert an appropriate adaptor for the glassware to be used into each of the four buc!ets. A. 3nsert the glassware, loaded with sample, into the adaptors, +A-T3(4$ T6( (" 8(-" SA,*1#S +A4 ;# +#4T"38-:#' AT T)# SA,# T3,#, +#4T"38-:34: (4# (" T)"## SA,*1#S 6311 +A-S# A4 3,;A1A4+# (8 T)# "(T(" A4' ,A "#S-1T 34 'A,A:# T( T)# +#4T"38-:#. 38 (41 "(T(". B. +hec! tightness of rotor nut before operation. 6A"434:$ T)# ,AY3,-, 1(A'34: (8 T)# "(T(" A4' T)# ,AY3,-, *#",3SA;1# "#R(1-T3(4S *#" ,34-T# ,-ST 4(T ;# #Y+##'#' %S## 1A;#1 (4 "(T("&. C. *ush the lid closed and hold it until the latch is felt to start to pull the lid down onto the seal. D. *ress the S*##'."+8 !ey to toggle between speed %in rpm& and "elative +entrifugal 8orce %in g&. /0. "otate the Time +ontrol until the required value is shown on the Timer display. T6( SA,*1#S A"# ;#34: +#4T"38-:#', T)# :1ASS6A"# +(4TA3434: T)# SA,*1#S ,-ST ;# *1A+#' (**(S3T# #A+) (T)#" 34 T)#

//. The temperature to be set is entered into the Set Temperature display by rotating the Temperature control. /5. *ress the STA"T !ey to commence a run. RESULT AND DISCUSSION 6hat would be the expected result if a different centrifugation speed has been selectedZ CONCLUSION State your conclusion. REFERENCE State the reference used.

E8PERIMENT -: SEPARATION OF SOLID MI8TURE ,ixtures are not unique to chemistry, we use and consume them on a daily basis. The beverages we drin! each morning, the fuel we use in our automobiles, and the ground we wal! on are mixtures. Rery few materials we encounter are pure. Any material made up of two or more substances that are not chemically combined is a mixture. The isolation of pure components of a mixture requires the separation of one component from another. +hemist have developed techniques for doing this. These methods ta!e advantage of the differences in physical properties of the component. The technique to be demonstrated in this laboratory are the following$ #xtraction$ this uses a solvent to selectively dissolve one component of the solid mixture. 6ith this technique, a soluble solid can be separated from an insoluble solid. 'ecantation$ This separates a liquid from insoluble solid sediment by carefully pouring the liquid from the solid without disturbing the solid. "ecrystallization $This involves dissolving a mixture of solids in a hot solvent, followed by cooling, and crystallization of the more insoluble material. 8iltration $ This separates a solid from a liquid through the use of a porous material as a filter. *aper, charcoal, or sand can serve as filter. These materials allow the liquid to pass through but not the solid. O0:ect;<e : Separate the substances. 'etermine the percent of each in the original mixture.

M!ter;!=s !n# !33!r!tus$ Sand, benzoic acid, tap water, sodium chloride ;ea!er, hot plate, filter funnel, stirring rod.

Resu=t !n# C!=cu=!t;on: /. +alculate the percent of each component in the mixture. S>o6 2our c!=cu=!t;on. 5. +alculate the percent error in your result. S>o6 2our c!=cu=!t;on.

E8PERIMENT ?: NATURE OF FLO@. O0:ect;<e: To visually observe laminar and turbulent flow patterns. To determine the critical "eynolds number for transition from laminar to turbulent flow. To determine the friction factor and to verify the relationship between f and (R"

Resu=t !n# C!=cu=!t;on. /. 8or each run, comment on the observes characteristics of the flow. 5. +alculate the volumetric flow rate, linear velocity, friction factor and "eynold number. >. 'etermine the critical "eynolds number for the transition from laminar to turbulent flow, when the flow rate is increased in small steps. 3s it the same for the transition of turbulent to laminar flow when flow is decreased in small stepsZ ?. *lot the graph of f versus (Re and comment on the graph.