FACULTY OF ENGINEERING AND THE BUILT ENVIRONMENT DEPARTMENT OF CHEMICAL AND METALLURGICAL ENGINEERING

STUDENT LABORATORY GUIDE

NAME OF COURSE: CHEMICAL ENGINEERING PLANT (IIIA) NQF CREDIT S

NQF LEVEL

QUALIFICATION & SAQA ID

COURSE CODE

Diploma In CHEMICAL ENGINEERING (CMP33AT) SAQA ID No.: NLRD49744..

COMPILED BY : Mr M. Mosesane REVISED BY : Mr V. Hlongwane 2010

2009

COPYRIGHT : Tshwane University of Technology Private Bag X680 PRETORIA 0001

Printed and distributed by : FACULTY OF ENGINEERING AND BUILT ENVIRONMENT

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ORGANISATIONAL COMPONENT CONTENTS: 1. Welcome.....................................................................................................................5 2. LABORATORY Staff...................................................................................................6 2.1 Contact Details......................................................................................................6 2.2 Staff availability.....................................................................................................6 3. Requirements, resources and recommended material.............................................7 3.1 Requirements for the course.................................................................................8 4. Code of conduct.......................................................................................................10 5 Attendance............................................................................................................14 5.1 LABORATORY, HEALTH & SAFETY RULES AND REGULATIONS...............14 BASIC RULES...........................................................................................................14 5.2 Responsibilities of students................................................................................14 6. Assessment..............................................................................................................15 6.1 Assessment methods and criteria......................................................................15 6.2 Assessment rules................................................................................................15 6.3 Marking system .................................................................................................15 6.4 predicate/Year mark...........................................................................................16

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6.5 Moderation ........................................................................................................17 6.6 Promotion requirements.....................................................................................17 7. laboratory course content and schedule..................................................................17 7.1 schedule of laboratory sessions and assignments.............................................17 7.2 Learning outcomes and assessment criteria.....................................................19 7.3 Generic outcomes and critical cross-field outcomes.........................................21 8. Glossary of terms ....................................................................................................21 9. Assessment Records ..............................................................................................21 10 Example of a practical report...............................................................................22 11. Appendices ...........................................................................................................26 11.1 Flocculation and coagulation.............................................................................26 11.2 sedimentation experiment.....................................................................................29 Up = true particles hindered velocity (m/s).................................................31 12. Example of a practical report.................................................................35

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SECTION

ORGANISATIONAL COMPONENT

1. WELCOME Welcome to laboratory session of Chemical Engineering Plant IIIA. This part of the course provides an introduction and represents advanced knowledge in unity operation and is offered via experimental work, problem-based work or project-based work over 8 weeks. The course is structured in such a way as to master theoretical concepts and principles and various practical skills to provide a sound foundation for the study of Distillation, Absorption and Drying to complement the major courses in the qualification and pave the way for more advanced learning in B-Tech in Chemical engineering. We trust you will enjoy the course, and find it interesting and informative.

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2. LABORATORY STAFF 2.1 CONTACT DETAILS

NAME

CAMPU S

ROOM NO

TEL NO E-MAIL (012) 382 3513 mbayar@tut.ac .za

CONSULTA TION TIMES

ACADEMIC FUNCTION

Dr R. Mbaya

Pretoria

Lecturer

(012) 382 4655 Mr M.J Mosesane Pretoria B2 R127 mosesanejm@t ut.ac.za 08H00 16H00 Technologis t

Mentors

2.2 STAFF AVAILABILITY

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If, after attending class and making every effort from your side to master content, you still have problems with understanding key concepts or principles or their application, lecturers are available for consultation. To consult your lecturer, make an appointment by calling his office or see/ call the secretary at (012) 382 3597/3514 for an appointment. To consult your technologist, make an appointment by calling his office at ( 012) 382 4655 or call the secretary at (012) 382 3514.

3. REQUIREMENTS, MATERIAL.

RESOURCES

AND

RECOMMENDED

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3.1 REQUIREMENTS FOR THE COURSE 3.1.1 PRESCRIBED RESOURCES

The following tables indicate what literature and other resources are essential for successful completion of this course. You are strongly advised to acquire all the prescribed resources. PRESCRIBED RESOURCES CATEGORY DESCRIPTION WHERE TO FIND COST LEVY

CALCULATOR

Scientific

Bookstore

COMPUTER

Computer lab

HARDWARE

Laboratory Journal/Notebook ( page or exam pad )

not

SOFTWARE

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EQUIPMENT

Sedimentation Study Kit and Jar test equipment

COMPONENT S

3.1.2

RECOMMENDED RESOURCES

The following recommend resources will enhance your understanding and knowledge in this course, and you are encouraged to use the following additional resources.

RECOMMENDED RESOURCES CATEGORY AUTHOR NAME PUBLISHE R ISBN NO

BOOKS MANUALS Laboratory Manual

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GUIDES RECOMMENDED ELECTRONIC MATERIAL & WEBSITES VIDEO

CD

DVD

WEBSITES

4. CODE OF CONDUCT Safety Laboratory safety is the top priority and this requires all people in the lab to be observing safe practices at all times!

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 Safety glasses must always be worn by everyone in the laboratory. Make sure you understand how the experimental apparatus works and what all of the adjustments do before you attempt to operate it. Be sure you have asked, and received an answer, from the Technician about any possible hazards related to your experiment before attempting to operate it. Care must be used in the handling of chemicals to avoid spills and to avoid contact with the skin. B. Laboratory Format and Procedures 1. Organization of Student Groups and Laboratory Projects Students will organize into groups of five persons. Each group is to perform three projects during the semester. (A roster of the groups and a schedule of projects will be supplied separately.) A group leader, who is in charge of directing the work for the lab, should be selected by, and from among, the members of the group. (This responsibility should rotate among the members.) All group members must be prepared for the laboratory and contribute equally to the laboratory work and preparation of the reports. However, the group leader is in charge of assigning and coordinating tasks for the laboratory period and maintaining the group notebook. He or she is ultimately responsible for making sure that everything is done to ensure a successful experiment. 2. Laboratory Session 1 At the beginning of the first session for a given experiment, a paragraph describing the experimental plan and procedure should be submitted to the Technician who is in charge at

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that time. A discussion between the Technician and the students will take place to ensure that students have an accurate plan of action. 3. Laboratory Session 2 The Technical report should be submitted to the Technician in charge of the experiment. A summary discussion of the report with the instructor will be conducted in the laboratory.

4. Session 3 The laboratory will be open to gather additional data if needed. The lecturer will be available for consultations during the first hour of the laboratory period. During this session examination of the experimental apparatus for the next assigned project should be performed by each group. 5. Final Technical Report . The final Technical report is due at the beginning of the next scheduled laboratory period following Session 3. There are no exceptions to this deadline. The reports are to be submitted to one of the department secretaries in the Chemical Engineering office or to the Technician. During the week following the day on which the final report was submitted, the group should schedule a meeting with the lecturer for the discussion of the written report. Each member of the group should be prepared to defend and/or discuss any part of the final report. 6. Laboratory Notebook Part of the purpose of the chemical engineering laboratories is to learn good laboratory and research practices. An important aspect of this is safety. Another important aspect is record-keeping and documentation. In industry you will find that all experiments have to be carefully recorded in an official laboratory notebook and signed by the investigator on a daily basis. To help foster these professional practices, each group is required to
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keep a laboratory notebook documenting the group's work. In the notebook should be kept a neat, labeled and dated record of all work associated with the experiment, including a copy of the precis, all raw data, the settings on the experimental controls, any problems encountered in the experiment and what was done to fix them and why, all calculations, a copy of your progress report, etc. The laboratory notebooks will be handed in at the end of the semester and will contribute to the laboratory participation portion of your grade. 7. Student Responsibilities in the Laboratory Condition of Working Area. Students are responsible for the condition of their working area at the end of each laboratory period . All power to the equipment and instruments should be turned off, and steam and cooling water flows should be shut off. Glassware used should be cleaned and dried. Any equipment or instrumentation malfunctions should be reported promptly to the Technician or assistants.

Checkout before Leaving Laboratory. The students must have their notebooks initialed by a Technician prior to leaving at the end of the laboratory period. At that time the Technician will check the working area and take information about any equipment or instrumentation problems. 8. Grading/Marking Report grading is done by the lecturers who are in charge of a given experiment. This grade will be based on the written report, the oral defense and other pertinent factors (e.g., if you are totally unprepared to do an experiment, you will be docked.) Grades for this course will be determined by the grades on the three experiments as well as your laboratory participation. The laboratory participation portion of your grade in will include how well you followed laboratory safety guidelines (did you wear safety glasses at all times in the lab? did you follow the special safety precautions required for each experiment?), attendance, tardiness, participation, professionalism, how effective a group leader you were, and the quality of your laboratory notebook. Both laboratory instructors and teaching assistants will contribute towards this portion of your grade.

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ATTENDANCE

Regular attendance of the chemical engineering plant (IIIA) lectures is of primary importance. It is the learners responsibility to sign the register each week. A minimum attendance of 75% is mandatory for all courses including practical In a 30 week year, 8 classes that have not been attended and for which you have not furnished a valid doctors letter or other proof of extenuating circumstances, amounts to 25% absenteeism. This level of absenteeism will lead to exclusion from the final moderation at the end of the year, which means that you will fail the course and will have to repeat it the following year. 5.1 LABORATORY, HEALTH & SAFETY RULES AND REGULATIONS 5.1.1. LABORATORY RULES

BASIC RULES Always wear a laboratory coat in the laboratory. Do not wear open shoes in the laboratory. Do not eat or drink in the laboratory. No horse-playing in the laboratory. Always ask the technician if you are not sure of anything.

5.2 RESPONSIBILITIES OF STUDENTS It is your responsibility to make a success of learning in this course. To this end you are encouraged to attend class, write practical reports and hand in your assignments/projects on the set due dates.

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SECTION

LEARNING COMPONENT

6. ASSESSMENT 6.1 ASSESSMENT METHODS AND CRITERIA

Assessment of this laboratory course will include experimental work, problem-based work, Project-based works and assignments, as indicated in the schedule under section 2.2. The purpose of assessment is to determine whether you have achieved the learning outcomes. The various assessment methods therefore will focus on criteria that will enable the lecturer(s) to determine whether you have achieved the learning outcomes and mastered the required skills. The assessment criteria relevant to each learning outcome are detailed in section 2. 6.2 ASSESSMENT RULES The general rules of TUT regarding assessment apply. You are advised to familiarise yourself with these rules, as they are applied stringently.

6.3 MARKING SYSTEM

Subject 1. 2. Title Page Abstract

Max Mark 1 6

Actual Mark

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3. 4. 5. 6. 7. 8.

Introduction Theoretical Background Procedure Results Discussion of Results Conclusion and Recommendations Literature Cited Nomenclature Organization and Neatness

2 3 2 6 10 4

9. 10. 11.

1 1 2

Appendix A1 A2 Raw Data Data analysis and Sample Calculations TOTAL 2 10

50

6.4 PREDICATE/YEAR MARK (Indicate how the laboratory mark will be calculated and any rules you have in this regard. Also indicate the percentage it contributes to the predicate/year mark. Distinguish between semester modules and year subjects) Predicate marks are put on the faculty notice boards. If you

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have queries about your mark, you must immediately consult your course lecturer (contact details are given above), before predicate day. Once the predicate mark is entered on TUTs mainframe computer, the mark cannot be changed. 6.5 MODERATION

The lecturer of the subject will be responsible to moderate all practical report. 6.6 PROMOTION REQUIREMENTS The leaner has to obtain the minimum of 50% in the practical report in order to pass. 7. LABORATORY COURSE CONTENT AND SCHEDULE This course comprises of an experimental component, problem-based component and a project-based component. Your mastery of the required skills is assessed at regular intervals. More importantly, the application of theory is assessed through problem-based- or project-based assignments or projects. The following outline provides an overview of the content to be covered in this course and the ways in which your progress will be assessed.

7.1 SCHEDULE OF LABORATORY SESSIONS AND ASSIGNMENTS

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EXPERIMENTAL/ DURATION THEME PROBLEMBASED/ PROJECT-BASED Week 1-4 SEDIMENTATION (Learning Outcome 1) To study different settling regimes and to determine the relationship between concentration and settling velocity. To study the concepts of flocculation and anti-flocculation and apply them to thickener operation and design. To be able to size thickeners based on particle sizes, fluid viscosities, and desired consistencies. Coagulation and flocculation SEDIMENTATION COMPLETI ON DATE*

Week 5-8

Coagulation and flocculation (Learning Outcomes 2 ) To conduct jar test on a natural

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surface water in order to estimate an optimum dosage of aluminium sulphate or ferric sulphate for the removal of suspended matter or colour. To observe the rate of floc formation and sedimentation.

7.2 LEARNING OUTCOMES AND ASSESSMENT CRITERIA The following tables clearly indicate what you have to achieve (the learning outcomes) and how you will be assessed (assessment criteria) to determine whether you have achieved the required knowledge and competences:

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LEARNING OUTCOME 1: SEDIMENTATION, COAGULATION AND FLOCCULATION Assessment criteria Report writing skills Data collection and interpretation Task performance Assessment method Written report(marking the report) Questions and Answers Observation

LEARNING OUTCOME 2

Assessment criteria

Assessment method

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7.3 GENERIC OUTCOMES AND CRITICAL CROSS-FIELD OUTCOMES Compliance with cross-field Outcomes Critical Compliance Engineering with and Generic Built

Environment Outcomes Mathematics and Statistics Communication and written skills

8. GLOSSARY OF TERMS The following technical terms are used in this course, and you should be familiar with these terms and their meanings. Flocculants, coagulation, settling velocity, rate of settling, sedimentation, thickener

Sources used for the compilation of the glossary: 9. ASSESSMENT RECORDS The following guideline for the preparation of report writing are attached to serve as examples of the implementation of the assessment criteria and assessment method, as listed in the table 3.1, and you should be familiar with these examples to prepare and orientate yourself of how the various assessment criteria are used and applied in the various assessment methods.

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10

EXAMPLE OF A PRACTICAL REPORT

Guidelines for the Preparation of Written Reports A technical report is a medium commonly used by scientists and engineers to communicate the results of their work. Frequently the report is the only tangible product and thus the only evidence for evaluation of the work. Consequently, it deserves careful attention to quality, packaging, and distribution. It is important that the writer(s) of an engineering report keep in mind the needs and interests of the anticipated readers of the report. The laboratory report should be written with the same professionalism that would be used to present the results of a major industrial project. The people who will read it, and need to draw conclusions from it, can be expected to have technical training, but probably would not be familiar with the details of the work. A good report of technical work quantitatively states significant results of experiments and computations and explains how they were obtained, what they mean, and how they are useful. The report should be clear, concise, and accurate. Often the structure of the report must conform to specific conventions. A format for laboratory reports that is to be used in this course is given below.

1. Title Page The title of the report is followed by names of the authors and laboratory group, the date of submission, and identification of the institution or organization supporting the work (Tshwane University of Technology, Department of Chemical & Metallurgical Engineering, CMP33BT). 2. Abstract

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The abstract is a tightly written summary, typically 100 to 300 words long. This section is important because it is the first impression your report will make to a reader, and it could very well be the only part of it he or she will read! (Because of its importance, it is a significant part of the overall grade.) The abstract should be written as stand alone section of just text. Its independence means that the use of symbols, tables, and graphs as well as literature references should be avoided. A good abstract states the principal objective of the investigation, describes the methodology used and summarizes the results and conclusions in statements as quantitative and as general as possible. The abstract should provide ranges of the experimental parameters (e.g. the Reynolds number was varied from 100 to 10000), report the most important results and state how these values compare to expected (i.e., literature) ones. (e.g., values for the friction factor in the laminar flow regime were consistently 15% higher that the predictions of Poiseuille flow). If the value of a single variable or a short list of numbers is given, the numbers should give the uncertainty (e.g., solubility at 25C was 25 3 moles/liter) and of course units should be included. We recommend that you write the abstract last, when your thoughts are most clearly in focus (i.e., you know all the answers and thus know what to say!). 3. Table of Contents A Table of Contents should be included in the report, including a listing of the Abstract. Appendices should also be listed. All pages should be numbered, including tables, figures, and appendices. 4. Introduction The purpose of the Introduction is to place the work in the perspective of prior work including key literature references, demonstrate its importance, and state the specific objectives. The Introduction should not exceed two pages.

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5. Theory This section is a short, concise statement of the essential empirical and theoretical relations to be used in interpreting the data or to be tested by the data. Equations are usually stated with a reference, along with the pertinent assumptions and limitations. Brief manipulations may be appropriate, but long derivations are relegated to an appendix. The physical significance of equation parameters should be pointed out. 6. Experimental A. Apparatus The objective of this section of the report is to describe the experimental set-up in enough quantitative detail to enable the reader to completely understand the experiment. Ranges of independent variables are cited. The model and supplier of any unique equipment should be cited. Also, a schematic diagram of the experimental apparatus should be included. B. Procedure The objective of this section of the report is to describe the materials and methods used to obtain the experimental data. Emphasis is placed on general procedures that are not routine 7. Results The data, or a representative fraction of them, must be included in this section. They should be presented graphically. If there are only a few (i.e. 2-3) numbers, these could put into a table if they can be understood. Data are often not presented in raw form, but are reduced and shown in the way most clearly supporting the conclusions. Representation of scatter in data is essential. For example, the experimentally determined heat transfer coefficient is meaningless unless it is accompanied by units and an estimated uncertainty. Comparison of data with theoretical predictions and/or previously published values should be included whenever possible. This may require searching for information in reference books or research

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articles. Comment briefly on unique aspects of the results, in particular its accuracy. Also comment on the range of the variables covered. Each graph or diagram is assigned a number (e.g., Figure 1) and should have a caption that is descriptive of the information contained in the figure. A restatement of the information on the axes is not an acceptable title. 8. Discussion All important interpretations which follow from the results and the underlying theory are logically and quantitatively compared in the Discussion section. The positive conclusions, comparison with literature data, and the significance applicability, and reproducibility of the results are stressed. Quantitative statements about the accuracy and precision of the results are required. However, when a detailed error analysis is essential to the work, it should be relegated to an Appendix. 9. Conclusions and Recommendations This section is a summary of the most significant conclusions developed in the preceding section. Quantitative statements are best. Useful recommendations to improve the experiment and to extend the work to other systems, should be included here. 10. Literature Cited Only references cited in the report are to be listed is this section since it is not a bibliography covering all references but only the most pertinent ones. Footnotes on individual pages of the report are not to be used. References cited in the text of the final project report should give the last name of the author (both authors when only two; first author et. al. when more than two) and the corresponding page numbers. An example is given below. The Reynolds number can be interpreted as the ratio of inertial to viscous forces at work in the fluid (Denn 37-39). References are to be listed in alphabetical order according to author or equivalent and should not be numbered. Use Chemical Abstracts Service

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Source Index journal abbreviations. For the previous example the citation would be the following:

Richard, J.F. and Zaki, W.N. 1954. Sedimentation and fluidization, Part 1, Transactions of the Institution of Chemical Engineers

. Coulson, J.M., Backhorst, J.R., Harker, J.H., and Richardson J.F. vol 2 4th ed,. Particle technology and separation process. 1991

11. Nomenclature Symbols used in the report are defined immediately after they are presented the first time. This section of the report lists all of the symbols used. Units should be included. 12. Appendices The appendices contain material of secondary importance: sample calculations (a sample of all calculations done for the experiment must be included in the report), error analysis, derivation of theoretical relations, and perhaps graphs, calibration curves and/or schematics. Note that the appendices should be named in the order of which they appear in the final project report. In other words Appendix A should be the first appendix referred to in the text of the report. 11. APPENDICES

11.1 FLOCCULATION AND COAGULATION JAR TEST PRACTICAL BACKGROUND

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Coagulation and flocculation processes are an important part of water and wastewater treatment. Coagulation or destabilization of a colloidal suspension results in joining of minute particles by physical and chemical processes. Flocculation results in formation of a larger settleable structure by bridging. These processes commonly used to remove suspended matter or colour. Adsorption of ionic forms also occurs to varying degrees depending on the constituents in the water or wastewater. The jar test is a laboratory technique for determining the most effective coagulant, chemical dose, and operating pH for coagulation and flocculation, aluminium or iron salts may be used to coagulate particles and to form settleable flocs composed of the hydrous metal oxide precipitates and impurities. Coagulation and flocculation experiments may also be used, in conjunction with other tests, to study basic processes including, for example, the kinetics of reaction, and the removal of trace constituents from aqueous solution. OBJECTIVES 1. To conduct jar test on a natural surface water in order to estimate an optimum dosage of aluminium sulphate or ferric sulphate for the removal of suspended matter or colour. 2. To observe the rate of floc formation and sedimentation. PROCEDURE A. DETERMINE OF OPTIMUM COAGULANT DOSAGE Collect 20 to 50 litres of natural surface water. Analyze the water for pH, turbidity, colour after filtration, and alkalinity. Alternatively, make up a synthetic water sample for testing. Record both the water temperature and ambient air temperature. Calculate the amount of alkalinity required to react with the maximum dosage of aluminium or ferric sulphate. If necessary, augment the natural alkalinity by the addition of 0.1 N Na2CO3 so that the alkalinity will be at least 0.5 meq/l (25 mg/l as CaCO3). Measure exact 1 litre of water into each jar test reactor. Prepare portions of the aluminium or ferric sulphate solution which will yield 10 to 50 mg/l as Al2O3 or Fe2O3 when added to the sample aliquots. Mix at 50 rpm to ensure water is completely mixed. Measure chemical volumes to achieve desired dose in each reactor. Increase mixing speed to 250 rpm. Add the chemicals to each reactor near the vortex. All reactors should be dosed at the same time. Rapidly mix for 1 min. Reduce mixing to 60 rpm for 9 min.; Observe the reactors at 3 min.

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intervals to detect the formation of flocs. Reduce mixing to 25 rpm for 4 min.; Reduce mixing to 10 rpm for 2 min. Turn off mixers and allow particles to settle for 20 min. Measure the turbidity or colour, alkalinity, and pH of the liquid in each jar by sampling at the top, taking care not to disturb the sediment in sampling. Measure the depth of sludge in the beaker.

B DETERMINATION OF OPTIMUM pH Repeat the jar test of Part A using the observed optimum dosage of ferric sulphate but adjusting sample pH to 6, 7, 8, and 9 with NaOH or H2SO4 prior to adding coagulant. Measure final pH, turbidity or colour of the supernatant of each sample. Measure the depth of sludge in the beaker. Plot turbidity or colour versus pH. EFFECT OF MIXING (AGGREGATION KINETICS) Prepare identical (optimum) coagulant dosages for all six beakers. Use the same rapid mix as before but vary the time of slow mix at 30 rpm. Use 5, 10, 15, 20, 30, and 45 minutes for the six jars respectively. Terminate mixing by carefully lifting the paddle from the beaker at appropriate time. Allow 30 minutes for settling. Measure the colour or turbidity and pH of the supernatant in each beaker. APPARATUS Jar test apparatus and beakers Magnetic stirrer plus magnetic stirring bars Spectrophotometer or colour comparator Turbidimeter pH meter Assorted measurement pipettes (1, 5, 10 ml) and volumetric pipettes to 50 ml Burette Glass or plastic funnels Ringstands and rings MATERIALS Aluminium sulphate solution, 1 g/l or ferric sulphate solution, 1 g/l H2SO4, 2 litres each, 5 x 10-2 M, 10-2 M NaOH,, 1 litre, 10-1 M Sodium carbonate, 1 litre each, 5 x 10-2 M, 10-2 M Indicators: methyl orange, phenolphthalein

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Synthetic water sample: Add suspended matter with a kaolin, montmorillonite, illite, or bentonite clay and/or the colour with extract from boiled leaves or with instant coffee to raw water. Turbidity might be increased to about 40 turbidity units and colour to about 80 colour units (Clay suspension sample should be mixed for 3 days). Buffer solution Whatman #1 filter paper

REPORT Prepare tables which facilitate comparisons of coagulant dosages with alkalinity, pH, colour, turbidity, and other changes observed. Plot the inverse of turbidity and colour versus coagulant dosage as part of the analysis. Plot turbidity versus coagulant dose at different settling times to determine the influence of floc formation and settling characteristics on the selection of coagulant dosage. Comment on the differences between coagulation with iron and aluminium salts. Define the pH ranges over which each salt should result in effective coagulation. Determine the rate of aggregation for a particular coagulant dose and pH by plotting the reciprocal of the turbidity versus time. (This would represent a second order reaction with respect to turbidity). Also plot the natural log of the reciprocal turbidity (representing a first order reaction) versus time. Determine which gives the best straight line fit of the data and determine the slope. References Richard, J.F. and Zaki, W.N. 1954. Sedimentation and fluidization, Part 1, Transactions of the Institution of Chemical Engineers. Coulson, J.M., Backhorst, J.R., Harker, J.H., and Richardson J.F. vol 2 4th ed,. Particle technology and separation process. 1991. Geankoplis, C.J Transport Processes and Unit Operations, 3rd., Prantice-Hall, 1993 11.2 SEDIMENTATION EXPERIMENT 1. INTRODUCTION

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Sedimentation is the partial separation or concentration of suspended solid particles from a liquid by gravity settling. It is a strong function of liquid viscosity and density, particle size, and concentration of the solution. With that in mind, experiments can be performed that will allow the engineer to determine settling times and velocities for liquid-solid suspensions and slurries. This would enable thickeners to be designed for specific industrial task.

The sedimentation process is particularly important in the preparation of industrial or domestic water and purification of wastewater. Many process applications are also found in metallurgical industry. The beer brewing industry also has many applications dealing with batch settling and use of flocculants. Certain clarifiers are added to the beer in order to flocculate sediment particles so they may later be filtered.

The objective of this experiment is to do settling experiments of the type that are used to size thickeners for specific industrial applications and to interpret the results in the context of equipment design.

Objectives: To study different settling regimes and to determine the relationship between concentration and settling velocity. To study the concepts of flocculation and anti-flocculation and apply them to thickener operation and design. To be able to size thickeners based on particle sizes, fluid viscosities, and desired consistencies.

2. Theory The theoretical ideas used in analysing sedimentation problems are studied extensively in Chemical Plant course. The methods and

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concepts and concepts covered in this experiment are dealt with in that class and can be found in the text (2). The main calculations in the lab are done using the Richardson-Zaki equation and the Kynch method. The student is urged to have a good grasp of these concepts when performing this experiment and discuss the aspects of them thoroughly in the report. Most correlations used to size thickeners require that the particles behave according to Stokes law operation is that the Reynolds number must be less than 0.3. Richardson and Zaki have developed a means to relate the actual velocity of the particle. With the terminal velocity calculated, Stokes law can be solved for the diameter of the particle. The Richardson-Zaki equation is as follows:

U U

P T

= Void fraction for the concentration

n = proportional exponent

UP = TRUE PARTICLES HINDERED VELOCITY (M/S)

UT = terminal velocity, from Stokes law (m/s)

The value of the proportional exponent can be found by:

n = 4.6 + x/D

Where x = particle diameter, in meters

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D = vessel diameter, in meters

Stokes law:

v =

d 2 g (Ps Pl) 18

The Kynch method is a graphical approach that is used to find the settling velocity of a slurry or suspension over time. However, there are several other constraints that apply to the Kynch method that should also be kept in mind, such as neglecting wall effects, assuming uniform particle shape and size, and that the particle velocity reaches zero at large times .The Kynch method involves constructing tangents to the settling height and times curves, and the slope of each of these tangents is the velocity at that time.

The most important restriction of the Kynch method is that system must obey Stokes law. Stokes law compares the drag force that resists a settling sphere in a fluid .the viscosity of that fluid and the shear it creates, and the pressure drag of the moving sphere, to the terminal velocity of the particle. To prove that a given system of the particles are within the

Stokes law region, the single particle Reynolds number is calculated. This value must be below 0.3 for Stokes law to the valid. If this is true, then the settling velocity of the

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particles can be as a function of system characteristics, like particle and fluid densities, as well as the diameter of the particle.

4. APPARATUS:

To perform this experiment, graduated glass cylinders with a total height of approximately 1 m are used. The diameter of the cylinder is 0.05 m. The cylinders should be thoroughly washed and filled with varying concentration of a suspension and glass beads for the experiment. The suspension to be examined is a

C aC O

, which is

combined with water to simulate batch settling of fine particles, while glass beads are mixed with octanol to simulate coarse particles. The settling times are kept by using the stopwatches provided.

5. METHOD:

The settling experiment is conducted in a cylinder. The suspension

C aC O

is prepared

at different concentration by weight (to be determined by laboratory supervisor). The suspension is prepared by mixing

C aC O

of known quantity with water. The test

column is filled with the suspension up to 0.7 m and agitated with compressed air or well shaken for about 1 min to provide uniform concentration throughout the depth. The solids profiles are then determined at different moments of time after agitation.

In addition to profile determination settling of the interface is measured as a function of time to estimate settling parameters. Graphs at height against time are plotted as the experiment proceeds. for final compaction reading, a period of 24 hours should

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elapse. Gradients of the initial settling period should be deduced, in order to plot the initial mass settling rate against concentration.

To determine concentration at any point on the settling curve, a graphical method employed by Kynch is employed. On the time vs. height graph, a tangent is drawn to the settling curve, it cuts the vertical axis at a certain point.

The following quantities should be tabulated from reassured data:

Concentration %

Initial solid weight used (kg)

Volume per unit 3 weight (m /kg) *

Height when critical point reached (m)

Sedimentation Volume

H CR T ubeA rea In itia lS o lid s W e ig h t

Final Sedimentation height (m)

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Final Volume =

T u b eA rea

In itia lS o lid s W e ig h t

Richard, J.F. and Zaki, W.N. 1954. Sedimentation and fluidization, Part 1, Transactions of the Institution of Chemical Engineers. Coulson, J.M., Backhorst, J.R., Harker, J.H., and Richardson J.F. vol 2 4th ed,. Particle technology and separation process. 1991. Geankoplis, C.J Transport Processes and Unit Operations, 3rd., Prantice-Hall, 1993

12.

EXAMPLE OF A PRACTICAL REPORT

TSHWANE UNIVERSITY OF TECHNOLOGY

DEPARTMENT OF CHEMICAL AND METTALURGICAL ENGINEERING

REPORT GRADING FORM

Name of Student: ____________________________________________________

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Student Number: _____________________________________________________

Title of Report: ______________________________________________________

Term: _______________________________

DATE: __________________

Subject 1. 2. 3. 4. 5. 6. 7. 8. Title Page Abstract Introduction Theoretical Background Procedure Results Discussion of Results Conclusion and Recommendations Literature Cited Nomenclature Organization and Neatness

Max Mark 1 6 2 3 2 6 10 4

Actual Mark

9. 10. 11.

1 1 2

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Appendix A1 A2 Raw Data Data analysis and Sample Calculations TOTAL 2 10

50

Signed: ____________________________________ Comments:

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